Crystal of the complex Ni2L (ClO4)2 was obtained by reaction of Ni(ClO4)2 and macrocyclic ligand H2L, where L2– is the dinucleating macrocycle with two 2,6-di(aminomethyl)-4-methyl phenolate entities combined by the same two lateral chains, –(CH2)2–NH–(CH2)2–, at the amino nitrogens. The thermal decomposition processes of the title complex were studied in a dynamic atmosphere of dry argon using TG-DTG. The kinetic analysis of the first and second thermal decomposition steps were performed via the TG-DTG curves, and the kinetic parameters were obtained from analysis of the TG-DTG curves with integral and differential methods. The most probable kinetic function was suggested by comparison of the kinetic parameters.