A reticulation mesh Ni 3 O 20 C 18 H 22 was synthesized by hydrothermal reaction of NiCl 2 ·6H 2 O and 1,3,5-benzenetricarboxylic acid as raw materials.The structure was characterized by elemental analysis and single crystal X-ray diffraction analysis.The result show that the coordination polymer crystallizes in triclinic,space group P-1(2),a = 1.001 38(4) nm,b = 1.009 01(4) nm,c = 1.322 26(5) nm,α = 75.346 6(8) °,β = 67.847 3(9) °,γ = 65.724 4(9) °,V = 1.120 36(8) nm3,Z =2,Dc =1.985 g/cm3,F(000) = 500,R gt(F) =0.025 7,wR ref(F2) =0.079 8.