The electrochemical oxidation of anodic Ti, Fe, Cd, Sn, and Pb (= M) into acetonitrile solutions of N, N'-bis(salicylidene)-o-phenylenediamine [SalophH(2)] gives the corresponding M(Saloph) complexes in high yield. The mechanism of the electrochemical reactions is discussed. SalophH(2) forms complexes (1:1 molar ratio) with titanium, iron, cadmium, tin, and lead ions. The complexes have been characterized by elemental analyses, molar conductivity measurements, and infrared and electronic spectral data. The SalophH(2) complexes of iron(II) and cadmium(II) have been further identified by H-1-NMR and mass spectra.