Abstract
Methylation of the molybdenum sulfide cluster unit [Mo6S8(PEt3)6] (1) with CH3OTf resulted in the formation of mono‐ and dimethylated cluster units, [Mo6S8–x(SCH3)x(PEt3)6]OTf·yCH2Cl2 {[2]OTf·0.5CH2Cl2 (x = 1, y = 0.5) and [3]OTf·CH2Cl2 (x = 2, y = 1)}. Structural and electrochemical investigations revealed that the methylation of the µ3‐S ligand(s) induced a characteristic structural distortion of the [Mo6S8] cluster core and enhanced its ability to accept multiple electrons.
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