The electrochemical oxidation of cobalt, nickel, copper, zinc or cadmium anodes in an acetonitrile solution containing N[(2-hydroxyphenyl)methylidine]-N'-tosylbenzene-1,2-diamine (H 2 L) yielded compounds of general formula [ML]. When 1,10-phenanthroline (phen) or 2,2'-bipyridine (bipy) is added to the cell, mixed ligand complexes are obtained. The crystal structures of {(1,10-phenanthroline)[N-(2-oxophenyl)methylidine]-N'-tosylbenzene-1,2-diami nato}nickel(II) (1) and {(1,10-phenanthroline)[N-(2-oxophenyl)methylidine]-N'-tosylbenzene-1,2-diami nato}copper(II) (2) were determined by X-ray diffraction. Compound 1 consists of a binuclear [Ni 2 L 2 1 (phen) 2 ] complex with phenolic oxygen atoms bridging both nickel atoms. Each nickel atom is in a distorted octahedral [NiN 4 O 2 ] environment. Compound 2 is monomeric, with the copper atom in a [CuN 4 O] distorted square pyramidal geometry. The electronic, IR and NMR spectra of the complexes are discussed and related to the structure.