A new three-nitro-group compound of 1-(2,4-dinitrophenyl)azo-1-nitrocyclohexane was prepared by the reaction of cyclohexanone-2,4dinitrophenylhydrazine with nitric oxide at ambient temperature. The single crystal structure has been determined by a four-circle X-ray diffractometer. The compound is monoclinic with space group P2(1)/c and unit-cell parameters aZ11.300(2) A ˚, bZ12.993(2) A ˚, cZ 10.155(1) A ˚, bZ98.33(1) o , F(000)Z672, the unit-cell volume VZ1475.2(5) A ˚3, the molecule number in one unit-cell ZZ4, the absorption coefficient mZ1.19 cm K1 , the calculated density D c Z1.456 g cm K3 . The exothermic decomposition reaction kinetics of the compound has been studied by DSC. The kinetic model function in differential form, apparent activation energy and pre-exponential constant of this reaction are (3/4)(1Ka)[Kln(1Ka)] 1/4 , 123.88 kJ mol K1 and 10 11.49 s K1 , respectively. The critical temperature of thermal explosion of the title compound is 161.15 o C and the entropy of activation ðDS s Þ, enthalpy of activation ðDH s Þ, and free energy of activation ðDG s Þ are K34.16 J mol K1 K K1 , 115.7, and 130.48 kJ mol K1 , respectively.