Thiosemicarbazides and their derivatives are well known for their use in biological activity and many applications in pharmaceutical and industrial fields. The cyclization of 1-benzoyl-4-(2-nitrophenyl)-3-thiosemicarbazide (BNPTSC) in dimethylformamide (DMF) medium furnished N-(2-nitrophenyl)-5-phenyl-1,3,4-oxadiazole-2-amine (NPPOA). The chemical structure of the above substituted 1,3,4-oxadiazole has been assigned by IR, mass and X-ray diffraction studies. The XRD studies reveal the presence of four types of hydrogen bonds (N–H路路路O, N–H路路路N, C–H路路路O, C–H路路路N) in the crystal packing. The crystal system was found to be orthorhombic with a space group Pca2(1) and the unit cell dimensions are: a = 26.873(3) 脜, b = 6.0827(7) 脜, c = 7.8502(10) 脜, α = 90掳, β = 90掳, γ = 90掳 and Z = 4.