3, 4-Bis(1H-5-tetrazolyl)furoxan was synthesized via cyclization reaction using 3, 4-dicyanofuroxan and sodium azide as raw materials and water as solvent under the ZnCl₂ catalysis with a total yield of 91.0%. The structure was fully characterized by IR, NMR, elemental analysis, and X-ray single-crystal diffraction. Results show that the crystal belongs to the orthorhombic system, and space group is P2₁2₁2₁ with crystal parameters of a=6.1172(14)Å, b=9.657(2)Å, c=14.220(3)Å, V=840.0(3)ų, Z=4, D_c=1.76 g·cm^-3, F(000)=448, μ=0.147 mm^-1, S=1.031, the final R=0.0800 and wR=0.2523. The structure of 3, 4-bis(1H-5-tetrazolyl) furoxan is almost in one plane, indicating that a strong conjugation effect exists in the molecules. At the same time, lots of weak bonds among nitrogen atoms in the molecules can improve the density of compounds and thermal stability.