TRIANGULAR M3SE7(4+) AND M3SE4(4+) COMPLEXES (M = MO, W) - AN X-RAY STUDY OF MO3SE7(ET2NCS2)4 AND W3SE7(ET2NCS2)4

被引：66

作者：

FEDIN, VP

SOKOLOV, MN

GERASKO, OA

VIROVETS, AV

PODBEREZSKAYA, NV

FEDOROV, VY

机构：

[1] Institute of Inorganic Chemistry, Siberian Branch, the Academy of Sciences, 630090 Novosibirsk

来源：

INORGANICA CHIMICA ACTA | 1991年 / 187卷 / 01期

关键词：

D O I：

10.1016/S0020-1693(00)82980-1

中图分类号：

O61 [无机化学];

学科分类号：

070301 ; 081704 ;

摘要：

New methods for the synthesis of triangular M3Se74+ and M3Se44+ complexes soluble in organic solvents have been developed which proceed from polymeric M3Se7X4 (M = Mo, W; X = Cl, Br). Heating of Mo3Se7Cl4 in a PPh4Cl melt has produced the (PPh4)2Mo3Se7Cl6 salt. Selenobromide complexes of molybdenum and tungsten are less stable and have been converted to M3Se7(dtc)4 complexes by reacting them with NaS2NCEt2.3H2O (Nadtc.3H2O) in CH3CN. The structure of M3Se7(dtc)4 (M = Mo, W) has been determined by X-ray structural analysis: a = 16.728(5), b = 18.604(7), c = 13.324(3) angstrom, beta = 99.12(3)-degrees, Z = 4, P2(1)/c, R(F) = 0.1344 for W3Se7(dtc)4; a = 16.652(5), b = 18.614(8), c = 13.337(3) angstrom, beta = 99.11(2)-degrees, Z = 4, P2(1)/c, R(F) = 0.0628 for Mo3Se7(dtc)4. Heating of M3Se7X4 in a melt of 1,10-phenanthroline (phen) produces salts containing M3Se7(phen)34+ with different anions (Cl-, Br-, ZnCl42-, ZnBr42-). The action of phosphines on M3Se74+ complexes gave M3Se44+ complexes Mo3Se4(dtc)4(PPh3) and Mo3Se4(dppe)3Cl4 (dppe is Ph2PCH2CH2PPh2).

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页码：81 / 90

页数：10

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