The Effect of Hydrothermal and Non‐Hydrothermal Synthesis on the Formation of 
Holmium(III) Succinate Hydrate Frameworks

Bernini, Maria C.; Brusau, Elena V.; Narda, Griselda E.; Echeverria, Gustavo E.; Pozzi, C. Gustavo; Punte, Graciela; Lehmann, Christian W.

doi:10.1002/ejic.200600860

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The Effect of Hydrothermal and Non‐Hydrothermal Synthesis on the Formation of Holmium(III) Succinate Hydrate Frameworks

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Lehmann, Christian W.
Service Department Lehmann (EMR), Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Citation

Bernini, M. C., Brusau, E. V., Narda, G. E., Echeverria, G. E., Pozzi, C. G., Punte, G., et al. (2007). The Effect of Hydrothermal and Non‐Hydrothermal Synthesis on the Formation of Holmium(III) Succinate Hydrate Frameworks. European Journal of Inorganic Chemistry, (5), 684-693. doi:10.1002/ejic.200600860.

Cite as: https://hdl.handle.net/11858/00-001M-0000-000F-91B3-B

Abstract

Two novel hydrated holmium(III) succinates with formula [Ho₂(C₄H₄O₄)₃(H₂O)₄]·6H₂O (1) and [Ho₂(C₄H₄O₄)₃(H₂O)₂]·H₂O (2) have been synthesized from aqueous solution under ambient and hydrothermal conditions, respectively. Single‐crystal X‐ray diffraction shows that Ho^III is nine‐coordinate in both compounds even though their structures are markedly different, the main distinctive features being the [H₂O]/[C₄H₄O₄^2–] ratio in the coordination sphere, the conformation and coordination ability of the succinate ions, and the resulting framework dimensionality. Compound 1 is a 2D hybrid polymer and its crystal structure is unprecedented for rare‐earth succinates. It consists of centrosymmetric dimers of edge‐sharing HoO₇(H₂O)₂ polyhedra linked by succinate ions in the [100] and [101] directions. Hydrogen‐bonded hydration water molecules connect layers to give three‐dimensional stability. Compound 2 is built up from infinite chains of HoO₈(H₂O) polyhedra linked by succinates that result in a 3D architecture. This structure shows that hydrothermal conditions favor an increase in the overall dimensionality of these hybrids, in agreement with theoretical considerations. The compounds were characterized by FTIR and Raman spectroscopy, thermal analysis, and variable‐temperature magnetic susceptibility measurements and the results are discussed in connection with the structural findings. The effect of the dimensionality on the thermal stability of both structures after removal of the hydration water molecules is also analyzed.