The reaction of V2O5 with mixed ligands in water leaded to the formation of complex [(VO3)(2)center dot(HL2-)(2)center dot(HL1)(2)] (1) (H3L = pyridine-2,4,6-tricarboxylic acid; HL1 = isonicotinic acid). This complex is characterized by SEM, X-ray single-crystal diffraction, TGA and UV-Visible diffuse reflectance spectroscopy (UV-Vis DRS). The results show that 1 belongs to the triclinic system, P-1 space group, with a = 8.5626(10) angstrom, b = 9.8337(12) angstrom, c = 10.7188(12) angstrom, alpha = 93.8250(10)degrees; beta = 112.3410(10)degrees; gamma = 109.8270(10)degrees, V = 765.20(16) angstrom(3), Mr = 832.34. Its band gap is 2.8 ev, surface area is 35.6 m(2)/g, and it can be stable within 200 degrees C. The photocatalytic degradation rate of methylene blue (MB) is 0.041 mg/L.min, which is 1.6 times of P-25.