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An unprecedented redox-neutral S-nitrosation of thiol has been achieved at dicopper(I,I) center. Treatment of dicopper (I,I) complex with excess NO• and thiol generates a dicopper (I,I) di-S-nitrosothiol complex [CuICuI(RSNO)2]2+ or dicopper (I,I) mono-S-nitrosothiol complex [CuICuI(RSNO)]2+, which readily release RSNO in 88-94% yield. The S-nitrosation reaction proceeds through a mixed-valence [CuIICuIII(m-O)(m-NO)]2+ species, which deprotonates RS-H at the basic m-O site and nitrosates thedoi:10.26434/chemrxiv.14160968.v1 fatcat:oe7amnvya5gdpoysmkli42tufq