The title complex [ CuL3 ] (C1O4)2 · 2H2O· 2CH3CN (L = 1, 10-phenanthroline-5, 6-dione) has been synthesized and characterized by elemental analysis, conductivity, infrared and UV-Vis spectra. X-ray diffraction analysis at room temperature indicates that the complex (C40H28Cl2 CuNsO16, Mr = 1011.14) crystallizes in orthorhombic system, space group P21 21 21 with a = 13. 983(1), b = 14. 310 (1), c =20.890(2) (A。), V = 4179.7(6) (A。)3, Z = 4, Dc= 1.607g/cm3, F(000) = 2026,μ(MoKa) = 0.736 mm-1. The final R and w,R factors are 0.0446 and 0. 1212 respectively with 8545 independent reflections. The title complex is composed of a discrete [CuL3 ]2+ cation, uncoordinated ClO4- anions, H2O and CH3CN molecules. The central Cu(Ⅱ) atom is six-coordinated by six nitrogen donors of three ligands. The coordination geometry of Cu(Ⅱ) could be considered as an approximately ideal octahedral configuration with little static Jahn-Teller distortion (the longest and shortest Cu- N bonds are 2. 102 vs 2. 139 (A。) with the mean length of 2. 122 (A。) ), which is very rare for a six-coordinated Cu(Ⅱ) complex.