Synthesis and Characterization of Indium Compounds with Phosphinothiol Ligands. The Crystal and Molecular Structures of [In{2-(Ph2P)C6H4S}3], [In{2-(Ph
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- 作者：Paulo Pé ; rez-Lourido ; Jaime Romero ; José ; Arturo Garcí ; a-Vá ; zquez ; Antonio Sousa ; Kevin Maresca ; and Jon Zubieta
- 刊名：Inorganic Chemistry
- 出版年：1999
- 出版时间：March 22, 1999
- 年：1999
- 卷：38
- 期：6
- 页码：1293 - 1298
- 全文大小：149K
- 年卷期：v.38,no.6(March 22, 1999)
- ISSN：1520-510X
文摘
The electrochemical oxidation of anodic indium metal in an acetonitrile solution of phosphinothiol ligands affords[In{2-(Ph2P)C6H4S}3] (1), [In{2-(Ph2P)-6-(Me3Si)C6H3S)}2{2-(Ph2PO)-6-(Me3Si)C6H3S}] (2), [In{2-(Ph2PO)-6-(Me3Si)C6H3S}3] (3), and [NMe4][In{PhP(C6H4S-2)2}2]·CH3CN (4) complexes exhibiting distorted six-coordinategeometries based on {InS3P3}, {InS3P2O}, and {InS4P2} cores, respectively. In all cases, the In-P bond distancesare anomalously long, presumably as a consequence of steric crowding. The anion of 4 provides an unusualexample of an In(III)-thiolate coordination complex ion. Crystal data: 1, C54H42InP3S3, monoclinic, P21/c, a =16.6579(1) Å, b = 12.6628(2) Å, c = 22.5520(3) Å, 
= 96.42(1)
, V = 4727.15(1) Å3, Z = 4, 6176 reflections,R = 0.0579; 2, C63H66InOP3S3Si3, monoclinic, P21/c, a = 11.53090(10) Å, b = 26.2505(3) Å, c = 20.4206(2)Å, = 94.0870(10), V = 6165.43(11) Å3, Z = 4, 10 699 reflections, R = 0.0621; 4, C42H41InN2P2S4, monoclinic,P2(1), a = 13.0052(2) Å, b = 11.2240(2) Å, c = 14.3070(3) Å, = 93.190(1), V = 2085.16(7) Å3, Z = 2, 6651reflections, R = 0.0352.
= 96.42(1), V = 4727.15(1) Å3, Z = 4, 6176 reflections,R = 0.0579; 2, C63H66InOP3S3Si3, monoclinic, P21/c, a = 11.53090(10) Å, b = 26.2505(3) Å, c = 20.4206(2)Å, = 94.0870(10), V = 6165.43(11) Å3, Z = 4, 10 699 reflections, R = 0.0621; 4, C42H41InN2P2S4, monoclinic,P2(1), a = 13.0052(2) Å, b = 11.2240(2) Å, c = 14.3070(3) Å, = 93.190(1), V = 2085.16(7) Å3, Z = 2, 6651reflections, R = 0.0352.