K28Li5H7[P8W48O184]•92H2O (0.050 g, 3.37 × 10−6 mol) and LiCl (0.2 g, 4.74 × 10−3 mol) were dissolved in 5 mL of a 1 M HCOOH/HCOONa buffer at pH = 3.7. The uranium salt UO2(NO3)2•6H2O (0.0133 g, 2.65 × 10−5 mol) was added, and the mixture was heated up to 160 °C during 30 h in a 23 mL Teflon-lined stainless autoclave. The large amount of LiCl is tentatively used to decrease the number of potassium cations encapsulated within the [P8W48O184]40− entity and also helps for the solubilization of the final product. The resulting solution was separated from an insoluble residue, and yellowish crystals were obtained after a few days by solvent evaporation in an opened beaker under air atmosphere.