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-cyclopropanedicarboxylic acid (H 2 -cpdc) generates one-dimensional hydrogen-bonded infinite chains [Ni(L)(H-cpdc) 2 ] (1) and [Cu(L)(H-cpdc) 2 ] (2) (H-cpdc = cyclopropane-1-carboxylic acid-1-carboxylate). These complexes have been characterized by X-ray crystallography, spectroscopy, and cyclic voltammetry. The crystal structures of (1) and (2) show a distorted octahedral coordination geometry around the metal ion, with four secondary amines and two oxygen atoms of the H-cpdc ligand at the trans position. Complexes (1) and (2) display the one-dimensional hydrogenbonded infinite chains. The cyclic voltammogram of the complexes display two one-electron 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-cpdc ligand.