Molybdenum monooxo compoundsMoO(OAr)4-nCln (n=0-2, Ar=2,6-Me2C6H3 or 2,6-i-Pr2C6H3) have been synthesized starting from the dioxo precursor MoO2Cl2. The complexes are characterized spectroscopically and by X-ray diffraction. The formation mechanism likely involves phenol precoordination followed by addition across the Mo=O bond.