A new cobaloxime was synthesized by the reaction of cobalt chloride and diphenylglyoxime in methanol, followed by the addition of 4 '-(4-pyridyl)-2,2 ':6 ',2 ''-terpyridine, pytpy. This complex was characterized by UV-Vis spectroscopy, H-1-NMR spectroscopy, cyclic voltammetry, and single-crystal X-ray diffraction analysis. In cyclic voltammetry experiments an irreversible reduction wave assigned to Co(III)/Co(II) at Ecp = -0.31 V vs. Ag/AgCl and a quasi-reversible process assigned to the Co(II)/Co(I) reduction at -0.72 V vs. Ag/AgCl were observed. The crystal of the complex belongs to the triclinic space group P1 with a = 12.4698(6) angstrom, b = 14.1285(8) angstrom, c = 15.5801(8) angstrom, alpha = 109.681(4)degrees, beta = 112.975(4)degrees, gamma = 81.67(96.414(4)degrees 3)degrees, V = 2284.0(2) angstrom(3), Z = 2, Dc = 1.408 mg.m (-3), mu = 0.66 mm(-1), F(000) = 996, and final R1 = 0.0564, omega R2 = 0.1502.