A novel templated uranium oxalate/glycolate, (UO2)4(O)2(C2O4)(H2C2O3)2.2[(C8H20)N] (a = 7.9230(8) A, b = 13.3793(13) A, c = 17.4141(18) A, beta = 96.006(2) degrees , monoclinic, P21/n, Z = 2), has been synthesized under hydrothermal conditions via in-situ ligand synthesis. The oxalate and glycolate anions have been formed through the oxidation of 1,4-diazabicyclo[2.2.2]octane, which proceeds through intermediates such as piperazine and ethylene glycol. Reported herein is the synthesis of this compound, crystal structure, and mechanistic information regarding the oxidation pathway.