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.
The N-methyl-2-(methylamino)troponimine [(Me)(2)ATI]H reacts with bis[bis(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 Å) at 183 K: [(Me)(2)ATI](2)Sn, C(18)H(22)N(4)Sn, a = 8.4347(11) Å, b = 10.5564(13) Å, c = 11.5527(11) Å, alpha = 66.931(8) degrees, beta = 73.579(9) degrees, gamma = 67.437(7) degrees, V = 863.3(2) Å(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) Å, b = 9.5834(9) Å, c = 16.0132(12) Å, beta = 107.418(8) degrees, V = 1895.8(3) Å(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) Å, b = 8.004(2) Å, c = 19.339(3) Å, beta = 101.537(13) degrees, V = 3691.1(11) Å(3), monoclinic, space group C2/c, Z = 8, R = 0.0224.
Dias
H. V. Rasika
HV
Department of Chemistry and Biochemistry, The University of Texas at Arlington, Arlington, Texas 76019-0065.
Jin
Wiechang
W