A new energetic MOFs, {[Ni-2(C2H5N5)(2)(C3H2O4)(2)(H2O)]center dot 3H(2)O}(n) (Hdatrz (C2H5N5) = 3,5-diamino-1,2,4-triazole, H(2)mal (C3H4O4) = malonic acid), has been synthesized and characterized by element analysis, chemical analysis, IR spectroscopy, single-crystal X-ray diffraction and thermal analysis. X-ray diffraction analysis confirmed that the compound featured a 2D layer structure with dinuclear Ni(II) unit. Thermal analysis demonstrated that the compound after dehydration have good thermostability with decomposition temperature up to 633 K. The non-isothermal kinetics for the compound was studied by Kissinger's and Ozawa's methods. The Arrhenius equation of initial thermal decomposition process of compound can be expressed as lnk = 55.89 - 332.01 x 10(3)/RT. Furthermore, a reasonable thermochemical cycle was designed based on the preparation reaction of the compound, and standard molar enthalpy of dissolution of reactants and products were measured by RD496-2000 calorimeter. Finally, the standard molar enthalpy of formation of the compound was determined to be -(2766.3 +/- 2.3) kJ . mol (1) in accordance with Hess's law. In addition, the specific heat capacity of the compound at T = 298.15 K was determined to be 1.42 +/- 0.11 J . K (1) . g (1) by RD496-2000 calorimeter. (C) 2015 Elsevier Ltd. All rights reserved.