The reaction of [Ni(L)]Cl(2)center dot 2H(2)O (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo [14,4,0(1.18),0(7.12)] docosane) with trans-1,2-cyclopentanedicarboxylic acid (H(2)-cpdc) yields a 1D hydrogen-bonded infinite chain with formula [Ni(L)(H-cpdc(-))(2)] (1). This complex has been characterized by X-ray crystallography, spectroscopy and cyclic voltammetry. The crystal structure of 1 exhibits a distorted octahedral geometry about Ni atom with four nitrogen atoms of the macrocycle and two oxygen atoms of the H-cpdc(-) ligand at the axial position. Compound 1 crystallizes in the monoclinic system P2(1)/c with a = 8.7429(17), b = 10.488(2), c = 18.929(4) angstrom, beta = 91.82(2), V = 1734.8(6) angstrom(3), Z = 2. Electronic spectrum of 1 reveals a high-spin octahedral environment. Cyclic voltammetry of 1 undergoes two waves of a one-electron transfer corresponding to Ni(II)/Ni(III) and Ni(II)/Ni(I) processes.