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The metal‐stabilized thiyl radical complex [Ru(SP)3]+, [Ru‐1]+, {SP = 2‐(diphenylphosphanyl)benzenethiolate} adds 1‐octyne across the cis‐sulfur sites to yield the S‐alkylated dithiolene product [Ru‐1·octyne]+. The product complex exists as a pair of inseparable geometric isomers, which were characterized by X‐ray crystallography, 31P NMR spectroscopy, and cyclic voltammetry. By using electrochemical...
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