Abstract
The first organogallium four-membered ring compounds with arsenic, halogen mixed bridging to be characterized completely, Ph 2 GaAs(SiMe 3) 2Ga(Ph) 2X (X = Cl ( 1) and X = Br ( 2)) were prepared by the reaction of (Me 3Si) 3As ( 3) with Ph 2GaCl and Ph 2GaBr, respectively. X-ray crystallographic analyses show the compounds to be isostructural with each containing a non-planar Ga-As-Ga-X four membered ring. Isomorphous crystals of 1 and 2 belong to the monoclinic system, space group P2 1/ c ( C 5 2 h ), with four molecules in unit cells of dimensions: a 10.560(3), b 15.797(3), c 20.591(4) Å, β 92.17(2)°, V 3433(2) Å 3 for 1, and a 10.653(1), b 15.777(2), c 20.517(2) Å, β 91.97(1)°, V 3446(1) Å 3 for 2. The non-planarity of the rings is manifested in the halogen atom displacements of 0.256 Å in 1 and 0.293 Å in 2 from the respective Ga-As-Ga′ planes. Deviations from overall C 2 v symmetry serve to relieve unfavorable intramolecular bulky ring substituent interactions present in such a symmetric form. The dimer [Ph 2GaAs(SiMe 3) 2] 2 ( 4), obtained from the reaction of Ph 2GaCl and LiAs(SiMe 3) 2, has been characterized by partial elemental analysis, NMR spectroscopy and cryoscopic molecular weight determination. An alternative route to the synthesis of 1 by reaction of 4 and Ph 2GaCl was investigated via NMR spectroscopy.
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