Dioxomolybdenum(VI) complexes of the type MoO2X2L2 (X, L = Cl, OPPh3 (1); Br, OPPh3 (2); Cl, OPMePh2 (3); Br, OPMePh2 (4)) were synthesized and characterized by the melting point, elemental analysis, infrared spectroscopy (IR), and nuclear magnetic resonance (H-1 NMR and P-31 NMR). Using a static analytical method, the solubilities of 1 to 4 were measured in dichloromethane in the temperature range from (283.16 to 310.41) K and in H2O2 (30 % (by weight)) + H2O solution from (298.02 to 358.82) K, respectively. It was found that the solubilities of 1 to 4 in dichloromethane and H2O2 (30 % (by weight)) + H2O solution decreased in the order 3 > 4 > 1 > 2. The solubility data were correlated with an empirical equation.