Salicylaldehyde or 5-bromosalicylaldehyde reacted with 2,3-diaminophenol in absolute EtOH in a 2:1 molar ratio to give new unsymmetrical Schiff bases (H 2 L). The bases were used as ligands to coordinate Mn(III), Ni(II) and Cu(II) chlorides leading to [Mn III ClL] AE EtOH and [M II L] or [M II L] AE 2H 2 O (M=Ni or Cu) complexes. Their structures were determined using mass spectroscopy, IR, u.v.-vis and 1 H-n.m.r. The cyclic voltammetry in acetonitrile showed irreversible waves for both ligands. Under the same experimental conditions, the complexes exhibited mainly the non-reversible reduction of the Ni(II) or Cu(II) ion to Ni(0) or Cu(0), while the reduction of Mn(III) to Mn(II) was found to be a quite reversible phenomenon.