The binuclear copper complex [Cu(H 2 slox)] 2 (1) and heterobinuclear copper and molybdenum complexes [Cu(slox)MoO 2 (A) 2 ] (slox ¼ tetranegative disalicylaldehyde oxaloyldihydrazone) (A ¼ H 2 O (2), py (3), 2-pic (4), 3-pic (5), 4-pic (6)) and [Cu(slox)MoO 2 (NN)] (NN ¼ bpy (7) and phen (8)) have been synthesized from disalicylaldehyde oxaloyldihydrazone in methanol and characterized by various physico-chemical and spectroscopic techniques. The stoichiometry of the complexes has been established based on elemental analyses and thermoanalytical studies. The m eff values for the complexes rule out metal-metal interaction between the metal centers in the structural unit of the complexes. The dihydrazone has keto-enol forms; in 1, it is a dibasic tetradentate bridging ligand in enol form and in heterobinuclear complexes as a tetrabasic hexadentate bridging ligand. Electronic spectra of the complexes show that copper(II) is square-planar in binuclear and heterobinuclear complexes; molybdenum is a distorted octahedral stereochemistry in heterobinuclear complexes. EPR spectra suggest that in all complexes, the unpaired electron is in the d x2Ày2 orbital of copper and that the copper in heterobinuclear complexes is tetrahedrally distorted.