SYNTHESES, STRUCTURES, AND EQUILIBRIA OF O-TOLYLANTIMONY, M-TOLYLANTIMONY, P-TOLYLANTIMONY AND PHENYLANTIMONY RINGS

Exchange reactions of R(3)Sb (R = o-Tol, m-Tol, p-Tol) with SbCl3 in a 1:2 molar ratio give RSbCl(2). Silylstibanes RSb(SiMe(3))(2) were obtained by reaction of RSbCl(2) and Me(3)SiCl with Mg in THF. Slow access of air to solutions of RSb(SiMe(3))(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 Sb ... Sb distances of 420 pm. Solutions of (RSb)(n) (R = Ph, o-Tol, m-Tol, p-Tol) in CGD, were analyzed by H-1-NMR spectroscopy. They contain (RSb)(5) and (RSb)(4) in equilibria. Raman spectra of (PhSb)(6) or (p-TolSb)(n) show signals for Sb-n at (v) over tilde = 151 or 153 cm(-1). C-13-CP-MAS-NMR data of (p-TolSb)(n) are reported.