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Issue 23, 2007
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Synthesis and structural studies of germyl and germyl/stannyl substituted tungstenocenes

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Abstract

One-pot reactions of [WCp2(H)2] and [WCp2(H)(SnMe3)] with nBuLi followed by an equivalent of GeMe2Cl2 afford mono(germyl) substituted tungstenocenes [WCp2(H)(GeMe2Cl)] (1) and [WCp2(SnMe3)(GeMe2Cl)] (7). Reactions of the products with tin halides in the presence NEt3 afford the mixed complexes [WCp2(SnR2X)(GeMe2Y)] (X, Y = Cl, Br, R[double bond, length as m-dash]Me, Et), which were further converted to moderately stable compounds [WCp2(SnR2H)(GeMe2H)] (R = Me (10), Et (11)). A number of asymmetric mono(halo)-substituted germyl/stannyl tungstenocenes [WCp2(SnMe2X)(GeMe2H)] (X = Cl (12), Br (13)) and [WCp2(SnEt2Y)(GeMe2H)] (Y = Br (14), I (15)) were prepared by selective halogenation of the Sn–H bond in 10 and 11. X-Ray studies of [WCp2(H)(GeMe2Cl)] (1), [WCp2(SnEt2Br)(GeMe2Cl)] (4), and [WCp2(SnEt2Br)(GeMe2H)] (14) established classical structures of these compounds. X-Ray study of complex [WCp2(SnMe2Cl)(GeMe2Cl)] (3) revealed the presence of interligand Ge–Cl⋯Sn–Cl interactions in a highly Ge/Sn disordered structure. Analyses of molecular parameters of 1, 4, and 14 suggest the presence of a negative hyperconjugation between metal lone pairs and the σ*-orbital of the E–X bond, which is stronger in bromo substituted complexes in comparison with chloro substituted ones.

Graphical abstract: Synthesis and structural studies of germyl and germyl/stannyl substituted tungstenocenes

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Supplementary files

Article information


Submitted
02 Jan 2007
Accepted
26 Mar 2007
First published
13 Apr 2007

Dalton Trans., 2007, 2440-2449
Article type
Paper

Synthesis and structural studies of germyl and germyl/stannyl substituted tungstenocenes

A. Yu. Khalimon, K. Yu. Dorogov, A. V. Churakov, L. G. Kuzmina, D. A. Lemenovskii, J. A. K. Howard and G. I. Nikonov, Dalton Trans., 2007, 2440
DOI: 10.1039/B618806K

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