Six-coordinate molybdenum(Ⅴ)-oxo complexes (PyH)[MoOCl2L] and (R4N)-[MoOCl2L] (R=CH3 and C2H5) with N-salicylidene-2-aminophenol(L1) and its derivatives(L2=5-CH3, L3=3-CH3O, L4=5,6-C4H4 and L5=5-NO2) as ONO-donor ligands have been synthesized and the spectral and electrochemical properties of the complexes by elemental analysis, molar conductivity, UV-vis, IR, 1H NMR and CV have been studied.