3, 4-Bis(3-nitrofurazan-4-oxy)furazan (1) was synthesized from 3, 4-diaminofurazan by Caro′s acid oxidation, hydrolysis, neutralization and substituent reactions, and its structure was characterized by IR, NMR, elemental analysis, and X-ray single-crystal diffraction analysis. The crystal belongs to the monoclinic system, space group P2₁/c with a=15.256(3)Å, b=11.579(3)Å, c=14.981(3)Å, β=117.624(4)°, M_r=328.14, V=2344.7(9)ų, Z=8, D_c=1.859 g·cm^-3, F(000)=1312, μ=0.177 mm^-1, S=1.012, the final R=0.0433 and wR=0.0987. X-ray single-crystal diffraction analysis indicate that compound 1 crystallizes in two crystallographic independent host molecules with different conformation and several intermolecular interactions among oxygen atoms and nitrogen atoms lead to a high density. The thermal behavior of compound 1 was studied by TG-DTG and DSC techniques. Results show that it melts at 72.9 ℃ and is highly exothermic from 245 ℃ to 346 ℃.