The molecular structure oftrans-dichlorodioxobis(triphenylphosphate) molybdenum(VI), MoO2Cl2[OP(OPh)3]2has been determined. Crystal data: Monoclinic,Pn, a = 11.767(2), b = 10.341(2), c = 15.682(3) Å,β= 92.27(3)°, V = 1906.8(7) Å-3, Z = 2. Trans-dichlorodioxobis(triphenylphosphate)molybdenum(VI) was obtained by the reaction of molybdenum oxide, HCl and triphenylphosphate and was characterized by elemental analysis, IR, and1H-NMR spectroscopy.