Triangular [MoS] clusters are known to serve as platforms to accommodate a metal atom M, furnishing cubic [MoSM] clusters. In this study, three [MoS] clusters supported by η-cyclopentadienyl (Cp) ligands, [CpMoS] (Cp = CMeSiMe, CMeSiEt, and CMeH), were synthesized via half-sandwich molybdenum chlorides CpMoCl. In the cyclic voltammogram of the [MoS] cluster having CMeH ligands, a weak feature appeared in addition to the [CpMoS] redox process, indicating the interaction between [CpMoS] and the [NBu] cation of the electrolyte, while such a feature was less significant for the CMeSiR variants. The [MoS] clusters with bulky CMeSiR ligands were successfully applied as platforms to accommodate an Fe atom to furnish cubic [MoSFe] clusters. On the other hand, the corresponding reactions of the less bulky CMeH analogue gave complex mixtures.
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