Abstract: The synthesis and characterization of a novel mixed-valent uranium oxyfluoride is described; the inorganic network consists of 2-D [U2F10]2- sheets constructed from corner- and edge-sharing UIVF9 tricapped trigonal prisms and 1-D [UO2F3]- chains constructed from edge-sharing UVIO2F5 pentagonal bipyramids with the organic cations and water molecules between the sheets. This is the first example with a hybrid network structure in the system of uranium fluoride or oxyfluoride. The variable-temperature magnetic susceptibility confirms the oxidation state of the uranium ions. Crystal data follow: C6H25N4O4F13U3, monoclinic, space group P21 (No. 4); a = 8.6876(4) Å, b = 7.3158(4) Å, c = 16.3376(8) Å, β = 93.7285(9)°, V = 1036.2(2) Å3, and Z = 2.