The effect of sucrose on the structure of molecular assemblies formed in an MO/H 2 O mixture has been studied using a small-angle X-ray scattering method. It was found that the phase transition Ia3d → Pn3m → H II occurs with increased sucrose concentration in the mixture with the composition 70 wt% MO at 20 °C. This structural change induced by sucrose addition would be ascribed to a cosmotropic property of sucrose, which leads to the dehydration of the MO head group and hence causes a decrease in the effective area occupied by the MO molecule at the polar/apolar interface, which facilitates the formation of molecular assemblies with a high curvature for the reversed liquid-crystal mesophase.