A oxovanadium(Ⅴ) complex of [VOL(C9H6NO)] ·CH2Cl2 [H2L=2-hydroxy-1-naphthaldehyde 4-methoxybenzoylhydrazone, C9H6NO-=8-hydroxyquinoline anion] has been synthesized and characterized by elemental analyses, IR and single crystal X-ray diffraction. The crystal crystallizes in triclinic system, the space group is P1,with the crystal cell parameters a=1.087 0(2) nm, b=1.107 1(2) nm, c=1.269 3(3) nm, α=67.84(3)°, β=79.26(3)°,γ=73.85(3)° and V=1.353 1(6) nm3, Mr=614.34, R=0.0503, wR=0.1409. The V(Ⅴ) atom is six-coordinated by one O atom of oxo group, two O atoms and one N atom of the tridentate hydrazone ligand, as well as one N atom and one O atom of 8-hydroxyquinoline ligand, thus defining a distorted octahedral VO(ONO)(NO) geometry. A twodimensional supramolecular layer structure is formed through π-π stacking interactions.CCDC:268672.