Abstract
AbstractExchange reactions of R3Sb (R = o‐Tol, m‐Tol, p‐Tol) with SbCl3 in a 1:2 molar ratio give RSbCl2. Silylstibanes RSb(SiMe3)2 were obtained by reaction of RSbCl2 and Me3SiCl with Mg in THF. Slow access of air to solutions of RSb(SiMe3)2 afforded orange crystals of the composition (RSb)n. Crystal structures were determined by X‐ray crystallography for R = o‐Tol and m‐Tol as stacks of (RSb)6 rings in the chair conformation with equatorial substituents. In the crystals of (m‐TolSb)6 there are short intermolecular Sbb distances of 420 pm. Solutions of (RSb)n (R = Ph, o‐Tol, m‐Tol, p‐Tol) in C6D6 were analyzed by 1H‐NMR spectroscopy. They contain (RSb)5 and (RSb)4 in equilibria. Raman spectra of (PhSb)6 or (p‐TolSb)n show signals for Sbn at β = 151 or 153 cm‐1. 13C‐CP‐MAS‐NMR data of (p‐TolSb)n are reported.
Published Version
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