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キーワード:
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要旨:
Known procedures for the synthesis of K[CpRu-(CO)(2)] (KRp) via reductive cleavage of the ruthenium dimer Rp(2) were found to be inconsistent and have thus been revisited, and a revised protocol using K[HB(sec-Bu)(3)] (K-Selectride) as the reducing agent is now reported that gives yellow KRp in crystalline form in around 40% yield. The structure of KRp THF has been determined by X-ray diffraction, representing the first crystallographic characterization of an Rp(-) salt. Inevitably the reductive cleavage of Rp(2) also gives a poorly soluble black solid as an additional product, which has now been analyzed by a variety of methods, including C-13 MAS NMR spectroscopy using (CO)-C-13-labeled material. The black solid has been identified as a polymeric Cp/Ru/CO compound with both bridging and terminal CO ligands in a 3:1 ratio. The present report may stimulate the use of the [CpRu(CO)(2)](-) (Rp(-)) anion, which has been barely exploited as yet in comparison to its popular congener [CpFe(CO)(2)](-) (Fp(-)).
