[NH3(CH2)2NH3]3[(UO2)2O2(C2O4)4]·4H2O (1), [NH3(CH2)2NH2(CH2)2NH3]2[(UO2)2O2(C2O4)4]·2H2O (2) and [NH3(CH2)2NH2(CH2)2NH3]2[(UO2)2O2(C2O4)4] (3) were synthesized in situ under room temperature and laboratory lamp condition, using 1,2-diaminoethane and 2,2'-diaminodiethylamine separately as templates. Structures and properties were characterized by single-crystal X-ray diffraction, Raman spectra, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The dihedral angle of U-O2-U in 1 and 2 is 180°, which deviates from the natural angle of peroxide. The peroxide bond length of 2 and 3 is shorter than that of the reported peroxide, and the bond lenth of 2 is close to superoxide bond length. However, both valence and Raman spectra indicated that 2 and 3 are peroxide bonds.