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The synthesis and characterization of a {CuNO}¹⁰ complex, namely, [Cu(CH₃NO₂)₅(NO)][PF₆]₂, has been achieved by the addition of [NO][PF₆] to copper metal powder in the presence of nitromethane. In the solid state, this complex exhibits a bent Cu−N−O moiety [Cu−N−O = 121.0(3)°] and a long Cu−N bond. This complex readily reacts with mesitylene to form [mesitylene, NO][PF₆] and [Cu(η²-1,3,5-Me₃C₆H₃)₂][PF₆] by transfer of NO⁺ to the mesitylene ring.