Isolation and characterisation by X-ray studies of palladium µ2-nitrosyl clusters in the reduction of nitric acid by carbon monoxide mediated by palladium acetate

Abstract

In the reduction by CO of HNO₃ to NO, mediated by [Pd₃(O₂CMe)₆] in acetic acid, [Pd₃(O₂CMe)₅(η²-NO₂)](1) is formed first, but is converted under the reaction conditions into the known cluster [Pd₄(O₂CMe)₆(µ₂-NO)₂](2); slow crystallization of (1) from wet benzene and pentane gives (2) and [Pd₆(O₂CMe)₈(µ₂-NO)₂](3), the structures of (1) and (3) having been determined by X-ray crystallography.