Synthesis of bis(tert-butyl)(2-thioxo-1,3-dithiole-4,5-dithiolato)stannane, (Bu2Sn)-Sn-t(dmit), and bis(tert-butyl)(2-oxo-1,3-dithiole-4,5-dithiolato)stannane, (Bu2Sn)-Sn-t(dmio): Crystal structures, at 120 K, of polymeric (Bu2Sn)-Sn-t(dmit), and two polymorphs of But2Sn(dmio). a polymer and a cyclic tetramer.

摘要

The syntheses of bis(tert-butyl)(2-thioxo-1,3-dithiole-4,5-dithiolato)stannane, (Bu2Sn)-Sn-t(dmit) 1, and bis(tert-butyl)(2-oxo-1,3-dithiole-4,5-dithiolato)stannane, (Bu2Sn)-Sn-t(dmio) 2, are reported. Compounds 1 and 2 were prepared by the exchange reactions of (Bu2SnCl2)-Sn-t with [NEt4](2)[Zn(dmit)(2)] and [NEt4](2)[Zn(dmio)(2)], respectively. X-ray structure determinations reveal the existance of two polymorphs of 2, 2m and 2o. In all three phases, intermolecular Sn-S-thioxo or Sn-O-oxo, as appropriate, create five-coordinate, trigonal bipyramidal tin centres. In 1 and 2o these intermolecular contacts link the molecules in chains, while in 2m they create a centrosymmetric cyclic tetramer, with a 24 membered, Sn4C8O4S8, ring. These findings of aggregated structures are in contrast to the published report that the simpler ethane-1,2-dithiolato compound, (Bu2Sn)-Sn-t(edt), is a molecular species in the solid state. (C) 2008 Elsevier B.V. All rights reserved.