The synthesis and spectroscopic characterization of the first silylated mixed‐chalcogen reagent, Me3Si–SeS–SiMe3, is presented. This reagent is shown to be an effective and efficient delivery source of both sulfur and selenium as demonstrated in the synthesis of a [Cu84Se42–xSx(PEt2Ph)24] (x ≈ 15) cluster. The reaction proceeds with chalcogen‐chalcogen bond cleavage and the resulting X‐ray crystal structure of [Cu84Se42–xSx(PEt2Ph)24] illustrates the intimate mixing of sulfur and selenium within the cluster core.
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Turner et al. (2007) studied this question.
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