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Synthesis and Characterization of Indium Compounds with Phosphinothiol Ligands. The Crystal and Molecular Structures of [In{2-(Ph(2)P)C(6)H(4)S}(3)], [In{2-(Ph(2)P)-6-(Me(3)Si)C(6)H(3)S}(2){2-(Ph(2)PO)-6-(Me(3)Si)C(6)H(3)S}], and [NMe(4)][In{PhP(C(6)H(4)S-2)(2)}(2)].CH(3)CN. 1999

Paulo Pérez-Lourido, and Jaime Romero, and José Arturo García-Vázquez, and Antonio Sousa, and Kevin Maresca, and Jon Zubieta
Department of Chemistry, Syracuse University, Syracuse, New York 13244.

The electrochemical oxidation of anodic indium metal in an acetonitrile solution of phosphinothiol ligands affords [In{2-(Ph(2)P)C(6)H(4)S}(3)] (1), [In{2-(Ph(2)P)-6-(Me(3)Si)C(6)H(3)S)}(2){2-(Ph(2)PO)-6-(Me(3)Si)C(6)H(3)S}] (2), [In{2-(Ph(2)PO)-6-(Me(3)Si)C(6)H(3)S}(3)] (3), and [NMe(4)][In{PhP(C(6)H(4)S-2)(2)}(2)].CH(3)CN (4) complexes exhibiting distorted six-coordinate geometries based on {InS(3)P(3)}, {InS(3)P(2)O}, and {InS(4)P(2)} cores, respectively. In all cases, the In-P bond distances are anomalously long, presumably as a consequence of steric crowding. The anion of 4 provides an unusual example of an In(III)-thiolate coordination complex ion. Crystal data: 1, C(54)H(42)InP(3)S(3), monoclinic, P2(1)/c, a = 16.6579(1) Å, b = 12.6628(2) Å, c = 22.5520(3) Å, beta = 96.42(1) degrees, V = 4727.15(1) Å(3), Z = 4, 6176 reflections, R = 0.0579; 2, C(63)H(66)InOP(3)S(3)Si(3), monoclinic, P2(1)/c, a = 11.53090(10) Å, b = 26.2505(3) Å, c = 20.4206(2) Å, beta = 94.0870(10) degrees, V = 6165.43(11) Å(3), Z = 4, 10 699 reflections, R = 0.0621; 4, C(42)H(41)InN(2)P(2)S(4), monoclinic, P2(1), a = 13.0052(2) Å, b = 11.2240(2) Å, c = 14.3070(3) Å, beta = 93.190(1) degrees, V = 2085.16(7) Å(3), Z = 2, 6651 reflections, R = 0.0352.

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