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 (UF9)-F-IV tricapped trigonal prisms and 1-D [UO2F3](-) chains constructed from edge-sharing (UO2F5)-O-VI 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 P2(1) (No. 4); a = 8.6876(4) Angstrom, b = 7.3158(4) Angstrom, c = 16.3376(8) Angstrom, 93.7285(9)degrees, V = 1036.2(2) Angstrom(3), and Z = 2.