The preparation method and structure analysis results were obtained for the salt made from semicarbazide and picric acid. The molecular structure was characterized by elemental analysis, IR and DSC. Its crystal structure was determined by the single-crystal X-ray diffraction method with a four-circle diffractometer. The results show that the crystal is of triclinic system. Space group is Pī with crystal parameters of a=5.024(1)Å， b=10.209(1)Å，c=11.551(1)Å；α=79.00(1)°，β=81.11(1)°，γ=82.47(1)°；V=571.42(14)ų，Z=2，Dc=1.768 g·cm^-3，μ=0.162 mm^-1，F(000)=312， R₁=0.032 4，Rw₂=0.087 4。