# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_3 _database_code_depnum_ccdc_archive 'CCDC 914763' _audit_creation_date 2012-12-06 _audit_block_code RKI-RF-151-01_6912 _chemical_name_systematic ; P-triphenyl-P'-2-pyridyl-diphenyl-carbodiphorphorane ; _chemical_melting_point ? _chemical_compound_source toluene _chemical_formula_moiety '2(C36 H29 N P2), C7 H8' _chemical_formula_sum 'C79 H66 N2 P4' _chemical_formula_weight 1167.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-p 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5881(12) _cell_length_b 11.7546(14) _cell_length_c 13.4581(16) _cell_angle_alpha 73.849(2) _cell_angle_beta 73.626(2) _cell_angle_gamma 78.953(2) _cell_volume 1531.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9641 _cell_measurement_theta_min 2.8830 _cell_measurement_theta_max 31.7733 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 -1.00 0.00 0.0100 0.00 1.00 0.00 0.0100 -1.00 0.00 -1.00 0.0100 1.00 0.00 1.00 0.0100 -1.00 0.00 1.00 0.0300 1.00 0.00 -1.00 0.0200 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.265 _exptl_crystal_density_method ? _exptl_crystal_F_000 614 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.99209 _exptl_absorpt_correction_T_max 0.99724 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_special_details ; Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75 ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_monochromator 'Incoatec Helios mirrors' _diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 66.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47413 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 32.04 _reflns_number_total 10542 _reflns_number_gt 7527 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT software (Bruker AXS, 2004)' _computing_data_reduction 'SAINT software (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The minimum and maximum estimated transmissions from the multi-scan scaling are 0.8494 and 1.0000 (SADABS). Reflections above 4 angstroem were affected by the beamstop and removed from the final refinement cycles. The position of the N atom could not be determined by refining the structure using all C atoms in the 6-membered rings, which indicates that the pyridyl group may be distributed at different positions in the molecule. Nevertheless, the lack of electron density in a region where the H atom of a C-H group would be expected suggests that N1 is a likely position of the N atom. The crystal contains a disordered toluene molecule about a crystallographic centre of symmetry. Disordered atoms were refined with isotropic atomic displacement parameters and half occupancy. Highest peak 0.90 at 0.5471 0.4216 0.1307 [ 0.57 A from C42 ] Deepest hole -0.71 at 0.6380 0.4038 0.0844 [ 0.53 A from C37 ] ; _iucr_refine_instructions_details ; TITL 6912sadabs in P-1 #2 CELL 0.71073 10.5881 11.7546 13.4581 73.849 73.626 78.953 ZERR 1 0.0012 0.0014 0.0016 0.002 0.002 0.002 LATT 1 SFAC C H N P UNIT 79 66 2 4 LIST 4 L.S. 10 PLAN 20 TEMP -173 BOND $H FMAP 2 ACTA 60 WGHT 0.104900 0.420200 FVAR 0.20549 C1 1 0.245493 0.922436 0.267135 11.00000 0.01603 0.01330 = 0.01674 -0.00209 -0.00463 -0.00142 C2 1 0.448325 0.710354 0.295481 11.00000 0.01408 0.01535 = 0.01568 -0.00375 -0.00382 -0.00102 C3 1 0.526507 0.759168 0.196946 11.00000 0.01946 0.01606 = 0.01664 -0.00392 -0.00159 -0.00216 AFIX 43 H3 2 0.494420 0.831920 0.154229 11.00000 -1.20000 AFIX 0 C4 1 0.652127 0.701893 0.160249 11.00000 0.01918 0.02444 = 0.02608 -0.00978 0.00140 -0.00353 AFIX 43 H4 2 0.706132 0.735386 0.092698 11.00000 -1.20000 AFIX 0 C5 1 0.697412 0.596391 0.222617 11.00000 0.01632 0.02695 = 0.03711 -0.01334 -0.00707 0.00396 AFIX 43 H5 2 0.782103 0.555687 0.197406 11.00000 -1.20000 AFIX 0 C6 1 0.619914 0.549678 0.321738 11.00000 0.03381 0.02442 = 0.03207 -0.00292 -0.01377 0.00662 AFIX 43 H6 2 0.653021 0.477964 0.365104 11.00000 -1.20000 AFIX 0 C7 1 0.176831 0.689149 0.319009 11.00000 0.01360 0.01511 = 0.01642 -0.00398 -0.00323 -0.00218 C8 1 0.095940 0.736768 0.247657 11.00000 0.02077 0.01819 = 0.01731 -0.00260 -0.00698 -0.00396 AFIX 43 H8 2 0.094469 0.818426 0.210620 11.00000 -1.20000 AFIX 0 C9 1 0.017565 0.665167 0.230608 11.00000 0.02637 0.02388 = 0.02650 -0.00649 -0.01248 -0.00406 AFIX 43 H9 2 -0.038183 0.698040 0.182673 11.00000 -1.20000 AFIX 0 C10 1 0.020952 0.545533 0.283786 11.00000 0.02457 0.02138 = 0.03989 -0.00915 -0.01332 -0.00548 AFIX 43 H10 2 -0.031680 0.495987 0.271844 11.00000 -1.20000 AFIX 0 C11 1 0.101480 0.498806 0.354345 11.00000 0.02854 0.01422 = 0.04974 -0.00061 -0.01826 -0.00513 AFIX 43 H11 2 0.103216 0.417025 0.391032 11.00000 -1.20000 AFIX 0 C12 1 0.179480 0.569443 0.372231 11.00000 0.02164 0.01627 = 0.03146 -0.00024 -0.01356 -0.00344 AFIX 43 H12 2 0.234543 0.536229 0.420656 11.00000 -1.20000 AFIX 0 C13 1 0.255177 0.764279 0.478025 11.00000 0.01468 0.01389 = 0.01411 -0.00152 -0.00378 -0.00151 C14 1 0.352981 0.791510 0.515251 11.00000 0.01495 0.02728 = 0.01692 -0.00611 -0.00233 -0.00607 AFIX 43 H14 2 0.436765 0.807112 0.468211 11.00000 -1.20000 AFIX 0 C15 1 0.328233 0.795878 0.620853 11.00000 0.02033 0.04160 = 0.02314 -0.01260 -0.00569 -0.00569 AFIX 43 H15 2 0.395649 0.813559 0.646190 11.00000 -1.20000 AFIX 0 C16 1 0.206478 0.774760 0.689528 11.00000 0.02564 0.03236 = 0.01567 -0.00856 -0.00372 -0.00124 AFIX 43 H16 2 0.189417 0.779801 0.761459 11.00000 -1.20000 AFIX 0 C17 1 0.108945 0.746137 0.653359 11.00000 0.01784 0.02185 = 0.01808 -0.00470 -0.00043 -0.00058 AFIX 43 H17 2 0.025401 0.730614 0.700852 11.00000 -1.20000 AFIX 0 C18 1 0.133117 0.740103 0.547792 11.00000 0.01436 0.01751 = 0.01737 -0.00393 -0.00292 -0.00068 AFIX 43 H18 2 0.066625 0.719564 0.523321 11.00000 -1.20000 AFIX 0 C19 1 0.211942 1.166737 0.164361 11.00000 0.01412 0.01379 = 0.01292 -0.00371 -0.00205 0.00042 C20 1 0.115538 1.135135 0.128456 11.00000 0.01742 0.01286 = 0.01620 -0.00388 -0.00413 -0.00045 AFIX 43 H20 2 0.100944 1.053895 0.145795 11.00000 -1.20000 AFIX 0 C21 1 0.040442 1.221451 0.067442 11.00000 0.01645 0.01900 = 0.01817 -0.00361 -0.00535 -0.00053 AFIX 43 H21 2 -0.024863 1.199307 0.042776 11.00000 -1.20000 AFIX 0 C22 1 0.061384 1.340244 0.042727 11.00000 0.02067 0.01659 = 0.02090 -0.00297 -0.00479 0.00481 AFIX 43 H22 2 0.009545 1.399755 0.001832 11.00000 -1.20000 AFIX 0 C23 1 0.158287 1.372115 0.077856 11.00000 0.02483 0.01295 = 0.02392 -0.00423 -0.00441 -0.00014 AFIX 43 H23 2 0.172660 1.453414 0.060511 11.00000 -1.20000 AFIX 0 C24 1 0.233893 1.286097 0.137928 11.00000 0.01822 0.01492 = 0.02081 -0.00434 -0.00370 -0.00243 AFIX 43 H24 2 0.300540 1.308224 0.161107 11.00000 -1.20000 AFIX 0 C25 1 0.474813 1.058837 0.189567 11.00000 0.01471 0.01224 = 0.01569 -0.00498 -0.00234 -0.00199 C26 1 0.519158 1.088446 0.078841 11.00000 0.01733 0.01882 = 0.01653 -0.00468 -0.00364 -0.00344 AFIX 43 H26 2 0.456822 1.119459 0.036216 11.00000 -1.20000 AFIX 0 C27 1 0.653778 1.073048 0.030098 11.00000 0.01922 0.02406 = 0.01738 -0.00618 -0.00144 -0.00413 AFIX 43 H27 2 0.683231 1.092033 -0.045451 11.00000 -1.20000 AFIX 0 C28 1 0.744746 1.029755 0.092621 11.00000 0.01665 0.02622 = 0.02560 -0.01025 -0.00297 -0.00248 AFIX 43 H28 2 0.836775 1.018813 0.059715 11.00000 -1.20000 AFIX 0 C29 1 0.701826 1.002316 0.203202 11.00000 0.02036 0.02479 = 0.02523 -0.00733 -0.00968 -0.00030 AFIX 43 H29 2 0.764630 0.974399 0.245651 11.00000 -1.20000 AFIX 0 C30 1 0.567265 1.015689 0.251618 11.00000 0.01977 0.01874 = 0.01612 -0.00491 -0.00594 -0.00045 AFIX 43 H30 2 0.538036 0.995422 0.327171 11.00000 -1.20000 AFIX 0 C31 1 0.269026 1.109874 0.369598 11.00000 0.01612 0.01620 = 0.01496 -0.00570 -0.00545 0.00233 C32 1 0.338370 1.198569 0.367899 11.00000 0.01735 0.01959 = 0.01800 -0.00650 -0.00605 -0.00026 AFIX 43 H32 2 0.404147 1.228325 0.306206 11.00000 -1.20000 AFIX 0 C33 1 0.310906 1.243516 0.457049 11.00000 0.02601 0.02575 = 0.02853 -0.01152 -0.01208 0.00274 AFIX 43 H33 2 0.358724 1.304460 0.456385 11.00000 -1.20000 AFIX 0 C34 1 0.215051 1.201633 0.547519 11.00000 0.03095 0.02948 = 0.02075 -0.01401 -0.01118 0.01042 AFIX 43 H34 2 0.197486 1.233576 0.608278 11.00000 -1.20000 AFIX 0 C35 1 0.144997 1.112999 0.548931 11.00000 0.02627 0.02711 = 0.01557 -0.00629 -0.00247 0.00671 AFIX 43 H35 2 0.078518 1.084221 0.610469 11.00000 -1.20000 AFIX 0 C36 1 0.172420 1.066073 0.459578 11.00000 0.01841 0.02056 = 0.01739 -0.00469 -0.00311 0.00173 AFIX 43 H36 2 0.125413 1.004587 0.460176 11.00000 -1.20000 AFIX 0 N1 3 0.494263 0.605752 0.359204 11.00000 0.03435 0.02705 = 0.02962 -0.00151 -0.00871 0.00444 P1 4 0.280840 0.786140 0.335262 11.00000 0.01186 0.01179 = 0.01263 -0.00159 -0.00312 -0.00149 P2 4 0.299047 1.049770 0.251815 11.00000 0.01302 0.01198 = 0.01196 -0.00278 -0.00258 -0.00119 PART -1 C37 1 0.359203 0.641746 0.912307 10.50000 0.05775 AFIX 137 H37A 2 0.408157 0.709478 0.871129 10.50000 -1.50000 H37B 2 0.281882 0.668379 0.964424 10.50000 -1.50000 H37C 2 0.329676 0.609552 0.864000 10.50000 -1.50000 AFIX 0 C38 1 0.444094 0.550580 0.967100 10.50000 0.02890 C39 1 0.541550 0.475444 0.917933 10.50000 0.02490 AFIX 43 H39 2 0.556975 0.482661 0.843525 10.50000 -1.20000 AFIX 0 C40 1 0.617496 0.388887 0.977265 10.50000 0.04261 AFIX 43 H40 2 0.684304 0.335203 0.944358 10.50000 -1.20000 AFIX 0 C41 1 0.593090 0.381019 1.093409 10.50000 0.05716 AFIX 43 H41 2 0.643120 0.322467 1.136531 10.50000 -1.20000 AFIX 0 C42 1 0.501706 0.456549 1.132957 10.50000 0.04657 AFIX 43 H42 2 0.486153 0.452777 1.206791 10.50000 -1.20000 AFIX 0 C43 1 0.420924 0.547079 1.072009 10.50000 0.03258 AFIX 43 H43 2 0.354602 0.601593 1.104254 10.50000 -1.20000 PART 0 HKLF 4 REM 6912sadabs in P-1 #2 REM R1 = 0.0535 for 7542 Fo > 4sig(Fo) and 0.0912 for all 10574 data REM 381 parameters refined using 0 restraints END WGHT 0.1049 0.4202 REM Highest difference peak 1.074, deepest hole -0.837, 1-sigma level 0.192 Q1 1 0.5470 0.4231 1.1318 11.00000 0.05 1.07 Q2 1 0.5341 0.5150 0.8572 11.00000 0.05 0.94 Q3 1 0.6238 0.3626 1.1298 11.00000 0.05 0.91 Q4 1 0.3794 0.6208 0.9550 11.00000 0.05 0.89 Q5 1 0.3245 0.8306 0.3418 11.00000 0.05 -0.84 Q6 1 0.3368 1.0808 0.1847 11.00000 0.05 -0.83 Q7 1 0.3561 0.9642 0.2685 11.00000 0.05 -0.82 Q8 1 0.4037 0.9416 0.2422 11.00000 0.05 -0.80 Q9 1 0.3551 0.9992 0.2108 11.00000 0.05 -0.80 Q10 1 0.3232 0.8075 0.2871 11.00000 0.05 -0.76 Q11 1 0.3675 0.8856 0.2754 11.00000 0.05 -0.75 Q12 1 0.2643 1.0221 0.3042 11.00000 0.05 -0.75 Q13 1 0.2789 1.0373 0.2256 11.00000 0.05 -0.73 Q14 1 0.2492 0.8197 0.3610 11.00000 0.05 -0.72 Q15 1 0.4113 0.9970 0.1967 11.00000 0.05 -0.71 Q16 1 0.2054 1.0638 0.2560 11.00000 0.05 -0.71 Q17 1 0.2592 0.7422 0.3882 11.00000 0.05 -0.70 Q18 1 0.1831 0.8061 0.3388 11.00000 0.05 -0.70 Q19 1 0.3269 0.9031 0.2873 11.00000 0.05 -0.69 Q20 1 0.5269 0.6265 0.3258 11.00000 0.05 -0.69 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.7848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10542 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1524 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.24549(16) 0.92252(14) 0.26722(13) 0.0161(3) Uani 1 1 d . . . C2 C 0.44827(16) 0.71046(15) 0.29548(12) 0.0157(3) Uani 1 1 d . . . C3 C 0.52658(17) 0.75916(15) 0.19691(13) 0.0185(3) Uani 1 1 d . . . H3 H 0.4945 0.8319 0.1542 0.022 Uiso 1 1 calc R . . C4 C 0.65213(18) 0.70194(17) 0.16014(15) 0.0244(4) Uani 1 1 d . . . H4 H 0.7061 0.7355 0.0926 0.029 Uiso 1 1 calc R . . C5 C 0.69753(18) 0.59636(18) 0.22246(17) 0.0270(4) Uani 1 1 d . . . H5 H 0.7822 0.5556 0.1972 0.032 Uiso 1 1 calc R . . C6 C 0.6199(2) 0.54963(19) 0.32178(17) 0.0318(4) Uani 1 1 d . . . H6 H 0.6530 0.4779 0.3652 0.038 Uiso 1 1 calc R . . C7 C 0.17684(16) 0.68917(14) 0.31895(12) 0.0156(3) Uani 1 1 d . . . C8 C 0.09592(17) 0.73667(15) 0.24782(13) 0.0190(3) Uani 1 1 d . . . H8 H 0.0943 0.8184 0.2109 0.023 Uiso 1 1 calc R . . C9 C 0.01769(19) 0.66509(17) 0.23067(15) 0.0247(4) Uani 1 1 d . . . H9 H -0.0380 0.6979 0.1827 0.030 Uiso 1 1 calc R . . C10 C 0.0211(2) 0.54550(17) 0.28389(17) 0.0274(4) Uani 1 1 d . . . H10 H -0.0316 0.4960 0.2720 0.033 Uiso 1 1 calc R . . C11 C 0.1016(2) 0.49877(17) 0.35432(19) 0.0308(4) Uani 1 1 d . . . H11 H 0.1034 0.4170 0.3910 0.037 Uiso 1 1 calc R . . C12 C 0.17943(18) 0.56949(16) 0.37213(15) 0.0233(3) Uani 1 1 d . . . H12 H 0.2345 0.5363 0.4206 0.028 Uiso 1 1 calc R . . C13 C 0.25527(16) 0.76439(14) 0.47809(12) 0.0152(3) Uani 1 1 d . . . C14 C 0.35297(17) 0.79161(16) 0.51524(13) 0.0199(3) Uani 1 1 d . . . H14 H 0.4368 0.8072 0.4682 0.024 Uiso 1 1 calc R . . C15 C 0.32824(19) 0.7960(2) 0.62054(15) 0.0275(4) Uani 1 1 d . . . H15 H 0.3956 0.8138 0.6459 0.033 Uiso 1 1 calc R . . C16 C 0.20632(19) 0.77465(18) 0.68939(14) 0.0253(4) Uani 1 1 d . . . H16 H 0.1894 0.7795 0.7614 0.030 Uiso 1 1 calc R . . C17 C 0.10891(17) 0.74619(16) 0.65334(14) 0.0210(3) Uani 1 1 d . . . H17 H 0.0253 0.7307 0.7008 0.025 Uiso 1 1 calc R . . C18 C 0.13322(16) 0.74020(15) 0.54794(13) 0.0175(3) Uani 1 1 d . . . H18 H 0.0668 0.7196 0.5234 0.021 Uiso 1 1 calc R . . C19 C 0.21202(15) 1.16671(14) 0.16455(12) 0.0147(3) Uani 1 1 d . . . C20 C 0.11562(16) 1.13516(14) 0.12854(12) 0.0163(3) Uani 1 1 d . . . H20 H 0.1010 1.0539 0.1459 0.020 Uiso 1 1 calc R . . C21 C 0.04055(17) 1.22164(15) 0.06733(13) 0.0187(3) Uani 1 1 d . . . H21 H -0.0247 1.1995 0.0426 0.022 Uiso 1 1 calc R . . C22 C 0.06145(18) 1.34031(16) 0.04269(14) 0.0214(3) Uani 1 1 d . . . H22 H 0.0096 1.3998 0.0018 0.026 Uiso 1 1 calc R . . C23 C 0.15819(18) 1.37216(15) 0.07783(14) 0.0218(3) Uani 1 1 d . . . H23 H 0.1726 1.4535 0.0605 0.026 Uiso 1 1 calc R . . C24 C 0.23388(17) 1.28600(15) 0.13808(13) 0.0187(3) Uani 1 1 d . . . H24 H 0.3005 1.3082 0.1613 0.022 Uiso 1 1 calc R . . C25 C 0.47479(16) 1.05882(14) 0.18966(12) 0.0147(3) Uani 1 1 d . . . C26 C 0.51918(17) 1.08846(15) 0.07901(13) 0.0179(3) Uani 1 1 d . . . H26 H 0.4569 1.1196 0.0364 0.021 Uiso 1 1 calc R . . C27 C 0.65379(17) 1.07296(16) 0.03031(14) 0.0210(3) Uani 1 1 d . . . H27 H 0.6832 1.0919 -0.0452 0.025 Uiso 1 1 calc R . . C28 C 0.74464(18) 1.02969(17) 0.09272(15) 0.0229(3) Uani 1 1 d . . . H28 H 0.8367 1.0187 0.0599 0.028 Uiso 1 1 calc R . . C29 C 0.70159(18) 1.00229(17) 0.20316(15) 0.0233(3) Uani 1 1 d . . . H29 H 0.7644 0.9743 0.2456 0.028 Uiso 1 1 calc R . . C30 C 0.56706(17) 1.01566(15) 0.25157(13) 0.0185(3) Uani 1 1 d . . . H30 H 0.5378 0.9953 0.3271 0.022 Uiso 1 1 calc R . . C31 C 0.26906(16) 1.10987(15) 0.36944(12) 0.0163(3) Uani 1 1 d . . . C32 C 0.33824(17) 1.19851(15) 0.36784(13) 0.0184(3) Uani 1 1 d . . . H32 H 0.4039 1.2284 0.3061 0.022 Uiso 1 1 calc R . . C33 C 0.3110(2) 1.24342(18) 0.45723(16) 0.0260(4) Uani 1 1 d . . . H33 H 0.3590 1.3042 0.4566 0.031 Uiso 1 1 calc R . . C34 C 0.2152(2) 1.20167(18) 0.54753(15) 0.0271(4) Uani 1 1 d . . . H34 H 0.1977 1.2336 0.6083 0.032 Uiso 1 1 calc R . . C35 C 0.14510(19) 1.11296(18) 0.54890(14) 0.0254(4) Uani 1 1 d . . . H35 H 0.0786 1.0842 0.6104 0.030 Uiso 1 1 calc R . . C36 C 0.17249(17) 1.06606(16) 0.45947(13) 0.0202(3) Uani 1 1 d . . . H36 H 0.1255 1.0046 0.4601 0.024 Uiso 1 1 calc R . . N1 N 0.49417(19) 0.60574(16) 0.35927(15) 0.0335(4) Uani 1 1 d . . . P1 P 0.28084(4) 0.78615(4) 0.33525(3) 0.01299(9) Uani 1 1 d . . . P2 P 0.29905(4) 1.04978(4) 0.25183(3) 0.01311(9) Uani 1 1 d . . . C37 C 0.3588(8) 0.6422(7) 0.9131(6) 0.0587(18) Uiso 0.50 1 d P A -1 H37A H 0.4076 0.7100 0.8719 0.088 Uiso 0.50 1 calc PR A -1 H37B H 0.2819 0.6686 0.9657 0.088 Uiso 0.50 1 calc PR A -1 H37C H 0.3285 0.6105 0.8648 0.088 Uiso 0.50 1 calc PR A -1 C38 C 0.4440(4) 0.5507(4) 0.9670(3) 0.0298(8) Uiso 0.50 1 d P A -1 C39 C 0.5411(5) 0.4758(4) 0.9177(4) 0.0260(9) Uiso 0.50 1 d P A -1 H39 H 0.5564 0.4829 0.8433 0.031 Uiso 0.50 1 calc PR A -1 C40 C 0.6176(5) 0.3886(5) 0.9777(4) 0.0438(11) Uiso 0.50 1 d P A -1 H40 H 0.6844 0.3350 0.9447 0.053 Uiso 0.50 1 calc PR A -1 C41 C 0.5936(8) 0.3803(7) 1.0939(6) 0.0573(17) Uiso 0.50 1 d P A -1 H41 H 0.6435 0.3217 1.1371 0.069 Uiso 0.50 1 calc PR A -1 C42 C 0.5020(6) 0.4563(5) 1.1332(5) 0.0475(12) Uiso 0.50 1 d P A -1 H42 H 0.4864 0.4528 1.2070 0.057 Uiso 0.50 1 calc PR A -1 C43 C 0.4215(6) 0.5466(5) 1.0723(4) 0.0325(10) Uiso 0.50 1 d P A -1 H43 H 0.3552 0.6010 1.1047 0.039 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0166(7) 0.0138(7) 0.0170(7) -0.0021(5) -0.0048(6) -0.0015(6) C2 0.0148(7) 0.0160(7) 0.0163(6) -0.0040(5) -0.0041(5) -0.0011(5) C3 0.0200(8) 0.0165(7) 0.0173(7) -0.0040(6) -0.0018(6) -0.0022(6) C4 0.0198(8) 0.0250(9) 0.0266(8) -0.0098(7) 0.0012(7) -0.0035(7) C5 0.0170(8) 0.0275(9) 0.0378(10) -0.0135(8) -0.0074(7) 0.0037(7) C6 0.0347(11) 0.0249(9) 0.0329(10) -0.0033(8) -0.0140(8) 0.0065(8) C7 0.0143(7) 0.0158(7) 0.0169(6) -0.0043(5) -0.0033(5) -0.0022(5) C8 0.0216(8) 0.0185(8) 0.0179(7) -0.0026(6) -0.0069(6) -0.0041(6) C9 0.0271(9) 0.0246(9) 0.0271(8) -0.0066(7) -0.0130(7) -0.0042(7) C10 0.0253(9) 0.0221(9) 0.0406(10) -0.0095(8) -0.0135(8) -0.0056(7) C11 0.0291(10) 0.0151(8) 0.0502(12) -0.0007(8) -0.0180(9) -0.0053(7) C12 0.0221(8) 0.0170(8) 0.0323(9) -0.0004(7) -0.0138(7) -0.0034(6) C13 0.0156(7) 0.0143(7) 0.0147(6) -0.0017(5) -0.0040(5) -0.0015(5) C14 0.0157(7) 0.0277(9) 0.0172(7) -0.0061(6) -0.0023(6) -0.0063(6) C15 0.0213(9) 0.0418(11) 0.0236(8) -0.0125(8) -0.0061(7) -0.0059(8) C16 0.0266(9) 0.0329(10) 0.0163(7) -0.0087(7) -0.0040(6) -0.0012(7) C17 0.0186(8) 0.0223(8) 0.0188(7) -0.0048(6) -0.0006(6) -0.0008(6) C18 0.0151(7) 0.0179(7) 0.0183(7) -0.0041(6) -0.0033(6) -0.0006(6) C19 0.0146(7) 0.0144(7) 0.0136(6) -0.0039(5) -0.0021(5) 0.0004(5) C20 0.0180(7) 0.0135(7) 0.0169(7) -0.0040(5) -0.0040(6) -0.0006(6) C21 0.0171(7) 0.0199(8) 0.0186(7) -0.0039(6) -0.0054(6) -0.0006(6) C22 0.0213(8) 0.0175(8) 0.0213(7) -0.0031(6) -0.0051(6) 0.0047(6) C23 0.0252(8) 0.0136(7) 0.0245(8) -0.0044(6) -0.0043(7) -0.0003(6) C24 0.0189(7) 0.0156(7) 0.0212(7) -0.0047(6) -0.0038(6) -0.0025(6) C25 0.0153(7) 0.0129(7) 0.0162(6) -0.0053(5) -0.0025(5) -0.0021(5) C26 0.0178(7) 0.0193(8) 0.0172(7) -0.0049(6) -0.0039(6) -0.0035(6) C27 0.0200(8) 0.0248(9) 0.0178(7) -0.0066(6) -0.0013(6) -0.0045(6) C28 0.0171(8) 0.0267(9) 0.0262(8) -0.0106(7) -0.0030(6) -0.0025(7) C29 0.0212(8) 0.0253(9) 0.0261(8) -0.0078(7) -0.0102(7) -0.0002(7) C30 0.0204(8) 0.0192(8) 0.0167(7) -0.0052(6) -0.0060(6) -0.0008(6) C31 0.0167(7) 0.0169(7) 0.0157(6) -0.0059(6) -0.0056(6) 0.0023(6) C32 0.0180(7) 0.0200(8) 0.0186(7) -0.0064(6) -0.0061(6) -0.0003(6) C33 0.0266(9) 0.0260(9) 0.0297(9) -0.0116(7) -0.0124(7) 0.0026(7) C34 0.0319(10) 0.0300(10) 0.0214(8) -0.0142(7) -0.0115(7) 0.0107(8) C35 0.0268(9) 0.0281(9) 0.0160(7) -0.0064(7) -0.0026(6) 0.0067(7) C36 0.0193(8) 0.0211(8) 0.0179(7) -0.0049(6) -0.0033(6) 0.0016(6) N1 0.0354(9) 0.0282(9) 0.0307(8) -0.0016(7) -0.0090(7) 0.0041(7) P1 0.01252(18) 0.01250(18) 0.01321(17) -0.00177(13) -0.00325(13) -0.00154(13) P2 0.01372(18) 0.01264(18) 0.01255(17) -0.00296(13) -0.00277(13) -0.00126(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 P2 1.6398(17) . y C1 P1 1.6416(16) . y C2 N1 1.381(2) . y C2 C3 1.384(2) . y C2 P1 1.8292(16) . y C3 C4 1.391(2) . y C3 H3 0.9500 . y C4 C5 1.376(3) . y C4 H4 0.9500 . y C5 C6 1.382(3) . y C5 H5 0.9500 . y C6 N1 1.390(3) . y C6 H6 0.9500 . y C7 C12 1.389(2) . y C7 C8 1.394(2) . y C7 P1 1.8211(17) . y C8 C9 1.389(3) . y C8 H8 0.9500 . y C9 C10 1.388(3) . y C9 H9 0.9500 . y C10 C11 1.383(3) . y C10 H10 0.9500 . y C11 C12 1.383(3) . y C11 H11 0.9500 . y C12 H12 0.9500 . y C13 C14 1.389(2) . y C13 C18 1.393(2) . y C13 P1 1.8150(16) . y C14 C15 1.380(2) . y C14 H14 0.9500 . y C15 C16 1.381(3) . y C15 H15 0.9500 . y C16 C17 1.384(3) . y C16 H16 0.9500 . y C17 C18 1.388(2) . y C17 H17 0.9500 . y C18 H18 0.9500 . y C19 C20 1.392(2) . y C19 C24 1.395(2) . y C19 P2 1.8289(16) . y C20 C21 1.392(2) . y C20 H20 0.9500 . y C21 C22 1.387(3) . y C21 H21 0.9500 . y C22 C23 1.390(3) . y C22 H22 0.9500 . y C23 C24 1.387(2) . y C23 H23 0.9500 . y C24 H24 0.9500 . y C25 C26 1.393(2) . y C25 C30 1.393(2) . y C25 P2 1.8227(16) . y C26 C27 1.391(2) . y C26 H26 0.9500 . y C27 C28 1.386(3) . y C27 H27 0.9500 . y C28 C29 1.389(3) . y C28 H28 0.9500 . y C29 C30 1.388(2) . y C29 H29 0.9500 . y C30 H30 0.9500 . y C31 C32 1.376(2) . y C31 C36 1.391(2) . y C31 P2 1.8324(16) . y C32 C33 1.381(2) . y C32 H32 0.9500 . y C33 C34 1.382(3) . y C33 H33 0.9500 . y C34 C35 1.385(3) . y C34 H34 0.9500 . y C35 C36 1.396(2) . y C35 H35 0.9500 . y C36 H36 0.9500 . y C37 C38 1.435(8) . y C37 H37A 0.9800 . y C37 H37B 0.9800 . y C37 H37C 0.9800 . y C38 C43 1.358(6) . y C38 C39 1.366(6) . y C39 C40 1.396(7) . y C39 H39 0.9500 . y C40 C41 1.491(9) . y C40 H40 0.9500 . y C41 C42 1.288(9) . y C41 H41 0.9500 . y C42 C43 1.445(8) . y C42 H42 0.9500 . y C43 H43 0.9500 . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 C1 P1 133.25(10) . . y N1 C2 C3 120.62(15) . . y N1 C2 P1 121.58(13) . . y C3 C2 P1 117.76(12) . . y C2 C3 C4 120.23(16) . . y C2 C3 H3 119.9 . . y C4 C3 H3 119.9 . . y C5 C4 C3 119.46(17) . . y C5 C4 H4 120.3 . . y C3 C4 H4 120.3 . . y C4 C5 C6 119.95(17) . . y C4 C5 H5 120.0 . . y C6 C5 H5 120.0 . . y C5 C6 N1 121.11(18) . . y C5 C6 H6 119.4 . . y N1 C6 H6 119.4 . . y C12 C7 C8 119.55(16) . . y C12 C7 P1 122.06(13) . . y C8 C7 P1 118.36(13) . . y C9 C8 C7 120.32(16) . . y C9 C8 H8 119.8 . . y C7 C8 H8 119.8 . . y C10 C9 C8 119.80(17) . . y C10 C9 H9 120.1 . . y C8 C9 H9 120.1 . . y C11 C10 C9 119.67(18) . . y C11 C10 H10 120.2 . . y C9 C10 H10 120.2 . . y C12 C11 C10 120.91(18) . . y C12 C11 H11 119.5 . . y C10 C11 H11 119.5 . . y C11 C12 C7 119.76(17) . . y C11 C12 H12 120.1 . . y C7 C12 H12 120.1 . . y C14 C13 C18 119.64(15) . . y C14 C13 P1 118.16(12) . . y C18 C13 P1 121.37(12) . . y C15 C14 C13 119.97(16) . . y C15 C14 H14 120.0 . . y C13 C14 H14 120.0 . . y C14 C15 C16 120.51(17) . . y C14 C15 H15 119.7 . . y C16 C15 H15 119.7 . . y C15 C16 C17 119.90(16) . . y C15 C16 H16 120.1 . . y C17 C16 H16 120.1 . . y C16 C17 C18 120.07(16) . . y C16 C17 H17 120.0 . . y C18 C17 H17 120.0 . . y C17 C18 C13 119.89(16) . . y C17 C18 H18 120.1 . . y C13 C18 H18 120.1 . . y C20 C19 C24 119.47(15) . . y C20 C19 P2 118.03(12) . . y C24 C19 P2 122.40(13) . . y C21 C20 C19 120.54(15) . . y C21 C20 H20 119.7 . . y C19 C20 H20 119.7 . . y C22 C21 C20 119.66(16) . . y C22 C21 H21 120.2 . . y C20 C21 H21 120.2 . . y C21 C22 C23 120.01(16) . . y C21 C22 H22 120.0 . . y C23 C22 H22 120.0 . . y C24 C23 C22 120.42(16) . . y C24 C23 H23 119.8 . . y C22 C23 H23 119.8 . . y C23 C24 C19 119.88(16) . . y C23 C24 H24 120.1 . . y C19 C24 H24 120.1 . . y C26 C25 C30 119.25(15) . . y C26 C25 P2 120.13(12) . . y C30 C25 P2 119.63(12) . . y C27 C26 C25 120.67(15) . . y C27 C26 H26 119.7 . . y C25 C26 H26 119.7 . . y C28 C27 C26 119.55(16) . . y C28 C27 H27 120.2 . . y C26 C27 H27 120.2 . . y C27 C28 C29 120.22(16) . . y C27 C28 H28 119.9 . . y C29 C28 H28 119.9 . . y C30 C29 C28 120.12(16) . . y C30 C29 H29 119.9 . . y C28 C29 H29 119.9 . . y C29 C30 C25 120.16(15) . . y C29 C30 H30 119.9 . . y C25 C30 H30 119.9 . . y C32 C31 C36 120.70(15) . . y C32 C31 P2 120.73(12) . . y C36 C31 P2 118.55(13) . . y C31 C32 C33 119.11(17) . . y C31 C32 H32 120.4 . . y C33 C32 H32 120.4 . . y C32 C33 C34 121.30(19) . . y C32 C33 H33 119.3 . . y C34 C33 H33 119.3 . . y C33 C34 C35 119.58(16) . . y C33 C34 H34 120.2 . . y C35 C34 H34 120.2 . . y C34 C35 C36 119.70(17) . . y C34 C35 H35 120.2 . . y C36 C35 H35 120.2 . . y C31 C36 C35 119.60(18) . . y C31 C36 H36 120.2 . . y C35 C36 H36 120.2 . . y C2 N1 C6 118.60(17) . . y C1 P1 C13 116.81(8) . . y C1 P1 C7 108.95(8) . . y C13 P1 C7 105.68(7) . . y C1 P1 C2 117.89(8) . . y C13 P1 C2 103.20(7) . . y C7 P1 C2 102.82(7) . . y C1 P2 C25 116.55(8) . . y C1 P2 C19 108.67(8) . . y C25 P2 C19 105.09(7) . . y C1 P2 C31 118.29(8) . . y C25 P2 C31 103.98(7) . . y C19 P2 C31 102.68(7) . . y C43 C38 C39 122.4(4) . . y C43 C38 C37 113.7(5) . . y C39 C38 C37 123.8(5) . . y C38 C39 C40 119.4(4) . . y C38 C39 H39 120.3 . . y C40 C39 H39 120.3 . . y C39 C40 C41 119.5(5) . . y C39 C40 H40 120.3 . . y C41 C40 H40 120.3 . . y C42 C41 C40 116.9(7) . . y C42 C41 H41 121.5 . . y C40 C41 H41 121.5 . . y C41 C42 C43 124.3(6) . . y C41 C42 H42 117.9 . . y C43 C42 H42 117.9 . . y C38 C43 C42 117.5(5) . . y C38 C43 H43 121.2 . . y C42 C43 H43 121.2 . . y _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.902 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.079 data_4 _database_code_depnum_ccdc_archive 'CCDC 914764' _audit_creation_date 2012-04-21 _audit_block_code RKI-RF-155-04_6945 _chemical_name_systematic ; (diphenyl-2-pyridyl-phosphorane)(triphenylphosphorane)idene- triphenylphosphine-gold(i) hexafluoroantimonate dichloromethane solute ; _chemical_melting_point ? _chemical_compound_source 'dichloromethane, pentane' _chemical_formula_moiety 'C54 H44 Au N P3, F6 Sb, C H2 Cl2' _chemical_formula_sum 'C55 H46 Au Cl2 F6 N P3 Sb' _chemical_formula_weight 1317.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-p 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0585(17) _cell_length_b 15.106(2) _cell_length_c 16.288(2) _cell_angle_alpha 63.058(2) _cell_angle_beta 68.541(3) _cell_angle_gamma 83.121(3) _cell_volume 2457.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 7316 _cell_measurement_theta_min 2.3006 _cell_measurement_theta_max 23.2555 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0050 1.00 0.00 1.00 0.0020 -1.00 0.00 -1.00 0.0020 0.00 -1.00 0.00 0.0050 0.00 1.00 0.00 0.0050 0.00 0.00 -1.00 0.0050 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.004 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method ? _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 3.800 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.95624 _exptl_absorpt_correction_T_max 0.98694 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_special_details ; Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75 ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_monochromator 'Incoatec Helios mirrors' _diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 66.67 _diffrn_reflns_number 7175 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.44 _reflns_number_total 7175 _reflns_number_gt 5917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT software (Bruker AXS, 2004)' _computing_data_reduction 'SAINT software (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The minimum and maximum estimated transmissions from the multi-scan scaling are 0.8432 and 1.0000 (SADABS). Diffracted intensities above 12 Angstroem resolution were affected by the beamstop and were removed. The crystal contains disordered dichloromethane. Intensity statistics for the dataset are given below: Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 2.44 360 361 99.7 5.57 78.5 38.26 0.0327 0.0196 2.44 - 1.93 371 374 99.2 5.52 52.9 32.13 0.0418 0.0243 1.93 - 1.68 369 369 100.0 5.55 44.9 28.36 0.0451 0.0265 1.68 - 1.52 373 373 100.0 5.44 36.9 25.27 0.0518 0.0300 1.52 - 1.42 365 365 100.0 5.46 35.9 24.49 0.0532 0.0313 1.42 - 1.33 409 409 100.0 5.37 30.1 21.00 0.0609 0.0361 1.33 - 1.26 382 382 100.0 5.28 23.7 17.94 0.0772 0.0436 1.26 - 1.20 421 421 100.0 5.08 22.4 16.21 0.0798 0.0484 1.20 - 1.15 428 428 100.0 4.87 20.2 14.86 0.0929 0.0550 1.15 - 1.11 388 388 100.0 4.81 16.7 12.61 0.1043 0.0653 1.11 - 1.07 464 464 100.0 4.56 18.4 13.18 0.1039 0.0648 1.07 - 1.04 373 373 100.0 4.49 14.9 10.91 0.1257 0.0785 1.04 - 1.01 437 437 100.0 4.29 14.1 9.98 0.1286 0.0852 1.01 - 0.98 501 501 100.0 4.29 13.6 9.38 0.1338 0.0912 0.98 - 0.96 362 362 100.0 4.02 13.0 8.59 0.1466 0.0986 0.96 - 0.94 392 392 100.0 4.05 11.4 7.53 0.1597 0.1132 0.94 - 0.92 424 424 100.0 3.93 10.0 6.76 0.1749 0.1287 0.92 - 0.89 359 392 91.6 2.80 8.9 5.35 0.1843 0.1889 #----------------------------------------------------------------------------- Inf - 0.89 7178 7215 99.5 4.72 25.2 16.46 0.0705 0.0483 #------------------------------------------------------------------------------ The crystal appears to be twinned about (0 0 1) [-2 -2 5] with a rotation matrix of [-1 0 0 0 -1 0 -0.854 -0.895 1.0] (according to PLATON). The refined fractional contribution of the second component was 0.09987(154). The crystal diffracted so pooly that the non-merohedral intensity data of this minor second component could not be collected. It cannot be ruled out that the reflections for which the measured intensities were significantly higher than the calculated ones based on the model, are not a result of loss of solvent from the crystal and corresponding crystallinity with retention of the gold contribution. The probable position of the N atom was determined by refining atomic displacement parameters of all atoms in the 6-membered rings as C atoms. The C atom, with the smallest atomic displacement parameter and no adjacent electron density that could be construed as an H atom, was chosen to be N. Subsequent refinement cycles with atomic displacement parameters of all ring atoms restrained to be similar with a standard uncertainty of 0.001 suggested that this choice was likely but not certain. We cannot rule out that the N atom is disordered over several pyridyl rings Assuming that the final model is correct, the larger than unity goodness-of-fit of 1.835 at the end of refinement suggests that the errors attributed to the measured intensities were underestimated. Highest peak 2.37 at 0.5768 0.2768 0.2681 [ 1.07 A from AU1 ] Deepest hole -1.22 at 0.6856 0.3704 0.1782 [ 0.74 A from AU1 ] ; _iucr_refine_instructions_details ; TITL 6945sadabs in P-1 #2 CELL 0.71073 12.0585 15.1062 16.2882 63.058 68.541 83.121 ZERR 2 0.0017 0.0021 0.0023 0.002 0.003 0.003 LATT 1 SFAC C H Au Cl F N P Sb UNIT 110 92 2 4 12 2 6 2 L.S. 10 PLAN 20 TEMP -173 SHEL 12.0 0.4 LIST 4 BOND $H FMAP 2 SIMU 0.001 C2 > C7 C8 > C13 C20 > C25 C32 > C37 C38 > C43 C44 > C49 C50 > C55 N1 ACTA WGHT 0.000000 4.847519 BASF 0.09987 FVAR 3.30947 C1 1 0.563265 0.301732 0.347339 11.00000 0.01410 0.01133 = 0.02433 -0.01234 -0.01044 0.00497 C2 1 0.363598 0.212260 0.348218 11.00000 0.04265 0.02924 = 0.03722 -0.01827 -0.02359 -0.00019 C3 1 0.365890 0.273542 0.253282 11.00000 0.04413 0.03050 = 0.03815 -0.01727 -0.02319 -0.00074 AFIX 43 H3 2 0.396578 0.340527 0.220984 11.00000 -1.20000 AFIX 0 C4 1 0.324006 0.237413 0.206458 11.00000 0.04482 0.03123 = 0.03869 -0.01694 -0.02293 -0.00086 AFIX 43 H4 2 0.322943 0.279967 0.142382 11.00000 -1.20000 AFIX 0 C5 1 0.283317 0.139590 0.251712 11.00000 0.04414 0.03056 = 0.03842 -0.01799 -0.02304 -0.00094 AFIX 43 H5 2 0.258903 0.113901 0.217087 11.00000 -1.20000 AFIX 0 C6 1 0.277740 0.079790 0.344748 11.00000 0.04304 0.02957 = 0.03807 -0.01837 -0.02323 -0.00050 AFIX 43 H6 2 0.247127 0.012814 0.376708 11.00000 -1.20000 AFIX 0 C7 1 0.317223 0.117430 0.392835 11.00000 0.04254 0.02916 = 0.03736 -0.01845 -0.02334 -0.00006 AFIX 43 H7 2 0.311815 0.075899 0.458900 11.00000 -1.20000 AFIX 0 C8 1 0.316345 0.369072 0.401582 11.00000 0.02075 0.01721 = 0.02784 -0.01275 -0.01438 0.00532 C9 1 0.193371 0.349971 0.430819 11.00000 0.02089 0.01754 = 0.02825 -0.01198 -0.01404 0.00548 AFIX 43 H9 2 0.162333 0.283886 0.457575 11.00000 -1.20000 AFIX 0 C10 1 0.117120 0.427652 0.420634 11.00000 0.02093 0.01790 = 0.02852 -0.01170 -0.01405 0.00554 AFIX 43 H10 2 0.033753 0.414994 0.440820 11.00000 -1.20000 AFIX 0 C11 1 0.163040 0.522646 0.381264 11.00000 0.02127 0.01793 = 0.02875 -0.01189 -0.01386 0.00567 AFIX 43 H11 2 0.111232 0.576094 0.372741 11.00000 -1.20000 AFIX 0 C12 1 0.282681 0.541673 0.353992 11.00000 0.02161 0.01795 = 0.02905 -0.01206 -0.01360 0.00536 AFIX 43 H12 2 0.313110 0.607817 0.327888 11.00000 -1.20000 AFIX 0 C13 1 0.359611 0.464251 0.364488 11.00000 0.02112 0.01758 = 0.02839 -0.01250 -0.01408 0.00519 AFIX 43 H13 2 0.442509 0.477569 0.345812 11.00000 -1.20000 AFIX 0 C14 1 0.375763 0.176435 0.534458 11.00000 0.01778 0.01042 = 0.02624 -0.01085 -0.01656 0.00696 C16 1 0.409717 0.017193 0.649473 11.00000 0.02468 0.01816 = 0.03434 -0.01000 -0.02155 0.00655 AFIX 43 H16 2 0.451959 -0.042015 0.663546 11.00000 -1.20000 AFIX 0 C17 1 0.322582 0.029119 0.723593 11.00000 0.02738 0.02781 = 0.02048 -0.00536 -0.01571 0.00078 AFIX 43 H17 2 0.304031 -0.021582 0.789173 11.00000 -1.20000 AFIX 0 C18 1 0.260405 0.114310 0.704758 11.00000 0.02539 0.03464 = 0.02157 -0.01457 -0.00907 -0.00036 AFIX 43 H18 2 0.198738 0.122292 0.757116 11.00000 -1.20000 AFIX 0 C19 1 0.287712 0.187586 0.610255 11.00000 0.01369 0.02257 = 0.02604 -0.01432 -0.01087 0.00508 AFIX 43 H19 2 0.245110 0.246609 0.597311 11.00000 -1.20000 AFIX 0 C20 1 0.737946 0.428207 0.344744 11.00000 0.02160 0.02615 = 0.02893 -0.01993 -0.01091 0.00366 C21 1 0.754421 0.494976 0.247469 11.00000 0.02231 0.02672 = 0.02918 -0.01979 -0.01060 0.00311 AFIX 43 H21 2 0.722380 0.478963 0.210230 11.00000 -1.20000 AFIX 0 C22 1 0.817405 0.584389 0.205442 11.00000 0.02288 0.02714 = 0.02965 -0.01948 -0.01002 0.00314 AFIX 43 H22 2 0.830189 0.629371 0.138610 11.00000 -1.20000 AFIX 0 C23 1 0.862114 0.609187 0.259632 11.00000 0.02253 0.02682 = 0.02986 -0.01985 -0.00996 0.00358 AFIX 43 H23 2 0.905653 0.670964 0.229819 11.00000 -1.20000 AFIX 0 C24 1 0.844065 0.545334 0.355926 11.00000 0.02188 0.02634 = 0.02958 -0.01999 -0.01069 0.00388 AFIX 43 H24 2 0.874335 0.562950 0.393130 11.00000 -1.20000 AFIX 0 C25 1 0.781688 0.455096 0.399044 11.00000 0.02159 0.02616 = 0.02911 -0.01984 -0.01108 0.00392 AFIX 43 H25 2 0.768507 0.411053 0.466176 11.00000 -1.20000 AFIX 0 C26 1 0.773138 0.220080 0.399572 11.00000 0.01161 0.01660 = 0.01265 -0.00864 -0.00538 -0.00050 C27 1 0.871153 0.222627 0.423601 11.00000 0.01985 0.02353 = 0.02094 -0.01648 -0.00707 0.00223 AFIX 43 H27 2 0.879240 0.271952 0.442311 11.00000 -1.20000 AFIX 0 C28 1 0.957763 0.153644 0.420574 11.00000 0.02043 0.02548 = 0.02388 -0.01263 -0.01471 0.00290 AFIX 43 H28 2 1.024806 0.156247 0.437020 11.00000 -1.20000 AFIX 0 C29 1 0.947338 0.082342 0.394228 11.00000 0.02568 0.01423 = 0.02325 -0.00574 -0.01312 0.01352 AFIX 43 H29 2 1.007661 0.036072 0.391455 11.00000 -1.20000 AFIX 0 C30 1 0.849430 0.076923 0.371492 11.00000 0.02838 0.01390 = 0.02497 -0.01247 -0.01335 0.00364 AFIX 43 H30 2 0.842048 0.026796 0.353547 11.00000 -1.20000 AFIX 0 C31 1 0.762553 0.144573 0.374973 11.00000 0.01818 0.02140 = 0.01923 -0.01245 -0.00934 0.00675 AFIX 43 H31 2 0.694553 0.139984 0.360505 11.00000 -1.20000 AFIX 0 C32 1 0.585054 0.288703 0.527232 11.00000 0.01846 0.03463 = 0.02866 -0.02259 -0.01204 0.00132 C33 1 0.601401 0.207703 0.606718 11.00000 0.01902 0.03532 = 0.02908 -0.02200 -0.01153 0.00140 AFIX 43 H33 2 0.653490 0.158191 0.596828 11.00000 -1.20000 AFIX 0 C34 1 0.542144 0.198846 0.700207 11.00000 0.01965 0.03642 = 0.02977 -0.02106 -0.01101 0.00128 AFIX 43 H34 2 0.553341 0.143083 0.754917 11.00000 -1.20000 AFIX 0 C35 1 0.467178 0.269937 0.714782 11.00000 0.01990 0.03645 = 0.03015 -0.02150 -0.01072 0.00079 AFIX 43 H35 2 0.426094 0.263393 0.779533 11.00000 -1.20000 AFIX 0 C36 1 0.451355 0.350541 0.636028 11.00000 0.01939 0.03564 = 0.03025 -0.02195 -0.01102 0.00109 AFIX 43 H36 2 0.399207 0.399820 0.646432 11.00000 -1.20000 AFIX 0 C37 1 0.510048 0.360782 0.542344 11.00000 0.01863 0.03480 = 0.02929 -0.02219 -0.01174 0.00151 AFIX 43 H37 2 0.499222 0.417239 0.487956 11.00000 -1.20000 AFIX 0 C38 1 0.819604 0.467819 -0.042327 11.00000 0.06194 0.04166 = 0.02986 -0.01446 -0.01281 -0.00880 C39 1 0.863275 0.501947 -0.142619 11.00000 0.06211 0.04175 = 0.03021 -0.01424 -0.01206 -0.00860 AFIX 43 H39 2 0.844547 0.464514 -0.170000 11.00000 -1.20000 AFIX 0 C40 1 0.931591 0.586537 -0.203167 11.00000 0.06199 0.04199 = 0.03021 -0.01360 -0.01190 -0.00854 AFIX 43 H40 2 0.962169 0.606706 -0.272065 11.00000 -1.20000 AFIX 0 C41 1 0.958075 0.644775 -0.166531 11.00000 0.06187 0.04212 = 0.03006 -0.01331 -0.01266 -0.00876 AFIX 43 H41 2 1.003913 0.705984 -0.209199 11.00000 -1.20000 AFIX 0 C42 1 0.916565 0.611570 -0.068341 11.00000 0.06253 0.04248 = 0.03013 -0.01366 -0.01284 -0.00948 AFIX 43 H42 2 0.934054 0.650146 -0.041519 11.00000 -1.20000 AFIX 0 C43 1 0.849487 0.523350 -0.005527 11.00000 0.06260 0.04226 = 0.03004 -0.01407 -0.01284 -0.00934 AFIX 43 H43 2 0.823798 0.500856 0.063599 11.00000 -1.20000 AFIX 0 C44 1 0.627313 0.350421 -0.014566 11.00000 0.09412 0.06901 = 0.08643 -0.04802 -0.06895 0.02695 C45 1 0.581048 0.434432 -0.062729 11.00000 0.09404 0.06907 = 0.08652 -0.04776 -0.06870 0.02740 AFIX 43 H45 2 0.607371 0.496336 -0.072285 11.00000 -1.20000 AFIX 0 C46 1 0.491579 0.430908 -0.099945 11.00000 0.09425 0.06957 = 0.08672 -0.04732 -0.06863 0.02752 AFIX 43 H46 2 0.457008 0.490755 -0.131714 11.00000 -1.20000 AFIX 0 C47 1 0.458491 0.352935 -0.091929 11.00000 0.09439 0.07016 = 0.08678 -0.04747 -0.06917 0.02662 AFIX 43 H47 2 0.400215 0.353852 -0.118787 11.00000 -1.20000 AFIX 0 C48 1 0.504922 0.262271 -0.043873 11.00000 0.09488 0.07021 = 0.08745 -0.04732 -0.06897 0.02626 AFIX 43 H48 2 0.476943 0.201880 -0.036292 11.00000 -1.20000 AFIX 0 C49 1 0.595264 0.262602 -0.006511 11.00000 0.09458 0.06972 = 0.08727 -0.04743 -0.06900 0.02652 AFIX 43 H49 2 0.631908 0.203173 0.023116 11.00000 -1.20000 AFIX 0 C50 1 0.833498 0.255028 0.033541 11.00000 0.07668 0.03028 = 0.03160 -0.01887 -0.02326 0.01129 C51 1 0.870046 0.233842 -0.045728 11.00000 0.07732 0.03094 = 0.03218 -0.01842 -0.02274 0.01145 AFIX 43 H51 2 0.840419 0.269039 -0.098017 11.00000 -1.20000 AFIX 0 C52 1 0.950395 0.160793 -0.048804 11.00000 0.07785 0.03096 = 0.03258 -0.01842 -0.02224 0.01160 AFIX 43 H52 2 0.976055 0.146184 -0.103648 11.00000 -1.20000 AFIX 0 C53 1 0.992645 0.110121 0.025326 11.00000 0.07784 0.03082 = 0.03254 -0.01835 -0.02211 0.01178 AFIX 43 H53 2 1.047865 0.060335 0.022001 11.00000 -1.20000 AFIX 0 C54 1 0.956616 0.129774 0.105679 11.00000 0.07740 0.03058 = 0.03214 -0.01842 -0.02247 0.01168 AFIX 43 H54 2 0.986275 0.094219 0.157901 11.00000 -1.20000 AFIX 0 C55 1 0.877287 0.201573 0.108342 11.00000 0.07690 0.03031 = 0.03162 -0.01884 -0.02294 0.01141 AFIX 43 H55 2 0.851311 0.215189 0.163807 11.00000 -1.20000 AFIX 0 PART -1 C56A 1 0.695488 -0.009916 -0.053188 10.50000 0.08152 AFIX 23 H56A 2 0.767278 0.036245 -0.092580 10.50000 -1.20000 H56B 2 0.641599 0.007634 -0.091193 10.50000 -1.20000 AFIX 0 PART -2 C56B 1 0.569121 0.006351 0.008758 10.50000 0.08809 AFIX 23 H56C 2 0.598160 0.062872 -0.057698 10.50000 -1.20000 H56D 2 0.506264 -0.034818 0.014385 10.50000 -1.20000 AFIX 0 PART 0 AU1 3 0.641917 0.328319 0.201680 11.00000 0.02906 0.02268 = 0.02453 -0.01206 -0.01649 0.00507 PART -1 CL1A 4 0.736636 -0.143789 -0.015486 10.50000 0.10446 CL2A 4 0.624879 -0.008703 0.057874 10.50000 0.09864 PART -2 CL1B 4 0.692302 -0.067772 0.048741 10.50000 0.25194 CL2B 4 0.534579 0.036262 0.088573 10.50000 0.34991 PART 0 F1 5 0.202456 0.917417 0.293993 11.00000 0.04563 0.02010 = 0.04841 -0.01435 -0.02214 -0.00686 F2 5 -0.006817 0.739675 0.312097 11.00000 0.04010 0.02651 = 0.05732 -0.02998 -0.03616 0.01584 F3 5 0.135954 0.725469 0.406241 11.00000 0.04102 0.02362 = 0.03482 -0.01611 -0.03116 0.01296 F4 5 0.220681 0.794134 0.214204 11.00000 0.05280 0.03548 = 0.04170 -0.02345 -0.01650 0.00283 F5 5 -0.026121 0.861069 0.393515 11.00000 0.03885 0.04207 = 0.06614 -0.04405 -0.03200 0.02219 F6 5 0.059441 0.929746 0.200377 11.00000 0.10680 0.02742 = 0.06595 -0.01549 -0.06600 0.02141 N1 6 0.438917 0.090442 0.552337 11.00000 0.03237 0.03445 = 0.05705 -0.02507 -0.02201 0.00079 P1 7 0.416299 0.268154 0.406468 11.00000 0.01566 0.01373 = 0.02603 -0.01328 -0.01352 0.00695 P2 7 0.656802 0.308271 0.401984 11.00000 0.01444 0.01764 = 0.01848 -0.01319 -0.00970 0.00624 P3 7 0.730866 0.352001 0.042819 11.00000 0.04038 0.02958 = 0.02709 -0.01209 -0.01796 0.00396 SB1 8 0.097879 0.827664 0.303905 11.00000 0.03340 0.01410 = 0.03169 -0.01342 -0.02399 0.00871 HKLF 5 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+4.8475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7175 _refine_ls_number_parameters 620 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.835 _refine_ls_restrained_S_all 1.806 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5633(8) 0.3017(6) 0.3473(7) 0.014(2) Uani 1 1 d . . . C2 C 0.3636(10) 0.2123(8) 0.3482(8) 0.0317(12) Uani 1 1 d U . . C3 C 0.3659(10) 0.2735(8) 0.2533(8) 0.0337(12) Uani 1 1 d U . . H3 H 0.3966 0.3405 0.2210 0.040 Uiso 1 1 calc R . . C4 C 0.3240(10) 0.2374(8) 0.2065(8) 0.0348(12) Uani 1 1 d U . . H4 H 0.3229 0.2800 0.1424 0.042 Uiso 1 1 calc R . . C5 C 0.2833(10) 0.1396(8) 0.2517(8) 0.0336(12) Uani 1 1 d U . . H5 H 0.2589 0.1139 0.2171 0.040 Uiso 1 1 calc R . . C6 C 0.2777(9) 0.0798(8) 0.3447(8) 0.0325(12) Uani 1 1 d U . . H6 H 0.2471 0.0128 0.3767 0.039 Uiso 1 1 calc R . . C7 C 0.3172(9) 0.1174(8) 0.3928(8) 0.0317(12) Uani 1 1 d U . . H7 H 0.3118 0.0759 0.4589 0.038 Uiso 1 1 calc R . . C8 C 0.3163(8) 0.3691(7) 0.4016(7) 0.0194(11) Uani 1 1 d U . . C9 C 0.1934(8) 0.3500(7) 0.4308(7) 0.0202(11) Uani 1 1 d U . . H9 H 0.1623 0.2839 0.4576 0.024 Uiso 1 1 calc R . . C10 C 0.1171(9) 0.4277(7) 0.4206(7) 0.0206(11) Uani 1 1 d U . . H10 H 0.0338 0.4150 0.4408 0.025 Uiso 1 1 calc R . . C11 C 0.1630(8) 0.5226(7) 0.3813(7) 0.0209(11) Uani 1 1 d U . . H11 H 0.1112 0.5761 0.3727 0.025 Uiso 1 1 calc R . . C12 C 0.2827(8) 0.5417(7) 0.3540(7) 0.0211(11) Uani 1 1 d U . . H12 H 0.3131 0.6078 0.3279 0.025 Uiso 1 1 calc R . . C13 C 0.3596(8) 0.4643(7) 0.3645(7) 0.0201(11) Uani 1 1 d U . . H13 H 0.4425 0.4776 0.3458 0.024 Uiso 1 1 calc R . . C14 C 0.3758(8) 0.1764(6) 0.5345(7) 0.015(2) Uani 1 1 d . . . C16 C 0.4097(9) 0.0172(7) 0.6495(7) 0.023(2) Uani 1 1 d . . . H16 H 0.4520 -0.0420 0.6635 0.028 Uiso 1 1 calc R . . C17 C 0.3226(9) 0.0291(7) 0.7236(7) 0.025(2) Uani 1 1 d . . . H17 H 0.3040 -0.0216 0.7892 0.030 Uiso 1 1 calc R . . C18 C 0.2604(9) 0.1143(7) 0.7048(7) 0.026(2) Uani 1 1 d . . . H18 H 0.1987 0.1223 0.7571 0.031 Uiso 1 1 calc R . . C19 C 0.2877(8) 0.1876(7) 0.6103(7) 0.018(2) Uani 1 1 d . . . H19 H 0.2451 0.2466 0.5973 0.022 Uiso 1 1 calc R . . C20 C 0.7379(8) 0.4282(7) 0.3447(7) 0.0220(11) Uani 1 1 d U . . C21 C 0.7544(8) 0.4950(7) 0.2475(7) 0.0227(11) Uani 1 1 d U . . H21 H 0.7224 0.4790 0.2102 0.027 Uiso 1 1 calc R . . C22 C 0.8174(8) 0.5844(7) 0.2054(7) 0.0237(11) Uani 1 1 d U . . H22 H 0.8302 0.6294 0.1386 0.028 Uiso 1 1 calc R . . C23 C 0.8621(8) 0.6092(7) 0.2596(7) 0.0234(11) Uani 1 1 d U . . H23 H 0.9057 0.6710 0.2298 0.028 Uiso 1 1 calc R . . C24 C 0.8441(8) 0.5453(7) 0.3559(7) 0.0226(11) Uani 1 1 d U . . H24 H 0.8743 0.5629 0.3931 0.027 Uiso 1 1 calc R . . C25 C 0.7817(8) 0.4551(7) 0.3990(7) 0.0221(11) Uani 1 1 d U . . H25 H 0.7685 0.4111 0.4662 0.027 Uiso 1 1 calc R . . C26 C 0.7731(7) 0.2201(6) 0.3996(6) 0.012(2) Uani 1 1 d . . . C27 C 0.8712(8) 0.2226(7) 0.4236(7) 0.019(2) Uani 1 1 d . . . H27 H 0.8792 0.2720 0.4423 0.023 Uiso 1 1 calc R . . C28 C 0.9578(8) 0.1536(7) 0.4206(7) 0.021(2) Uani 1 1 d . . . H28 H 1.0248 0.1562 0.4370 0.025 Uiso 1 1 calc R . . C29 C 0.9473(9) 0.0823(7) 0.3942(7) 0.022(2) Uani 1 1 d . . . H29 H 1.0077 0.0361 0.3915 0.026 Uiso 1 1 calc R . . C30 C 0.8494(8) 0.0769(7) 0.3715(7) 0.020(2) Uani 1 1 d . . . H30 H 0.8420 0.0268 0.3535 0.024 Uiso 1 1 calc R . . C31 C 0.7626(8) 0.1446(7) 0.3750(6) 0.018(2) Uani 1 1 d . . . H31 H 0.6946 0.1400 0.3605 0.021 Uiso 1 1 calc R . . C32 C 0.5851(8) 0.2887(7) 0.5272(7) 0.0226(11) Uani 1 1 d U . . C33 C 0.6014(8) 0.2077(7) 0.6067(7) 0.0237(11) Uani 1 1 d U . . H33 H 0.6535 0.1582 0.5968 0.028 Uiso 1 1 calc R . . C34 C 0.5421(8) 0.1988(8) 0.7002(7) 0.0253(11) Uani 1 1 d U . . H34 H 0.5533 0.1431 0.7549 0.030 Uiso 1 1 calc R . . C35 C 0.4672(8) 0.2699(7) 0.7148(7) 0.0254(11) Uani 1 1 d U . . H35 H 0.4261 0.2634 0.7795 0.030 Uiso 1 1 calc R . . C36 C 0.4514(8) 0.3505(7) 0.6360(7) 0.0247(11) Uani 1 1 d U . . H36 H 0.3992 0.3998 0.6464 0.030 Uiso 1 1 calc R . . C37 C 0.5100(8) 0.3608(7) 0.5423(7) 0.0233(11) Uani 1 1 d U . . H37 H 0.4992 0.4172 0.4880 0.028 Uiso 1 1 calc R . . C38 C 0.8196(11) 0.4678(9) -0.0423(8) 0.0450(14) Uani 1 1 d U . . C39 C 0.8633(11) 0.5019(9) -0.1426(8) 0.0456(14) Uani 1 1 d U . . H39 H 0.8445 0.4645 -0.1700 0.055 Uiso 1 1 calc R . . C40 C 0.9316(11) 0.5865(9) -0.2032(9) 0.0460(14) Uani 1 1 d U . . H40 H 0.9622 0.6067 -0.2721 0.055 Uiso 1 1 calc R . . C41 C 0.9581(11) 0.6448(9) -0.1665(8) 0.0458(14) Uani 1 1 d U . . H41 H 1.0039 0.7060 -0.2092 0.055 Uiso 1 1 calc R . . C42 C 0.9166(11) 0.6116(9) -0.0683(8) 0.0459(14) Uani 1 1 d U . . H42 H 0.9341 0.6501 -0.0415 0.055 Uiso 1 1 calc R . . C43 C 0.8495(11) 0.5234(9) -0.0055(9) 0.0457(14) Uani 1 1 d U . . H43 H 0.8238 0.5009 0.0636 0.055 Uiso 1 1 calc R . . C44 C 0.6273(14) 0.3504(11) -0.0146(11) 0.0681(18) Uani 1 1 d U . . C45 C 0.5810(13) 0.4344(11) -0.0627(10) 0.0684(18) Uani 1 1 d U . . H45 H 0.6074 0.4963 -0.0723 0.082 Uiso 1 1 calc R . . C46 C 0.4916(13) 0.4309(11) -0.0999(11) 0.0690(18) Uani 1 1 d U . . H46 H 0.4570 0.4908 -0.1317 0.083 Uiso 1 1 calc R . . C47 C 0.4585(14) 0.3529(11) -0.0919(11) 0.0690(18) Uani 1 1 d U . . H47 H 0.4002 0.3539 -0.1188 0.083 Uiso 1 1 calc R . . C48 C 0.5049(13) 0.2623(11) -0.0439(11) 0.0696(18) Uani 1 1 d U . . H48 H 0.4769 0.2019 -0.0363 0.084 Uiso 1 1 calc R . . C49 C 0.5953(13) 0.2626(11) -0.0065(11) 0.0692(18) Uani 1 1 d U . . H49 H 0.6319 0.2032 0.0231 0.083 Uiso 1 1 calc R . . C50 C 0.8335(12) 0.2550(8) 0.0335(8) 0.0436(14) Uani 1 1 d U . . C51 C 0.8700(11) 0.2338(8) -0.0457(8) 0.0447(14) Uani 1 1 d U . . H51 H 0.8404 0.2690 -0.0980 0.054 Uiso 1 1 calc R . . C52 C 0.9504(11) 0.1608(8) -0.0488(8) 0.0453(14) Uani 1 1 d U . . H52 H 0.9761 0.1462 -0.1036 0.054 Uiso 1 1 calc R . . C53 C 0.9926(11) 0.1101(8) 0.0253(8) 0.0453(14) Uani 1 1 d U . . H53 H 1.0479 0.0603 0.0220 0.054 Uiso 1 1 calc R . . C54 C 0.9566(11) 0.1298(8) 0.1057(8) 0.0447(14) Uani 1 1 d U . . H54 H 0.9863 0.0942 0.1579 0.054 Uiso 1 1 calc R . . C55 C 0.8773(11) 0.2016(8) 0.1083(8) 0.0438(14) Uani 1 1 d U . . H55 H 0.8513 0.2152 0.1638 0.053 Uiso 1 1 calc R . . C56A C 0.695(3) -0.010(2) -0.053(2) 0.082(10) Uiso 0.50 1 d P A -1 H56A H 0.7673 0.0363 -0.0926 0.098 Uiso 0.50 1 calc PR A -1 H56B H 0.6416 0.0076 -0.0912 0.098 Uiso 0.50 1 calc PR A -1 C56B C 0.569(3) 0.006(3) 0.009(3) 0.088(10) Uiso 0.50 1 d P B -2 H56C H 0.5981 0.0629 -0.0577 0.106 Uiso 0.50 1 calc PR B -2 H56D H 0.5062 -0.0348 0.0144 0.106 Uiso 0.50 1 calc PR B -2 Au1 Au 0.64192(4) 0.32832(3) 0.20168(3) 0.02290(13) Uani 1 1 d . . . Cl1A Cl 0.7366(9) -0.1438(8) -0.0155(7) 0.104(3) Uiso 0.50 1 d P A -1 Cl2A Cl 0.6249(10) -0.0087(8) 0.0579(8) 0.099(3) Uiso 0.50 1 d P A -1 Cl1B Cl 0.692(2) -0.0678(17) 0.0487(17) 0.252(9) Uiso 0.50 1 d P B -2 Cl2B Cl 0.535(3) 0.036(2) 0.089(2) 0.350(15) Uiso 0.50 1 d P B -2 F1 F 0.2025(5) 0.9174(4) 0.2940(4) 0.0358(15) Uani 1 1 d . . . F2 F -0.0068(5) 0.7397(4) 0.3121(4) 0.0320(15) Uani 1 1 d . . . F3 F 0.1360(5) 0.7255(4) 0.4062(4) 0.0273(14) Uani 1 1 d . . . F4 F 0.2207(5) 0.7941(4) 0.2142(4) 0.0408(16) Uani 1 1 d . . . F5 F -0.0261(5) 0.8611(4) 0.3935(5) 0.0385(16) Uani 1 1 d . . . F6 F 0.0594(7) 0.9297(5) 0.2004(5) 0.059(2) Uani 1 1 d . . . N1 N 0.4389(8) 0.0904(7) 0.5523(7) 0.037(2) Uani 1 1 d . . . P1 P 0.4163(2) 0.26815(17) 0.40647(18) 0.0153(6) Uani 1 1 d . . . P2 P 0.6568(2) 0.30827(17) 0.40198(17) 0.0140(5) Uani 1 1 d . . . P3 P 0.7309(3) 0.3520(2) 0.0428(2) 0.0308(7) Uani 1 1 d . . . Sb1 Sb 0.09788(6) 0.82766(5) 0.30391(5) 0.02183(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.014(5) 0.011(5) 0.024(6) -0.012(4) -0.010(4) 0.005(4) C2 0.043(3) 0.029(2) 0.037(3) -0.018(2) -0.024(3) 0.000(2) C3 0.044(3) 0.030(2) 0.038(3) -0.017(2) -0.023(3) -0.001(2) C4 0.045(3) 0.031(2) 0.039(3) -0.017(2) -0.023(3) -0.001(2) C5 0.044(3) 0.031(2) 0.038(3) -0.018(2) -0.023(3) -0.001(2) C6 0.043(3) 0.030(2) 0.038(3) -0.018(2) -0.023(3) -0.001(2) C7 0.043(3) 0.029(2) 0.037(3) -0.018(2) -0.023(3) 0.000(2) C8 0.021(2) 0.017(2) 0.028(2) -0.013(2) -0.014(2) 0.0053(19) C9 0.021(2) 0.018(2) 0.028(2) -0.012(2) -0.014(2) 0.0055(19) C10 0.021(2) 0.018(2) 0.029(2) -0.012(2) -0.014(2) 0.0055(19) C11 0.021(2) 0.018(2) 0.029(2) -0.012(2) -0.014(2) 0.0057(19) C12 0.022(2) 0.018(2) 0.029(2) -0.012(2) -0.014(2) 0.0054(19) C13 0.021(2) 0.018(2) 0.028(2) -0.013(2) -0.014(2) 0.0052(19) C14 0.018(5) 0.010(5) 0.026(6) -0.011(4) -0.017(5) 0.007(4) C16 0.025(6) 0.018(6) 0.034(7) -0.010(5) -0.022(5) 0.007(5) C17 0.027(6) 0.028(6) 0.020(6) -0.005(5) -0.016(5) 0.001(5) C18 0.025(6) 0.035(6) 0.022(6) -0.015(5) -0.009(5) 0.000(5) C19 0.014(5) 0.023(6) 0.026(6) -0.014(5) -0.011(5) 0.005(4) C20 0.022(2) 0.026(2) 0.029(2) -0.020(2) -0.011(2) 0.0037(19) C21 0.022(2) 0.027(2) 0.029(2) -0.020(2) -0.011(2) 0.0031(19) C22 0.023(2) 0.027(2) 0.030(2) -0.019(2) -0.010(2) 0.0031(19) C23 0.023(2) 0.027(2) 0.030(2) -0.020(2) -0.010(2) 0.0036(19) C24 0.022(2) 0.026(2) 0.030(2) -0.020(2) -0.011(2) 0.0039(19) C25 0.022(2) 0.026(2) 0.029(2) -0.020(2) -0.011(2) 0.0039(19) C26 0.012(5) 0.017(5) 0.013(5) -0.009(4) -0.005(4) -0.001(4) C27 0.020(5) 0.024(6) 0.021(5) -0.016(5) -0.007(5) 0.002(4) C28 0.020(5) 0.025(6) 0.024(6) -0.013(5) -0.015(5) 0.003(5) C29 0.026(6) 0.014(5) 0.023(6) -0.006(5) -0.013(5) 0.014(5) C30 0.028(6) 0.014(5) 0.025(6) -0.012(5) -0.013(5) 0.004(5) C31 0.018(5) 0.021(5) 0.019(5) -0.012(5) -0.009(4) 0.007(4) C32 0.018(2) 0.035(3) 0.029(2) -0.023(2) -0.012(2) 0.001(2) C33 0.019(2) 0.035(3) 0.029(2) -0.022(2) -0.012(2) 0.001(2) C34 0.020(2) 0.036(3) 0.030(2) -0.021(2) -0.011(2) 0.001(2) C35 0.020(2) 0.036(3) 0.030(2) -0.021(2) -0.011(2) 0.001(2) C36 0.019(2) 0.036(3) 0.030(2) -0.022(2) -0.011(2) 0.001(2) C37 0.019(2) 0.035(3) 0.029(2) -0.022(2) -0.012(2) 0.002(2) C38 0.062(3) 0.042(3) 0.030(3) -0.014(2) -0.013(3) -0.009(3) C39 0.062(3) 0.042(3) 0.030(3) -0.014(2) -0.012(3) -0.009(3) C40 0.062(3) 0.042(3) 0.030(3) -0.014(2) -0.012(3) -0.009(3) C41 0.062(3) 0.042(3) 0.030(3) -0.013(2) -0.013(3) -0.009(3) C42 0.063(3) 0.042(3) 0.030(3) -0.014(2) -0.013(3) -0.009(3) C43 0.063(3) 0.042(3) 0.030(3) -0.014(2) -0.013(3) -0.009(3) C44 0.094(4) 0.069(4) 0.086(4) -0.048(4) -0.069(4) 0.027(4) C45 0.094(4) 0.069(4) 0.087(4) -0.048(4) -0.069(4) 0.027(4) C46 0.094(4) 0.070(4) 0.087(4) -0.047(4) -0.069(4) 0.028(4) C47 0.094(4) 0.070(4) 0.087(4) -0.047(4) -0.069(4) 0.027(4) C48 0.095(4) 0.070(4) 0.087(4) -0.047(4) -0.069(4) 0.026(4) C49 0.095(4) 0.070(4) 0.087(4) -0.047(4) -0.069(4) 0.027(4) C50 0.077(4) 0.030(3) 0.032(3) -0.019(2) -0.023(3) 0.011(3) C51 0.077(4) 0.031(3) 0.032(3) -0.018(2) -0.023(3) 0.011(3) C52 0.078(4) 0.031(3) 0.033(3) -0.018(2) -0.022(3) 0.012(3) C53 0.078(4) 0.031(3) 0.033(3) -0.018(2) -0.022(3) 0.012(3) C54 0.077(4) 0.031(3) 0.032(3) -0.018(2) -0.022(3) 0.012(3) C55 0.077(4) 0.030(3) 0.032(3) -0.019(2) -0.023(3) 0.011(3) Au1 0.0291(2) 0.0227(2) 0.0245(2) -0.01206(19) -0.01649(19) 0.00507(18) F1 0.046(4) 0.020(3) 0.048(4) -0.014(3) -0.022(3) -0.007(3) F2 0.040(4) 0.027(3) 0.057(4) -0.030(3) -0.036(3) 0.016(3) F3 0.041(4) 0.024(3) 0.035(3) -0.016(3) -0.031(3) 0.013(3) F4 0.053(4) 0.035(4) 0.042(4) -0.023(3) -0.017(3) 0.003(3) F5 0.039(4) 0.042(4) 0.066(4) -0.044(4) -0.032(3) 0.022(3) F6 0.107(6) 0.027(4) 0.066(5) -0.015(4) -0.066(5) 0.021(4) N1 0.032(5) 0.034(6) 0.057(7) -0.025(5) -0.022(5) 0.001(5) P1 0.0157(13) 0.0137(13) 0.0260(15) -0.0133(12) -0.0135(12) 0.0069(11) P2 0.0144(13) 0.0176(13) 0.0185(14) -0.0132(12) -0.0097(11) 0.0062(11) P3 0.0404(18) 0.0296(16) 0.0271(16) -0.0121(14) -0.0180(14) 0.0040(14) Sb1 0.0334(4) 0.0141(4) 0.0317(4) -0.0134(3) -0.0240(4) 0.0087(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 P1 1.688(9) . y C1 P2 1.707(9) . y C1 Au1 2.067(9) . y C2 C7 1.358(14) . y C2 C3 1.388(14) . y C2 P1 1.820(10) . y C3 C4 1.364(14) . y C3 H3 0.9500 . y C4 C5 1.375(14) . y C4 H4 0.9500 . y C5 C6 1.348(14) . y C5 H5 0.9500 . y C6 C7 1.380(13) . y C6 H6 0.9500 . y C7 H7 0.9500 . y C8 C13 1.366(13) . y C8 C9 1.404(13) . y C8 P1 1.817(9) . y C9 C10 1.388(12) . y C9 H9 0.9500 . y C10 C11 1.369(13) . y C10 H10 0.9500 . y C11 C12 1.370(13) . y C11 H11 0.9500 . y C12 C13 1.390(12) . y C12 H12 0.9500 . y C13 H13 0.9500 . y C14 C19 1.366(12) . y C14 N1 1.391(11) . y C14 P1 1.818(9) . y C16 C17 1.348(13) . y C16 N1 1.397(13) . y C16 H16 0.9500 . y C17 C18 1.375(13) . y C17 H17 0.9500 . y C18 C19 1.370(13) . y C18 H18 0.9500 . y C19 H19 0.9500 . y C20 C21 1.392(13) . y C20 C25 1.394(12) . y C20 P2 1.826(10) . y C21 C22 1.377(13) . y C21 H21 0.9500 . y C22 C23 1.381(13) . y C22 H22 0.9500 . y C23 C24 1.367(13) . y C23 H23 0.9500 . y C24 C25 1.382(13) . y C24 H24 0.9500 . y C25 H25 0.9500 . y C26 C27 1.384(12) . y C26 C31 1.402(12) . y C26 P2 1.818(8) . y C27 C28 1.388(12) . y C27 H27 0.9500 . y C28 C29 1.360(13) . y C28 H28 0.9500 . y C29 C30 1.381(13) . y C29 H29 0.9500 . y C30 C31 1.378(12) . y C30 H30 0.9500 . y C31 H31 0.9500 . y C32 C33 1.380(13) . y C32 C37 1.381(13) . y C32 P2 1.795(10) . y C33 C34 1.375(13) . y C33 H33 0.9500 . y C34 C35 1.367(13) . y C34 H34 0.9500 . y C35 C36 1.368(13) . y C35 H35 0.9500 . y C36 C37 1.369(13) . y C36 H36 0.9500 . y C37 H37 0.9500 . y C38 C43 1.371(16) . y C38 C39 1.373(15) . y C38 P3 1.815(12) . y C39 C40 1.342(16) . y C39 H39 0.9500 . y C40 C41 1.384(16) . y C40 H40 0.9500 . y C41 C42 1.344(15) . y C41 H41 0.9500 . y C42 C43 1.376(16) . y C42 H42 0.9500 . y C43 H43 0.9500 . y C44 C45 1.336(17) . y C44 C49 1.362(18) . y C44 P3 1.821(13) . y C45 C46 1.434(17) . y C45 H45 0.9500 . y C46 C47 1.224(18) . y C46 H46 0.9500 . y C47 C48 1.403(17) . y C47 H47 0.9500 . y C48 C49 1.430(17) . y C48 H48 0.9500 . y C49 H49 0.9500 . y C50 C51 1.374(14) . y C50 C55 1.376(14) . y C50 P3 1.825(11) . y C51 C52 1.385(15) . y C51 H51 0.9500 . y C52 C53 1.350(15) . y C52 H52 0.9500 . y C53 C54 1.377(14) . y C53 H53 0.9500 . y C54 C55 1.363(14) . y C54 H54 0.9500 . y C55 H55 0.9500 . y C56A Cl2A 1.70(3) . y C56A Cl1A 1.89(3) . y C56A H56A 0.9900 . y C56A H56B 0.9900 . y C56B Cl2B 1.47(4) . y C56B Cl1B 1.88(4) . y C56B H56C 0.9900 . y C56B H56D 0.9900 . y Au1 P3 2.280(3) . y Cl1B Cl2B 2.41(4) . y F1 Sb1 1.875(5) . y F2 Sb1 1.870(5) . y F3 Sb1 1.852(5) . y F4 Sb1 1.869(6) . y F5 Sb1 1.874(6) . y F6 Sb1 1.866(6) . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 C1 P2 124.3(5) . . y P1 C1 Au1 119.5(5) . . y P2 C1 Au1 116.1(5) . . y C7 C2 C3 118.5(9) . . y C7 C2 P1 124.6(8) . . y C3 C2 P1 116.8(8) . . y C4 C3 C2 119.9(10) . . y C4 C3 H3 120.1 . . y C2 C3 H3 120.1 . . y C3 C4 C5 120.2(10) . . y C3 C4 H4 119.9 . . y C5 C4 H4 119.9 . . y C6 C5 C4 120.6(10) . . y C6 C5 H5 119.7 . . y C4 C5 H5 119.7 . . y C5 C6 C7 118.9(10) . . y C5 C6 H6 120.5 . . y C7 C6 H6 120.5 . . y C2 C7 C6 121.7(10) . . y C2 C7 H7 119.1 . . y C6 C7 H7 119.1 . . y C13 C8 C9 119.4(8) . . y C13 C8 P1 121.1(7) . . y C9 C8 P1 119.4(7) . . y C10 C9 C8 120.0(9) . . y C10 C9 H9 120.0 . . y C8 C9 H9 120.0 . . y C11 C10 C9 119.5(9) . . y C11 C10 H10 120.3 . . y C9 C10 H10 120.3 . . y C10 C11 C12 120.9(9) . . y C10 C11 H11 119.6 . . y C12 C11 H11 119.6 . . y C11 C12 C13 120.0(9) . . y C11 C12 H12 120.0 . . y C13 C12 H12 120.0 . . y C8 C13 C12 120.2(9) . . y C8 C13 H13 119.9 . . y C12 C13 H13 119.9 . . y C19 C14 N1 120.4(9) . . y C19 C14 P1 123.7(7) . . y N1 C14 P1 115.9(7) . . y C17 C16 N1 121.1(9) . . y C17 C16 H16 119.5 . . y N1 C16 H16 119.5 . . y C16 C17 C18 120.3(9) . . y C16 C17 H17 119.8 . . y C18 C17 H17 119.8 . . y C19 C18 C17 119.8(9) . . y C19 C18 H18 120.1 . . y C17 C18 H18 120.1 . . y C14 C19 C18 120.5(9) . . y C14 C19 H19 119.8 . . y C18 C19 H19 119.8 . . y C21 C20 C25 119.1(9) . . y C21 C20 P2 120.7(7) . . y C25 C20 P2 120.2(8) . . y C22 C21 C20 119.7(9) . . y C22 C21 H21 120.2 . . y C20 C21 H21 120.2 . . y C21 C22 C23 120.6(10) . . y C21 C22 H22 119.7 . . y C23 C22 H22 119.7 . . y C24 C23 C22 120.3(10) . . y C24 C23 H23 119.8 . . y C22 C23 H23 119.8 . . y C23 C24 C25 119.8(9) . . y C23 C24 H24 120.1 . . y C25 C24 H24 120.1 . . y C24 C25 C20 120.5(9) . . y C24 C25 H25 119.8 . . y C20 C25 H25 119.8 . . y C27 C26 C31 118.1(8) . . y C27 C26 P2 122.6(7) . . y C31 C26 P2 119.2(6) . . y C26 C27 C28 120.5(8) . . y C26 C27 H27 119.8 . . y C28 C27 H27 119.8 . . y C29 C28 C27 120.5(9) . . y C29 C28 H28 119.8 . . y C27 C28 H28 119.8 . . y C28 C29 C30 120.3(8) . . y C28 C29 H29 119.9 . . y C30 C29 H29 119.9 . . y C31 C30 C29 119.7(8) . . y C31 C30 H30 120.2 . . y C29 C30 H30 120.2 . . y C30 C31 C26 120.9(8) . . y C30 C31 H31 119.6 . . y C26 C31 H31 119.6 . . y C33 C32 C37 119.6(9) . . y C33 C32 P2 124.0(7) . . y C37 C32 P2 116.4(7) . . y C34 C33 C32 119.9(9) . . y C34 C33 H33 120.1 . . y C32 C33 H33 120.1 . . y C35 C34 C33 120.3(10) . . y C35 C34 H34 119.9 . . y C33 C34 H34 119.9 . . y C34 C35 C36 119.9(9) . . y C34 C35 H35 120.0 . . y C36 C35 H35 120.0 . . y C35 C36 C37 120.6(9) . . y C35 C36 H36 119.7 . . y C37 C36 H36 119.7 . . y C36 C37 C32 119.7(9) . . y C36 C37 H37 120.1 . . y C32 C37 H37 120.1 . . y C43 C38 C39 117.3(12) . . y C43 C38 P3 119.0(9) . . y C39 C38 P3 123.7(9) . . y C40 C39 C38 122.0(12) . . y C40 C39 H39 119.0 . . y C38 C39 H39 119.0 . . y C39 C40 C41 120.8(11) . . y C39 C40 H40 119.6 . . y C41 C40 H40 119.6 . . y C42 C41 C40 117.6(12) . . y C42 C41 H41 121.2 . . y C40 C41 H41 121.2 . . y C41 C42 C43 122.0(12) . . y C41 C42 H42 119.0 . . y C43 C42 H42 119.0 . . y C38 C43 C42 120.3(11) . . y C38 C43 H43 119.9 . . y C42 C43 H43 119.9 . . y C45 C44 C49 120.0(13) . . y C45 C44 P3 120.4(11) . . y C49 C44 P3 119.6(10) . . y C44 C45 C46 119.8(14) . . y C44 C45 H45 120.1 . . y C46 C45 H45 120.1 . . y C47 C46 C45 121.8(14) . . y C47 C46 H46 119.1 . . y C45 C46 H46 119.1 . . y C46 C47 C48 121.3(14) . . y C46 C47 H47 119.3 . . y C48 C47 H47 119.3 . . y C47 C48 C49 118.6(13) . . y C47 C48 H48 120.7 . . y C49 C48 H48 120.7 . . y C44 C49 C48 118.2(13) . . y C44 C49 H49 120.9 . . y C48 C49 H49 120.9 . . y C51 C50 C55 118.5(10) . . y C51 C50 P3 122.7(9) . . y C55 C50 P3 118.8(8) . . y C50 C51 C52 119.5(11) . . y C50 C51 H51 120.3 . . y C52 C51 H51 120.3 . . y C53 C52 C51 120.7(11) . . y C53 C52 H52 119.7 . . y C51 C52 H52 119.7 . . y C52 C53 C54 120.7(11) . . y C52 C53 H53 119.6 . . y C54 C53 H53 119.6 . . y C55 C54 C53 118.3(11) . . y C55 C54 H54 120.9 . . y C53 C54 H54 120.9 . . y C54 C55 C50 122.3(10) . . y C54 C55 H55 118.8 . . y C50 C55 H55 118.8 . . y Cl2A C56A Cl1A 101.8(17) . . y Cl2A C56A H56A 111.4 . . y Cl1A C56A H56A 111.4 . . y Cl2A C56A H56B 111.4 . . y Cl1A C56A H56B 111.4 . . y H56A C56A H56B 109.3 . . y Cl2B C56B Cl1B 91(2) . . y Cl2B C56B H56C 113.4 . . y Cl1B C56B H56C 113.4 . . y Cl2B C56B H56D 113.4 . . y Cl1B C56B H56D 113.4 . . y H56C C56B H56D 110.7 . . y C1 Au1 P3 178.0(2) . . y C56B Cl2B Cl1B 51.2(17) . . y C14 N1 C16 117.9(9) . . y C1 P1 C8 116.0(4) . . y C1 P1 C14 114.9(4) . . y C8 P1 C14 107.5(4) . . y C1 P1 C2 111.0(5) . . y C8 P1 C2 100.9(4) . . y C14 P1 C2 105.1(5) . . y C1 P2 C32 115.0(4) . . y C1 P2 C26 111.8(4) . . y C32 P2 C26 107.5(4) . . y C1 P2 C20 115.3(4) . . y C32 P2 C20 102.0(4) . . y C26 P2 C20 104.3(4) . . y C38 P3 C44 104.1(6) . . y C38 P3 C50 104.8(6) . . y C44 P3 C50 105.5(6) . . y C38 P3 Au1 115.8(4) . . y C44 P3 Au1 114.3(5) . . y C50 P3 Au1 111.5(4) . . y F3 Sb1 F6 179.5(3) . . y F3 Sb1 F4 89.6(2) . . y F6 Sb1 F4 90.0(3) . . y F3 Sb1 F2 89.8(2) . . y F6 Sb1 F2 89.7(3) . . y F4 Sb1 F2 89.2(3) . . y F3 Sb1 F5 90.6(2) . . y F6 Sb1 F5 89.8(3) . . y F4 Sb1 F5 179.6(3) . . y F2 Sb1 F5 90.4(2) . . y F3 Sb1 F1 91.0(2) . . y F6 Sb1 F1 89.4(3) . . y F4 Sb1 F1 90.7(3) . . y F2 Sb1 F1 179.1(2) . . y F5 Sb1 F1 89.7(3) . . y _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.44 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.368 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.173 data_5 _database_code_depnum_ccdc_archive 'CCDC 914765' _audit_creation_date 2012-12-07 _audit_block_code RKI-RF-202-02_7057 _chemical_name_systematic ; ? RKI-RF-202-02 ; _chemical_melting_point ? _chemical_compound_source dichloromethane,diethylether,hexane _chemical_formula_moiety 'C54 H44 Au Cl Cu N P3, F6 Sb, C4 H10 O, 1.26(C H2 Cl2)' _chemical_formula_sum 'C59.26 H56.52 Au Cl3.52 Cu F6 N O P3 Sb' _chemical_formula_weight 1512.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'c 2/c' _symmetry_space_group_name_Hall '-c 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.703(8) _cell_length_b 11.136(3) _cell_length_c 38.620(11) _cell_angle_alpha 90.00 _cell_angle_beta 114.233(4) _cell_angle_gamma 90.00 _cell_volume 12433(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9906 _cell_measurement_theta_min 2.3132 _cell_measurement_theta_max 28.4891 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 1.00 0.00 0.0600 -1.00 -1.00 0.00 0.0400 1.00 0.00 -0.50 0.0100 -1.00 0.00 0.50 0.0100 0.00 0.00 1.00 0.0050 0.00 0.00 -1.00 0.0050 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method ? _exptl_crystal_F_000 5959 _exptl_absorpt_coefficient_mu 3.410 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.73288 _exptl_absorpt_correction_T_max 0.96823 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_special_details ; Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75 ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_monochromator 'Incoatec Helios mirrors' _diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 66.67 _diffrn_reflns_number 94800 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 27.88 _reflns_number_total 14815 _reflns_number_gt 12024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT software (Bruker AXS, 2004)' _computing_data_reduction 'SAINT software (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The minimum and maximum estimated transmissions from the multi-scan scaling are 0.5084 and 1.0000 (SADABS). Several low angle reflections were shaded by the beamstop and were not used in the final refinement cycles. The Cu and Cl atoms in the cation are each disordered over two positions with refined occupancy of 0.8:0.2. Bond distances, angles and vectors indicate that in the major component (80%), Cu1A is bonded to N1 of the pyridyl group with a Cu1A-N1 bond distance of 2.267(6) \%A. As a result, the Cl atom, Cl1A, which bonded to Cu1A, is bent away from N1 in the plane of Au1, Cu1A, N1, such that the C1-Cu1A-Cl1A bond angle is 148.3(2) \%. Bond angles around the Cu atom of the minor component indicate that Cu1B undergoes interaction with an N atom of a minor pyridyl ring component near to the position of C20. Due to the partial occupancy of solute and the presence of Au, Cu and Cl in the structure, it was not possible to locate the exact position of this pyridyl group, but it is probably bonded to P2. In addition, the large anisotropic atomic displacement parameter of Cl1B indicate that the partial pyridyl group is itself disordered. The crystal contains both solute ether and dichloromethane. Both dichloromethane molecules are present with refined partial occupancy of 63%. Highest peak 1.88 at 0.2192 0.1002 0.1118 [ 0.91 A from AU1 ] Deepest hole -2.68 at 0.2190 0.1776 0.1112 [ 0.05 A from AU1 ] ; _iucr_refine_instructions_details ; TITL 7057sadabs in C2/c #15 CELL 0.71073 31.7033 11.1359 38.6203 90 114.233 90 ZERR 8 0.0084 0.0031 0.0106 0.0 0.0044 0.0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Au Cl Cu F N O P Sb UNIT 474.08 452.15 8 28.15 8 48 8 8 24 8 L.S. 10 SHEL 9.3 0.76 BOND FMAP 2 ACTA PLAN 20 SIZE 0.011 0.021 0.137 TEMP -173 WGHT 0.046900 1.934372 FVAR 0.02730 0.80230 0.62938 C1 1 0.175895 0.034124 0.109298 11.00000 0.01115 0.01771 = 0.01495 0.00257 0.00440 -0.00159 C2 1 0.131571 0.192498 0.142625 11.00000 0.01905 0.01535 = 0.01387 -0.00036 0.00277 -0.00282 C3 1 0.097646 0.272401 0.140793 11.00000 0.02713 0.03313 = 0.01525 0.00214 0.00052 0.00779 AFIX 43 H3 2 0.068519 0.273265 0.119593 11.00000 -1.20000 AFIX 0 C4 1 0.107188 0.352093 0.170909 11.00000 0.06415 0.02275 = 0.03456 -0.00318 0.02324 0.00931 AFIX 43 H4 2 0.084604 0.408796 0.170509 11.00000 -1.20000 AFIX 0 C5 1 0.149518 0.347732 0.201108 11.00000 0.07723 0.03518 = 0.02064 -0.01025 0.01870 -0.02487 AFIX 43 H5 2 0.156947 0.403338 0.221417 11.00000 -1.20000 AFIX 0 C6 1 0.181905 0.260220 0.201800 11.00000 0.03209 0.06015 = 0.01684 -0.00207 0.00583 -0.01440 AFIX 43 H6 2 0.210683 0.255096 0.223278 11.00000 -1.20000 AFIX 0 C7 1 0.086681 -0.031881 0.115405 11.00000 0.02101 0.01600 = 0.01862 -0.00355 0.00980 -0.00169 C8 1 0.039104 -0.017201 0.101235 11.00000 0.01833 0.03029 = 0.02017 -0.00067 0.00652 -0.00278 AFIX 43 H8 2 0.024655 0.048856 0.085172 11.00000 -1.20000 AFIX 0 C9 1 0.012652 -0.100070 0.110734 11.00000 0.01848 0.05455 = 0.02987 0.00215 0.00899 -0.00700 AFIX 43 H9 2 -0.019993 -0.091097 0.100846 11.00000 -1.20000 AFIX 0 C10 1 0.033931 -0.195993 0.134677 11.00000 0.03148 0.04435 = 0.03837 0.00117 0.01816 -0.01515 AFIX 43 H10 2 0.015694 -0.253309 0.140598 11.00000 -1.20000 AFIX 0 C11 1 0.081625 -0.208112 0.149895 11.00000 0.03276 0.02757 = 0.03263 0.00420 0.01600 -0.00368 AFIX 43 H11 2 0.096176 -0.272426 0.166736 11.00000 -1.20000 AFIX 0 C12 1 0.107945 -0.126072 0.140438 11.00000 0.01977 0.01927 = 0.02707 0.00185 0.01123 0.00131 AFIX 43 H12 2 0.140665 -0.133801 0.151020 11.00000 -1.20000 AFIX 0 C13 1 0.085802 0.149058 0.060647 11.00000 0.01437 0.01731 = 0.01862 0.00083 0.00589 0.00150 C14 1 0.059370 0.075999 0.030515 11.00000 0.01743 0.02054 = 0.02353 -0.00221 0.00520 -0.00361 AFIX 43 H14 2 0.056618 -0.007350 0.034408 11.00000 -1.20000 AFIX 0 C15 1 0.036937 0.125562 -0.005416 11.00000 0.02244 0.04005 = 0.01694 -0.00955 0.00320 -0.01246 AFIX 43 H15 2 0.018875 0.075694 -0.026183 11.00000 -1.20000 AFIX 0 C16 1 0.040674 0.247911 -0.011306 11.00000 0.02269 0.03414 = 0.02339 0.00615 0.00348 0.00073 AFIX 43 H16 2 0.024910 0.281147 -0.035956 11.00000 -1.20000 AFIX 0 C17 1 0.067310 0.321005 0.018698 11.00000 0.03030 0.02636 = 0.03016 0.00832 0.00992 0.00507 AFIX 43 H17 2 0.069741 0.404435 0.014717 11.00000 -1.20000 AFIX 0 C18 1 0.090385 0.272130 0.054516 11.00000 0.02333 0.01732 = 0.02546 0.00096 0.00674 0.00141 AFIX 43 H18 2 0.109363 0.321690 0.075019 11.00000 -1.20000 AFIX 0 C19 1 0.154430 -0.217773 0.083380 11.00000 0.02585 0.01703 = 0.02856 -0.00556 0.01651 -0.00606 C20 1 0.180285 -0.289683 0.115091 11.00000 0.03375 0.01759 = 0.03898 0.00305 0.02396 0.00292 AFIX 43 H20 2 0.211351 -0.268919 0.130892 11.00000 -1.20000 AFIX 0 C21 1 0.160416 -0.390650 0.123235 11.00000 0.03397 0.01958 = 0.04214 0.00845 0.02284 0.00588 AFIX 43 H21 2 0.177691 -0.439105 0.144633 11.00000 -1.20000 AFIX 0 C22 1 0.114986 -0.420330 0.099803 11.00000 0.04425 0.01794 = 0.04561 -0.00185 0.02963 -0.00545 AFIX 43 H22 2 0.101191 -0.488449 0.105770 11.00000 -1.20000 AFIX 0 C23 1 0.089686 -0.353532 0.068312 11.00000 0.03277 0.02520 = 0.03849 -0.00985 0.02083 -0.00873 AFIX 43 H23 2 0.058984 -0.376661 0.052271 11.00000 -1.20000 AFIX 0 C24 1 0.109327 -0.250479 0.059791 11.00000 0.03469 0.01791 = 0.03307 -0.00252 0.02222 -0.00043 AFIX 43 H24 2 0.091901 -0.203506 0.038062 11.00000 -1.20000 AFIX 0 C25 1 0.241111 -0.113598 0.090937 11.00000 0.03330 0.01849 = 0.03588 0.00764 0.02444 0.00230 C26 1 0.250566 -0.193575 0.067568 11.00000 0.04432 0.03020 = 0.04753 0.01148 0.03191 0.00889 AFIX 43 H26 2 0.225941 -0.227717 0.046295 11.00000 -1.20000 AFIX 0 C27 1 0.295661 -0.223593 0.075172 11.00000 0.05993 0.03787 = 0.06588 0.02939 0.04676 0.02389 AFIX 43 H27 2 0.301976 -0.278786 0.059149 11.00000 -1.20000 AFIX 0 C28 1 0.332131 -0.173608 0.106209 11.00000 0.03929 0.04698 = 0.08136 0.03876 0.03523 0.01755 AFIX 43 H28 2 0.363264 -0.193422 0.111284 11.00000 -1.20000 AFIX 0 C29 1 0.322351 -0.096386 0.128953 11.00000 0.04444 0.03840 = 0.06719 0.02640 0.01024 0.00701 AFIX 43 H29 2 0.347075 -0.061583 0.150005 11.00000 -1.20000 AFIX 0 C30 1 0.276609 -0.066271 0.122275 11.00000 0.03181 0.02545 = 0.03836 0.00799 0.01127 0.00524 AFIX 43 H30 2 0.270335 -0.014241 0.139081 11.00000 -1.20000 AFIX 0 C31 1 0.156844 -0.033787 0.029081 11.00000 0.01987 0.02389 = 0.02154 -0.00001 0.01130 -0.00479 C32 1 0.139935 -0.119115 -0.000366 11.00000 0.03257 0.02646 = 0.03267 -0.00375 0.02044 -0.00751 AFIX 43 H32 2 0.140297 -0.202160 0.005379 11.00000 -1.20000 AFIX 0 C33 1 0.122559 -0.080491 -0.038235 11.00000 0.02957 0.04828 = 0.02751 -0.01144 0.01409 -0.01095 AFIX 43 H33 2 0.110664 -0.137749 -0.058155 11.00000 -1.20000 AFIX 0 C34 1 0.122538 0.039648 -0.046895 11.00000 0.01936 0.05017 = 0.02478 0.00215 0.01164 -0.00095 AFIX 43 H34 2 0.110461 0.064945 -0.072647 11.00000 -1.20000 AFIX 0 C35 1 0.140342 0.124115 -0.017664 11.00000 0.02111 0.03670 = 0.02313 0.00570 0.00983 0.00019 AFIX 43 H35 2 0.140718 0.206766 -0.023624 11.00000 -1.20000 AFIX 0 C36 1 0.157335 0.088166 0.019718 11.00000 0.02225 0.02349 = 0.02962 -0.00139 0.01464 -0.00368 AFIX 43 H36 2 0.169503 0.146236 0.039366 11.00000 -1.20000 AFIX 0 C37 1 0.240696 0.417737 0.067508 11.00000 0.02704 0.01843 = 0.02580 0.00092 0.01391 -0.00209 C38 1 0.194801 0.452926 0.054615 11.00000 0.02020 0.03127 = 0.02266 0.00209 0.00617 0.00060 AFIX 43 H38 2 0.178091 0.435312 0.069547 11.00000 -1.20000 AFIX 0 C39 1 0.172606 0.513503 0.020280 11.00000 0.01861 0.03076 = 0.02858 0.00466 0.00346 0.00181 AFIX 43 H39 2 0.141067 0.536329 0.011752 11.00000 -1.20000 AFIX 0 C40 1 0.197079 0.539714 -0.001062 11.00000 0.03315 0.03720 = 0.02260 0.00664 0.00743 0.00346 AFIX 43 H40 2 0.182461 0.581146 -0.024497 11.00000 -1.20000 AFIX 0 C41 1 0.242706 0.506000 0.011491 11.00000 0.03262 0.06461 = 0.02850 0.01910 0.01668 0.00954 AFIX 43 H41 2 0.259320 0.524403 -0.003460 11.00000 -1.20000 AFIX 0 C42 1 0.264769 0.445748 0.045526 11.00000 0.02338 0.05037 = 0.03164 0.01238 0.01553 0.00442 AFIX 43 H42 2 0.296347 0.423522 0.053875 11.00000 -1.20000 AFIX 0 C43 1 0.322353 0.280633 0.115913 11.00000 0.02083 0.01664 = 0.02443 0.00268 0.00988 0.00087 C44 1 0.362510 0.319300 0.144277 11.00000 0.02461 0.04968 = 0.03238 -0.01666 0.00682 0.00083 AFIX 43 H44 2 0.361952 0.378404 0.161823 11.00000 -1.20000 AFIX 0 C45 1 0.404668 0.270537 0.147177 11.00000 0.02002 0.07206 = 0.04967 -0.02446 0.00396 0.00068 AFIX 43 H45 2 0.432877 0.296353 0.166868 11.00000 -1.20000 AFIX 0 C46 1 0.405178 0.184917 0.121388 11.00000 0.02258 0.04637 = 0.04891 -0.00627 0.01530 0.00951 AFIX 43 H46 2 0.433762 0.152567 0.123258 11.00000 -1.20000 AFIX 0 C47 1 0.364602 0.146792 0.093213 11.00000 0.03087 0.02746 = 0.04265 -0.00665 0.01944 -0.00153 AFIX 43 H47 2 0.365055 0.087471 0.075691 11.00000 -1.20000 AFIX 0 C48 1 0.323238 0.193937 0.090169 11.00000 0.03075 0.02271 = 0.03613 -0.00351 0.01791 -0.00197 AFIX 43 H48 2 0.295143 0.167459 0.070480 11.00000 -1.20000 AFIX 0 C49 1 0.277794 0.444311 0.148906 11.00000 0.02052 0.02118 = 0.01992 0.00106 0.00766 0.00102 C50 1 0.268878 0.415357 0.180083 11.00000 0.04462 0.03209 = 0.03093 0.00102 0.01847 -0.00761 AFIX 43 H50 2 0.256355 0.339046 0.181612 11.00000 -1.20000 AFIX 0 C51 1 0.278436 0.499390 0.209478 11.00000 0.06299 0.05527 = 0.03091 -0.00325 0.02767 0.00028 AFIX 43 H51 2 0.272796 0.479436 0.231118 11.00000 -1.20000 AFIX 0 C52 1 0.295679 0.608811 0.207024 11.00000 0.07179 0.04245 = 0.03436 -0.01330 0.01844 0.00629 AFIX 43 H52 2 0.301096 0.666111 0.226616 11.00000 -1.20000 AFIX 0 C53 1 0.305416 0.637804 0.176505 11.00000 0.07672 0.02209 = 0.03030 0.00068 0.00818 0.00304 AFIX 43 H53 2 0.318740 0.713484 0.175571 11.00000 -1.20000 AFIX 0 C54 1 0.295813 0.556867 0.147249 11.00000 0.05858 0.01993 = 0.02497 -0.00081 0.01812 -0.00035 AFIX 43 H54 2 0.301562 0.578202 0.125761 11.00000 -1.20000 AFIX 0 C55 1 0.407287 0.449894 0.260596 31.00000 0.06759 0.05169 = 0.05005 0.00492 0.01370 -0.00166 AFIX 23 H55A 2 0.404362 0.375806 0.273609 31.00000 -1.20000 H55B 2 0.378370 0.458678 0.237357 31.00000 -1.20000 AFIX 0 C56 1 0.468097 0.698672 0.180699 31.00000 0.05966 0.06885 = 0.09287 0.02813 0.03970 0.02136 AFIX 23 H56A 2 0.477937 0.753605 0.165254 31.00000 -1.20000 H56B 2 0.496084 0.659859 0.199769 31.00000 -1.20000 AFIX 0 C60 1 0.318448 0.195911 0.260238 11.00000 0.02431 0.05760 = 0.04987 0.01151 0.00160 -0.00068 AFIX 137 H60A 2 0.323670 0.150108 0.283309 11.00000 -1.50000 H60B 2 0.285535 0.193251 0.243121 11.00000 -1.50000 H60C 2 0.327919 0.279501 0.266993 11.00000 -1.50000 AFIX 0 C59 1 0.348437 0.138092 0.239316 11.00000 0.05526 0.07130 = 0.07401 0.00439 0.00466 -0.00931 AFIX 23 H59A 2 0.336075 0.058358 0.228599 11.00000 -1.20000 H59B 2 0.348010 0.190888 0.218550 11.00000 -1.20000 AFIX 0 C57 1 0.425418 0.073597 0.255489 11.00000 0.08833 0.14275 = 0.09338 -0.01185 0.05549 0.01596 AFIX 23 H57A 2 0.425316 0.118175 0.233276 11.00000 -1.20000 H57B 2 0.415890 -0.010303 0.247697 11.00000 -1.20000 AFIX 0 C58 1 0.473272 0.076390 0.287672 11.00000 0.09477 0.21521 = 0.07541 0.01487 0.04188 0.04916 AFIX 137 H58A 2 0.483252 0.159928 0.293843 11.00000 -1.50000 H58B 2 0.495076 0.034044 0.279904 11.00000 -1.50000 H58C 2 0.472415 0.037005 0.310066 11.00000 -1.50000 AFIX 0 Au1 3 0.218648 0.182008 0.111599 11.00000 0.01745 0.01582 = 0.02165 0.00192 0.00687 -0.00253 Cl1A 4 0.254533 -0.089055 0.212847 21.00000 0.03601 0.03421 = 0.01936 0.00472 0.00410 0.01001 Cl1B 4 0.267603 -0.046041 0.215393 -21.00000 0.06078 0.12489 = 0.03172 0.02805 0.01894 0.05272 Cl2 4 0.411496 0.572322 0.290465 31.00000 0.07164 0.05565 = 0.05569 -0.00483 0.03297 0.00748 Cl3 4 0.448892 0.431966 0.248081 31.00000 0.13480 0.11746 = 0.12491 -0.04811 0.09204 -0.01933 Cl4 4 0.439706 0.782743 0.204369 31.00000 0.08956 0.10602 = 0.08619 -0.04035 0.00476 0.01921 Cl5 4 0.431950 0.591113 0.151943 31.00000 0.08402 0.05977 = 0.05048 -0.00642 0.01797 0.00884 Cu1A 5 0.210143 0.018195 0.165017 21.00000 0.02203 0.02647 = 0.02175 0.00717 0.00266 0.00108 Cu1B 5 0.222331 -0.027300 0.157452 -21.00000 0.03308 0.02385 = 0.02036 0.00226 0.00280 0.00297 F1 6 0.516468 0.741854 0.417612 11.00000 0.03069 0.03027 = 0.07969 -0.01065 0.01231 -0.00829 F2 6 0.480834 0.947187 0.425724 11.00000 0.03629 0.04870 = 0.12587 0.00022 0.03811 0.00502 F3 6 0.516803 0.927955 0.375473 11.00000 0.15256 0.09050 = 0.02395 0.00681 0.01427 -0.02532 F4 6 0.558800 1.060591 0.436464 11.00000 0.06437 0.02344 = 0.06383 -0.01123 0.04418 -0.01345 F5 6 0.595367 0.855621 0.428975 11.00000 0.04559 0.04530 = 0.13394 -0.02069 0.05625 -0.00685 F6 6 0.560518 0.874421 0.479347 11.00000 0.08859 0.07250 = 0.02879 0.00981 0.01202 -0.01903 N1 7 0.172885 0.183262 0.172502 11.00000 0.02551 0.04234 = 0.01880 0.00341 0.00611 -0.00651 O1 8 0.395164 0.127283 0.268804 11.00000 0.05837 0.10294 = 0.06925 -0.00194 0.02050 0.00302 P1 9 0.122066 0.080386 0.105610 11.00000 0.01716 0.01210 = 0.01835 -0.00041 0.00566 -0.00124 P2 9 0.180364 -0.076844 0.078882 11.00000 0.02264 0.01394 = 0.02522 -0.00010 0.01315 -0.00215 P3 9 0.265925 0.335148 0.111617 11.00000 0.01786 0.01502 = 0.02094 0.00024 0.00854 -0.00157 Sb1 10 0.537564 0.901622 0.426950 11.00000 0.02332 0.02245 = 0.02669 -0.00136 0.00812 -0.00295 HKLF 4 REM 7057sadabs in C2/c #15 REM R1 = 0.0516 for 12024 Fo > 4sig(Fo) and 0.0712 for all 14815 data REM 734 parameters refined using 0 restraints END REM Highest difference peak 1.884, deepest hole -2.679, 1-sigma level 0.166 Q1 1 0.2192 0.1002 0.1118 11.00000 0.05 1.88 Q2 1 0.5186 0.5417 0.2031 11.00000 0.05 1.81 Q3 1 0.2198 0.2638 0.1110 11.00000 0.05 1.73 Q4 1 0.2310 0.1805 0.1331 11.00000 0.05 1.72 Q5 1 0.4312 0.5298 0.2796 11.00000 0.05 1.39 Q6 1 0.3505 0.1790 0.2025 11.00000 0.05 1.38 Q7 1 0.2518 0.1263 0.1267 11.00000 0.05 1.37 Q8 1 0.2009 0.1652 0.0873 11.00000 0.05 1.33 Q9 1 0.4988 0.6356 0.1760 11.00000 0.05 1.31 Q10 1 0.2395 0.1423 0.1114 11.00000 0.05 1.30 Q11 1 0.1893 0.1312 0.0990 11.00000 0.05 1.26 Q12 1 0.1894 0.2391 0.0848 11.00000 0.05 1.17 Q13 1 0.2494 0.2470 0.1366 11.00000 0.05 1.15 Q14 1 0.5261 0.9065 0.4041 11.00000 0.05 1.14 Q15 1 0.2339 0.2417 0.1438 11.00000 0.05 1.11 Q16 1 0.4777 0.9712 0.3831 11.00000 0.05 1.01 Q17 1 0.5397 0.9835 0.4257 11.00000 0.05 0.98 Q18 1 0.3892 0.1277 0.2036 11.00000 0.05 0.91 Q19 1 0.5388 0.8009 0.4275 11.00000 0.05 0.91 Q20 1 0.1669 0.1837 0.0781 11.00000 0.05 0.81 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+1.9344P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14815 _refine_ls_number_parameters 734 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.319 _refine_ls_restrained_S_all 1.319 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.17590(17) 0.0341(4) 0.10930(13) 0.0149(10) Uani 1 1 d . . . C2 C 0.13157(19) 0.1925(4) 0.14262(14) 0.0174(10) Uani 1 1 d . . . C3 C 0.0976(2) 0.2724(5) 0.14079(15) 0.0279(12) Uani 1 1 d . . . H3 H 0.0685 0.2733 0.1196 0.033 Uiso 1 1 calc R . . C4 C 0.1072(3) 0.3521(5) 0.17091(18) 0.0395(17) Uani 1 1 d . . . H4 H 0.0846 0.4088 0.1705 0.047 Uiso 1 1 calc R . . C5 C 0.1495(3) 0.3477(5) 0.20111(17) 0.0448(19) Uani 1 1 d . . . H5 H 0.1569 0.4033 0.2214 0.054 Uiso 1 1 calc R . . C6 C 0.1819(2) 0.2602(6) 0.20180(16) 0.0377(15) Uani 1 1 d . . . H6 H 0.2107 0.2551 0.2233 0.045 Uiso 1 1 calc R . . C7 C 0.08668(19) -0.0319(4) 0.11541(14) 0.0180(10) Uani 1 1 d . . . C8 C 0.0391(2) -0.0172(4) 0.10123(15) 0.0234(11) Uani 1 1 d . . . H8 H 0.0247 0.0489 0.0852 0.028 Uiso 1 1 calc R . . C9 C 0.0127(2) -0.1001(5) 0.11073(17) 0.0346(14) Uani 1 1 d . . . H9 H -0.0200 -0.0911 0.1008 0.042 Uiso 1 1 calc R . . C10 C 0.0339(2) -0.1960(5) 0.13468(18) 0.0368(15) Uani 1 1 d . . . H10 H 0.0157 -0.2533 0.1406 0.044 Uiso 1 1 calc R . . C11 C 0.0816(2) -0.2081(5) 0.14989(17) 0.0301(13) Uani 1 1 d . . . H11 H 0.0962 -0.2724 0.1667 0.036 Uiso 1 1 calc R . . C12 C 0.1079(2) -0.1261(4) 0.14044(15) 0.0215(11) Uani 1 1 d . . . H12 H 0.1407 -0.1338 0.1510 0.026 Uiso 1 1 calc R . . C13 C 0.08580(18) 0.1491(4) 0.06065(14) 0.0171(10) Uani 1 1 d . . . C14 C 0.05937(19) 0.0760(4) 0.03051(15) 0.0216(11) Uani 1 1 d . . . H14 H 0.0566 -0.0074 0.0344 0.026 Uiso 1 1 calc R . . C15 C 0.0369(2) 0.1256(5) -0.00542(15) 0.0281(12) Uani 1 1 d . . . H15 H 0.0189 0.0757 -0.0262 0.034 Uiso 1 1 calc R . . C16 C 0.0407(2) 0.2479(5) -0.01131(16) 0.0287(12) Uani 1 1 d . . . H16 H 0.0249 0.2811 -0.0360 0.034 Uiso 1 1 calc R . . C17 C 0.0673(2) 0.3210(5) 0.01870(17) 0.0298(13) Uani 1 1 d . . . H17 H 0.0697 0.4044 0.0147 0.036 Uiso 1 1 calc R . . C18 C 0.0904(2) 0.2721(4) 0.05452(15) 0.0231(11) Uani 1 1 d . . . H18 H 0.1094 0.3217 0.0750 0.028 Uiso 1 1 calc R . . C19 C 0.1544(2) -0.2178(4) 0.08338(15) 0.0221(12) Uani 1 1 d . . . C20 C 0.1803(2) -0.2897(4) 0.11509(17) 0.0271(13) Uani 1 1 d . . . H20 H 0.2114 -0.2689 0.1309 0.033 Uiso 1 1 calc R . . C21 C 0.1604(2) -0.3906(4) 0.12324(17) 0.0295(13) Uani 1 1 d . . . H21 H 0.1777 -0.4391 0.1446 0.035 Uiso 1 1 calc R . . C22 C 0.1150(2) -0.4203(4) 0.09980(17) 0.0323(14) Uani 1 1 d . . . H22 H 0.1012 -0.4884 0.1058 0.039 Uiso 1 1 calc R . . C23 C 0.0897(2) -0.3535(5) 0.06831(17) 0.0301(13) Uani 1 1 d . . . H23 H 0.0590 -0.3767 0.0523 0.036 Uiso 1 1 calc R . . C24 C 0.1093(2) -0.2505(4) 0.05979(16) 0.0258(12) Uani 1 1 d . . . H24 H 0.0919 -0.2035 0.0381 0.031 Uiso 1 1 calc R . . C25 C 0.2411(2) -0.1136(4) 0.09094(16) 0.0259(13) Uani 1 1 d . . . C26 C 0.2506(3) -0.1936(5) 0.06757(19) 0.0364(15) Uani 1 1 d . . . H26 H 0.2259 -0.2277 0.0463 0.044 Uiso 1 1 calc R . . C27 C 0.2957(3) -0.2236(6) 0.0752(2) 0.048(2) Uani 1 1 d . . . H27 H 0.3020 -0.2788 0.0591 0.057 Uiso 1 1 calc R . . C28 C 0.3321(3) -0.1736(6) 0.1062(3) 0.052(2) Uani 1 1 d . . . H28 H 0.3633 -0.1934 0.1113 0.063 Uiso 1 1 calc R . . C29 C 0.3224(3) -0.0964(6) 0.1290(2) 0.054(2) Uani 1 1 d . . . H29 H 0.3471 -0.0616 0.1500 0.065 Uiso 1 1 calc R . . C30 C 0.2766(2) -0.0663(5) 0.12228(18) 0.0329(14) Uani 1 1 d . . . H30 H 0.2703 -0.0142 0.1391 0.039 Uiso 1 1 calc R . . C31 C 0.15684(19) -0.0338(4) 0.02908(14) 0.0208(11) Uani 1 1 d . . . C32 C 0.1399(2) -0.1191(5) -0.00037(16) 0.0282(13) Uani 1 1 d . . . H32 H 0.1403 -0.2022 0.0054 0.034 Uiso 1 1 calc R . . C33 C 0.1226(2) -0.0805(5) -0.03823(17) 0.0343(14) Uani 1 1 d . . . H33 H 0.1107 -0.1377 -0.0582 0.041 Uiso 1 1 calc R . . C34 C 0.1225(2) 0.0396(5) -0.04690(16) 0.0306(13) Uani 1 1 d . . . H34 H 0.1105 0.0649 -0.0726 0.037 Uiso 1 1 calc R . . C35 C 0.1403(2) 0.1241(5) -0.01766(15) 0.0267(12) Uani 1 1 d . . . H35 H 0.1407 0.2068 -0.0236 0.032 Uiso 1 1 calc R . . C36 C 0.15734(19) 0.0882(4) 0.01972(16) 0.0238(12) Uani 1 1 d . . . H36 H 0.1695 0.1462 0.0394 0.029 Uiso 1 1 calc R . . C37 C 0.2407(2) 0.4177(4) 0.06751(15) 0.0227(12) Uani 1 1 d . . . C38 C 0.1948(2) 0.4529(5) 0.05461(15) 0.0256(12) Uani 1 1 d . . . H38 H 0.1781 0.4353 0.0695 0.031 Uiso 1 1 calc R . . C39 C 0.1726(2) 0.5135(5) 0.02028(16) 0.0280(12) Uani 1 1 d . . . H39 H 0.1411 0.5363 0.0118 0.034 Uiso 1 1 calc R . . C40 C 0.1971(2) 0.5397(5) -0.00106(16) 0.0323(13) Uani 1 1 d . . . H40 H 0.1825 0.5811 -0.0245 0.039 Uiso 1 1 calc R . . C41 C 0.2427(2) 0.5060(6) 0.01149(17) 0.0405(16) Uani 1 1 d . . . H41 H 0.2593 0.5244 -0.0035 0.049 Uiso 1 1 calc R . . C42 C 0.2648(2) 0.4457(5) 0.04553(17) 0.0337(14) Uani 1 1 d . . . H42 H 0.2963 0.4235 0.0539 0.040 Uiso 1 1 calc R . . C43 C 0.32235(19) 0.2806(4) 0.11591(15) 0.0204(11) Uani 1 1 d . . . C44 C 0.3625(2) 0.3193(5) 0.14428(18) 0.0372(15) Uani 1 1 d . . . H44 H 0.3620 0.3784 0.1618 0.045 Uiso 1 1 calc R . . C45 C 0.4047(2) 0.2705(7) 0.1472(2) 0.0506(19) Uani 1 1 d . . . H45 H 0.4329 0.2964 0.1669 0.061 Uiso 1 1 calc R . . C46 C 0.4052(2) 0.1849(5) 0.1214(2) 0.0391(15) Uani 1 1 d . . . H46 H 0.4338 0.1526 0.1233 0.047 Uiso 1 1 calc R . . C47 C 0.3646(2) 0.1468(5) 0.09321(18) 0.0322(14) Uani 1 1 d . . . H47 H 0.3651 0.0875 0.0757 0.039 Uiso 1 1 calc R . . C48 C 0.3232(2) 0.1939(4) 0.09017(17) 0.0285(13) Uani 1 1 d . . . H48 H 0.2951 0.1675 0.0705 0.034 Uiso 1 1 calc R . . C49 C 0.27779(19) 0.4443(4) 0.14891(14) 0.0207(11) Uani 1 1 d . . . C50 C 0.2689(2) 0.4154(5) 0.18008(17) 0.0349(15) Uani 1 1 d . . . H50 H 0.2564 0.3390 0.1816 0.042 Uiso 1 1 calc R . . C51 C 0.2784(3) 0.4994(6) 0.20948(19) 0.0470(18) Uani 1 1 d . . . H51 H 0.2728 0.4794 0.2311 0.056 Uiso 1 1 calc R . . C52 C 0.2957(3) 0.6088(6) 0.20702(19) 0.0506(19) Uani 1 1 d . . . H52 H 0.3011 0.6661 0.2266 0.061 Uiso 1 1 calc R . . C53 C 0.3054(3) 0.6378(5) 0.17651(18) 0.0476(19) Uani 1 1 d . . . H53 H 0.3187 0.7135 0.1756 0.057 Uiso 1 1 calc R . . C54 C 0.2958(2) 0.5569(4) 0.14725(16) 0.0342(15) Uani 1 1 d . . . H54 H 0.3016 0.5782 0.1258 0.041 Uiso 1 1 calc R . . C55 C 0.4073(5) 0.4499(11) 0.2606(4) 0.060(3) Uani 0.629(4) 1 d P . . H55A H 0.4044 0.3758 0.2736 0.072 Uiso 0.629(4) 1 calc PR . . H55B H 0.3784 0.4587 0.2374 0.072 Uiso 0.629(4) 1 calc PR . . C56 C 0.4681(5) 0.6987(12) 0.1807(5) 0.071(4) Uani 0.629(4) 1 d P . . H56A H 0.4779 0.7536 0.1653 0.085 Uiso 0.629(4) 1 calc PR . . H56B H 0.4961 0.6599 0.1998 0.085 Uiso 0.629(4) 1 calc PR . . C60 C 0.3184(3) 0.1959(6) 0.2602(2) 0.0484(18) Uani 1 1 d . . . H60A H 0.3237 0.1501 0.2833 0.073 Uiso 1 1 calc R . . H60B H 0.2855 0.1933 0.2431 0.073 Uiso 1 1 calc R . . H60C H 0.3279 0.2795 0.2670 0.073 Uiso 1 1 calc R . . C59 C 0.3484(3) 0.1381(8) 0.2393(3) 0.074(3) Uani 1 1 d . . . H59A H 0.3361 0.0584 0.2286 0.089 Uiso 1 1 calc R . . H59B H 0.3480 0.1909 0.2186 0.089 Uiso 1 1 calc R . . C57 C 0.4254(4) 0.0736(11) 0.2555(3) 0.102(4) Uani 1 1 d . . . H57A H 0.4253 0.1182 0.2333 0.123 Uiso 1 1 calc R . . H57B H 0.4159 -0.0103 0.2477 0.123 Uiso 1 1 calc R . . C58 C 0.4733(5) 0.0764(13) 0.2877(3) 0.126(5) Uani 1 1 d . . . H58A H 0.4833 0.1599 0.2938 0.189 Uiso 1 1 calc R . . H58B H 0.4951 0.0340 0.2799 0.189 Uiso 1 1 calc R . . H58C H 0.4724 0.0370 0.3101 0.189 Uiso 1 1 calc R . . Au1 Au 0.218648(7) 0.182008(15) 0.111599(5) 0.01869(7) Uani 1 1 d . . . Cl1A Cl 0.25453(15) -0.0891(3) 0.21285(12) 0.0322(7) Uani 0.802(7) 1 d P . . Cl1B Cl 0.2676(8) -0.046(2) 0.2154(6) 0.072(6) Uani 0.198(7) 1 d P . . Cl2 Cl 0.41150(12) 0.5723(3) 0.29047(9) 0.0587(10) Uani 0.629(4) 1 d P . . Cl3 Cl 0.4489(2) 0.4320(4) 0.24808(15) 0.1130(19) Uani 0.629(4) 1 d P . . Cl4 Cl 0.43971(17) 0.7827(4) 0.20437(13) 0.1042(18) Uani 0.629(4) 1 d P . . Cl5 Cl 0.43195(14) 0.5911(3) 0.15194(9) 0.0679(11) Uani 0.629(4) 1 d P . . Cu1A Cu 0.21014(5) 0.01819(18) 0.16502(4) 0.0255(5) Uani 0.802(7) 1 d P . . Cu1B Cu 0.2223(2) -0.0273(7) 0.15745(14) 0.0285(19) Uani 0.198(7) 1 d P . . F1 F 0.51647(13) 0.7419(3) 0.41761(12) 0.0503(10) Uani 1 1 d . . . F2 F 0.48083(15) 0.9472(4) 0.42572(16) 0.0687(14) Uani 1 1 d . . . F3 F 0.5168(2) 0.9280(5) 0.37547(12) 0.096(2) Uani 1 1 d . . . F4 F 0.55880(14) 1.0606(3) 0.43646(11) 0.0447(10) Uani 1 1 d . . . F5 F 0.59537(15) 0.8556(4) 0.42897(16) 0.0686(14) Uani 1 1 d . . . F6 F 0.56052(18) 0.8744(4) 0.47935(11) 0.0673(13) Uani 1 1 d . . . N1 N 0.17289(18) 0.1833(4) 0.17250(13) 0.0299(11) Uani 1 1 d . . . O1 O 0.3952(2) 0.1273(6) 0.26880(18) 0.0787(18) Uani 1 1 d . . . P1 P 0.12207(5) 0.08039(10) 0.10561(4) 0.0164(3) Uani 1 1 d . . . P2 P 0.18036(5) -0.07684(10) 0.07888(4) 0.0195(3) Uani 1 1 d . . . P3 P 0.26593(5) 0.33515(10) 0.11162(4) 0.0177(3) Uani 1 1 d . . . Sb1 Sb 0.537564(14) 0.90162(3) 0.426950(10) 0.02486(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.011(3) 0.018(2) 0.015(2) 0.0026(17) 0.004(2) -0.0016(18) C2 0.019(3) 0.015(2) 0.014(2) -0.0004(17) 0.003(2) -0.0028(18) C3 0.027(4) 0.033(3) 0.015(2) 0.002(2) 0.001(3) 0.008(2) C4 0.064(5) 0.023(3) 0.035(3) -0.003(2) 0.023(4) 0.009(3) C5 0.077(6) 0.035(3) 0.021(3) -0.010(2) 0.019(4) -0.025(3) C6 0.032(4) 0.060(4) 0.017(3) -0.002(3) 0.006(3) -0.014(3) C7 0.021(3) 0.016(2) 0.019(2) -0.0036(17) 0.010(2) -0.0017(19) C8 0.018(3) 0.030(3) 0.020(3) -0.001(2) 0.007(3) -0.003(2) C9 0.018(4) 0.055(4) 0.030(3) 0.002(3) 0.009(3) -0.007(3) C10 0.031(4) 0.044(3) 0.038(4) 0.001(3) 0.018(3) -0.015(3) C11 0.033(4) 0.028(3) 0.033(3) 0.004(2) 0.016(3) -0.004(2) C12 0.020(3) 0.019(2) 0.027(3) 0.0018(19) 0.011(3) 0.001(2) C13 0.014(3) 0.017(2) 0.019(2) 0.0008(17) 0.006(2) 0.0015(18) C14 0.017(3) 0.021(2) 0.024(3) -0.0022(19) 0.005(3) -0.004(2) C15 0.022(4) 0.040(3) 0.017(3) -0.010(2) 0.003(3) -0.012(2) C16 0.023(4) 0.034(3) 0.023(3) 0.006(2) 0.003(3) 0.001(2) C17 0.030(4) 0.026(3) 0.030(3) 0.008(2) 0.010(3) 0.005(2) C18 0.023(3) 0.017(2) 0.025(3) 0.0010(19) 0.007(3) 0.001(2) C19 0.026(3) 0.017(2) 0.029(3) -0.0056(19) 0.017(3) -0.006(2) C20 0.034(4) 0.018(2) 0.039(3) 0.003(2) 0.024(3) 0.003(2) C21 0.034(4) 0.020(2) 0.042(3) 0.008(2) 0.023(3) 0.006(2) C22 0.044(4) 0.018(2) 0.046(4) -0.002(2) 0.030(4) -0.005(2) C23 0.033(4) 0.025(2) 0.038(3) -0.010(2) 0.021(3) -0.009(2) C24 0.035(4) 0.018(2) 0.033(3) -0.003(2) 0.022(3) 0.000(2) C25 0.033(4) 0.018(2) 0.036(3) 0.008(2) 0.024(3) 0.002(2) C26 0.044(5) 0.030(3) 0.048(4) 0.011(2) 0.032(4) 0.009(3) C27 0.060(6) 0.038(3) 0.066(5) 0.029(3) 0.047(5) 0.024(3) C28 0.039(5) 0.047(4) 0.081(6) 0.039(4) 0.035(5) 0.018(3) C29 0.044(5) 0.038(3) 0.067(5) 0.026(3) 0.010(4) 0.007(3) C30 0.032(4) 0.025(3) 0.038(3) 0.008(2) 0.011(3) 0.005(2) C31 0.020(3) 0.024(2) 0.022(3) 0.0000(19) 0.011(3) -0.005(2) C32 0.033(4) 0.026(3) 0.033(3) -0.004(2) 0.020(3) -0.008(2) C33 0.030(4) 0.048(3) 0.028(3) -0.011(3) 0.014(3) -0.011(3) C34 0.019(4) 0.050(3) 0.025(3) 0.002(2) 0.012(3) -0.001(3) C35 0.021(3) 0.037(3) 0.023(3) 0.006(2) 0.010(3) 0.000(2) C36 0.022(3) 0.023(2) 0.030(3) -0.001(2) 0.015(3) -0.004(2) C37 0.027(4) 0.018(2) 0.026(3) 0.0009(19) 0.014(3) -0.002(2) C38 0.020(3) 0.031(3) 0.023(3) 0.002(2) 0.006(3) 0.001(2) C39 0.019(3) 0.031(3) 0.029(3) 0.005(2) 0.003(3) 0.002(2) C40 0.033(4) 0.037(3) 0.023(3) 0.007(2) 0.007(3) 0.003(3) C41 0.033(4) 0.065(4) 0.029(3) 0.019(3) 0.017(3) 0.010(3) C42 0.023(4) 0.050(3) 0.032(3) 0.012(3) 0.016(3) 0.004(3) C43 0.021(3) 0.017(2) 0.024(3) 0.0027(18) 0.010(3) 0.001(2) C44 0.025(4) 0.050(4) 0.032(3) -0.017(3) 0.007(3) 0.001(3) C45 0.020(4) 0.072(5) 0.050(4) -0.024(4) 0.004(4) 0.001(3) C46 0.023(4) 0.046(3) 0.049(4) -0.006(3) 0.015(4) 0.010(3) C47 0.031(4) 0.027(3) 0.043(4) -0.007(2) 0.019(3) -0.002(2) C48 0.031(4) 0.023(2) 0.036(3) -0.004(2) 0.018(3) -0.002(2) C49 0.021(3) 0.021(2) 0.020(3) 0.0011(19) 0.008(3) 0.001(2) C50 0.045(4) 0.032(3) 0.031(3) 0.001(2) 0.018(3) -0.008(3) C51 0.063(6) 0.055(4) 0.031(3) -0.003(3) 0.028(4) 0.000(3) C52 0.072(6) 0.042(4) 0.034(4) -0.013(3) 0.018(4) 0.006(3) C53 0.077(6) 0.022(3) 0.030(3) 0.001(2) 0.008(4) 0.003(3) C54 0.059(5) 0.020(2) 0.025(3) -0.001(2) 0.018(3) 0.000(3) C55 0.068(10) 0.052(7) 0.050(7) 0.005(5) 0.014(7) -0.002(6) C56 0.060(10) 0.069(8) 0.093(11) 0.028(7) 0.040(10) 0.021(7) C60 0.024(4) 0.058(4) 0.050(4) 0.012(3) 0.002(4) -0.001(3) C59 0.055(7) 0.071(5) 0.074(6) 0.004(5) 0.005(6) -0.009(5) C57 0.088(10) 0.143(10) 0.093(9) -0.012(7) 0.055(8) 0.016(7) C58 0.095(11) 0.215(15) 0.075(8) 0.015(8) 0.042(9) 0.049(10) Au1 0.01745(13) 0.01582(9) 0.02165(11) 0.00192(7) 0.00687(9) -0.00253(7) Cl1A 0.036(2) 0.0342(12) 0.0194(10) 0.0047(9) 0.0041(12) 0.0100(10) Cl1B 0.061(14) 0.125(17) 0.032(7) 0.028(11) 0.019(9) 0.053(11) Cl2 0.072(3) 0.0557(17) 0.0557(19) -0.0048(13) 0.0330(19) 0.0075(15) Cl3 0.135(5) 0.117(4) 0.125(4) -0.048(3) 0.092(4) -0.019(3) Cl4 0.090(4) 0.106(3) 0.086(3) -0.040(2) 0.005(3) 0.019(3) Cl5 0.084(3) 0.0598(18) 0.0505(19) -0.0064(14) 0.018(2) 0.0088(17) Cu1A 0.0220(6) 0.0265(8) 0.0218(5) 0.0072(5) 0.0027(5) 0.0011(5) Cu1B 0.033(3) 0.024(3) 0.020(2) 0.0023(17) 0.003(2) 0.003(2) F1 0.031(2) 0.0303(18) 0.080(3) -0.0107(18) 0.012(2) -0.0083(16) F2 0.036(3) 0.049(2) 0.126(4) 0.000(2) 0.038(3) 0.0050(19) F3 0.153(6) 0.091(4) 0.024(2) 0.007(2) 0.014(3) -0.025(4) F4 0.064(3) 0.0234(16) 0.064(2) -0.0112(15) 0.044(2) -0.0135(16) F5 0.046(3) 0.045(2) 0.134(5) -0.021(2) 0.056(3) -0.0068(19) F6 0.089(4) 0.073(3) 0.029(2) 0.0098(19) 0.012(2) -0.019(3) N1 0.026(3) 0.042(3) 0.019(2) 0.0034(19) 0.006(2) -0.007(2) O1 0.058(5) 0.103(5) 0.069(4) -0.002(4) 0.021(4) 0.003(4) P1 0.0172(8) 0.0121(5) 0.0184(6) -0.0004(4) 0.0057(6) -0.0012(5) P2 0.0226(8) 0.0139(5) 0.0252(7) -0.0001(5) 0.0131(7) -0.0021(5) P3 0.0179(8) 0.0150(5) 0.0209(6) 0.0002(4) 0.0085(6) -0.0016(5) Sb1 0.0233(2) 0.02245(16) 0.0267(2) -0.00136(13) 0.00812(18) -0.00295(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 P1 1.732(5) . y C1 P2 1.750(5) . y C1 Cu1B 1.961(7) . y C1 Cu1A 1.981(5) . y C1 Au1 2.111(4) . y C2 N1 1.348(7) . y C2 C3 1.375(7) . y C2 P1 1.827(5) . y C3 C4 1.394(8) . y C4 C5 1.371(10) . y C5 C6 1.408(10) . y C6 N1 1.353(7) . y C7 C8 1.387(8) . y C7 C12 1.398(7) . y C7 P1 1.820(5) . y C8 C9 1.394(7) . y C9 C10 1.393(9) . y C10 C11 1.386(9) . y C11 C12 1.384(7) . y C13 C14 1.385(7) . y C13 C18 1.408(6) . y C13 P1 1.812(5) . y C14 C15 1.388(7) . y C15 C16 1.394(8) . y C16 C17 1.384(8) . y C17 C18 1.384(8) . y C19 C24 1.392(8) . y C19 C20 1.410(8) . y C19 P2 1.813(5) . y C20 C21 1.387(7) . y C21 C22 1.390(9) . y C22 C23 1.369(9) . y C23 C24 1.408(7) . y C25 C30 1.375(8) . y C25 C26 1.386(7) . y C25 P2 1.832(6) . y C26 C27 1.377(10) . y C27 C28 1.395(11) . y C28 C29 1.353(11) . y C29 C30 1.405(10) . y C31 C36 1.407(6) . y C31 C32 1.408(7) . y C31 P2 1.819(5) . y C32 C33 1.402(8) . y C33 C34 1.379(8) . y C34 C35 1.398(8) . y C35 C36 1.377(7) . y C37 C38 1.387(8) . y C37 C42 1.390(7) . y C37 P3 1.808(5) . y C38 C39 1.394(7) . y C39 C40 1.375(8) . y C40 C41 1.376(9) . y C41 C42 1.383(8) . y C43 C44 1.364(8) . y C43 C48 1.394(7) . y C43 P3 1.831(5) . y C44 C45 1.404(9) . y C45 C46 1.384(9) . y C46 C47 1.367(9) . y C47 C48 1.372(8) . y C49 C50 1.383(7) . y C49 C54 1.390(7) . y C49 P3 1.802(5) . y C50 C51 1.405(8) . y C51 C52 1.355(9) . y C52 C53 1.374(9) . y C53 C54 1.378(8) . y C55 Cl3 1.593(14) . y C55 Cl2 1.755(12) . y C56 Cl5 1.714(16) . y C56 Cl4 1.788(14) . y C60 C59 1.613(12) . y C59 O1 1.456(11) . y C57 O1 1.395(11) . y C57 C58 1.516(15) . y Au1 P3 2.2702(13) . y Au1 Cu1A 2.8483(10) . y Au1 Cu1B 2.900(4) . y Cl1A Cl1B 0.61(2) . y Cl1A Cu1B 2.073(6) . y Cl1A Cu1A 2.165(4) . y Cl1B Cu1B 2.12(2) . y Cl1B Cu1A 2.17(2) . y Cu1A Cu1B 0.764(9) . y Cu1A N1 2.267(6) . y Cu1A P1 2.8778(19) . y Cu1B P2 2.823(6) . y F1 Sb1 1.883(3) . y F2 Sb1 1.851(4) . y F3 Sb1 1.843(4) . y F4 Sb1 1.876(3) . y F5 Sb1 1.873(4) . y F6 Sb1 1.873(4) . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 C1 P2 120.2(3) . . y P1 C1 Cu1B 120.8(4) . . y P2 C1 Cu1B 98.9(4) . . y P1 C1 Cu1A 101.4(2) . . y P2 C1 Cu1A 120.4(3) . . y P1 C1 Au1 111.4(2) . . y P2 C1 Au1 110.6(2) . . y Cu1B C1 Au1 90.7(2) . . y Cu1A C1 Au1 88.16(19) . . y N1 C2 C3 123.9(5) . . y N1 C2 P1 114.1(4) . . y C3 C2 P1 121.8(4) . . y C2 C3 C4 118.1(6) . . y C5 C4 C3 119.3(6) . . y C4 C5 C6 119.5(5) . . y N1 C6 C5 121.4(6) . . y C8 C7 C12 119.9(4) . . y C8 C7 P1 120.0(4) . . y C12 C7 P1 119.7(4) . . y C7 C8 C9 119.5(5) . . y C10 C9 C8 120.2(6) . . y C11 C10 C9 120.2(5) . . y C12 C11 C10 119.7(5) . . y C11 C12 C7 120.4(5) . . y C14 C13 C18 119.9(5) . . y C14 C13 P1 119.0(3) . . y C18 C13 P1 120.2(4) . . y C13 C14 C15 119.4(4) . . y C14 C15 C16 120.6(5) . . y C17 C16 C15 120.1(5) . . y C18 C17 C16 119.8(5) . . y C17 C18 C13 120.1(5) . . y C24 C19 C20 119.6(5) . . y C24 C19 P2 123.2(4) . . y C20 C19 P2 116.7(4) . . y C21 C20 C19 120.1(6) . . y C20 C21 C22 119.4(5) . . y C23 C22 C21 121.4(5) . . y C22 C23 C24 119.8(6) . . y C19 C24 C23 119.6(5) . . y C30 C25 C26 120.1(6) . . y C30 C25 P2 122.2(4) . . y C26 C25 P2 117.6(5) . . y C27 C26 C25 120.0(7) . . y C26 C27 C28 120.5(7) . . y C29 C28 C27 118.8(7) . . y C28 C29 C30 121.8(8) . . y C25 C30 C29 118.7(6) . . y C36 C31 C32 119.0(5) . . y C36 C31 P2 118.9(4) . . y C32 C31 P2 122.1(4) . . y C33 C32 C31 119.5(5) . . y C34 C33 C32 120.8(5) . . y C33 C34 C35 119.8(5) . . y C36 C35 C34 120.4(5) . . y C35 C36 C31 120.6(5) . . y C38 C37 C42 118.4(5) . . y C38 C37 P3 118.4(4) . . y C42 C37 P3 123.2(5) . . y C37 C38 C39 121.6(5) . . y C40 C39 C38 119.0(6) . . y C39 C40 C41 120.1(5) . . y C40 C41 C42 121.1(5) . . y C41 C42 C37 119.9(6) . . y C44 C43 C48 120.4(5) . . y C44 C43 P3 121.5(4) . . y C48 C43 P3 118.0(4) . . y C43 C44 C45 119.1(5) . . y C46 C45 C44 120.1(6) . . y C47 C46 C45 120.1(6) . . y C46 C47 C48 120.2(5) . . y C47 C48 C43 120.1(6) . . y C50 C49 C54 119.0(5) . . y C50 C49 P3 119.2(4) . . y C54 C49 P3 121.8(4) . . y C49 C50 C51 119.7(5) . . y C52 C51 C50 120.1(6) . . y C51 C52 C53 120.7(6) . . y C52 C53 C54 119.9(6) . . y C53 C54 C49 120.6(5) . . y Cl3 C55 Cl2 116.6(8) . . y Cl5 C56 Cl4 110.7(8) . . y O1 C59 C60 105.1(7) . . y O1 C57 C58 107.3(9) . . y C1 Au1 P3 176.59(12) . . y C1 Au1 Cu1A 44.03(13) . . y P3 Au1 Cu1A 137.70(4) . . y C1 Au1 Cu1B 42.54(16) . . y P3 Au1 Cu1B 137.93(10) . . y Cu1A Au1 Cu1B 15.24(17) . . y Cl1B Cl1A Cu1B 85(2) . . y Cl1B Cl1A Cu1A 82(2) . . y Cl1A Cl1B Cu1B 78(2) . . y Cl1A Cl1B Cu1A 81(2) . . y Cu1B Cu1A C1 77.4(4) . . y Cu1B Cu1A Cl1A 72.9(3) . . y C1 Cu1A Cl1A 148.3(2) . . y Cu1B Cu1A Cl1B 75.8(6) . . y C1 Cu1A Cl1B 152.6(6) . . y Cl1A Cu1A Cl1B 16.3(6) . . y Cu1B Cu1A N1 163.4(3) . . y C1 Cu1A N1 89.08(19) . . y Cl1A Cu1A N1 121.93(18) . . y Cl1B Cu1A N1 116.3(6) . . y Cu1B Cu1A Au1 86.3(3) . . y C1 Cu1A Au1 47.81(13) . . y Cl1A Cu1A Au1 138.57(11) . . y Cl1B Cu1A Au1 124.5(6) . . y N1 Cu1A Au1 77.42(12) . . y Cu1B Cu1A P1 109.4(3) . . y C1 Cu1A P1 36.14(14) . . y Cl1A Cu1A P1 153.05(10) . . y Cl1B Cu1A P1 167.7(6) . . y N1 Cu1A P1 61.35(14) . . y Au1 Cu1A P1 67.53(4) . . y Cu1A Cu1B C1 80.3(5) . . y Cu1A Cu1B Cl1A 86.4(4) . . y C1 Cu1B Cl1A 162.6(5) . . y Cu1A Cu1B Cl1B 83.7(7) . . y C1 Cu1B Cl1B 163.1(10) . . y Cl1A Cu1B Cl1B 16.8(6) . . y Cu1A Cu1B P2 116.8(4) . . y C1 Cu1B P2 37.78(18) . . y Cl1A Cu1B P2 149.3(4) . . y Cl1B Cu1B P2 159.0(9) . . y Cu1A Cu1B Au1 78.5(3) . . y C1 Cu1B Au1 46.71(15) . . y Cl1A Cu1B Au1 140.9(3) . . y Cl1B Cu1B Au1 124.4(8) . . y P2 Cu1B Au1 67.52(9) . . y C2 N1 C6 117.7(5) . . y C2 N1 Cu1A 109.1(3) . . y C6 N1 Cu1A 132.7(5) . . y C57 O1 C59 112.3(8) . . y C1 P1 C13 114.9(2) . . y C1 P1 C7 116.7(2) . . y C13 P1 C7 106.6(2) . . y C1 P1 C2 107.4(2) . . y C13 P1 C2 107.3(2) . . y C7 P1 C2 103.0(2) . . y C13 P1 Cu1A 153.12(17) . . y C7 P1 Cu1A 98.52(18) . . y C2 P1 Cu1A 75.30(18) . . y C1 P2 C19 112.5(2) . . y C1 P2 C31 114.4(2) . . y C19 P2 C31 108.9(2) . . y C1 P2 C25 110.7(2) . . y C19 P2 C25 104.7(2) . . y C31 P2 C25 105.0(2) . . y C19 P2 Cu1B 95.65(19) . . y C31 P2 Cu1B 153.3(2) . . y C25 P2 Cu1B 77.8(3) . . y C49 P3 C37 106.0(2) . . y C49 P3 C43 106.0(2) . . y C37 P3 C43 107.0(2) . . y C49 P3 Au1 115.35(17) . . y C37 P3 Au1 110.19(18) . . y C43 P3 Au1 111.80(15) . . y F3 Sb1 F2 90.9(3) . . y F3 Sb1 F6 178.2(3) . . y F2 Sb1 F6 90.8(2) . . y F3 Sb1 F5 89.9(3) . . y F2 Sb1 F5 179.2(2) . . y F6 Sb1 F5 88.3(2) . . y F3 Sb1 F4 90.1(2) . . y F2 Sb1 F4 90.75(17) . . y F6 Sb1 F4 89.54(18) . . y F5 Sb1 F4 89.06(17) . . y F3 Sb1 F1 90.1(2) . . y F2 Sb1 F1 89.38(17) . . y F6 Sb1 F1 90.23(19) . . y F5 Sb1 F1 90.81(17) . . y F4 Sb1 F1 179.7(2) . . y _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.884 _refine_diff_density_min -2.679 _refine_diff_density_rms 0.166 data_6 _database_code_depnum_ccdc_archive 'CCDC 914766' _audit_creation_date 2012-12-07 _audit_block_code RKI-RF-204-01_7089 _chemical_name_systematic ; Au-chloro-Au'-triphenylphosphine-Au,Au'-mu^2^-(diphenyl-2-pyridyl- phosphorane)-(triphenylphosphorane)-idenyl-digold hexafluoroantimonate dichloromethane solute ; _chemical_melting_point ? _chemical_formula_moiety 'C54 H44 Au2 Cl N P3, F6 Sb, 2(C H2 Cl2)' _chemical_compound_source dichlormethane/diethylether _chemical_formula_sum 'C56 H48 Au2 Cl5 F6 N P3 Sb' _chemical_formula_weight 1634.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-p 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0964(17) _cell_length_b 16.611(3) _cell_length_c 17.876(3) _cell_angle_alpha 63.214(2) _cell_angle_beta 74.097(3) _cell_angle_gamma 71.051(3) _cell_volume 2750.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.1804 _cell_measurement_theta_max 26.3670 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0050 0.00 0.00 -1.00 0.0050 -1.00 0.00 0.00 0.0180 1.00 0.00 0.00 0.0180 0.00 -1.00 0.00 0.0180 0.00 1.00 0.00 0.0180 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.036 _exptl_crystal_size_mid 0.036 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method ? _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 6.199 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.77426 _exptl_absorpt_correction_T_max 0.94267 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_special_details ; Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75 ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_monochromator 'Incoatec Helios mirrors' _diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 66.67 _diffrn_reflns_number 58526 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.78 _reflns_number_total 11609 _reflns_number_gt 8203 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT software (Bruker AXS, 2004)' _computing_data_reduction 'SAINT software (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The minimum and maximum estimated transmissions from the multi-scan scaling are 0.7261 and 0.9958 (SADABS). Several low angle reflections were shaded by the beamstop and were not included in the final refinement cycles. One of the phenyl/pyridyl groups attached to P was rotationally disordered over two positions about C19. The location of the single 2-pyridyl group attached to P could not be determined with certainty. However, refinement of all the six-membered ring atoms as C resulted in smaller than average C atomic displacement parameters for C01 and C20A, indicating that these positions are the preferential locations of N. Position C20A and half of position C01 were refined as N atoms (N1A and N1B, respectively). Distances of these two N atoms to the Au atom Au2 (N1A...Au2 3.31(1) and N1B...Au2 3.41(1) \%A) indicate that the 2-pyridyl group is not bonded to Au2. This is confirmed by the almost linear C1-Au2-Cl1 angle of 178.8(2) \%. The crystal contains two solute dichlormethane molecules. The adp of one Cl atom (Cl4) is somewhat anisotropic. Attempts to model the disorder of this atom by two atoms with half occupancy were unsuccessful, since the close proximity of a centre of symmetry, and associated symmetry related molecule, prevented an otherwise chemically sensible interpretation of the disorder. Highest peak 3.26 at 0.2635 0.4021 0.0895 [ 0.92 A from AU2 ] Deepest hole -1.93 at 0.5019 0.0809 0.0176 [ 0.80 A from CL4 ] ; _iucr_refine_instructions_details ; TITL 7089sadabs in P-1 CELL 0.71073 11.0964 16.6114 17.8756 63.214 74.097 71.051 ZERR 2.00 0.0017 0.0026 0.0028 0.002 0.003 0.003 LATT 1 SFAC C H Au Cl F N P Sb UNIT 112 96 4 10 12 2 6 2 L.S. 10 SHEL 10.0 0.3 ACTA SIZE 0.012 0.048 0.051 TEMP -173 BOND EADP N1A C01 EXYZ N1A C01 FMAP 2 PLAN 20 WGHT 0.055400 4.772717 FVAR 0.05023 C1 1 0.206658 0.364741 0.249650 11.00000 0.01968 0.02840 = 0.03505 -0.01541 -0.00211 -0.00507 PART 1 C01 1 0.216040 0.167500 0.241356 10.50000 0.04615 AFIX 43 H01 2 0.271946 0.206792 0.203644 10.50000 -1.20000 AFIX 0 C2 1 0.123393 0.191098 0.303298 11.00000 0.03377 0.02533 = 0.05271 -0.01592 -0.02006 -0.00289 C3 1 0.039499 0.134866 0.355424 11.00000 0.04104 0.02154 = 0.05733 -0.01290 -0.02142 -0.00529 AFIX 43 H3 2 -0.025882 0.151810 0.396334 11.00000 -1.20000 AFIX 0 C4 1 0.052692 0.051114 0.346791 11.00000 0.04588 0.03592 = 0.08073 -0.00801 -0.03840 -0.01357 AFIX 43 H4 2 -0.003848 0.011603 0.382549 11.00000 -1.20000 AFIX 0 C5 1 0.144381 0.027651 0.288531 11.00000 0.06373 0.02983 = 0.06874 -0.01538 -0.04057 -0.00222 AFIX 43 H5 2 0.152845 -0.028909 0.284161 11.00000 -1.20000 AFIX 0 C6 1 0.224295 0.082754 0.236353 11.00000 0.05311 0.02834 = 0.06756 -0.02663 -0.03416 0.01203 AFIX 43 H6 2 0.287713 0.064823 0.195211 11.00000 -1.20000 AFIX 0 PART 0 C7 1 0.127403 0.246469 0.432308 11.00000 0.02956 0.02335 = 0.04170 -0.01618 -0.00787 -0.00266 C8 1 0.252310 0.223650 0.448892 11.00000 0.03535 0.02199 = 0.04764 -0.01388 -0.00676 -0.00637 AFIX 43 H8 2 0.321980 0.234837 0.403593 11.00000 -1.20000 AFIX 0 C9 1 0.273964 0.184512 0.532018 11.00000 0.04892 0.01923 = 0.05622 -0.01008 -0.02339 -0.00129 AFIX 43 H9 2 0.359085 0.170076 0.543179 11.00000 -1.20000 AFIX 0 C10 1 0.175235 0.165903 0.599105 11.00000 0.05649 0.02223 = 0.03640 -0.00896 -0.01541 -0.00646 AFIX 43 H10 2 0.190986 0.139641 0.655978 11.00000 -1.20000 AFIX 0 C11 1 0.051478 0.186830 0.580898 11.00000 0.04768 0.03046 = 0.03982 -0.01186 -0.00527 -0.01315 AFIX 43 H11 2 -0.017402 0.173427 0.626431 11.00000 -1.20000 AFIX 0 C12 1 0.026314 0.225995 0.499618 11.00000 0.03416 0.03216 = 0.03456 -0.01015 -0.00397 -0.00707 AFIX 43 H12 2 -0.058725 0.239191 0.488867 11.00000 -1.20000 AFIX 0 C13 1 -0.063517 0.354100 0.312828 11.00000 0.02544 0.02819 = 0.05111 -0.01371 -0.00772 -0.00808 C14 1 -0.136344 0.402792 0.362458 11.00000 0.04276 0.03082 = 0.04355 -0.00708 -0.01370 -0.01119 AFIX 43 H14 2 -0.102681 0.399296 0.407587 11.00000 -1.20000 AFIX 0 C15 1 -0.258026 0.456351 0.345846 11.00000 0.03549 0.02859 = 0.06211 -0.01245 0.00029 -0.00325 AFIX 43 H15 2 -0.309892 0.487779 0.381058 11.00000 -1.20000 AFIX 0 C16 1 -0.304187 0.464205 0.278236 11.00000 0.02304 0.04507 = 0.06179 -0.00884 -0.01528 -0.00654 AFIX 43 H16 2 -0.386675 0.503050 0.265759 11.00000 -1.20000 AFIX 0 C17 1 -0.232300 0.416485 0.228567 11.00000 0.03078 0.03695 = 0.05876 -0.01402 -0.01808 -0.00867 AFIX 43 H17 2 -0.265179 0.422294 0.182126 11.00000 -1.20000 AFIX 0 C18 1 -0.112770 0.360346 0.246178 11.00000 0.03111 0.02254 = 0.04659 -0.00739 -0.01313 -0.01052 AFIX 43 H18 2 -0.063898 0.325899 0.212954 11.00000 -1.20000 AFIX 0 C19 1 0.320282 0.528128 0.178602 11.00000 0.03609 0.03108 = 0.03017 -0.01023 -0.00583 -0.01271 PART 1 C20B 1 0.418660 0.486855 0.151631 10.50000 0.03968 AFIX 43 H20B 2 0.432558 0.421537 0.171120 10.50000 -1.20000 AFIX 0 PART 2 C21A 1 0.502870 0.548827 0.065168 10.50000 0.03131 AFIX 43 H21A 2 0.564863 0.530001 0.024014 10.50000 -1.20000 AFIX 0 PART 1 C21B 1 0.512197 0.528571 0.094280 10.50000 0.04925 AFIX 43 H21B 2 0.585230 0.493688 0.070437 10.50000 -1.20000 AFIX 0 PART 0 C22 1 0.500042 0.625231 0.070049 11.00000 0.04417 0.06202 = 0.05607 -0.01276 -0.00027 -0.01557 AFIX 43 H22 2 0.564163 0.656848 0.031744 11.00000 -1.20000 AFIX 0 PART 2 C23A 1 0.326338 0.610383 0.182432 10.50000 0.02748 AFIX 43 H24A 2 0.266322 0.631987 0.222586 10.50000 -1.20000 AFIX 0 PART 1 C23B 1 0.388579 0.668433 0.106519 10.50000 0.08433 AFIX 43 H24B 2 0.375654 0.732137 0.094818 10.50000 -1.20000 AFIX 0 PART 2 C24A 1 0.417692 0.659599 0.128976 10.50000 0.02877 AFIX 43 H23A 2 0.423998 0.713607 0.132190 10.50000 -1.20000 AFIX 0 PART 1 C24B 1 0.292091 0.621107 0.161087 10.50000 0.06260 AFIX 43 H23B 2 0.212782 0.651697 0.184171 10.50000 -1.20000 AFIX 0 PART 0 C25 1 0.046485 0.556179 0.238218 11.00000 0.03675 0.02466 = 0.02615 -0.00766 -0.00411 -0.00842 C26 1 -0.026991 0.565639 0.182663 11.00000 0.03785 0.02357 = 0.03330 -0.00982 -0.01204 -0.00731 AFIX 43 H26 2 -0.000669 0.524900 0.154206 11.00000 -1.20000 AFIX 0 C27 1 -0.138374 0.634088 0.168506 11.00000 0.04340 0.02649 = 0.04124 -0.00776 -0.01638 -0.00199 AFIX 43 H27 2 -0.188768 0.640708 0.129959 11.00000 -1.20000 AFIX 0 C28 1 -0.177692 0.693249 0.209710 11.00000 0.04258 0.02920 = 0.04385 -0.01630 -0.01202 0.00875 AFIX 43 H28 2 -0.256568 0.738932 0.201263 11.00000 -1.20000 AFIX 0 C29 1 -0.102729 0.686034 0.262916 11.00000 0.05342 0.03260 = 0.04410 -0.01710 -0.01256 -0.00168 AFIX 43 H29 2 -0.128033 0.728399 0.289602 11.00000 -1.20000 AFIX 0 C30 1 0.010772 0.616620 0.278080 11.00000 0.05347 0.02806 = 0.02363 -0.00755 -0.01444 -0.01442 AFIX 43 H30 2 0.062622 0.611101 0.315295 11.00000 -1.20000 AFIX 0 C31 1 0.229925 0.447772 0.358272 11.00000 0.03298 0.01941 = 0.03966 -0.01327 -0.01241 -0.00372 C32 1 0.130245 0.438356 0.424021 11.00000 0.02551 0.02349 = 0.02656 -0.00551 -0.00666 -0.00115 AFIX 43 H32 2 0.045576 0.447485 0.414813 11.00000 -1.20000 AFIX 0 C33 1 0.153366 0.415706 0.503104 11.00000 0.03096 0.03009 = 0.04517 -0.01494 -0.00382 -0.00130 AFIX 43 H33 2 0.084256 0.409912 0.549004 11.00000 -1.20000 AFIX 0 C34 1 0.277218 0.401116 0.516769 11.00000 0.06063 0.03086 = 0.02927 -0.00948 -0.01373 -0.00662 AFIX 43 H34 2 0.292979 0.383847 0.572249 11.00000 -1.20000 AFIX 0 C35 1 0.374991 0.411283 0.451934 11.00000 0.03871 0.03737 = 0.05012 -0.01738 -0.02136 -0.00611 AFIX 43 H35 2 0.459507 0.402160 0.461388 11.00000 -1.20000 AFIX 0 C36 1 0.352638 0.434930 0.371789 11.00000 0.02871 0.02847 = 0.03776 -0.00740 -0.01064 -0.00652 AFIX 43 H36 2 0.421644 0.442410 0.325792 11.00000 -1.20000 AFIX 0 C37 1 0.600538 0.078943 0.245795 11.00000 0.02934 0.03099 = 0.03159 -0.01403 -0.01006 -0.00524 C38 1 0.683484 0.052970 0.183507 11.00000 0.06678 0.04545 = 0.04812 -0.02257 0.00499 -0.03198 AFIX 43 H38 2 0.741406 0.089746 0.143992 11.00000 -1.20000 AFIX 0 C39 1 0.681154 -0.030648 0.179142 11.00000 0.08771 0.05303 = 0.07347 -0.04159 0.00653 -0.03224 AFIX 43 H39 2 0.739542 -0.051571 0.138076 11.00000 -1.20000 AFIX 0 C40 1 0.592252 -0.079937 0.235901 11.00000 0.07051 0.04563 = 0.06104 -0.02583 -0.01318 -0.02795 AFIX 43 H40 2 0.585360 -0.132469 0.230363 11.00000 -1.20000 AFIX 0 C41 1 0.513406 -0.055731 0.300097 11.00000 0.03343 0.02623 = 0.06344 -0.01895 -0.00611 -0.00258 AFIX 43 H41 2 0.457897 -0.093754 0.340994 11.00000 -1.20000 AFIX 0 C42 1 0.515740 0.024731 0.304532 11.00000 0.03555 0.02760 = 0.04715 -0.01753 -0.00169 -0.00766 AFIX 43 H42 2 0.459544 0.043237 0.347628 11.00000 -1.20000 AFIX 0 C43 1 0.723617 0.230125 0.172387 11.00000 0.02988 0.02205 = 0.03210 -0.00553 -0.01395 -0.00962 C44 1 0.853074 0.189301 0.181867 11.00000 0.03626 0.05407 = 0.03965 0.00111 -0.01088 -0.01905 AFIX 43 H44 2 0.874784 0.136493 0.231967 11.00000 -1.20000 AFIX 0 C45 1 0.948650 0.224061 0.120368 11.00000 0.02970 0.07807 = 0.06440 -0.02356 -0.00842 -0.01668 AFIX 43 H45 2 1.036504 0.196863 0.127734 11.00000 -1.20000 AFIX 0 C46 1 0.915335 0.300213 0.046455 11.00000 0.05511 0.05193 = 0.04927 -0.01204 0.00726 -0.02756 AFIX 43 H46 2 0.981585 0.325102 0.003527 11.00000 -1.20000 AFIX 0 C47 1 0.793377 0.338831 0.034538 11.00000 0.06368 0.05668 = 0.04470 0.00909 0.00933 -0.00890 AFIX 43 H47 2 0.773669 0.389036 -0.017503 11.00000 -1.20000 AFIX 0 C48 1 0.694850 0.306549 0.097272 11.00000 0.03949 0.05409 = 0.04047 -0.00448 -0.00762 0.00070 AFIX 43 H48 2 0.607616 0.336275 0.089357 11.00000 -1.20000 AFIX 0 C49 1 0.646013 0.150972 0.354090 11.00000 0.03785 0.03011 = 0.02944 0.00168 -0.01211 -0.01617 C50 1 0.634649 0.220232 0.380520 11.00000 0.03847 0.02699 = 0.04485 -0.01619 -0.01366 -0.00899 AFIX 43 H50 2 0.599428 0.282909 0.346428 11.00000 -1.20000 AFIX 0 C51 1 0.673374 0.199870 0.455057 11.00000 0.04156 0.02944 = 0.04840 -0.02115 -0.01527 -0.00409 AFIX 43 H51 2 0.664175 0.247804 0.472815 11.00000 -1.20000 AFIX 0 C52 1 0.725778 0.108872 0.503717 11.00000 0.06057 0.04336 = 0.02608 -0.00974 -0.01760 -0.01333 AFIX 43 H52 2 0.754424 0.093735 0.554932 11.00000 -1.20000 AFIX 0 C53 1 0.736461 0.039938 0.477798 11.00000 0.06755 0.02151 = 0.04665 -0.00714 -0.03150 -0.00285 AFIX 43 H53 2 0.770306 -0.022837 0.512387 11.00000 -1.20000 AFIX 0 C54 1 0.699622 0.060108 0.404036 11.00000 0.05107 0.02463 = 0.04903 -0.01983 -0.01516 -0.00365 AFIX 43 H54 2 0.710498 0.011841 0.386331 11.00000 -1.20000 AFIX 0 C55 1 0.860740 0.110554 0.888423 11.00000 0.16674 AFIX 23 H55A 2 0.800229 0.070018 0.923565 11.00000 -1.20000 H55B 2 0.812201 0.166736 0.846912 11.00000 -1.20000 AFIX 0 C56 1 0.383563 0.169553 0.976577 11.00000 0.15015 AFIX 23 H56A 2 0.424259 0.180949 0.917134 11.00000 -1.20000 H56B 2 0.345699 0.230871 0.979874 11.00000 -1.20000 AFIX 0 AU1 3 0.399231 0.283408 0.246585 11.00000 0.02536 0.02939 = 0.03574 -0.01530 -0.00911 -0.00268 AU2 3 0.189326 0.392375 0.126910 11.00000 0.02695 0.03048 = 0.03478 -0.01405 -0.00712 -0.00764 CL1 4 0.173832 0.419853 -0.006791 11.00000 0.04322 0.06266 = 0.03595 -0.01753 -0.00552 -0.02032 CL2 4 0.901182 0.144093 0.952672 11.00000 0.30770 0.19366 = 0.14293 -0.08981 -0.04696 -0.01680 CL3 4 0.973610 0.056199 0.834987 11.00000 0.20732 0.20873 = 0.17275 -0.12172 -0.05126 0.00895 CL4 4 0.492215 0.117077 1.033239 11.00000 0.25584 0.68779 = 0.41816 0.33915 -0.17553 -0.22676 CL5 4 0.264516 0.119880 0.997854 11.00000 0.32452 0.24323 = 0.22241 -0.12782 -0.07078 -0.05035 F1 5 0.781674 0.304745 0.678927 11.00000 0.05897 0.09785 = 0.13379 -0.08069 -0.02460 -0.01757 F2 5 0.538119 0.389043 0.680829 11.00000 0.06656 0.05630 = 0.15205 -0.05838 0.01664 -0.01405 F3 5 0.670924 0.364153 0.543411 11.00000 0.11643 0.08435 = 0.07349 -0.00751 -0.00395 -0.05939 F4 5 0.497561 0.268118 0.636306 11.00000 0.05565 0.06023 = 0.08883 -0.01726 -0.03304 -0.01480 F5 5 0.605158 0.210184 0.768596 11.00000 0.15218 0.08350 = 0.07271 -0.00689 -0.03707 -0.06093 F6 5 0.742793 0.190405 0.630320 11.00000 0.07163 0.06747 = 0.13098 -0.06921 -0.04462 0.01028 PART 2 N1A 6 0.216040 0.167500 0.241356 10.50000 0.04615 N1B 6 0.417170 0.494387 0.118862 10.50000 0.03639 PART 0 P1 7 0.198278 0.468859 0.256386 11.00000 0.02849 0.02382 = 0.03363 -0.01171 -0.00916 -0.00639 P2 7 0.102808 0.293927 0.321971 11.00000 0.02568 0.02439 = 0.04200 -0.01290 -0.01056 -0.00371 P3 7 0.596936 0.185282 0.252721 11.00000 0.02667 0.02302 = 0.02971 -0.00991 -0.00666 -0.00469 SB1 8 0.639023 0.288673 0.658779 11.00000 0.04154 0.03012 = 0.06740 -0.01927 -0.01550 -0.00394 HKLF 4 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+4.7727P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11609 _refine_ls_number_parameters 648 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1244 _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_restrained_S_all 1.270 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2067(8) 0.3647(6) 0.2496(6) 0.0272(19) Uani 1 1 d . A . C01 C 0.2160(9) 0.1675(7) 0.2414(6) 0.046(2) Uiso 0.50 1 d P A 1 H01 H 0.2719 0.2068 0.2036 0.055 Uiso 0.50 1 calc PR A 1 C2 C 0.1234(9) 0.1911(6) 0.3033(6) 0.035(2) Uani 1 1 d . A 1 C3 C 0.0395(10) 0.1349(6) 0.3554(7) 0.039(2) Uani 1 1 d . A 1 H3 H -0.0259 0.1518 0.3963 0.046 Uiso 1 1 calc R A 1 C4 C 0.0527(11) 0.0511(7) 0.3468(8) 0.053(3) Uani 1 1 d . A 1 H4 H -0.0038 0.0116 0.3825 0.063 Uiso 1 1 calc R A 1 C5 C 0.1444(12) 0.0277(7) 0.2885(8) 0.051(3) Uani 1 1 d . A 1 H5 H 0.1528 -0.0289 0.2842 0.062 Uiso 1 1 calc R A 1 C6 C 0.2243(11) 0.0828(7) 0.2364(8) 0.047(3) Uani 1 1 d . A 1 H6 H 0.2877 0.0648 0.1952 0.056 Uiso 1 1 calc R A 1 C7 C 0.1274(9) 0.2465(6) 0.4323(6) 0.031(2) Uani 1 1 d . A . C8 C 0.2523(9) 0.2237(6) 0.4489(6) 0.035(2) Uani 1 1 d . . . H8 H 0.3220 0.2348 0.4036 0.042 Uiso 1 1 calc R . . C9 C 0.2740(10) 0.1845(6) 0.5320(7) 0.042(3) Uani 1 1 d . . . H9 H 0.3591 0.1701 0.5432 0.050 Uiso 1 1 calc R . . C10 C 0.1752(10) 0.1659(6) 0.5991(6) 0.038(2) Uani 1 1 d . . . H10 H 0.1910 0.1396 0.6560 0.046 Uiso 1 1 calc R . . C11 C 0.0515(10) 0.1868(6) 0.5809(7) 0.039(2) Uani 1 1 d . . . H11 H -0.0174 0.1734 0.6264 0.047 Uiso 1 1 calc R . . C12 C 0.0263(9) 0.2260(6) 0.4996(6) 0.035(2) Uani 1 1 d . . . H12 H -0.0587 0.2392 0.4889 0.042 Uiso 1 1 calc R . . C13 C -0.0635(9) 0.3541(6) 0.3128(7) 0.035(2) Uani 1 1 d . A . C14 C -0.1363(10) 0.4028(6) 0.3625(7) 0.040(2) Uani 1 1 d . . . H14 H -0.1027 0.3993 0.4076 0.048 Uiso 1 1 calc R . . C15 C -0.2580(10) 0.4564(7) 0.3458(7) 0.047(3) Uani 1 1 d . . . H15 H -0.3099 0.4878 0.3811 0.057 Uiso 1 1 calc R . . C16 C -0.3042(9) 0.4642(7) 0.2782(7) 0.047(3) Uani 1 1 d . . . H16 H -0.3867 0.5030 0.2658 0.056 Uiso 1 1 calc R . . C17 C -0.2323(9) 0.4165(7) 0.2286(7) 0.041(2) Uani 1 1 d . . . H17 H -0.2652 0.4223 0.1821 0.050 Uiso 1 1 calc R . . C18 C -0.1128(9) 0.3603(6) 0.2462(6) 0.033(2) Uani 1 1 d . . . H18 H -0.0639 0.3259 0.2130 0.040 Uiso 1 1 calc R . . C19 C 0.3203(9) 0.5281(6) 0.1786(6) 0.032(2) Uani 1 1 d . . . C20B C 0.419(2) 0.4869(17) 0.1516(16) 0.040(6) Uiso 0.50 1 d P B 1 H20B H 0.4326 0.4215 0.1711 0.048 Uiso 0.50 1 calc PR B 1 C21A C 0.503(2) 0.5488(15) 0.0652(15) 0.031(5) Uiso 0.50 1 d P B 2 H21A H 0.5649 0.5300 0.0240 0.038 Uiso 0.50 1 calc PR B 2 C21B C 0.512(3) 0.5286(19) 0.0943(18) 0.049(7) Uiso 0.50 1 d P B 1 H21B H 0.5852 0.4937 0.0704 0.059 Uiso 0.50 1 calc PR B 1 C22 C 0.5000(11) 0.6252(9) 0.0700(8) 0.059(3) Uani 1 1 d . . . H22 H 0.5642 0.6568 0.0317 0.071 Uiso 1 1 calc R B 1 C23A C 0.326(2) 0.6104(13) 0.1824(13) 0.027(4) Uiso 0.50 1 d P B 2 H24A H 0.2663 0.6320 0.2226 0.033 Uiso 0.50 1 calc PR B 2 C23B C 0.389(4) 0.668(3) 0.107(2) 0.084(12) Uiso 0.50 1 d P B 1 H24B H 0.3757 0.7321 0.0948 0.101 Uiso 0.50 1 calc PR B 1 C24A C 0.418(2) 0.6596(14) 0.1290(13) 0.029(5) Uiso 0.50 1 d P B 2 H23A H 0.4240 0.7136 0.1322 0.035 Uiso 0.50 1 calc PR B 2 C24B C 0.292(3) 0.621(2) 0.1611(19) 0.063(8) Uiso 0.50 1 d P B 1 H23B H 0.2128 0.6517 0.1842 0.075 Uiso 0.50 1 calc PR B 1 C25 C 0.0465(9) 0.5562(6) 0.2382(6) 0.030(2) Uani 1 1 d . . . C26 C -0.0270(9) 0.5656(6) 0.1827(6) 0.031(2) Uani 1 1 d . B . H26 H -0.0007 0.5249 0.1542 0.037 Uiso 1 1 calc R . . C27 C -0.1384(10) 0.6341(6) 0.1685(6) 0.039(2) Uani 1 1 d . . . H27 H -0.1888 0.6407 0.1300 0.046 Uiso 1 1 calc R B . C28 C -0.1777(10) 0.6932(7) 0.2097(6) 0.041(2) Uani 1 1 d . B . H28 H -0.2566 0.7389 0.2013 0.049 Uiso 1 1 calc R . . C29 C -0.1027(10) 0.6860(7) 0.2629(7) 0.044(3) Uani 1 1 d . . . H29 H -0.1280 0.7284 0.2896 0.052 Uiso 1 1 calc R B . C30 C 0.0108(10) 0.6166(6) 0.2781(6) 0.033(2) Uani 1 1 d . B . H30 H 0.0626 0.6111 0.3153 0.039 Uiso 1 1 calc R . . C31 C 0.2299(9) 0.4478(6) 0.3583(6) 0.029(2) Uani 1 1 d . . . C32 C 0.1302(8) 0.4384(6) 0.4240(5) 0.0276(19) Uani 1 1 d . B . H32 H 0.0456 0.4475 0.4148 0.033 Uiso 1 1 calc R . . C33 C 0.1534(9) 0.4157(6) 0.5031(6) 0.037(2) Uani 1 1 d . . . H33 H 0.0843 0.4099 0.5490 0.045 Uiso 1 1 calc R B . C34 C 0.2772(11) 0.4011(7) 0.5168(6) 0.041(2) Uani 1 1 d . B . H34 H 0.2930 0.3838 0.5722 0.049 Uiso 1 1 calc R . . C35 C 0.3750(10) 0.4113(7) 0.4519(7) 0.040(2) Uani 1 1 d . . . H35 H 0.4595 0.4022 0.4614 0.047 Uiso 1 1 calc R B . C36 C 0.3526(9) 0.4349(6) 0.3718(6) 0.033(2) Uani 1 1 d . B . H36 H 0.4216 0.4424 0.3258 0.039 Uiso 1 1 calc R . . C37 C 0.6005(8) 0.0789(6) 0.2458(6) 0.029(2) Uani 1 1 d . . . C38 C 0.6835(12) 0.0530(7) 0.1835(7) 0.050(3) Uani 1 1 d . . . H38 H 0.7414 0.0897 0.1440 0.060 Uiso 1 1 calc R . . C39 C 0.6812(14) -0.0306(8) 0.1791(8) 0.065(4) Uani 1 1 d . . . H39 H 0.7395 -0.0516 0.1381 0.078 Uiso 1 1 calc R . . C40 C 0.5923(12) -0.0799(8) 0.2359(7) 0.053(3) Uani 1 1 d . . . H40 H 0.5854 -0.1325 0.2304 0.063 Uiso 1 1 calc R . . C41 C 0.5134(10) -0.0557(6) 0.3001(7) 0.042(3) Uani 1 1 d . . . H41 H 0.4579 -0.0938 0.3410 0.050 Uiso 1 1 calc R . . C42 C 0.5157(9) 0.0247(6) 0.3045(7) 0.037(2) Uani 1 1 d . . . H42 H 0.4595 0.0432 0.3476 0.044 Uiso 1 1 calc R . . C43 C 0.7236(8) 0.2301(6) 0.1724(6) 0.0271(19) Uani 1 1 d . . . C44 C 0.8531(10) 0.1893(8) 0.1819(7) 0.048(3) Uani 1 1 d . . . H44 H 0.8748 0.1365 0.2320 0.057 Uiso 1 1 calc R . . C45 C 0.9486(10) 0.2241(9) 0.1204(8) 0.058(3) Uani 1 1 d . . . H45 H 1.0365 0.1969 0.1277 0.069 Uiso 1 1 calc R . . C46 C 0.9153(12) 0.3002(8) 0.0465(7) 0.055(3) Uani 1 1 d . . . H46 H 0.9816 0.3251 0.0035 0.066 Uiso 1 1 calc R . . C47 C 0.7934(13) 0.3388(9) 0.0345(8) 0.072(4) Uani 1 1 d . . . H47 H 0.7737 0.3890 -0.0175 0.086 Uiso 1 1 calc R . . C48 C 0.6948(11) 0.3065(8) 0.0973(7) 0.053(3) Uani 1 1 d . . . H48 H 0.6076 0.3363 0.0894 0.064 Uiso 1 1 calc R . . C49 C 0.6460(9) 0.1510(6) 0.3541(6) 0.034(2) Uani 1 1 d . . . C50 C 0.6346(9) 0.2202(6) 0.3805(6) 0.034(2) Uani 1 1 d . . . H50 H 0.5994 0.2829 0.3464 0.041 Uiso 1 1 calc R . . C51 C 0.6734(9) 0.1999(6) 0.4551(6) 0.037(2) Uani 1 1 d . . . H51 H 0.6642 0.2478 0.4728 0.044 Uiso 1 1 calc R . . C52 C 0.7258(11) 0.1089(7) 0.5037(6) 0.042(3) Uani 1 1 d . . . H52 H 0.7544 0.0937 0.5549 0.051 Uiso 1 1 calc R . . C53 C 0.7365(11) 0.0399(7) 0.4778(7) 0.045(3) Uani 1 1 d . . . H53 H 0.7703 -0.0228 0.5124 0.054 Uiso 1 1 calc R . . C54 C 0.6996(10) 0.0601(6) 0.4040(6) 0.039(2) Uani 1 1 d . . . H54 H 0.7105 0.0118 0.3863 0.047 Uiso 1 1 calc R . . C55 C 0.861(3) 0.1106(19) 0.8884(17) 0.167(10) Uiso 1 1 d . . . H55A H 0.8002 0.0700 0.9236 0.200 Uiso 1 1 calc R . . H55B H 0.8122 0.1667 0.8469 0.200 Uiso 1 1 calc R . . C56 C 0.384(2) 0.1696(18) 0.9766(16) 0.150(9) Uiso 1 1 d . . . H56A H 0.4243 0.1809 0.9171 0.180 Uiso 1 1 calc R . . H56B H 0.3457 0.2309 0.9799 0.180 Uiso 1 1 calc R . . Au1 Au 0.39923(3) 0.28341(2) 0.24659(2) 0.02924(11) Uani 1 1 d . . . Au2 Au 0.18933(3) 0.39237(2) 0.12691(2) 0.02953(11) Uani 1 1 d . . . Cl1 Cl 0.1738(3) 0.4199(2) -0.00679(16) 0.0461(6) Uani 1 1 d . . . Cl2 Cl 0.9012(10) 0.1441(6) 0.9527(5) 0.214(4) Uani 1 1 d . . . Cl3 Cl 0.9736(9) 0.0562(6) 0.8350(5) 0.189(3) Uani 1 1 d . . . Cl4 Cl 0.4922(14) 0.1171(15) 1.0332(11) 0.61(2) Uani 1 1 d . . . Cl5 Cl 0.2645(13) 0.1199(8) 0.9979(7) 0.247(5) Uani 1 1 d . . . F1 F 0.7817(7) 0.3047(6) 0.6789(6) 0.081(2) Uani 1 1 d . . . F2 F 0.5381(7) 0.3890(5) 0.6808(6) 0.092(3) Uani 1 1 d . . . F3 F 0.6709(9) 0.3642(6) 0.5434(5) 0.094(3) Uani 1 1 d . . . F4 F 0.4976(7) 0.2681(5) 0.6363(5) 0.068(2) Uani 1 1 d . . . F5 F 0.6052(10) 0.2102(6) 0.7686(5) 0.099(3) Uani 1 1 d . . . F6 F 0.7428(7) 0.1904(5) 0.6303(6) 0.079(2) Uani 1 1 d . . . N1A N 0.2160(9) 0.1675(7) 0.2414(6) 0.046(2) Uiso 0.50 1 d P C 2 N1B N 0.4172(18) 0.4944(13) 0.1189(13) 0.036(5) Uiso 0.50 1 d P B 2 P1 P 0.1983(2) 0.46886(15) 0.25639(15) 0.0275(5) Uani 1 1 d . A . P2 P 0.1028(2) 0.29393(16) 0.32197(16) 0.0302(5) Uani 1 1 d . . . P3 P 0.5969(2) 0.18528(15) 0.25272(15) 0.0265(5) Uani 1 1 d . . . Sb1 Sb 0.63902(7) 0.28867(5) 0.65878(5) 0.0460(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(4) 0.028(4) 0.035(5) -0.015(4) -0.002(4) -0.005(4) C2 0.034(5) 0.025(5) 0.053(6) -0.016(4) -0.020(5) -0.003(4) C3 0.041(6) 0.022(4) 0.057(7) -0.013(5) -0.021(5) -0.005(4) C4 0.046(7) 0.036(6) 0.081(9) -0.008(6) -0.038(7) -0.014(5) C5 0.064(8) 0.030(5) 0.069(8) -0.015(6) -0.041(7) -0.002(5) C6 0.053(7) 0.028(5) 0.068(8) -0.027(5) -0.034(6) 0.012(5) C7 0.030(5) 0.023(4) 0.042(5) -0.016(4) -0.008(4) -0.003(4) C8 0.035(5) 0.022(4) 0.048(6) -0.014(4) -0.007(5) -0.006(4) C9 0.049(6) 0.019(4) 0.056(7) -0.010(5) -0.023(5) -0.001(4) C10 0.056(7) 0.022(5) 0.036(6) -0.009(4) -0.015(5) -0.006(4) C11 0.048(6) 0.030(5) 0.040(6) -0.012(4) -0.005(5) -0.013(5) C12 0.034(5) 0.032(5) 0.035(5) -0.010(4) -0.004(4) -0.007(4) C13 0.025(5) 0.028(5) 0.051(6) -0.014(5) -0.008(4) -0.008(4) C14 0.043(6) 0.031(5) 0.044(6) -0.007(5) -0.014(5) -0.011(4) C15 0.035(6) 0.029(5) 0.062(7) -0.012(5) 0.000(5) -0.003(4) C16 0.023(5) 0.045(6) 0.062(7) -0.009(6) -0.015(5) -0.007(4) C17 0.031(5) 0.037(5) 0.059(7) -0.014(5) -0.018(5) -0.009(4) C18 0.031(5) 0.023(4) 0.047(6) -0.007(4) -0.013(4) -0.011(4) C19 0.036(5) 0.031(5) 0.030(5) -0.010(4) -0.006(4) -0.013(4) C22 0.044(7) 0.062(8) 0.056(8) -0.013(6) 0.000(6) -0.016(6) C25 0.037(5) 0.025(4) 0.026(5) -0.008(4) -0.004(4) -0.008(4) C26 0.038(5) 0.024(4) 0.033(5) -0.010(4) -0.012(4) -0.007(4) C27 0.043(6) 0.026(5) 0.041(6) -0.008(4) -0.016(5) -0.002(4) C28 0.043(6) 0.029(5) 0.044(6) -0.016(5) -0.012(5) 0.009(4) C29 0.053(7) 0.033(5) 0.044(6) -0.017(5) -0.013(5) -0.002(5) C30 0.053(6) 0.028(5) 0.024(5) -0.008(4) -0.014(4) -0.014(4) C31 0.033(5) 0.019(4) 0.040(5) -0.013(4) -0.012(4) -0.004(4) C32 0.026(4) 0.023(4) 0.027(5) -0.006(4) -0.007(4) -0.001(4) C33 0.031(5) 0.030(5) 0.045(6) -0.015(5) -0.004(4) -0.001(4) C34 0.061(7) 0.031(5) 0.029(5) -0.009(4) -0.014(5) -0.007(5) C35 0.039(6) 0.037(5) 0.050(6) -0.017(5) -0.021(5) -0.006(4) C36 0.029(5) 0.028(5) 0.038(5) -0.007(4) -0.011(4) -0.007(4) C37 0.029(5) 0.031(5) 0.032(5) -0.014(4) -0.010(4) -0.005(4) C38 0.067(8) 0.045(6) 0.048(7) -0.023(5) 0.005(6) -0.032(6) C39 0.088(10) 0.053(7) 0.073(9) -0.042(7) 0.007(7) -0.032(7) C40 0.071(8) 0.046(6) 0.061(8) -0.026(6) -0.013(6) -0.028(6) C41 0.033(5) 0.026(5) 0.063(7) -0.019(5) -0.006(5) -0.003(4) C42 0.036(5) 0.028(5) 0.047(6) -0.018(4) -0.002(5) -0.008(4) C43 0.030(5) 0.022(4) 0.032(5) -0.006(4) -0.014(4) -0.010(4) C44 0.036(6) 0.054(7) 0.040(6) 0.001(5) -0.011(5) -0.019(5) C45 0.030(6) 0.078(9) 0.064(8) -0.024(7) -0.008(5) -0.017(6) C46 0.055(7) 0.052(7) 0.049(7) -0.012(6) 0.007(6) -0.028(6) C47 0.064(9) 0.057(8) 0.045(7) 0.009(6) 0.009(6) -0.009(7) C48 0.039(6) 0.054(7) 0.040(6) -0.004(5) -0.008(5) 0.001(5) C49 0.038(5) 0.030(5) 0.029(5) 0.002(4) -0.012(4) -0.016(4) C50 0.038(5) 0.027(5) 0.045(6) -0.016(4) -0.014(4) -0.009(4) C51 0.042(6) 0.029(5) 0.048(6) -0.021(5) -0.015(5) -0.004(4) C52 0.061(7) 0.043(6) 0.026(5) -0.010(5) -0.018(5) -0.013(5) C53 0.068(7) 0.022(5) 0.047(6) -0.007(4) -0.031(6) -0.003(5) C54 0.051(6) 0.025(5) 0.049(6) -0.020(5) -0.015(5) -0.004(4) Au1 0.02536(19) 0.02939(19) 0.0357(2) -0.01530(16) -0.00911(15) -0.00268(14) Au2 0.02695(19) 0.03048(19) 0.0348(2) -0.01405(16) -0.00712(15) -0.00764(15) Cl1 0.0432(14) 0.0627(17) 0.0359(14) -0.0175(12) -0.0055(11) -0.0203(13) Cl2 0.308(12) 0.194(8) 0.143(6) -0.090(6) -0.047(7) -0.017(8) Cl3 0.207(8) 0.209(8) 0.173(7) -0.122(6) -0.051(6) 0.009(6) Cl4 0.256(14) 0.69(3) 0.42(2) 0.34(2) -0.176(15) -0.227(19) Cl5 0.325(14) 0.243(11) 0.222(10) -0.128(9) -0.071(9) -0.050(10) F1 0.059(5) 0.098(6) 0.134(7) -0.081(6) -0.025(5) -0.018(4) F2 0.067(5) 0.056(4) 0.152(8) -0.058(5) 0.017(5) -0.014(4) F3 0.116(7) 0.084(6) 0.073(5) -0.008(5) -0.004(5) -0.059(5) F4 0.056(4) 0.060(4) 0.089(5) -0.017(4) -0.033(4) -0.015(3) F5 0.152(9) 0.084(6) 0.073(6) -0.007(5) -0.037(6) -0.061(6) F6 0.072(5) 0.067(5) 0.131(7) -0.069(5) -0.045(5) 0.010(4) P1 0.0285(12) 0.0238(11) 0.0336(13) -0.0117(10) -0.0092(10) -0.0064(9) P2 0.0257(12) 0.0244(11) 0.0420(14) -0.0129(11) -0.0106(11) -0.0037(9) P3 0.0267(12) 0.0230(11) 0.0297(12) -0.0099(10) -0.0067(10) -0.0047(9) Sb1 0.0415(4) 0.0301(3) 0.0674(5) -0.0193(3) -0.0155(4) -0.0039(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 P2 1.754(9) . y C1 P1 1.758(9) . y C1 Au2 2.080(9) . y C1 Au1 2.127(8) . y C01 C2 1.394(14) . y C01 C6 1.422(14) . y C2 C3 1.383(13) . y C2 P2 1.817(9) . y C3 C4 1.425(14) . y C4 C5 1.341(17) . y C5 C6 1.341(16) . y C7 C8 1.391(13) . y C7 C12 1.400(13) . y C7 P2 1.828(10) . y C8 C9 1.383(14) . y C9 C10 1.378(14) . y C10 C11 1.395(14) . y C11 C12 1.366(14) . y C13 C14 1.387(14) . y C13 C18 1.392(14) . y C13 P2 1.803(9) . y C14 C15 1.380(14) . y C15 C16 1.376(16) . y C16 C17 1.374(16) . y C17 C18 1.374(13) . y C19 C20B 1.19(2) . y C19 C24B 1.37(3) . y C19 C23A 1.42(2) . y C19 N1B 1.46(2) . y C19 P1 1.826(9) . y C20B C21B 1.36(4) . y C21A C22 1.30(2) . y C21A N1B 1.39(3) . y C21B C22 1.43(3) . y C22 C23B 1.37(4) . y C22 C24A 1.40(2) . y C23A C24A 1.38(3) . y C23B C24B 1.41(4) . y C25 C26 1.377(12) . y C25 C30 1.380(13) . y C25 P1 1.826(9) . y C26 C27 1.373(13) . y C27 C28 1.377(14) . y C28 C29 1.370(14) . y C29 C30 1.397(14) . y C31 C32 1.365(12) . y C31 C36 1.380(12) . y C31 P1 1.805(9) . y C32 C33 1.365(13) . y C33 C34 1.386(14) . y C34 C35 1.342(14) . y C35 C36 1.376(13) . y C37 C38 1.373(14) . y C37 C42 1.398(13) . y C37 P3 1.813(9) . y C38 C39 1.435(15) . y C39 C40 1.379(16) . y C40 C41 1.372(15) . y C41 C42 1.383(13) . y C43 C44 1.396(13) . y C43 C48 1.397(13) . y C43 P3 1.790(9) . y C44 C45 1.361(15) . y C45 C46 1.393(16) . y C46 C47 1.326(17) . y C47 C48 1.381(16) . y C49 C54 1.387(12) . y C49 C50 1.388(13) . y C49 P3 1.820(9) . y C50 C51 1.374(13) . y C51 C52 1.379(13) . y C52 C53 1.378(14) . y C53 C54 1.351(14) . y C55 Cl3 1.64(3) . y C55 Cl2 1.69(3) . y C56 Cl4 1.56(3) . y C56 Cl5 1.65(3) . y Au1 P3 2.265(2) . y Au1 Au2 3.1274(6) . y Au2 Cl1 2.267(3) . y F1 Sb1 1.839(7) . y F2 Sb1 1.824(7) . y F3 Sb1 1.873(8) . y F4 Sb1 1.887(7) . y F5 Sb1 1.817(8) . y F6 Sb1 1.859(7) . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 C1 P1 119.3(5) . . y P2 C1 Au2 109.2(4) . . y P1 C1 Au2 109.3(4) . . y P2 C1 Au1 109.4(4) . . y P1 C1 Au1 111.1(4) . . y Au2 C1 Au1 96.0(4) . . y C2 C01 C6 117.9(10) . . y C3 C2 C01 120.2(9) . . y C3 C2 P2 115.6(8) . . y C01 C2 P2 124.2(8) . . y C2 C3 C4 118.9(11) . . y C5 C4 C3 120.5(11) . . y C6 C5 C4 121.1(11) . . y C5 C6 C01 121.3(11) . . y C8 C7 C12 119.8(9) . . y C8 C7 P2 118.2(7) . . y C12 C7 P2 121.7(7) . . y C9 C8 C7 119.3(9) . . y C10 C9 C8 121.7(10) . . y C9 C10 C11 117.9(9) . . y C12 C11 C10 122.0(10) . . y C11 C12 C7 119.2(9) . . y C14 C13 C18 120.0(9) . . y C14 C13 P2 122.3(8) . . y C18 C13 P2 117.3(8) . . y C15 C14 C13 119.6(10) . . y C16 C15 C14 120.0(11) . . y C17 C16 C15 120.7(10) . . y C16 C17 C18 119.9(10) . . y C17 C18 C13 119.8(10) . . y C20B C19 C24B 124.4(19) . . y C20B C19 C23A 115.7(16) . . y C24B C19 N1B 117.9(16) . . y C23A C19 N1B 118.1(12) . . y C20B C19 P1 121.7(13) . . y C24B C19 P1 113.7(14) . . y C23A C19 P1 116.0(10) . . y N1B C19 P1 125.8(9) . . y C19 C20B C21B 123(2) . . y C22 C21A N1B 121(2) . . y C20B C21B C22 120(2) . . y C21A C22 C23B 119(2) . . y C21A C22 C24A 125.6(16) . . y C23B C22 C21B 115(2) . . y C24A C22 C21B 113.7(16) . . y C24A C23A C19 121.4(18) . . y C22 C23B C24B 122(3) . . y C23A C24A C22 116.0(18) . . y C19 C24B C23B 116(3) . . y C26 C25 C30 120.5(9) . . y C26 C25 P1 121.5(7) . . y C30 C25 P1 118.0(7) . . y C27 C26 C25 119.8(9) . . y C26 C27 C28 120.6(10) . . y C29 C28 C27 119.8(9) . . y C28 C29 C30 120.3(10) . . y C25 C30 C29 119.0(9) . . y C32 C31 C36 120.2(9) . . y C32 C31 P1 118.1(7) . . y C36 C31 P1 121.6(7) . . y C33 C32 C31 119.4(9) . . y C32 C33 C34 120.3(9) . . y C35 C34 C33 120.3(9) . . y C34 C35 C36 119.9(9) . . y C35 C36 C31 119.9(9) . . y C38 C37 C42 120.8(9) . . y C38 C37 P3 120.7(7) . . y C42 C37 P3 118.5(7) . . y C37 C38 C39 118.9(10) . . y C40 C39 C38 118.5(11) . . y C41 C40 C39 122.3(10) . . y C40 C41 C42 119.2(10) . . y C41 C42 C37 120.2(9) . . y C44 C43 C48 118.2(9) . . y C44 C43 P3 121.5(7) . . y C48 C43 P3 120.4(7) . . y C45 C44 C43 121.0(10) . . y C44 C45 C46 118.8(10) . . y C47 C46 C45 121.6(11) . . y C46 C47 C48 120.4(11) . . y C47 C48 C43 119.9(10) . . y C54 C49 C50 118.5(9) . . y C54 C49 P3 123.5(8) . . y C50 C49 P3 118.0(7) . . y C51 C50 C49 121.2(9) . . y C50 C51 C52 119.1(9) . . y C53 C52 C51 119.8(9) . . y C54 C53 C52 121.1(9) . . y C53 C54 C49 120.3(9) . . y Cl3 C55 Cl2 119.8(17) . . y Cl4 C56 Cl5 117.9(18) . . y C1 Au1 P3 174.6(2) . . y C1 Au1 Au2 41.4(2) . . y P3 Au1 Au2 140.52(6) . . y C1 Au2 Cl1 178.8(2) . . y C1 Au2 Au1 42.5(2) . . y Cl1 Au2 Au1 136.34(7) . . y C21A N1B C19 117.4(16) . . y C1 P1 C31 111.3(4) . . y C1 P1 C25 116.1(4) . . y C31 P1 C25 107.0(4) . . y C1 P1 C19 111.7(4) . . y C31 P1 C19 105.4(4) . . y C25 P1 C19 104.5(4) . . y C1 P2 C13 111.1(4) . . y C1 P2 C2 112.8(5) . . y C13 P2 C2 104.9(4) . . y C1 P2 C7 114.4(4) . . y C13 P2 C7 109.8(5) . . y C2 P2 C7 103.2(4) . . y C43 P3 C37 105.0(4) . . y C43 P3 C49 106.6(4) . . y C37 P3 C49 106.3(4) . . y C43 P3 Au1 115.9(3) . . y C37 P3 Au1 113.0(3) . . y C49 P3 Au1 109.5(3) . . y F5 Sb1 F2 91.9(4) . . y F5 Sb1 F1 91.7(4) . . y F2 Sb1 F1 90.8(4) . . y F5 Sb1 F6 91.1(4) . . y F2 Sb1 F6 177.0(4) . . y F1 Sb1 F6 89.5(3) . . y F5 Sb1 F3 176.1(4) . . y F2 Sb1 F3 90.7(4) . . y F1 Sb1 F3 91.3(4) . . y F6 Sb1 F3 86.4(4) . . y F5 Sb1 F4 88.6(4) . . y F2 Sb1 F4 91.7(4) . . y F1 Sb1 F4 177.4(3) . . y F6 Sb1 F4 88.0(3) . . y F3 Sb1 F4 88.3(4) . . y _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.78 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.232 _refine_diff_density_min -1.984 _refine_diff_density_rms 0.208 data_9 _database_code_depnum_ccdc_archive 'CCDC 914767' _audit_creation_date 2012-12-07 _audit_block_code MEG-GL-051-03_7819 _chemical_name_systematic ; (mu-2-(2,3-bis(diisopropylamino)cycloprop-1(3)-en-2-ylium-1-yl- (2,4,6-triisopropyl-phenyl)-phosphanide)-dichloro-di-gold diethylether solute ; _chemical_melting_point ? _chemical_compound_source dichloromethane,diethylether _chemical_formula_moiety 'C30 H51 Au2 Cl2 N2 P, C4 H10 O' _chemical_formula_sum 'C34 H61 Au2 Cl2 N2 O P' _chemical_formula_weight 1009.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 21/n' _symmetry_space_group_name_Hall '-p 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2004(15) _cell_length_b 18.010(2) _cell_length_c 17.840(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.719(2) _cell_angle_gamma 90.00 _cell_volume 3893.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9130 _cell_measurement_theta_min 2.4244 _cell_measurement_theta_max 30.9659 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 0.00 -1.00 0.0500 1.00 0.00 1.00 0.0600 0.00 1.00 1.00 0.0500 0.00 -1.00 -1.00 0.0500 0.00 1.00 -1.00 0.0300 0.00 -1.00 1.00 0.0300 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.723 _exptl_crystal_density_method ? _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 7.733 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.35063 _exptl_absorpt_correction_T_max 0.67230 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_special_details ; Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75 ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_monochromator 'Incoatec Helios mirrors' _diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 66.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 112428 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 31.02 _reflns_number_total 12388 _reflns_number_gt 11258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT software (Bruker AXS, 2004)' _computing_data_reduction 'SAINT software (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The minimum and maximum estimated transmissions from the multi-scan scaling are 0.3773 and 0.6639 (SADABS). The crystal contains diethylether solute. Highest peak 1.93 at 0.3945 0.1315 0.7179 [ 0.68 A from AU2 ] Deepest hole -1.22 at 0.5211 -0.0013 0.3586 [ 0.73 A from CL2 ] ; _iucr_refine_instructions_details ; TITL 7819sadabs CELL 0.71073 12.2004 18.0104 17.8401 90 96.719 90 ZERR 4 0.0015 0.0022 0.0022 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Au Cl N O P UNIT 136 244 8 8 8 4 4 LIST 4 L.S. 4 PLAN 20 TEMP -173 BOND $H fmap 2 acta WGHT 0.014700 3.718400 WGHT 0.0146 3.7346 FVAR 0.05466 AU1 3 0.955995 0.812616 0.798623 11.00000 0.01582 0.01169 = 0.01463 -0.00030 0.00081 0.00151 AU2 3 1.054973 0.618662 0.788753 11.00000 0.02297 0.01216 = 0.01319 0.00127 -0.00008 0.00471 C1 1 0.907780 0.719137 0.654109 11.00000 0.01430 0.01155 = 0.01497 0.00089 0.00183 -0.00046 C2 1 0.848099 0.759162 0.597348 11.00000 0.01210 0.01374 = 0.01388 -0.00058 0.00056 -0.00059 C3 1 0.810647 0.688794 0.618575 11.00000 0.01532 0.01208 = 0.01556 0.00029 0.00190 0.00009 C4 1 0.756977 0.568215 0.662874 11.00000 0.01931 0.01368 = 0.02332 0.00438 0.00193 -0.00367 AFIX 13 H4 2 0.692956 0.534133 0.649539 11.00000 -1.20000 AFIX 0 C5 1 0.860367 0.525899 0.648292 11.00000 0.02443 0.01499 = 0.02879 0.00039 0.00131 -0.00027 AFIX 137 H5A 2 0.863389 0.478636 0.675676 11.00000 -1.50000 H5B 2 0.925772 0.555543 0.665718 11.00000 -1.50000 H5C 2 0.858514 0.516271 0.594093 11.00000 -1.50000 AFIX 0 C6 1 0.755673 0.589973 0.745009 11.00000 0.02518 0.02689 = 0.02380 0.00663 0.00553 -0.00071 AFIX 137 H6A 2 0.816344 0.624544 0.759939 11.00000 -1.50000 H6B 2 0.764595 0.545468 0.776742 11.00000 -1.50000 H6C 2 0.685239 0.613946 0.751347 11.00000 -1.50000 AFIX 0 C7 1 0.640187 0.635378 0.555413 11.00000 0.01523 0.02018 = 0.01992 0.00090 -0.00264 -0.00434 AFIX 13 H7 2 0.636843 0.685239 0.530588 11.00000 -1.20000 AFIX 0 C8 1 0.652854 0.577590 0.494764 11.00000 0.02686 0.02949 = 0.02261 -0.00597 -0.00169 -0.00411 AFIX 137 H8A 2 0.589982 0.580843 0.455333 11.00000 -1.50000 H8B 2 0.655349 0.527913 0.517312 11.00000 -1.50000 H8C 2 0.721386 0.586810 0.472599 11.00000 -1.50000 AFIX 0 C9 1 0.533536 0.625135 0.591276 11.00000 0.01740 0.02931 = 0.02766 0.00111 0.00059 -0.00408 AFIX 137 H9A 2 0.532586 0.575537 0.613783 11.00000 -1.50000 H9B 2 0.470144 0.630538 0.552527 11.00000 -1.50000 H9C 2 0.529425 0.662756 0.630536 11.00000 -1.50000 AFIX 0 C10 1 0.757000 0.840420 0.497090 11.00000 0.01417 0.02016 = 0.01818 0.00625 -0.00198 0.00109 AFIX 13 H10 2 0.779360 0.888157 0.474614 11.00000 -1.20000 AFIX 0 C11 1 0.751612 0.782631 0.435096 11.00000 0.02288 0.02941 = 0.01652 0.00328 -0.00188 0.00047 AFIX 137 H11A 2 0.696160 0.797375 0.393543 11.00000 -1.50000 H11B 2 0.731308 0.734507 0.455081 11.00000 -1.50000 H11C 2 0.823882 0.778620 0.416549 11.00000 -1.50000 AFIX 0 C12 1 0.646758 0.854393 0.526149 11.00000 0.01566 0.02859 = 0.02552 0.00566 0.00073 0.00410 AFIX 137 H12A 2 0.618951 0.807855 0.545220 11.00000 -1.50000 H12B 2 0.593904 0.873309 0.484984 11.00000 -1.50000 H12C 2 0.656247 0.891036 0.567003 11.00000 -1.50000 AFIX 0 C13 1 0.931160 0.877735 0.583703 11.00000 0.01555 0.01159 = 0.02275 0.00314 -0.00231 -0.00170 AFIX 13 H13 2 0.981135 0.855242 0.626098 11.00000 -1.20000 AFIX 0 C14 1 1.000966 0.894735 0.520808 11.00000 0.02031 0.02319 = 0.03460 0.00572 0.00655 -0.00390 AFIX 137 H14A 2 1.061689 0.927818 0.539851 11.00000 -1.50000 H14B 2 0.955206 0.918958 0.479019 11.00000 -1.50000 H14C 2 1.031095 0.848411 0.502926 11.00000 -1.50000 AFIX 0 C15 1 0.880389 0.946700 0.614525 11.00000 0.02644 0.01622 = 0.03338 -0.00180 0.00109 0.00094 AFIX 137 H15A 2 0.830123 0.970018 0.574477 11.00000 -1.50000 H15B 2 0.938998 0.981791 0.632561 11.00000 -1.50000 H15C 2 0.839301 0.932774 0.656416 11.00000 -1.50000 AFIX 0 C16 1 1.134353 0.753708 0.669558 11.00000 0.01253 0.01252 = 0.01344 0.00019 -0.00101 0.00183 C17 1 1.148097 0.714187 0.602780 11.00000 0.01349 0.01267 = 0.01522 -0.00090 -0.00112 0.00022 C18 1 1.220516 0.741439 0.554132 11.00000 0.01601 0.01551 = 0.01621 -0.00338 0.00133 0.00051 AFIX 43 H18 2 1.228597 0.714932 0.509069 11.00000 -1.20000 AFIX 0 C19 1 1.281023 0.806086 0.569661 11.00000 0.01371 0.01645 = 0.01491 0.00018 0.00111 0.00088 C20 1 1.273597 0.840511 0.638693 11.00000 0.01504 0.01524 = 0.01645 -0.00121 0.00029 -0.00221 AFIX 43 H20 2 1.318193 0.882895 0.651610 11.00000 -1.20000 AFIX 0 C21 1 1.203515 0.815514 0.689796 11.00000 0.01282 0.01309 = 0.01432 -0.00053 -0.00041 0.00069 C22 1 1.210286 0.856169 0.765156 11.00000 0.01781 0.01441 = 0.01494 -0.00207 0.00080 -0.00241 AFIX 13 H22 2 1.167202 0.827002 0.799374 11.00000 -1.20000 AFIX 0 C23 1 1.330216 0.861140 0.802461 11.00000 0.01795 0.02714 = 0.01864 -0.00269 -0.00260 -0.00308 AFIX 137 H23A 2 1.371361 0.896019 0.774182 11.00000 -1.50000 H23B 2 1.364644 0.811981 0.802421 11.00000 -1.50000 H23C 2 1.331084 0.878588 0.854559 11.00000 -1.50000 AFIX 0 C24 1 1.159510 0.933881 0.756301 11.00000 0.02348 0.01811 = 0.02311 -0.00371 0.00242 0.00060 AFIX 137 H24A 2 1.082687 0.929995 0.733428 11.00000 -1.50000 H24B 2 1.201447 0.963958 0.723819 11.00000 -1.50000 H24C 2 1.161901 0.957427 0.805989 11.00000 -1.50000 AFIX 0 C25 1 1.353537 0.840840 0.515640 11.00000 0.01444 0.01878 = 0.01651 -0.00130 0.00162 -0.00299 AFIX 13 H25 2 1.423121 0.857746 0.546051 11.00000 -1.20000 AFIX 0 C26 1 1.297156 0.909460 0.477868 11.00000 0.02354 0.02139 = 0.02189 0.00419 0.00303 -0.00081 AFIX 137 H26A 2 1.278773 0.944280 0.516721 11.00000 -1.50000 H26B 2 1.229462 0.894426 0.446503 11.00000 -1.50000 H26C 2 1.347162 0.933579 0.446215 11.00000 -1.50000 AFIX 0 C27 1 1.385552 0.787758 0.455548 11.00000 0.02141 0.02715 = 0.02064 -0.00483 0.00628 -0.00299 AFIX 137 H27A 2 1.319091 0.771945 0.423300 11.00000 -1.50000 H27B 2 1.422472 0.744221 0.479878 11.00000 -1.50000 H27C 2 1.435718 0.812911 0.424749 11.00000 -1.50000 AFIX 0 C28 1 1.093668 0.639783 0.582558 11.00000 0.01952 0.01213 = 0.01794 -0.00291 0.00241 -0.00194 AFIX 13 H28 2 1.039416 0.630196 0.619335 11.00000 -1.20000 AFIX 0 C29 1 1.179983 0.577798 0.592091 11.00000 0.03086 0.01459 = 0.04299 -0.00231 0.00333 0.00377 AFIX 137 H29A 2 1.218347 0.579121 0.643502 11.00000 -1.50000 H29B 2 1.233452 0.584945 0.555789 11.00000 -1.50000 H29C 2 1.143421 0.529637 0.583086 11.00000 -1.50000 AFIX 0 C30 1 1.030043 0.638198 0.503085 11.00000 0.03088 0.02453 = 0.01908 -0.00436 -0.00058 -0.00858 AFIX 137 H30A 2 1.082195 0.641747 0.465423 11.00000 -1.50000 H30B 2 0.978716 0.680211 0.497138 11.00000 -1.50000 H30C 2 0.988597 0.591625 0.495953 11.00000 -1.50000 AFIX 0 C31 1 0.506544 0.679254 0.824225 11.00000 0.03636 0.03545 = 0.02683 0.00186 0.00997 0.00976 AFIX 23 H31A 2 0.482947 0.710452 0.865123 11.00000 -1.20000 H31B 2 0.570383 0.648854 0.845388 11.00000 -1.20000 AFIX 0 C32 1 0.412475 0.629402 0.791844 11.00000 0.05446 0.03534 = 0.04363 -0.00601 0.01774 -0.00893 AFIX 137 H32A 2 0.438259 0.596238 0.754034 11.00000 -1.50000 H32B 2 0.351591 0.659971 0.768125 11.00000 -1.50000 H32C 2 0.386814 0.599797 0.832459 11.00000 -1.50000 AFIX 0 C33 1 0.616457 0.778948 0.791373 11.00000 0.02610 0.04186 = 0.02460 -0.00173 -0.00006 -0.00042 AFIX 23 H33A 2 0.685488 0.754666 0.813641 11.00000 -1.20000 H33B 2 0.588554 0.810540 0.830410 11.00000 -1.20000 AFIX 0 C34 1 0.637497 0.824985 0.724523 11.00000 0.02800 0.03802 = 0.02384 0.00229 0.00645 0.00095 AFIX 137 H34A 2 0.664031 0.792979 0.686041 11.00000 -1.50000 H34B 2 0.693347 0.862719 0.740284 11.00000 -1.50000 H34C 2 0.568869 0.849351 0.703543 11.00000 -1.50000 AFIX 0 CL1 4 0.875551 0.896168 0.872707 11.00000 0.02971 0.01920 = 0.02536 -0.00529 0.00222 0.00912 CL2 4 1.078510 0.513699 0.860416 11.00000 0.08925 0.02043 = 0.02583 0.00931 0.00756 0.02313 N1 5 0.844507 0.821711 0.559303 11.00000 0.01291 0.01369 = 0.01789 0.00376 -0.00243 -0.00117 N2 5 0.738429 0.634774 0.613195 11.00000 0.01550 0.01493 = 0.01835 0.00138 -0.00082 -0.00351 O1 6 0.536282 0.724504 0.765200 11.00000 0.02815 0.03185 = 0.02368 -0.00154 0.00239 0.00148 P1 7 1.024311 0.725453 0.726338 11.00000 0.01357 0.01078 = 0.01256 0.00066 -0.00038 0.00021 HKLF 4 REM REM R1 = 0.0148 for 11258 Fo > 4sig(Fo) and 0.0191 for all 12388 data REM 395 parameters refined using 0 restraints END WGHT 0.0146 3.7346 REM Highest difference peak 1.925, deepest hole -1.218, 1-sigma level 0.084 Q1 1 1.1055 0.6315 0.7821 11.00000 0.05 1.93 Q2 1 1.1404 0.5254 0.8599 11.00000 0.05 1.39 Q3 1 0.5666 0.7210 0.8395 11.00000 0.05 1.30 Q4 1 0.9054 0.8051 0.8183 11.00000 0.05 0.97 Q5 1 1.0004 0.6094 0.8244 11.00000 0.05 0.68 Q6 1 1.0177 0.8254 0.7912 11.00000 0.05 0.64 Q7 1 0.9139 0.8107 0.7605 11.00000 0.05 0.58 Q8 1 0.9977 0.8119 0.8381 11.00000 0.05 0.51 Q9 1 0.5473 0.9210 0.7022 11.00000 0.05 0.49 Q10 1 1.3092 0.8193 0.5402 11.00000 0.05 0.46 Q11 1 0.8044 0.5465 0.6599 11.00000 0.05 0.46 Q12 1 1.2304 0.8273 0.6618 11.00000 0.05 0.46 Q13 1 0.6417 0.8097 0.7562 11.00000 0.05 0.46 Q14 1 0.9805 0.6353 0.8003 11.00000 0.05 0.45 Q15 1 0.9002 0.9080 0.5991 11.00000 0.05 0.44 Q16 1 0.9589 0.8848 0.5484 11.00000 0.05 0.43 Q17 1 1.0787 0.7504 0.6996 11.00000 0.05 0.42 Q18 1 1.0530 0.7613 0.7863 11.00000 0.05 0.42 Q19 1 0.8877 0.7506 0.6326 11.00000 0.05 0.42 Q20 1 1.1954 0.8363 0.7257 11.00000 0.05 0.42 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+3.7346P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12388 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0191 _refine_ls_R_factor_gt 0.0148 _refine_ls_wR_factor_ref 0.0351 _refine_ls_wR_factor_gt 0.0336 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.955995(5) 0.812616(3) 0.798623(3) 0.01412(2) Uani 1 1 d . . . Au2 Au 1.054974(6) 0.618662(3) 0.788753(3) 0.01628(2) Uani 1 1 d . . . C1 C 0.90778(14) 0.71914(9) 0.65411(9) 0.0136(3) Uani 1 1 d . . . C2 C 0.84810(13) 0.75916(9) 0.59735(9) 0.0133(3) Uani 1 1 d . . . C3 C 0.81065(14) 0.68879(9) 0.61858(9) 0.0143(3) Uani 1 1 d . . . C4 C 0.75698(15) 0.56822(9) 0.66287(10) 0.0188(3) Uani 1 1 d . . . H4 H 0.6930 0.5341 0.6495 0.023 Uiso 1 1 calc R . . C5 C 0.86037(16) 0.52590(10) 0.64829(11) 0.0229(4) Uani 1 1 d . . . H5A H 0.8634 0.4786 0.6757 0.034 Uiso 1 1 calc R . . H5B H 0.9258 0.5555 0.6657 0.034 Uiso 1 1 calc R . . H5C H 0.8585 0.5163 0.5941 0.034 Uiso 1 1 calc R . . C6 C 0.75567(17) 0.58997(11) 0.74501(11) 0.0251(4) Uani 1 1 d . . . H6A H 0.8164 0.6245 0.7599 0.038 Uiso 1 1 calc R . . H6B H 0.7646 0.5455 0.7767 0.038 Uiso 1 1 calc R . . H6C H 0.6852 0.6140 0.7513 0.038 Uiso 1 1 calc R . . C7 C 0.64019(15) 0.63538(10) 0.55541(10) 0.0188(3) Uani 1 1 d . . . H7 H 0.6368 0.6852 0.5306 0.023 Uiso 1 1 calc R . . C8 C 0.65285(17) 0.57759(12) 0.49476(11) 0.0267(4) Uani 1 1 d . . . H8A H 0.5900 0.5808 0.4553 0.040 Uiso 1 1 calc R . . H8B H 0.6553 0.5279 0.5173 0.040 Uiso 1 1 calc R . . H8C H 0.7214 0.5868 0.4726 0.040 Uiso 1 1 calc R . . C9 C 0.53354(16) 0.62513(11) 0.59128(12) 0.0250(4) Uani 1 1 d . . . H9A H 0.5326 0.5755 0.6138 0.037 Uiso 1 1 calc R . . H9B H 0.4701 0.6305 0.5525 0.037 Uiso 1 1 calc R . . H9C H 0.5294 0.6628 0.6305 0.037 Uiso 1 1 calc R . . C10 C 0.75700(14) 0.84042(10) 0.49709(10) 0.0178(3) Uani 1 1 d . . . H10 H 0.7794 0.8882 0.4746 0.021 Uiso 1 1 calc R . . C11 C 0.75161(16) 0.78263(11) 0.43510(10) 0.0233(4) Uani 1 1 d . . . H11A H 0.6962 0.7974 0.3935 0.035 Uiso 1 1 calc R . . H11B H 0.7313 0.7345 0.4551 0.035 Uiso 1 1 calc R . . H11C H 0.8239 0.7786 0.4165 0.035 Uiso 1 1 calc R . . C12 C 0.64676(15) 0.85439(11) 0.52615(11) 0.0234(4) Uani 1 1 d . . . H12A H 0.6190 0.8079 0.5452 0.035 Uiso 1 1 calc R . . H12B H 0.5939 0.8733 0.4850 0.035 Uiso 1 1 calc R . . H12C H 0.6562 0.8910 0.5670 0.035 Uiso 1 1 calc R . . C13 C 0.93116(14) 0.87774(9) 0.58370(10) 0.0170(3) Uani 1 1 d . . . H13 H 0.9811 0.8552 0.6261 0.020 Uiso 1 1 calc R . . C14 C 1.00097(16) 0.89474(11) 0.52081(12) 0.0258(4) Uani 1 1 d . . . H14A H 1.0617 0.9278 0.5399 0.039 Uiso 1 1 calc R . . H14B H 0.9552 0.9190 0.4790 0.039 Uiso 1 1 calc R . . H14C H 1.0311 0.8484 0.5029 0.039 Uiso 1 1 calc R . . C15 C 0.88039(17) 0.94670(10) 0.61453(12) 0.0255(4) Uani 1 1 d . . . H15A H 0.8301 0.9700 0.5745 0.038 Uiso 1 1 calc R . . H15B H 0.9390 0.9818 0.6326 0.038 Uiso 1 1 calc R . . H15C H 0.8393 0.9328 0.6564 0.038 Uiso 1 1 calc R . . C16 C 1.13435(13) 0.75371(9) 0.66956(9) 0.0130(3) Uani 1 1 d . . . C17 C 1.14810(14) 0.71419(9) 0.60278(9) 0.0140(3) Uani 1 1 d . . . C18 C 1.22052(14) 0.74144(9) 0.55413(9) 0.0160(3) Uani 1 1 d . . . H18 H 1.2286 0.7149 0.5091 0.019 Uiso 1 1 calc R . . C19 C 1.28102(14) 0.80609(9) 0.56966(9) 0.0151(3) Uani 1 1 d . . . C20 C 1.27360(14) 0.84051(9) 0.63869(9) 0.0157(3) Uani 1 1 d . . . H20 H 1.3182 0.8829 0.6516 0.019 Uiso 1 1 calc R . . C21 C 1.20351(13) 0.81551(9) 0.68980(9) 0.0136(3) Uani 1 1 d . . . C22 C 1.21029(14) 0.85617(9) 0.76516(9) 0.0158(3) Uani 1 1 d . . . H22 H 1.1672 0.8270 0.7994 0.019 Uiso 1 1 calc R . . C23 C 1.33022(15) 0.86114(11) 0.80246(10) 0.0216(3) Uani 1 1 d . . . H23A H 1.3714 0.8960 0.7742 0.032 Uiso 1 1 calc R . . H23B H 1.3646 0.8120 0.8024 0.032 Uiso 1 1 calc R . . H23C H 1.3311 0.8786 0.8546 0.032 Uiso 1 1 calc R . . C24 C 1.15951(16) 0.93388(10) 0.75630(11) 0.0216(3) Uani 1 1 d . . . H24A H 1.0827 0.9300 0.7334 0.032 Uiso 1 1 calc R . . H24B H 1.2014 0.9640 0.7238 0.032 Uiso 1 1 calc R . . H24C H 1.1619 0.9574 0.8060 0.032 Uiso 1 1 calc R . . C25 C 1.35354(14) 0.84084(10) 0.51564(9) 0.0166(3) Uani 1 1 d . . . H25 H 1.4231 0.8577 0.5461 0.020 Uiso 1 1 calc R . . C26 C 1.29716(16) 0.90946(10) 0.47787(11) 0.0222(4) Uani 1 1 d . . . H26A H 1.2788 0.9443 0.5167 0.033 Uiso 1 1 calc R . . H26B H 1.2295 0.8944 0.4465 0.033 Uiso 1 1 calc R . . H26C H 1.3472 0.9336 0.4462 0.033 Uiso 1 1 calc R . . C27 C 1.38555(16) 0.78776(11) 0.45555(11) 0.0228(4) Uani 1 1 d . . . H27A H 1.3191 0.7719 0.4233 0.034 Uiso 1 1 calc R . . H27B H 1.4225 0.7442 0.4799 0.034 Uiso 1 1 calc R . . H27C H 1.4357 0.8129 0.4248 0.034 Uiso 1 1 calc R . . C28 C 1.09367(15) 0.63978(9) 0.58256(10) 0.0165(3) Uani 1 1 d . . . H28 H 1.0394 0.6302 0.6193 0.020 Uiso 1 1 calc R . . C29 C 1.17998(18) 0.57780(11) 0.59209(13) 0.0296(4) Uani 1 1 d . . . H29A H 1.2183 0.5791 0.6435 0.044 Uiso 1 1 calc R . . H29B H 1.2334 0.5849 0.5558 0.044 Uiso 1 1 calc R . . H29C H 1.1434 0.5296 0.5831 0.044 Uiso 1 1 calc R . . C30 C 1.03004(18) 0.63820(11) 0.50309(11) 0.0251(4) Uani 1 1 d . . . H30A H 1.0822 0.6417 0.4654 0.038 Uiso 1 1 calc R . . H30B H 0.9787 0.6802 0.4971 0.038 Uiso 1 1 calc R . . H30C H 0.9886 0.5916 0.4960 0.038 Uiso 1 1 calc R . . C31 C 0.5065(2) 0.67925(13) 0.82423(12) 0.0324(5) Uani 1 1 d . . . H31A H 0.4829 0.7105 0.8651 0.039 Uiso 1 1 calc R . . H31B H 0.5704 0.6489 0.8454 0.039 Uiso 1 1 calc R . . C32 C 0.4125(2) 0.62940(14) 0.79184(16) 0.0435(6) Uani 1 1 d . . . H32A H 0.4383 0.5962 0.7540 0.065 Uiso 1 1 calc R . . H32B H 0.3516 0.6600 0.7681 0.065 Uiso 1 1 calc R . . H32C H 0.3868 0.5998 0.8325 0.065 Uiso 1 1 calc R . . C33 C 0.61646(18) 0.77895(13) 0.79137(12) 0.0311(4) Uani 1 1 d . . . H33A H 0.6855 0.7547 0.8136 0.037 Uiso 1 1 calc R . . H33B H 0.5886 0.8105 0.8304 0.037 Uiso 1 1 calc R . . C34 C 0.63750(18) 0.82498(13) 0.72452(12) 0.0297(4) Uani 1 1 d . . . H34A H 0.6640 0.7930 0.6860 0.045 Uiso 1 1 calc R . . H34B H 0.6933 0.8627 0.7403 0.045 Uiso 1 1 calc R . . H34C H 0.5689 0.8493 0.7035 0.045 Uiso 1 1 calc R . . Cl1 Cl 0.87555(4) 0.89617(2) 0.87271(3) 0.02484(9) Uani 1 1 d . . . Cl2 Cl 1.07851(7) 0.51370(3) 0.86042(3) 0.04511(16) Uani 1 1 d . . . N1 N 0.84451(12) 0.82171(8) 0.55930(8) 0.0152(3) Uani 1 1 d . . . N2 N 0.73843(12) 0.63477(8) 0.61320(8) 0.0165(3) Uani 1 1 d . . . O1 O 0.53628(12) 0.72450(9) 0.76520(8) 0.0279(3) Uani 1 1 d . . . P1 P 1.02431(3) 0.72545(2) 0.72634(2) 0.01245(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01582(3) 0.01169(3) 0.01463(3) -0.00030(2) 0.00081(2) 0.00151(2) Au2 0.02297(3) 0.01216(3) 0.01319(3) 0.00127(2) -0.00008(2) 0.00471(2) C1 0.0143(7) 0.0115(6) 0.0150(7) 0.0009(5) 0.0018(6) -0.0005(5) C2 0.0121(7) 0.0137(7) 0.0139(7) -0.0006(5) 0.0006(5) -0.0006(5) C3 0.0153(7) 0.0121(7) 0.0156(7) 0.0003(5) 0.0019(6) 0.0001(6) C4 0.0193(8) 0.0137(7) 0.0233(8) 0.0044(6) 0.0019(6) -0.0037(6) C5 0.0244(9) 0.0150(7) 0.0288(9) 0.0004(7) 0.0013(7) -0.0003(7) C6 0.0252(9) 0.0269(9) 0.0238(9) 0.0066(7) 0.0055(7) -0.0007(7) C7 0.0152(8) 0.0202(8) 0.0199(8) 0.0009(6) -0.0026(6) -0.0043(6) C8 0.0269(10) 0.0295(10) 0.0226(9) -0.0060(7) -0.0017(7) -0.0041(8) C9 0.0174(9) 0.0293(10) 0.0277(9) 0.0011(7) 0.0006(7) -0.0041(7) C10 0.0142(8) 0.0202(8) 0.0182(7) 0.0062(6) -0.0020(6) 0.0011(6) C11 0.0229(9) 0.0294(9) 0.0165(8) 0.0033(7) -0.0019(7) 0.0005(7) C12 0.0157(8) 0.0286(9) 0.0255(9) 0.0057(7) 0.0007(7) 0.0041(7) C13 0.0156(8) 0.0116(7) 0.0228(8) 0.0031(6) -0.0023(6) -0.0017(6) C14 0.0203(9) 0.0232(9) 0.0346(10) 0.0057(8) 0.0066(8) -0.0039(7) C15 0.0264(10) 0.0162(8) 0.0334(10) -0.0018(7) 0.0011(8) 0.0009(7) C16 0.0125(7) 0.0125(7) 0.0134(7) 0.0002(5) -0.0010(5) 0.0018(5) C17 0.0135(7) 0.0127(7) 0.0152(7) -0.0009(5) -0.0011(6) 0.0002(6) C18 0.0160(8) 0.0155(7) 0.0162(7) -0.0034(6) 0.0013(6) 0.0005(6) C19 0.0137(7) 0.0164(7) 0.0149(7) 0.0002(6) 0.0011(6) 0.0009(6) C20 0.0150(7) 0.0152(7) 0.0165(7) -0.0012(6) 0.0003(6) -0.0022(6) C21 0.0128(7) 0.0131(7) 0.0143(7) -0.0005(5) -0.0004(5) 0.0007(5) C22 0.0178(8) 0.0144(7) 0.0149(7) -0.0021(6) 0.0008(6) -0.0024(6) C23 0.0180(8) 0.0271(9) 0.0186(8) -0.0027(7) -0.0026(6) -0.0031(7) C24 0.0235(9) 0.0181(8) 0.0231(8) -0.0037(6) 0.0024(7) 0.0006(7) C25 0.0144(8) 0.0188(7) 0.0165(7) -0.0013(6) 0.0016(6) -0.0030(6) C26 0.0235(9) 0.0214(8) 0.0219(8) 0.0042(7) 0.0030(7) -0.0008(7) C27 0.0214(9) 0.0271(9) 0.0206(8) -0.0048(7) 0.0063(7) -0.0030(7) C28 0.0195(8) 0.0121(7) 0.0179(7) -0.0029(6) 0.0024(6) -0.0019(6) C29 0.0309(11) 0.0146(8) 0.0430(12) -0.0023(8) 0.0033(9) 0.0038(7) C30 0.0309(10) 0.0245(9) 0.0191(8) -0.0044(7) -0.0006(7) -0.0086(8) C31 0.0364(12) 0.0355(11) 0.0268(10) 0.0019(8) 0.0100(9) 0.0098(9) C32 0.0545(16) 0.0353(12) 0.0436(14) -0.0060(10) 0.0177(12) -0.0089(11) C33 0.0261(10) 0.0419(12) 0.0246(10) -0.0017(9) -0.0001(8) -0.0004(9) C34 0.0280(10) 0.0380(11) 0.0238(9) 0.0023(8) 0.0064(8) 0.0009(9) Cl1 0.0297(2) 0.01920(19) 0.0254(2) -0.00529(16) 0.00222(18) 0.00912(17) Cl2 0.0893(5) 0.0204(2) 0.0258(2) 0.00931(19) 0.0076(3) 0.0231(3) N1 0.0129(6) 0.0137(6) 0.0179(6) 0.0038(5) -0.0024(5) -0.0012(5) N2 0.0155(7) 0.0149(6) 0.0183(7) 0.0014(5) -0.0008(5) -0.0035(5) O1 0.0281(7) 0.0318(8) 0.0237(7) -0.0015(6) 0.0024(6) 0.0015(6) P1 0.01357(19) 0.01078(16) 0.01256(17) 0.00066(13) -0.00038(14) 0.00021(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2525(4) . y Au1 Cl1 2.2974(5) . y Au2 P1 2.2319(5) . y Au2 Cl2 2.2814(5) . y C1 C2 1.379(2) . y C1 C3 1.389(2) . y C1 P1 1.8072(17) . y C2 N1 1.313(2) . y C2 C3 1.414(2) . y C3 N2 1.309(2) . y C4 N2 1.492(2) . y C4 C6 1.519(3) . y C4 C5 1.522(3) . y C4 H4 1.0000 . y C5 H5A 0.9800 . y C5 H5B 0.9800 . y C5 H5C 0.9800 . y C6 H6A 0.9800 . y C6 H6B 0.9800 . y C6 H6C 0.9800 . y C7 N2 1.487(2) . y C7 C8 1.522(3) . y C7 C9 1.527(3) . y C7 H7 1.0000 . y C8 H8A 0.9800 . y C8 H8B 0.9800 . y C8 H8C 0.9800 . y C9 H9A 0.9800 . y C9 H9B 0.9800 . y C9 H9C 0.9800 . y C10 N1 1.486(2) . y C10 C11 1.515(3) . y C10 C12 1.518(3) . y C10 H10 1.0000 . y C11 H11A 0.9800 . y C11 H11B 0.9800 . y C11 H11C 0.9800 . y C12 H12A 0.9800 . y C12 H12B 0.9800 . y C12 H12C 0.9800 . y C13 N1 1.489(2) . y C13 C14 1.517(3) . y C13 C15 1.519(3) . y C13 H13 1.0000 . y C14 H14A 0.9800 . y C14 H14B 0.9800 . y C14 H14C 0.9800 . y C15 H15A 0.9800 . y C15 H15B 0.9800 . y C15 H15C 0.9800 . y C16 C17 1.414(2) . y C16 C21 1.418(2) . y C16 P1 1.8455(17) . y C17 C18 1.398(2) . y C17 C28 1.520(2) . y C18 C19 1.389(2) . y C18 H18 0.9500 . y C19 C20 1.391(2) . y C19 C25 1.518(2) . y C20 C21 1.395(2) . y C20 H20 0.9500 . y C21 C22 1.525(2) . y C22 C24 1.531(2) . y C22 C23 1.538(2) . y C22 H22 1.0000 . y C23 H23A 0.9800 . y C23 H23B 0.9800 . y C23 H23C 0.9800 . y C24 H24A 0.9800 . y C24 H24B 0.9800 . y C24 H24C 0.9800 . y C25 C27 1.521(2) . y C25 C26 1.532(3) . y C25 H25 1.0000 . y C26 H26A 0.9800 . y C26 H26B 0.9800 . y C26 H26C 0.9800 . y C27 H27A 0.9800 . y C27 H27B 0.9800 . y C27 H27C 0.9800 . y C28 C29 1.530(3) . y C28 C30 1.535(3) . y C28 H28 1.0000 . y C29 H29A 0.9800 . y C29 H29B 0.9800 . y C29 H29C 0.9800 . y C30 H30A 0.9800 . y C30 H30B 0.9800 . y C30 H30C 0.9800 . y C31 O1 1.412(3) . y C31 C32 1.517(4) . y C31 H31A 0.9900 . y C31 H31B 0.9900 . y C32 H32A 0.9800 . y C32 H32B 0.9800 . y C32 H32C 0.9800 . y C33 O1 1.425(3) . y C33 C34 1.499(3) . y C33 H33A 0.9900 . y C33 H33B 0.9900 . y C34 H34A 0.9800 . y C34 H34B 0.9800 . y C34 H34C 0.9800 . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 175.919(17) . . y P1 Au2 Cl2 175.130(19) . . y C2 C1 C3 61.42(12) . . y C2 C1 P1 142.58(13) . . y C3 C1 P1 155.26(13) . . y N1 C2 C1 144.15(16) . . y N1 C2 C3 156.22(16) . . y C1 C2 C3 59.62(11) . . y N2 C3 C1 149.01(16) . . y N2 C3 C2 151.98(17) . . y C1 C3 C2 58.96(11) . . y N2 C4 C6 110.35(15) . . y N2 C4 C5 111.83(15) . . y C6 C4 C5 113.36(16) . . y N2 C4 H4 107.0 . . y C6 C4 H4 107.0 . . y C5 C4 H4 107.0 . . y C4 C5 H5A 109.5 . . y C4 C5 H5B 109.5 . . y H5A C5 H5B 109.5 . . y C4 C5 H5C 109.5 . . y H5A C5 H5C 109.5 . . y H5B C5 H5C 109.5 . . y C4 C6 H6A 109.5 . . y C4 C6 H6B 109.5 . . y H6A C6 H6B 109.5 . . y C4 C6 H6C 109.5 . . y H6A C6 H6C 109.5 . . y H6B C6 H6C 109.5 . . y N2 C7 C8 110.32(15) . . y N2 C7 C9 111.47(15) . . y C8 C7 C9 112.19(16) . . y N2 C7 H7 107.5 . . y C8 C7 H7 107.5 . . y C9 C7 H7 107.5 . . y C7 C8 H8A 109.5 . . y C7 C8 H8B 109.5 . . y H8A C8 H8B 109.5 . . y C7 C8 H8C 109.5 . . y H8A C8 H8C 109.5 . . y H8B C8 H8C 109.5 . . y C7 C9 H9A 109.5 . . y C7 C9 H9B 109.5 . . y H9A C9 H9B 109.5 . . y C7 C9 H9C 109.5 . . y H9A C9 H9C 109.5 . . y H9B C9 H9C 109.5 . . y N1 C10 C11 110.83(14) . . y N1 C10 C12 111.74(14) . . y C11 C10 C12 113.51(16) . . y N1 C10 H10 106.8 . . y C11 C10 H10 106.8 . . y C12 C10 H10 106.8 . . y C10 C11 H11A 109.5 . . y C10 C11 H11B 109.5 . . y H11A C11 H11B 109.5 . . y C10 C11 H11C 109.5 . . y H11A C11 H11C 109.5 . . y H11B C11 H11C 109.5 . . y C10 C12 H12A 109.5 . . y C10 C12 H12B 109.5 . . y H12A C12 H12B 109.5 . . y C10 C12 H12C 109.5 . . y H12A C12 H12C 109.5 . . y H12B C12 H12C 109.5 . . y N1 C13 C14 111.18(15) . . y N1 C13 C15 110.74(15) . . y C14 C13 C15 112.99(15) . . y N1 C13 H13 107.2 . . y C14 C13 H13 107.2 . . y C15 C13 H13 107.2 . . y C13 C14 H14A 109.5 . . y C13 C14 H14B 109.5 . . y H14A C14 H14B 109.5 . . y C13 C14 H14C 109.5 . . y H14A C14 H14C 109.5 . . y H14B C14 H14C 109.5 . . y C13 C15 H15A 109.5 . . y C13 C15 H15B 109.5 . . y H15A C15 H15B 109.5 . . y C13 C15 H15C 109.5 . . y H15A C15 H15C 109.5 . . y H15B C15 H15C 109.5 . . y C17 C16 C21 118.94(15) . . y C17 C16 P1 119.28(12) . . y C21 C16 P1 121.75(12) . . y C18 C17 C16 119.47(15) . . y C18 C17 C28 116.90(14) . . y C16 C17 C28 123.50(15) . . y C19 C18 C17 122.02(15) . . y C19 C18 H18 119.0 . . y C17 C18 H18 119.0 . . y C18 C19 C20 117.51(15) . . y C18 C19 C25 123.70(15) . . y C20 C19 C25 118.79(15) . . y C19 C20 C21 122.88(15) . . y C19 C20 H20 118.6 . . y C21 C20 H20 118.6 . . y C20 C21 C16 118.61(15) . . y C20 C21 C22 116.55(14) . . y C16 C21 C22 124.81(15) . . y C21 C22 C24 111.62(14) . . y C21 C22 C23 111.12(14) . . y C24 C22 C23 110.15(15) . . y C21 C22 H22 107.9 . . y C24 C22 H22 107.9 . . y C23 C22 H22 107.9 . . y C22 C23 H23A 109.5 . . y C22 C23 H23B 109.5 . . y H23A C23 H23B 109.5 . . y C22 C23 H23C 109.5 . . y H23A C23 H23C 109.5 . . y H23B C23 H23C 109.5 . . y C22 C24 H24A 109.5 . . y C22 C24 H24B 109.5 . . y H24A C24 H24B 109.5 . . y C22 C24 H24C 109.5 . . y H24A C24 H24C 109.5 . . y H24B C24 H24C 109.5 . . y C19 C25 C27 113.90(15) . . y C19 C25 C26 110.31(14) . . y C27 C25 C26 109.64(15) . . y C19 C25 H25 107.6 . . y C27 C25 H25 107.6 . . y C26 C25 H25 107.6 . . y C25 C26 H26A 109.5 . . y C25 C26 H26B 109.5 . . y H26A C26 H26B 109.5 . . y C25 C26 H26C 109.5 . . y H26A C26 H26C 109.5 . . y H26B C26 H26C 109.5 . . y C25 C27 H27A 109.5 . . y C25 C27 H27B 109.5 . . y H27A C27 H27B 109.5 . . y C25 C27 H27C 109.5 . . y H27A C27 H27C 109.5 . . y H27B C27 H27C 109.5 . . y C17 C28 C29 109.93(15) . . y C17 C28 C30 113.28(14) . . y C29 C28 C30 110.86(16) . . y C17 C28 H28 107.5 . . y C29 C28 H28 107.5 . . y C30 C28 H28 107.5 . . y C28 C29 H29A 109.5 . . y C28 C29 H29B 109.5 . . y H29A C29 H29B 109.5 . . y C28 C29 H29C 109.5 . . y H29A C29 H29C 109.5 . . y H29B C29 H29C 109.5 . . y C28 C30 H30A 109.5 . . y C28 C30 H30B 109.5 . . y H30A C30 H30B 109.5 . . y C28 C30 H30C 109.5 . . y H30A C30 H30C 109.5 . . y H30B C30 H30C 109.5 . . y O1 C31 C32 107.85(19) . . y O1 C31 H31A 110.1 . . y C32 C31 H31A 110.1 . . y O1 C31 H31B 110.1 . . y C32 C31 H31B 110.1 . . y H31A C31 H31B 108.5 . . y C31 C32 H32A 109.5 . . y C31 C32 H32B 109.5 . . y H32A C32 H32B 109.5 . . y C31 C32 H32C 109.5 . . y H32A C32 H32C 109.5 . . y H32B C32 H32C 109.5 . . y O1 C33 C34 107.15(17) . . y O1 C33 H33A 110.3 . . y C34 C33 H33A 110.3 . . y O1 C33 H33B 110.3 . . y C34 C33 H33B 110.3 . . y H33A C33 H33B 108.5 . . y C33 C34 H34A 109.5 . . y C33 C34 H34B 109.5 . . y H34A C34 H34B 109.5 . . y C33 C34 H34C 109.5 . . y H34A C34 H34C 109.5 . . y H34B C34 H34C 109.5 . . y C2 N1 C10 123.93(14) . . y C2 N1 C13 116.78(14) . . y C10 N1 C13 119.22(13) . . y C3 N2 C7 121.78(14) . . y C3 N2 C4 119.98(15) . . y C7 N2 C4 118.14(14) . . y C31 O1 C33 112.29(17) . . y C1 P1 C16 100.84(7) . . y C1 P1 Au2 111.93(5) . . y C16 P1 Au2 114.91(5) . . y C1 P1 Au1 98.00(5) . . y C16 P1 Au1 117.63(5) . . y Au2 P1 Au1 111.506(19) . . y _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.925 _refine_diff_density_min -1.218 _refine_diff_density_rms 0.084 #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 914768' _audit_creation_date 2012-12-07 _audit_block_code MEG-Gl-041-03_7758 _chemical_name_systematic ; chloro-(1-(cyclooctadienyl-rhodium-chloride)(2,4,6-triisopropyl-phenyl)- phosphino-2,3-bis(diisopropylamino)cyclopropenium-P)-gold ; _chemical_melting_point ? _chemical_compound_source 'dichloromethane, ether' _chemical_formula_moiety 'C38 H63 Au Cl2 N2 P Rh' _chemical_formula_sum 'C38 H63 Au Cl2 N2 P Rh' _chemical_formula_weight 949.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-c 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.580(3) _cell_length_b 26.348(4) _cell_length_c 15.250(2) _cell_angle_alpha 90.00 _cell_angle_beta 126.810(2) _cell_angle_gamma 90.00 _cell_volume 7907.5(19) _cell_formula_units_Z 8 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9828 _cell_measurement_theta_min 2.2743 _cell_measurement_theta_max 35.8921 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 1.00 0.00 0.0650 0.00 -1.00 0.00 0.0540 0.00 0.00 -1.00 0.1050 0.00 0.00 1.00 0.0810 1.00 1.00 0.00 0.0130 -1.00 -1.00 0.00 0.0260 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method ? _exptl_crystal_F_000 3824 _exptl_absorpt_coefficient_mu 4.327 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.18962 _exptl_absorpt_correction_T_max 0.76362 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2008)' _exptl_special_details ; Crystal mounted on a MiTeGen loop using Perfluoropolyether PFO-XR75 ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source '0.2 x 2mm^2^ focus rotating anode' _diffrn_radiation_monochromator 'Incoatec Helios mirrors' _diffrn_measurement_device_type 'Bruker-AXS Kappa Mach3 APEX-II' _diffrn_measurement_method 'CCD \f- and \w-scans' _diffrn_detector_area_resol_mean 66.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 110186 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 30.51 _reflns_number_total 12070 _reflns_number_gt 10548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT software (Bruker AXS, 2004)' _computing_data_reduction 'SAINT software (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Crystal Impact GbR, 2005)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The minimum and maximum estimated transmissions from the multi-scan scaling are 0.2029 and 0.7182 (SADABS). Reflections above 9 Angstroems resolution were shaded by the beamstop and removed from the final least- squares refinement cycles. Highest peak 1.56 at 0.8590 0.1496 0.3891 [ 0.92 A from RH2 ] Deepest hole -1.04 at 0.7809 0.0323 0.2979 [ 0.76 A from AU1 ] ; _iucr_refine_instructions_details ; TITL 7758sadabs CELL 0.71073 24.5802 26.3483 15.25 90 126.81 90 ZERR 8 0.0034 0.0037 0.0021 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Au Cl N P Rh UNIT 304 504 8 16 16 8 8 LIST 4 L.S. 4 PLAN 20 SHEL 9.0 0.7 SIZE 0.052 0.245 0.38 TEMP -173 FMAP 2 ACTA WGHT 0.015000 4.979500 FVAR 0.02233 AU1 3 0.281872 0.503459 0.300797 11.00000 0.01231 0.01000 = 0.01404 -0.00031 0.00777 0.00007 RH2 7 0.392934 0.625296 0.423912 11.00000 0.01309 0.00987 = 0.01757 -0.00096 0.00963 -0.00030 CL1 4 0.291284 0.416321 0.308307 11.00000 0.02314 0.01134 = 0.02567 -0.00078 0.01339 -0.00026 CL2 4 0.344942 0.705727 0.405314 11.00000 0.02104 0.01236 = 0.04000 -0.00286 0.01540 0.00179 P3 6 0.284640 0.589141 0.291154 11.00000 0.01303 0.01035 = 0.01394 0.00058 0.00906 0.00085 N1 5 0.161673 0.708422 0.220869 11.00000 0.02064 0.01280 = 0.02225 0.00349 0.01624 0.00408 N2 5 0.192381 0.619621 0.437627 11.00000 0.01784 0.01345 = 0.02021 0.00268 0.01395 0.00332 C1 1 0.227401 0.623819 0.307539 11.00000 0.01471 0.01136 = 0.01464 0.00056 0.00876 -0.00056 C2 1 0.188475 0.667140 0.281179 11.00000 0.01489 0.01211 = 0.01839 0.00093 0.01073 0.00014 C3 1 0.199447 0.633264 0.361497 11.00000 0.01405 0.01061 = 0.01748 0.00019 0.00869 0.00024 C4 1 0.175548 0.721268 0.140637 11.00000 0.02378 0.01470 = 0.01961 0.00382 0.01552 0.00338 AFIX 13 H4 2 0.204757 0.693703 0.144127 11.00000 -1.20000 AFIX 0 C5 1 0.214574 0.770822 0.169788 11.00000 0.02944 0.01857 = 0.02392 0.00451 0.01712 -0.00033 AFIX 137 H5A 2 0.186519 0.798843 0.164488 11.00000 -1.50000 H5B 2 0.225837 0.776747 0.118910 11.00000 -1.50000 H5C 2 0.256523 0.768818 0.244756 11.00000 -1.50000 AFIX 0 C6 1 0.110000 0.722652 0.023740 11.00000 0.02857 0.02226 = 0.02209 0.00564 0.01257 0.00248 AFIX 137 H6A 2 0.085366 0.690634 0.007619 11.00000 -1.50000 H6B 2 0.121031 0.727334 -0.027748 11.00000 -1.50000 H6C 2 0.081549 0.750877 0.016353 11.00000 -1.50000 AFIX 0 C7 1 0.118207 0.743669 0.230244 11.00000 0.03283 0.01566 = 0.03897 0.00979 0.02893 0.01145 AFIX 13 H7 2 0.107469 0.772748 0.180079 11.00000 -1.20000 AFIX 0 C8 1 0.050327 0.718958 0.187588 11.00000 0.02713 0.03072 = 0.04359 0.01865 0.02556 0.01420 AFIX 137 H8A 2 0.026582 0.709493 0.110588 11.00000 -1.50000 H8B 2 0.022425 0.742986 0.193952 11.00000 -1.50000 H8C 2 0.058397 0.688529 0.230839 11.00000 -1.50000 AFIX 0 C9 1 0.156363 0.765954 0.344623 11.00000 0.05709 0.01767 = 0.05194 -0.00295 0.04527 0.00098 AFIX 137 H9A 2 0.174402 0.738408 0.398411 11.00000 -1.50000 H9B 2 0.125354 0.786848 0.349678 11.00000 -1.50000 H9C 2 0.193956 0.786988 0.359584 11.00000 -1.50000 AFIX 0 C10 1 0.140539 0.644008 0.444195 11.00000 0.01900 0.01648 = 0.02129 0.00320 0.01521 0.00522 AFIX 13 H10 2 0.124744 0.675345 0.398069 11.00000 -1.20000 AFIX 0 C11 1 0.169330 0.660332 0.559651 11.00000 0.03642 0.04217 = 0.02925 -0.00720 0.02046 0.01229 AFIX 137 H11A 2 0.181431 0.630236 0.605716 11.00000 -1.50000 H11B 2 0.135236 0.680201 0.558593 11.00000 -1.50000 H11C 2 0.209955 0.681125 0.589368 11.00000 -1.50000 AFIX 0 C12 1 0.079404 0.609662 0.395900 11.00000 0.01744 0.02976 = 0.04522 0.00430 0.01810 0.00457 AFIX 137 H12A 2 0.062627 0.599507 0.321792 11.00000 -1.50000 H12B 2 0.043516 0.627861 0.392802 11.00000 -1.50000 H12C 2 0.092508 0.579394 0.441852 11.00000 -1.50000 AFIX 0 C13 1 0.228544 0.573461 0.504783 11.00000 0.01890 0.01361 = 0.01690 0.00354 0.01269 0.00393 AFIX 13 H13 2 0.218338 0.570272 0.558927 11.00000 -1.20000 AFIX 0 C14 1 0.202464 0.525431 0.435434 11.00000 0.02847 0.01419 = 0.02733 0.00018 0.02075 0.00109 AFIX 137 H14A 2 0.153010 0.523430 0.394373 11.00000 -1.50000 H14B 2 0.223561 0.495694 0.483172 11.00000 -1.50000 H14C 2 0.214036 0.526255 0.384122 11.00000 -1.50000 AFIX 0 C15 1 0.305050 0.579804 0.569874 11.00000 0.01783 0.02582 = 0.02267 0.00501 0.01177 0.00500 AFIX 137 H15A 2 0.317044 0.583074 0.519342 11.00000 -1.50000 H15B 2 0.327951 0.550074 0.616844 11.00000 -1.50000 H15C 2 0.319458 0.610353 0.615381 11.00000 -1.50000 AFIX 0 C16 1 0.433916 0.554603 0.502313 11.00000 0.01285 0.01152 = 0.01731 0.00073 0.00760 0.00132 AFIX 13 H16 2 0.398701 0.528264 0.481111 11.00000 -1.20000 AFIX 0 C17 1 0.446636 0.561315 0.424830 11.00000 0.01566 0.01077 = 0.02176 -0.00191 0.01142 0.00076 AFIX 13 H17 2 0.418844 0.539009 0.358896 11.00000 -1.20000 AFIX 0 C18 1 0.515940 0.575299 0.454560 11.00000 0.01739 0.01774 = 0.02839 -0.00218 0.01626 0.00008 AFIX 23 H18A 2 0.520678 0.560005 0.400155 11.00000 -1.20000 H18B 2 0.551702 0.560600 0.527039 11.00000 -1.20000 AFIX 0 C19 1 0.527184 0.632671 0.458375 11.00000 0.01865 0.01913 = 0.03298 -0.00153 0.01740 -0.00306 AFIX 23 H19A 2 0.576328 0.639834 0.512110 11.00000 -1.20000 H19B 2 0.513102 0.644056 0.385638 11.00000 -1.20000 AFIX 0 C20 1 0.488712 0.663034 0.488997 11.00000 0.01505 0.01505 = 0.02772 -0.00390 0.01215 -0.00522 AFIX 13 H20 2 0.484318 0.699957 0.470678 11.00000 -1.20000 AFIX 0 C21 1 0.487855 0.652078 0.576950 11.00000 0.01696 0.01582 = 0.02433 -0.00766 0.01033 -0.00491 AFIX 13 H21 2 0.482147 0.682441 0.610086 11.00000 -1.20000 AFIX 0 C22 1 0.528616 0.609433 0.657113 11.00000 0.01755 0.02324 = 0.02015 -0.00523 0.00790 -0.00287 AFIX 23 H22A 2 0.544849 0.620080 0.731418 11.00000 -1.20000 H22B 2 0.568882 0.602279 0.659100 11.00000 -1.20000 AFIX 0 C23 1 0.485768 0.560941 0.624756 11.00000 0.01824 0.01816 = 0.01944 -0.00003 0.00886 -0.00017 AFIX 23 H23A 2 0.516459 0.531170 0.654371 11.00000 -1.20000 H23B 2 0.461889 0.561632 0.658821 11.00000 -1.20000 AFIX 0 C24 1 0.239938 0.601390 0.142694 11.00000 0.01863 0.01235 = 0.01594 0.00060 0.01128 0.00283 C25 1 0.169917 0.589562 0.067220 11.00000 0.01931 0.01426 = 0.01799 -0.00118 0.00974 0.00398 C26 1 0.137053 0.600560 -0.043640 11.00000 0.02087 0.02083 = 0.01857 -0.00179 0.00620 0.00223 AFIX 43 H26 2 0.089680 0.594137 -0.093882 11.00000 -1.20000 AFIX 0 C27 1 0.170915 0.620561 -0.083504 11.00000 0.03541 0.02185 = 0.01845 0.00305 0.01471 0.00522 C28 1 0.239939 0.629611 -0.008619 11.00000 0.03443 0.02285 = 0.02386 0.00362 0.02034 0.00281 AFIX 43 H28 2 0.264188 0.642379 -0.034342 11.00000 -1.20000 AFIX 0 C29 1 0.274960 0.620688 0.102721 11.00000 0.02558 0.01590 = 0.02040 0.00114 0.01661 0.00218 C30 1 0.127930 0.562330 0.096929 11.00000 0.01336 0.02006 = 0.01850 -0.00178 0.00668 0.00073 AFIX 13 H30 2 0.157972 0.556944 0.178003 11.00000 -1.20000 AFIX 0 C31 1 0.065622 0.592313 0.067546 11.00000 0.01641 0.02625 = 0.03374 -0.00429 0.01198 0.00108 AFIX 137 H31A 2 0.080355 0.624499 0.107769 11.00000 -1.50000 H31B 2 0.040774 0.572461 0.087424 11.00000 -1.50000 H31C 2 0.035889 0.599154 -0.011345 11.00000 -1.50000 AFIX 0 C32 1 0.105977 0.510054 0.042382 11.00000 0.02343 0.02113 = 0.02362 -0.00274 0.01135 -0.00133 AFIX 137 H32A 2 0.078916 0.514050 -0.037255 11.00000 -1.50000 H32B 2 0.078628 0.493073 0.060949 11.00000 -1.50000 H32C 2 0.146332 0.489566 0.068523 11.00000 -1.50000 AFIX 0 C33 1 0.136529 0.630700 -0.204354 11.00000 0.03430 0.03671 = 0.01994 0.00381 0.01328 0.00083 AFIX 13 H33 2 0.173049 0.642783 -0.209620 11.00000 -1.20000 AFIX 0 C34 1 0.108765 0.582613 -0.270965 11.00000 0.04012 0.03749 = 0.01753 -0.00046 0.00980 0.00315 AFIX 137 H34A 2 0.145277 0.557487 -0.240697 11.00000 -1.50000 H34B 2 0.090398 0.589961 -0.347070 11.00000 -1.50000 H34C 2 0.072570 0.569128 -0.268436 11.00000 -1.50000 AFIX 0 C35 1 0.085280 0.672414 -0.249387 11.00000 0.08007 0.04066 = 0.02582 0.01113 0.02101 0.02348 AFIX 137 H35A 2 0.048801 0.662806 -0.244142 11.00000 -1.50000 H35B 2 0.066203 0.678278 -0.326299 11.00000 -1.50000 H35C 2 0.107202 0.703533 -0.207274 11.00000 -1.50000 AFIX 0 C36 1 0.350876 0.629663 0.173241 11.00000 0.02645 0.02271 = 0.02299 0.00306 0.01882 -0.00056 AFIX 13 H36 2 0.368496 0.625687 0.251378 11.00000 -1.20000 AFIX 0 C37 1 0.384494 0.588437 0.149160 11.00000 0.02903 0.04173 = 0.03054 0.00231 0.02201 0.00575 AFIX 137 H37A 2 0.373734 0.554915 0.162900 11.00000 -1.50000 H37B 2 0.433855 0.593354 0.196828 11.00000 -1.50000 H37C 2 0.367333 0.590750 0.072393 11.00000 -1.50000 AFIX 0 C38 1 0.369530 0.682990 0.160472 11.00000 0.03895 0.03273 = 0.03816 0.00781 0.02129 -0.00983 AFIX 137 H38A 2 0.353366 0.687976 0.084693 11.00000 -1.50000 H38B 2 0.418996 0.687148 0.210021 11.00000 -1.50000 H38C 2 0.348204 0.708088 0.178503 11.00000 -1.50000 HKLF 4 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+4.9795P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12070 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0491 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_restrained_S_all 1.228 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.281872(3) 0.503459(3) 0.300797(6) 0.01220(2) Uani 1 1 d . . . Rh2 Rh 0.392934(7) 0.625296(5) 0.423912(12) 0.01324(3) Uani 1 1 d . . . Cl1 Cl 0.29128(3) 0.416321(18) 0.30831(4) 0.02082(10) Uani 1 1 d . . . Cl2 Cl 0.34494(3) 0.705727(19) 0.40531(5) 0.02626(11) Uani 1 1 d . . . P3 P 0.28464(2) 0.589141(18) 0.29115(4) 0.01183(9) Uani 1 1 d . . . N1 N 0.16167(8) 0.70842(6) 0.22087(14) 0.0165(3) Uani 1 1 d . . . N2 N 0.19238(8) 0.61962(6) 0.43763(14) 0.0156(3) Uani 1 1 d . . . C1 C 0.22740(9) 0.62382(7) 0.30754(15) 0.0136(3) Uani 1 1 d . . . C2 C 0.18847(9) 0.66714(7) 0.28118(16) 0.0147(4) Uani 1 1 d . . . C3 C 0.19945(9) 0.63326(7) 0.36150(16) 0.0145(3) Uani 1 1 d . . . C4 C 0.17555(10) 0.72127(8) 0.14064(16) 0.0178(4) Uani 1 1 d . . . H4 H 0.2048 0.6937 0.1441 0.021 Uiso 1 1 calc R . . C5 C 0.21457(11) 0.77082(8) 0.16979(18) 0.0233(4) Uani 1 1 d . . . H5A H 0.1865 0.7988 0.1645 0.035 Uiso 1 1 calc R . . H5B H 0.2258 0.7767 0.1189 0.035 Uiso 1 1 calc R . . H5C H 0.2565 0.7688 0.2448 0.035 Uiso 1 1 calc R . . C6 C 0.11000(12) 0.72265(9) 0.02374(18) 0.0259(5) Uani 1 1 d . . . H6A H 0.0854 0.6906 0.0076 0.039 Uiso 1 1 calc R . . H6B H 0.1210 0.7273 -0.0277 0.039 Uiso 1 1 calc R . . H6C H 0.0815 0.7509 0.0164 0.039 Uiso 1 1 calc R . . C7 C 0.11821(11) 0.74367(8) 0.2302(2) 0.0245(5) Uani 1 1 d . . . H7 H 0.1075 0.7727 0.1801 0.029 Uiso 1 1 calc R . . C8 C 0.05033(12) 0.71896(9) 0.1876(2) 0.0311(5) Uani 1 1 d . . . H8A H 0.0266 0.7095 0.1106 0.047 Uiso 1 1 calc R . . H8B H 0.0224 0.7430 0.1940 0.047 Uiso 1 1 calc R . . H8C H 0.0584 0.6885 0.2308 0.047 Uiso 1 1 calc R . . C9 C 0.15636(14) 0.76595(9) 0.3446(2) 0.0344(6) Uani 1 1 d . . . H9A H 0.1744 0.7384 0.3984 0.052 Uiso 1 1 calc R . . H9B H 0.1254 0.7868 0.3497 0.052 Uiso 1 1 calc R . . H9C H 0.1940 0.7870 0.3596 0.052 Uiso 1 1 calc R . . C10 C 0.14054(10) 0.64401(8) 0.44420(17) 0.0170(4) Uani 1 1 d . . . H10 H 0.1247 0.6753 0.3981 0.020 Uiso 1 1 calc R . . C11 C 0.16933(13) 0.66033(11) 0.5597(2) 0.0355(6) Uani 1 1 d . . . H11A H 0.1814 0.6302 0.6057 0.053 Uiso 1 1 calc R . . H11B H 0.1352 0.6802 0.5586 0.053 Uiso 1 1 calc R . . H11C H 0.2100 0.6811 0.5894 0.053 Uiso 1 1 calc R . . C12 C 0.07940(11) 0.60966(9) 0.3959(2) 0.0312(5) Uani 1 1 d . . . H12A H 0.0626 0.5995 0.3218 0.047 Uiso 1 1 calc R . . H12B H 0.0435 0.6279 0.3928 0.047 Uiso 1 1 calc R . . H12C H 0.0925 0.5794 0.4419 0.047 Uiso 1 1 calc R . . C13 C 0.22854(10) 0.57346(7) 0.50478(16) 0.0152(4) Uani 1 1 d . . . H13 H 0.2183 0.5703 0.5589 0.018 Uiso 1 1 calc R . . C14 C 0.20246(11) 0.52543(8) 0.43543(18) 0.0208(4) Uani 1 1 d . . . H14A H 0.1530 0.5234 0.3944 0.031 Uiso 1 1 calc R . . H14B H 0.2236 0.4957 0.4832 0.031 Uiso 1 1 calc R . . H14C H 0.2140 0.5263 0.3841 0.031 Uiso 1 1 calc R . . C15 C 0.30505(10) 0.57980(9) 0.56987(18) 0.0223(4) Uani 1 1 d . . . H15A H 0.3170 0.5831 0.5193 0.034 Uiso 1 1 calc R . . H15B H 0.3280 0.5501 0.6168 0.034 Uiso 1 1 calc R . . H15C H 0.3195 0.6104 0.6154 0.034 Uiso 1 1 calc R . . C16 C 0.43392(9) 0.55460(7) 0.50231(16) 0.0148(4) Uani 1 1 d . . . H16 H 0.3987 0.5283 0.4811 0.018 Uiso 1 1 calc R . . C17 C 0.44664(10) 0.56132(7) 0.42483(17) 0.0159(4) Uani 1 1 d . . . H17 H 0.4188 0.5390 0.3589 0.019 Uiso 1 1 calc R . . C18 C 0.51594(10) 0.57530(8) 0.45456(18) 0.0196(4) Uani 1 1 d . . . H18A H 0.5207 0.5600 0.4002 0.024 Uiso 1 1 calc R . . H18B H 0.5517 0.5606 0.5270 0.024 Uiso 1 1 calc R . . C19 C 0.52718(10) 0.63267(8) 0.45837(19) 0.0224(4) Uani 1 1 d . . . H19A H 0.5763 0.6398 0.5121 0.027 Uiso 1 1 calc R . . H19B H 0.5131 0.6441 0.3856 0.027 Uiso 1 1 calc R . . C20 C 0.48871(10) 0.66303(8) 0.48900(17) 0.0197(4) Uani 1 1 d . . . H20 H 0.4843 0.7000 0.4707 0.024 Uiso 1 1 calc R . . C21 C 0.48786(10) 0.65208(8) 0.57695(18) 0.0203(4) Uani 1 1 d . . . H21 H 0.4821 0.6824 0.6101 0.024 Uiso 1 1 calc R . . C22 C 0.52862(10) 0.60943(8) 0.65711(17) 0.0224(4) Uani 1 1 d . . . H22A H 0.5448 0.6201 0.7314 0.027 Uiso 1 1 calc R . . H22B H 0.5689 0.6023 0.6591 0.027 Uiso 1 1 calc R . . C23 C 0.48577(10) 0.56094(8) 0.62476(17) 0.0201(4) Uani 1 1 d . . . H23A H 0.5165 0.5312 0.6544 0.024 Uiso 1 1 calc R . . H23B H 0.4619 0.5616 0.6588 0.024 Uiso 1 1 calc R . . C24 C 0.23994(10) 0.60139(7) 0.14269(16) 0.0151(4) Uani 1 1 d . . . C25 C 0.16992(10) 0.58956(8) 0.06722(17) 0.0181(4) Uani 1 1 d . . . C26 C 0.13705(11) 0.60056(8) -0.04364(17) 0.0236(4) Uani 1 1 d . . . H26 H 0.0897 0.5941 -0.0939 0.028 Uiso 1 1 calc R . . C27 C 0.17092(12) 0.62056(9) -0.08350(18) 0.0261(5) Uani 1 1 d . . . C28 C 0.23994(12) 0.62961(9) -0.00862(19) 0.0253(5) Uani 1 1 d . . . H28 H 0.2642 0.6424 -0.0343 0.030 Uiso 1 1 calc R . . C29 C 0.27496(11) 0.62069(8) 0.10272(17) 0.0189(4) Uani 1 1 d . . . C30 C 0.12793(10) 0.56233(8) 0.09693(17) 0.0191(4) Uani 1 1 d . . . H30 H 0.1580 0.5569 0.1780 0.023 Uiso 1 1 calc R . . C31 C 0.06562(11) 0.59231(9) 0.0675(2) 0.0274(5) Uani 1 1 d . . . H31A H 0.0804 0.6245 0.1078 0.041 Uiso 1 1 calc R . . H31B H 0.0408 0.5725 0.0874 0.041 Uiso 1 1 calc R . . H31C H 0.0359 0.5992 -0.0113 0.041 Uiso 1 1 calc R . . C32 C 0.10598(12) 0.51005(8) 0.04238(19) 0.0244(4) Uani 1 1 d . . . H32A H 0.0789 0.5141 -0.0373 0.037 Uiso 1 1 calc R . . H32B H 0.0786 0.4931 0.0609 0.037 Uiso 1 1 calc R . . H32C H 0.1463 0.4896 0.0685 0.037 Uiso 1 1 calc R . . C33 C 0.13653(13) 0.63070(10) -0.20435(19) 0.0322(5) Uani 1 1 d . . . H33 H 0.1730 0.6428 -0.2096 0.039 Uiso 1 1 calc R . . C34 C 0.10877(14) 0.58261(10) -0.27097(19) 0.0364(6) Uani 1 1 d . . . H34A H 0.1453 0.5575 -0.2407 0.055 Uiso 1 1 calc R . . H34B H 0.0904 0.5900 -0.3471 0.055 Uiso 1 1 calc R . . H34C H 0.0726 0.5691 -0.2684 0.055 Uiso 1 1 calc R . . C35 C 0.08528(18) 0.67241(12) -0.2494(2) 0.0555(9) Uani 1 1 d . . . H35A H 0.0488 0.6628 -0.2441 0.083 Uiso 1 1 calc R . . H35B H 0.0662 0.6783 -0.3263 0.083 Uiso 1 1 calc R . . H35C H 0.1072 0.7035 -0.2073 0.083 Uiso 1 1 calc R . . C36 C 0.35088(11) 0.62966(8) 0.17324(18) 0.0216(4) Uani 1 1 d . . . H36 H 0.3685 0.6257 0.2514 0.026 Uiso 1 1 calc R . . C37 C 0.38449(12) 0.58844(10) 0.1492(2) 0.0312(5) Uani 1 1 d . . . H37A H 0.3737 0.5549 0.1629 0.047 Uiso 1 1 calc R . . H37B H 0.4339 0.5934 0.1968 0.047 Uiso 1 1 calc R . . H37C H 0.3673 0.5908 0.0724 0.047 Uiso 1 1 calc R . . C38 C 0.36953(14) 0.68299(10) 0.1605(2) 0.0377(6) Uani 1 1 d . . . H38A H 0.3534 0.6880 0.0847 0.057 Uiso 1 1 calc R . . H38B H 0.4190 0.6871 0.2100 0.057 Uiso 1 1 calc R . . H38C H 0.3482 0.7081 0.1785 0.057 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01231(3) 0.01000(3) 0.01404(4) -0.00031(2) 0.00777(3) 0.00007(2) Rh2 0.01309(6) 0.00987(7) 0.01757(7) -0.00096(5) 0.00963(6) -0.00030(5) Cl1 0.0231(2) 0.0113(2) 0.0257(3) -0.00078(18) 0.0134(2) -0.00026(17) Cl2 0.0210(2) 0.0124(2) 0.0400(3) -0.0029(2) 0.0154(2) 0.00179(18) P3 0.0130(2) 0.0103(2) 0.0139(2) 0.00058(17) 0.00906(19) 0.00085(16) N1 0.0206(8) 0.0128(8) 0.0223(9) 0.0035(6) 0.0162(7) 0.0041(6) N2 0.0178(8) 0.0135(8) 0.0202(8) 0.0027(6) 0.0140(7) 0.0033(6) C1 0.0147(8) 0.0114(8) 0.0146(8) 0.0006(7) 0.0088(7) -0.0006(6) C2 0.0149(8) 0.0121(8) 0.0184(9) 0.0009(7) 0.0107(8) 0.0001(7) C3 0.0140(8) 0.0106(8) 0.0175(9) 0.0002(7) 0.0087(7) 0.0002(6) C4 0.0238(10) 0.0147(9) 0.0196(10) 0.0038(7) 0.0155(9) 0.0034(7) C5 0.0294(11) 0.0186(10) 0.0239(11) 0.0045(8) 0.0171(10) -0.0003(8) C6 0.0286(11) 0.0223(11) 0.0221(11) 0.0056(9) 0.0126(10) 0.0025(9) C7 0.0328(12) 0.0157(10) 0.0390(13) 0.0098(9) 0.0289(11) 0.0115(8) C8 0.0271(11) 0.0307(13) 0.0436(14) 0.0187(11) 0.0256(11) 0.0142(9) C9 0.0571(16) 0.0177(11) 0.0519(16) -0.0029(11) 0.0453(15) 0.0010(10) C10 0.0190(9) 0.0165(9) 0.0213(10) 0.0032(7) 0.0152(8) 0.0052(7) C11 0.0364(13) 0.0422(15) 0.0292(13) -0.0072(11) 0.0205(11) 0.0123(11) C12 0.0174(10) 0.0298(12) 0.0452(15) 0.0043(11) 0.0181(11) 0.0046(9) C13 0.0189(9) 0.0136(9) 0.0169(9) 0.0035(7) 0.0127(8) 0.0039(7) C14 0.0285(11) 0.0142(9) 0.0273(11) 0.0002(8) 0.0208(10) 0.0011(8) C15 0.0178(9) 0.0258(11) 0.0227(11) 0.0050(8) 0.0118(9) 0.0050(8) C16 0.0128(8) 0.0115(8) 0.0173(9) 0.0007(7) 0.0076(7) 0.0013(6) C17 0.0157(9) 0.0108(8) 0.0218(10) -0.0019(7) 0.0114(8) 0.0008(7) C18 0.0174(9) 0.0177(9) 0.0284(11) -0.0022(8) 0.0163(9) 0.0001(7) C19 0.0186(9) 0.0191(10) 0.0330(12) -0.0015(9) 0.0174(9) -0.0031(8) C20 0.0150(9) 0.0151(9) 0.0277(11) -0.0039(8) 0.0121(9) -0.0052(7) C21 0.0170(9) 0.0158(9) 0.0243(10) -0.0077(8) 0.0103(9) -0.0049(7) C22 0.0176(9) 0.0232(11) 0.0201(10) -0.0052(8) 0.0079(8) -0.0029(8) C23 0.0182(9) 0.0182(10) 0.0194(10) 0.0000(8) 0.0089(8) -0.0002(7) C24 0.0186(9) 0.0124(8) 0.0159(9) 0.0006(7) 0.0113(8) 0.0028(7) C25 0.0193(9) 0.0143(9) 0.0180(10) -0.0012(7) 0.0097(8) 0.0040(7) C26 0.0209(10) 0.0208(10) 0.0186(10) -0.0018(8) 0.0062(9) 0.0022(8) C27 0.0354(12) 0.0218(11) 0.0184(10) 0.0030(8) 0.0147(10) 0.0052(9) C28 0.0344(12) 0.0229(11) 0.0239(11) 0.0036(9) 0.0203(10) 0.0028(9) C29 0.0256(10) 0.0159(9) 0.0204(10) 0.0011(8) 0.0166(9) 0.0022(7) C30 0.0134(9) 0.0201(10) 0.0185(10) -0.0018(8) 0.0067(8) 0.0007(7) C31 0.0164(10) 0.0263(11) 0.0337(13) -0.0043(10) 0.0120(10) 0.0011(8) C32 0.0234(11) 0.0211(10) 0.0236(11) -0.0027(8) 0.0113(9) -0.0013(8) C33 0.0343(13) 0.0367(14) 0.0199(11) 0.0038(10) 0.0133(10) 0.0008(10) C34 0.0401(14) 0.0375(15) 0.0175(11) -0.0005(10) 0.0098(11) 0.0031(11) C35 0.080(2) 0.0407(17) 0.0258(14) 0.0111(12) 0.0210(16) 0.0235(16) C36 0.0264(10) 0.0227(11) 0.0230(10) 0.0031(8) 0.0188(9) -0.0006(8) C37 0.0290(12) 0.0417(15) 0.0305(13) 0.0023(11) 0.0220(11) 0.0057(10) C38 0.0389(14) 0.0327(14) 0.0382(15) 0.0078(11) 0.0213(12) -0.0098(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P3 2.2660(6) . y Au1 Cl1 2.3035(6) . y Rh2 C16 2.1143(19) . y Rh2 C17 2.1360(18) . y Rh2 C20 2.1717(19) . y Rh2 C21 2.205(2) . y Rh2 Cl2 2.3584(6) . y Rh2 P3 2.3736(6) . y P3 C1 1.8161(19) . y P3 C24 1.859(2) . y N1 C2 1.318(2) . y N1 C7 1.486(2) . y N1 C4 1.493(2) . y N2 C3 1.322(2) . y N2 C10 1.483(2) . y N2 C13 1.492(2) . y C1 C3 1.374(3) . y C1 C2 1.385(3) . y C2 C3 1.405(3) . y C4 C5 1.520(3) . y C4 C6 1.528(3) . y C7 C9 1.519(3) . y C7 C8 1.527(3) . y C10 C11 1.514(3) . y C10 C12 1.514(3) . y C13 C15 1.521(3) . y C13 C14 1.523(3) . y C16 C17 1.403(3) . y C16 C23 1.512(3) . y C17 C18 1.522(3) . y C18 C19 1.532(3) . y C19 C20 1.510(3) . y C20 C21 1.384(3) . y C21 C22 1.514(3) . y C22 C23 1.537(3) . y C24 C29 1.414(3) . y C24 C25 1.418(3) . y C25 C26 1.399(3) . y C25 C30 1.532(3) . y C26 C27 1.395(3) . y C27 C28 1.385(3) . y C27 C33 1.522(3) . y C28 C29 1.388(3) . y C29 C36 1.513(3) . y C30 C32 1.531(3) . y C30 C31 1.532(3) . y C33 C35 1.493(4) . y C33 C34 1.507(4) . y C36 C38 1.526(3) . y C36 C37 1.537(3) . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P3 Au1 Cl1 171.968(18) . . y C16 Rh2 C17 38.54(7) . . y C16 Rh2 C20 97.25(8) . . y C17 Rh2 C20 82.06(8) . . y C16 Rh2 C21 80.79(8) . . y C17 Rh2 C21 89.30(8) . . y C20 Rh2 C21 36.87(8) . . y C16 Rh2 Cl2 153.39(6) . . y C17 Rh2 Cl2 166.56(5) . . y C20 Rh2 Cl2 88.32(6) . . y C21 Rh2 Cl2 88.60(6) . . y C16 Rh2 P3 92.27(5) . . y C17 Rh2 P3 93.53(5) . . y C20 Rh2 P3 158.16(6) . . y C21 Rh2 P3 164.97(6) . . y Cl2 Rh2 P3 91.92(2) . . y C1 P3 C24 97.98(8) . . y C1 P3 Au1 115.88(6) . . y C24 P3 Au1 103.48(6) . . y C1 P3 Rh2 104.24(6) . . y C24 P3 Rh2 120.77(6) . . y Au1 P3 Rh2 113.98(2) . . y C2 N1 C7 122.43(16) . . y C2 N1 C4 119.67(16) . . y C7 N1 C4 117.89(16) . . y C3 N2 C10 120.77(16) . . y C3 N2 C13 119.11(15) . . y C10 N2 C13 119.30(15) . . y C3 C1 C2 61.21(13) . . y C3 C1 P3 151.64(15) . . y C2 C1 P3 146.30(15) . . y N1 C2 C1 148.44(19) . . y N1 C2 C3 152.54(18) . . y C1 C2 C3 59.01(13) . . y N2 C3 C1 148.45(18) . . y N2 C3 C2 151.70(18) . . y C1 C3 C2 59.78(13) . . y N1 C4 C5 111.66(17) . . y N1 C4 C6 111.27(17) . . y C5 C4 C6 111.12(17) . . y N1 C7 C9 111.55(18) . . y N1 C7 C8 110.96(18) . . y C9 C7 C8 114.8(2) . . y N2 C10 C11 112.32(17) . . y N2 C10 C12 110.53(17) . . y C11 C10 C12 111.8(2) . . y N2 C13 C15 110.70(16) . . y N2 C13 C14 111.77(16) . . y C15 C13 C14 112.71(17) . . y C17 C16 C23 125.30(17) . . y C17 C16 Rh2 71.56(11) . . y C23 C16 Rh2 111.37(13) . . y C16 C17 C18 123.64(18) . . y C16 C17 Rh2 69.90(11) . . y C18 C17 Rh2 112.82(13) . . y C17 C18 C19 113.23(16) . . y C20 C19 C18 113.72(17) . . y C21 C20 C19 124.4(2) . . y C21 C20 Rh2 72.89(11) . . y C19 C20 Rh2 108.92(13) . . y C20 C21 C22 123.37(19) . . y C20 C21 Rh2 70.25(12) . . y C22 C21 Rh2 112.68(13) . . y C21 C22 C23 111.28(17) . . y C16 C23 C22 113.37(17) . . y C29 C24 C25 119.04(18) . . y C29 C24 P3 121.27(15) . . y C25 C24 P3 119.65(15) . . y C26 C25 C24 118.46(19) . . y C26 C25 C30 116.80(18) . . y C24 C25 C30 124.63(18) . . y C27 C26 C25 122.8(2) . . y C28 C27 C26 117.5(2) . . y C28 C27 C33 119.0(2) . . y C26 C27 C33 123.4(2) . . y C27 C28 C29 122.3(2) . . y C28 C29 C24 119.8(2) . . y C28 C29 C36 116.08(18) . . y C24 C29 C36 124.04(18) . . y C32 C30 C25 109.97(17) . . y C32 C30 C31 109.87(17) . . y C25 C30 C31 113.86(18) . . y C35 C33 C34 113.1(2) . . y C35 C33 C27 112.9(2) . . y C34 C33 C27 111.5(2) . . y C29 C36 C38 112.95(19) . . y C29 C36 C37 109.29(18) . . y C38 C36 C37 112.00(19) . . y _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.561 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.096 #===END