A novel three-dimensional Zn(Ⅱ) coordination polymer, Zn3(C2H2N3)4(SiF6), has been synthesized under solvothermal conditions using 1H-1,2,4-triazole-3-carboxylic acid and zinc fluoride as the starting materials. The complex has been characterized by elemental analysis, IR, TG analysis and single-crystal X-ray diffraction analysis. The complex crystallizes in the tetragonal I4/mmm space group with a=11.592(0), c=7.526(1), V=1011.3(2)3 , Z=2, Mr=610.46, Dc=2.005 g/cm3 and F(000)=596. The final R=0.0312 and wR=0.067 for 319 observed reflections with I>2σ(I). In the title complex, the Zn centers are interconnected by μ 3 -bridging triazole ligands to form a microporous three-dimensional metal-organic framework. A novel three-dimensional Zn (Ⅱ) coordination polymer, Zn3 (C2H2N3) 4 (SiF6), has been synthesized under solvothermal conditions using 1H- 1,2,4-triazole-3-carboxylic acid and zinc fluoride as the starting materials. The complex has been characterized by elemental analysis, IR, TG analysis and single-crystal X-ray diffraction analysis. The complex crystallizes in the tetragonal I4 / mmm space group with a = 11.592 (0), c = V = 1011.3 (2) 3, Z = 2, Mr = 610.46, Dc = 2.005 g / cm3 and F (000) = 596. The final R = 0.0312 and wR = 0.067 for 319 observed reflections with I> 2σ (I In the title complex, the Zn centers are interconnected by μ 3 -bridging triazole ligands to form a microporous three-dimensional metal-organic framework.