Oxovanadium(IV/V) complexes of 2-hydroxyacetophenone-3-hydroxy-2-naphthoylhydrazone (H 2 L) have been synthesized and characterized. The complexes were characterized by elemental analyses, IR, electronic and EPR spectra. The oxovanadium(V) complex [VOL (OCH 3 )] is crystallized in two polymorphic forms, denoted by 1a and 1b, with space groups Pn2 1 a and P" 1 , respectively. Both have distorted square pyramidal structures.