Synthesis and Characterization of Molybdenum(0) and Tungsten(0) Complexes of Tetramethylthiourea: Single-Source Precursors for MoS2 and WS2

作者: John P. Shupp , Adam S. Kinne , Hadi D. Arman , Zachary J. Tonzetich

DOI: 10.1021/OM500567Y

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摘要: The molybdenum(0) and tungsten(0) carbonyl complexes, [M(CO)n(TMTU)6–n] (M = Mo W; TMTU tetramethylthiourea; n 4 5), have been prepared by addition of to the appropriate precursors. In solid state, compounds are monomeric feature octahedral coordination geometries about metal. case [M(CO)4(TMTU)2], ligands bound in a cis fashion. Dissolution cis-[M(CO)4(TMTU)2] produces an equilibrium mixture cis-[M(CO)4(TMTU)2], free TMTU, putative dimeric species, cis,cis-[M2(CO)8(μ-TMTU)2]. Attempts prepare tricarbonyl complex, [Mo(CO)3(TMTU)3], fac-[Mo(CO)3(η6-cycloheptatriene)] results isolation cis-[Mo(CO)4(TMTU)2], demonstrating that exchange CO is facile these compounds. Each decomposes readily state above 110 °C, ultimately forming tetravalent metal disulfide. Thermolysis reactions complexes at 300 °C under argon atmosph...

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