The reaction of warm EtOH solutions of FeX 3 . nH 2 O (X = Cl, NO 3 ) with tridentate ONX (X = O, S, N) pyridoxal semi-, thiosemi-and S-methylisothiosemicabazones (H 2 L 1 , H 2 L 2 , H 2 L 3 , respectively) yielded high-spin octahedral mono-and bis(ligand) complexes of the formula. H 2 O. The compounds were characterized by elemental analysis, conductometric and magnetochemical measurements, IR and UV-Vis spectra. Besides, a detailed voltammetric study of the complexes was carried out in DMF solution in the presence of several supporting electrolytes, to characterize the nature of the electrode processes and solution equilibria.