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Transition-metal Silacyclohexyl Derivatives. Crystal and Molecular Structure of Carbonyl(η-cyclopentadienyl)(1-phenyl-1-silacyclohex-1-yl)-(triphenylphosphine)iron(II)

DOI: 10.1039/DT9820002461

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 2461 - 2468 (1982)

Update date:2022-08-05

Topics:

Authors:

Holmes-Smith, Rupert D.Holmes-Smith, Rupert D.

Stobart, Stephen R.Stobart, Stephen R.

Atwood, Jerry L.Atwood, Jerry L.

Hunter, William E.Hunter, William E.

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Article abstract of DOI:10.1039/DT9820002461

Synthesis of transition-metal silacyclohexyl complexes (1-metallo-1-silacyclohexanes) is reported via two established preparative routes: (a) reaction of 1-chloro-1-silacyclohexanes with 5-C5H5)(CO)2>- to give Si-Fe compounds <*> 2=H, (8); R2=Me, (9); R2=Ph (10)> followed by photochemical substitution with PPh3 to give the corresponding complexes <*> 2=H, (11); R2=Me, (12); R2=Ph (13)> which are chiral at Fe; (b) hydrosilylation at the metal to give mononuclear complexes <*> 2=Me, (14); R2=Ph, (15), R2=Cl (16)> and <*>2=Me, (17); R2=Ph (18)>from or,binuclear complexes <*>2=Me, (19); or Ph (20); M=Os, R2=Me, (21)> with linear Si-M-M-Si skeletons from or , or <*> (22).Infrared and 1H, 13C, and 31P n.m.r. spectral data are reported, including resolution of diastereotopic shifts in 13C n.m.r. spectra for compounds (12) and (13) arising from asymmetry at the iron centre.The crystal and molecular structure of the title compound (13) has been determined using single-crystal X-ray diffraction; the silacyclohexyl substituent adopts a flattened chair conformation with Si-Fe =2.366(2) Angstroem.Angles at Fe between the three different unidentate ligands are markedly distorted from 90 deg <97.2(2), 98.43(6), and 83.2(2) deg>; this is interpreted in terms of steric congestion about the asymmetric metal centre and accordingly moderated reactivity of complex (15) towards a variety of reagents is observed compared with .

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