The single crystal of 3-amino-4-acylaminoximinofurazan (AAOF) was cultured using the mixed solvent of water and ethanol. The structure was characterized by 4-circle single-crystal X-ray diffraction analysis, IR and elemental analysis. The results indicate that the crystal belongs to monoclinic, space group P21/C with the crystallographcial parameters of a=0.7651(3) nm, b=1.1702(3) nm, c=1.9216(10) nm, M_r= 143.12, β=96.47 (4)°, V=1.7095(12) nm³, Z=4, D_c=1.668 g·cm^-3, F(000)=888. The AAOF molecule is good planar. There are inter- and intramolecular hydrogen bonds in the crystal.