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Synthesis of Thiolato Heterometalllc Clusters from the Reaction of Os 3 (CO) 9 (NCMe)(μ‐H)(μ‐SMe) with CpW(CO) 3 H
Author(s) -
Tsay ChyuanWu,
Tu WenCheng,
Chi Yun,
Peng ShieMing,
Lee GeneHsiang
Publication year - 1994
Publication title -
journal of the chinese chemical society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.329
H-Index - 45
eISSN - 2192-6549
pISSN - 0009-4536
DOI - 10.1002/jccs.199400086
Subject(s) - chemistry , acetonitrile , decarbonylation , crystal structure , crystallography , ligand (biochemistry) , cluster (spacecraft) , x ray crystallography , stereochemistry , metal , diffraction , catalysis , organic chemistry , receptor , physics , biochemistry , computer science , programming language , optics
Decarbonylation of triosmium methylthiolato cluster Os 3 (CO) 10 (μ‐H)(μ‐SMe) with Me 3 NO in acetonitrile solution gave cluster Os 3 (CO) 9 (NCMe)(μ‐H)(μ‐SMe) (1), in which one axial CO on the non‐bridged Os atom is replaced by an acetonitrile ligand. Crystal data for 2 : space group P bca, a = 14.491(1), b = 16.107(5), c = 16.639(5) Å, Z = 8; R F = 0.037, R w = 0.033. Treatment of 2 with CpW(CO) 3 H in refluxing THF solution yielded two cluster compounds with formula CpWOs 3 (CO) 11 (μ‐H) 2 (μ 3 ‐SMe) ( 2 ) and CpWOs 3 (CO) 11 (μ‐H) 2 (μ‐SMe) ( 3 ) as the principle products. The first possesses a spiked‐triangular geometry with a triply bridging thiolato ligand and the second adopts a butterfly metal core arrangement with an edge‐bridging thiolato grouping. The structure of 2 was characterized by single‐crystal X‐ray diffraction. Crystal data: space group P 1, a = 8.865(5), b = 8.959(3), c = 16.688(4) Å, α = 103.49(2), β = 93–58(3), γ = 113.03(4)°, Z = 2, R F = 0.034, R w = 0.035.