A new one-dimensional uranium(VI) coordination polymer, [UO2(μ-DMP)2(TMP)]n (1) (DMP is dimethyl phosphate and TMP is trimethyl phosphate), was prepared from the reaction of UO2(NO3)2.6H2O and TMP in in THF (THF is tetrahydrofuran) as a solvent. Suitable crystals of this complex for crystal structure determination were obtained by slow evaporation of the produced yellow solution at room temperature. Complex 1 was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The X-ray structural analysis indicated that the uranium(VI) is seven-coordinated in a pentagonal bipyramidal configuration by two axial uranyl oxygens, four bridged dimethyl phosphate and monodentate trimethyl phosphate ligands. Also, the thermal stability of 1 was studied by thermogravimetric and differential thermal analyses.