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Revisiting the synthesis and elucidating the structure of potassium Cyclopentadienyldicarbonylruthenate, K[CpRu(CO)(2)].

MPS-Authors
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Xiang,  S. Q.
Research Group of Solid-State NMR, MPI for biophysical chemistry, Max Planck Society;

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Lange,  A.
Research Group of Solid-State NMR, MPI for biophysical chemistry, Max Planck Society;

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Citation

Kalz, K. F., Kindermann, N., Xiang, S. Q., Kronz, A., & Lange, A. (2014). Revisiting the synthesis and elucidating the structure of potassium Cyclopentadienyldicarbonylruthenate, K[CpRu(CO)(2)]. Organometallics, 33(6), 1475-1479. doi:10.1021/om500107j.


Cite as: http://hdl.handle.net/11858/00-001M-0000-0019-12C4-0
Abstract
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(-)).