Abstract
The reaction of Cp ★ 2Mo 2S 4 ( 1) (Cp ★ = η 5-C 5Me 5) with CuCl gives the polynuclear clusters of Cp ★ 2Mo 2CuClS 4 ( 2, 4) and Cp ★ 2Mo 2Cu 2Cl 2S 4 ( 3, 5) under expansion of the MoS skeleton. The structures of these clusters are determined by the structures of the Mo-substrates ( 1A + CuCl → 2 + 3; 1C + CuCl → 3 + 5), thus permitting elucidation of the reaction pathway. The 62e-cluster 3 possesses a distorted cuban-like M 4S 4 core with 5 MM bonds as shown by an X-ray diffraction study. One or two CuCl moieties are replaced by Fe(NO) when 3 is irradiated in the presence of [N(PPh 3) 2][Fe(CO) 3NO]. In a metathetical reaction with NaSPh, 3 gives Cp ★ 2Mo 2Cu 2(SPh) 2S 4 ( 8).
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