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Preparation of Mononuclear Tungsten Tris(sulfido) and Molybdenum Sulfido−Tetrasulfido Complexes with Hydridotris(pyrazolyl)borate Coligand and Conversion of the Former into Sulfido-Bridged Bimetallic Complex Having Pt(μ-S)2WS Core

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posted on 02.03.2001, 00:00 by Hidetake Seino, Yasushi Arai, Naohisa Iwata, Shoken Nagao, Yasushi Mizobe, Masanobu Hidai
Treatment of [Et4N][(Me2Tp)W(CO)3] (Me2Tp = HB(3,5-dimethylpyrazol-1-yl)3) with S8 in DMF at room temperature afforded a tris(sulfido) complex [Et4N][(Me2Tp)WS3] (1a), while that of [Et4N][TpW(CO)3] (Tp = HB(pyrazol-1-yl)3) in MeCN resulted in the formation of [Et4N][TpWS3] (1b) along with [Et4N]2[{WO(S2)2}2(μ-S)] (6) as a byproduct. Under similar conditions, [Et4N][(Me2Tp)Mo(CO)3] gave a mixture of a sulfido−tetrasulfido complex [Et4N][(Me2Tp)MoS(S4)] (2a) and its monooxo analogue [Et4N][(Me2Tp)MoO(S4)], although a sulfido−tetrasulfido complex [Et4N][TpMoS(S4)] (2b) was exclusively obtained from [Et4N][TpMo(CO)3]. The reaction of 1a with [PtCl2(cod)] (cod = 1,5-cyclooctadiene) in MeCN at room temperature led to the formation of a sulfido-bridged mixed-metal complex [Et4N][(Me2Tp)WS(μ-S)2PtCl2] (10). The structures of new complexes have been determined in detail by the X-ray analyses for 1a·MeCN, 1b, 2a, 2b, 6, and 10.

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