The oxidation of Ru(NH 3) 5NCCH 2CN 2+ complex by the peroxydisulfate ion in the aqueous solution yields two products, (Equation Presented). The distribution of the products and the amount of oxidant required for the maximum yield of the binuclear complex depend on the acidity of the solution. The production of the binuclear complex was favored at lower acid concentrations. The formation of CC bond in the binuclear complex was characterized by both the spectral and the electrochemical results. A mechanism for the oxidation has been proposed by the kinetic studies in the region of 0.001-0.10 M acid concentrations. ? 2004 Elsevier B.V. All rights reserved.