Under hydrothermal conditions, a 1D chain-like Keggin-based hybrid, [Cu2(H3L)2] (SiMo12O40) (H2L=2,6-dimethyl-3,5-bis(pyrazol-3- yl)pyridine), was successfully prepared using utilizing CuCl2?2H2O, Na2SiO3, Na2MoO4 and 2,6-dimethyl-3,5-bis(pyrazol-3-yl) pyridine as starting materials. The crystal structure of the compound was characterized by single crystal X-ray diffraction analysis, TGA, IR spectra and elemental analysis.The results show that the compound crystallizes in the triclinic system, space group P-1 with a=1.168 9(5) nm, b=1.215 7(5) nm, c=1.223 3(5) nm, α=62.066(5)°, β= 62.833(5)°, γ=74.789(5)°, V=1.363 8(10) nm3, Z=2, R1=0.082 4, wR2=0.174 5. In addition, the electrochemical properties of the compound display better electrocatalytic activity toward the reduction of nitrite.