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N-Methyl-2-(methylamino)troponiminate Complexes of Tin(II), Gallium(III), and Indium(III). Syntheses of [(Me)(2)ATI](2)GaI and [(Me)(2)ATI](2)InCl Using the Tin(II) Reagent [(Me)(2)ATI](2)Sn
Authors:Dias H V Rasika  Jin Wiechang
Institution:Department of Chemistry and Biochemistry, The University of Texas at Arlington, Arlington, Texas 76019-0065.
Abstract:The N-methyl-2-(methylamino)troponimine (Me)(2)ATI]H reacts with bisbis(trimethylsilyl)amido]tin(II) to yield (Me)(2)ATI](2)Sn in excellent yield. The treatment of (Me)(2)ATI](2)Sn with GaI and InCl led to the bis(ligand)gallium(III) and -indium(III) compounds (Me)(2)ATI](2)GaI and (Me)(2)ATI](2)InCl. These metal complexes were characterized by elemental analysis, (1)H and (13)C NMR spectroscopy, and X-ray crystallography. All three metal adducts show fluxional behavior in solution at room temperature. (Me)(2)ATI](2)Sn exhibits a pseudo trigonal bipyramidal structure in the solid state. The gallium and indium atoms in (Me)(2)ATI](2)GaI and (Me)(2)ATI](2)InCl adopt trigonal bipyramidal geometry around the metal center with the halide occupying an equatorial site. A convenient, high-yield route to (Me)(2)ATI]H is also reported. Crystal data with Mo Kalpha (lambda = 0.710 73 ?) at 183 K: (Me)(2)ATI](2)Sn, C(18)H(22)N(4)Sn, a = 8.4347(11) ?, b = 10.5564(13) ?, c = 11.5527(11) ?, alpha = 66.931(8) degrees, beta = 73.579(9) degrees, gamma = 67.437(7) degrees, V = 863.3(2) ?(3), triclinic, space group P&onemacr;, Z = 2, R = 0.0224; (Me)(2)ATI](2)GaI, C(18)H(22)GaIN(4), a = 12.947(2) ?, b = 9.5834(9) ?, c = 16.0132(12) ?, beta = 107.418(8) degrees, V = 1895.8(3) ?(3), monoclinic, space group P2(1)/c, Z = 4, R = 0.0214; (Me)(2)ATI](2)InCl, C(18)H(22)ClInN(4), a = 24.337(3) ?, b = 8.004(2) ?, c = 19.339(3) ?, beta = 101.537(13) degrees, V = 3691.1(11) ?(3), monoclinic, space group C2/c, Z = 8, R = 0.0224.
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