A new uranium fluoride phosphate, UFPO4, was synthesized via a mild hydrothermal route and characterized optically, thermally, and magnetically. Two thermal transformation products, U2O(PO4)(2) and (UUO2)-U-IV-O-VI(PO4)(2), were discovered to be structurally related, and were subsequently synthesized for bulk property measurements. All three materials failed to follow Curie-Weiss behavior at low temperatures, attributed to the nearly ubiquitous singlet ground state of U(IV), transitioning into a Curie-Weiss paramagnetic regime at high temperatures. Neutron diffraction experiments were performed on UFPO4 and (UUO2)-U-IV-O-VI(PO4)(2) in order to characterize this unusual magnetic behavior.