A new hydrazone Schiff base, (E)-N'-(3-ethoxy-2-hydroxybenzylidene)isonicotinohydrazide (H 2 L), has been prepared and characterized by elemental analyses, spectroscopic methods, and single crystal X-ray diffraction. The corresponding dioxomolybdenum(VI) complex [Mo(O) 2 (L)(CH 3 OH)] was synthesized and characterized by spectroscopic methods and by single crystal X-ray diffraction. The hydrazone ligand coordinates to Mo through the phenolate O, imine N, and enolic O. The Mo center displays a distorted octahedral geometry, with the three donors of the ligands and an oxo defining the equatorial plane, and one methanol and another oxo occupying the axial positions.