The compound of ［NH₂NHC(NH₂)₂］NO₃ was prepared through the reaction of aminoguanidine bicarbonate and nitric acid solution. The crystal structure of ［NH₂NHC(NH₂)₂］NO₃ was determined by the single crystal diffraction. The result shows that there is not any double-bond in the compound, and it′s a typical nitrate. The crystal is triclinic with space group Pī, a=0.602 8(1) nm，b=0.734 4(1) nm，c = 0.772 3(1) nm； α=104.850(10)°，β=110.450(10)°，γ=102.660(10)°； V=0.291 1(7) nm³，Z=2，D_c=1.564 g·cm^-3，F(000)=144. The final R=0.032 7.