Two coordination compounds were synthesized based on 3-aminofurazan-4-carboxylic acid (AFCA) with copper(II) and nickel(II), and characterized by elemental analysis and FTIR characterization. Single-crystal X-ray diffraction analysis revealed that [Cu(H2O)4(AFCA)2·H2O] (1) belongs to monoclinic, pertains to P21/c space group, β= 132.451(17)°, D
c
= 1.921 g·cm–3, and [Ni(H2O)4(AFCA)2·H2O] (2) belongs to orthorhombic, pertains to Pnnm space group, D
c
= 1.913 g·cm–3. In 1 and 2, metal ion (Cu2 + and Ni2 +) was hexacoordinated with four water molecules and two AFCA anions, which of furazan-ring presents typical monodentate coordination mode. Differential scanning calorimetry (DSC) was applied to assess the thermal decomposition behavior of 1 and 2. The non-isothermal kinetics parameters were calculated by the Kissinger’s method, Ozawa’s method and Starink’s method, respectively. In the end, impact sensitivity was also determined by standard method.