Batsanov, A. S. and Cornet, S. M. and Dillon, K. B. and Goeta, A. E. and Thompson, A. L. and Xue, B. Y. (2003) 'The synthesis and characterisation of some group 14 compounds containing the 2,4,6-(CF3)(3)C6H2, 2,6-(CF3)(2)C6H3 or 2,4-(CF3)(2)C6H3 ligands.', Dalton transactions. (12). pp. 2496-2502.
New (aryl)(2)ECl2 and (aryl)ECl3 compounds [E = Si, Ge or Sn; aryl = 2,4,6-(CF3)(3)C6H2(Ar), 2,6-(CF3)(2)C6H3 (Ar') and/or 2,4-(CF3)(3)C6H3 (Ar")] were prepared by reactions of ECl4 with 2 equivalents of ArLi or of a Ar'Li/Ar"Li mixture. The latter gives predominantly the less sterically hindered product Ar"2ECl2 for E = Si or Ge, but Ar'2SnCl2 for the larger central atom. The products were characterised by elemental analysis, F-19 and (where appropriate) Sn-119 NMR spectroscopy, and single-crystal X-ray diffraction for Ar"2SiCl2, ArGeCl3, Ar2GeCl2, Ar"2GeCl2, Ar2SnCl2 and Ar'2SnCl2. For E = Si the synthesis is complicated by Cl/F exchange: besides Ar'2SiCl2 and Ar"2SiCl2, F-19 NMR spectroscopy identified in solution Ar'2SiF2 and Ar'2SiF2. The latter was isolated and its X-ray structure determined. In all compounds, the E atom has a strongly distorted tetrahedral coordination, supplemented by short intramolecular E...F contacts (secondary coordination) with o-CF3 group(s).
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|Publisher Web site:||http://dx.doi.org/10.1039/b302544f|
|Record Created:||20 Apr 2007|
|Last Modified:||20 Nov 2014 10:46|
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