The complexes [M(Hdamsm) 2 ]XÁH 2 O (M = Fe, X = NO 3 ; M = Ru, X = Cl), [Ru(Hdamsm)(PPh 3 ) 2 X 0 ] (X 0 = Cl, Br), and [VO(Hdamsm)(acac)] (H 2 damsm = diacetylmonoxime Schiff base of S-methyldithiocarbazate, Hacac = acetylacetone) have been prepared and characterized by spectroscopic techniques. Their redox properties were investigated by cyclic voltammetry. The X-ray crystal structure of [Fe(Hdamsm) 2 ]NO 3 .H 2 O has been determined and shows that the complex has a distorted octahedral geometry in which the Hdamsm behaves as a monoanionic NNS tridentate ligand coordinating via oxime nitrogen, hydrazinic imine nitrogen, and thiolate sulfur. The reactivity of these complexes toward oxidation of alcohols in the presence of t-BuOOH and H 2 O 2 as co-oxidants is reported.