Synthesis of Bis{(2-dimethylphosphino)ethane-1-thiolato}bis(<i>tert</i>-butylthiolato)- molybdenum(IV) and Its Cluster-Forming Reactions with FeCl<sub>2</sub> and CuBr
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Reaction of Mo(StBu)4 with 2 equiv of HSCH2CH2PMe2 (Hdmsp) produced Mo(dmsp)2(StBu)2 (1) in high yield. Treatment of 1 with FeCl2 and CuBr led to the formation of heterometallic clusters, [Mo(O)(dmsp)2]2FeCl2 (2) and [MoBr(dmsp)2(μ3-S)Cu2]2(μ2-StBu)2 (3), respectively. The structures of 1−3 were determined by X-ray analyses. Complex 1 assumes a distorted octahedral geometry with a cis-disposition of two tBuS ligands. In the structure of 2, an FeCl2 unit bridges two square-pyramidal Mo(O)(dmsp)2 fragments through interactions between Fe and dmsp sulfur atoms, where the MoS2Fe quadrilateral is puckered. Formation of 3 involves C−S bond cleavage of one tBuS ligand of 1 and rearrangement of ligands between the Mo and Cu coordination sites, resulting in the structure consisting of two MoCu2BrS(dmsp)2 cluster units and two tBuS bridges.
