The reaction of [M(L)]Cl 2 Á 2H 2 O (M = Ni 2+ and Cu 2+ , L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4, 0 1.18 ,0 7.12 ]docosane) with 1,1-cyclobutanedicarboxylic acid (H 2 -cbdc) generates 1D and 2D hydrogen-bonded infinite chains [Ni(L)(H-cbdc -) 2 ] (1) and [Cu(L)(H-cbdc -) 2 ] (2).(H-cbdc -= cyclobutane-1-carboxylic acid-1-carboxylate). These complexes have been characterized by X-ray crystallography, spectroscopy, and cyclic voltammetry. The crystal structure of 1 shows a distorted octahedral coordination geometry around the nickel(II) ion, with four secondary amines and two oxygen atoms of the H-cbdc -ligand at the trans position. In 2, the coordination environment around the central copper(II) ion shows a Jahn-Teller distorted octahedron with four Cu-N bonds and two long Cu-O distances. The cyclic voltammogram of the complexes undergoes two oneelectron waves corresponding to M II /M III and M II /M I processes. The electronic spectra and electrochemical behavior of the complexes are significantly affected by the nature of the axial H-cbdc -ligand.