In this paper, the compound (E)-N-(3,5-dimethylphenyl)-2-(3-chlorobenzylidene)thiosemicarb-azone was synthesized and characterized by elemental analysis, Fourier transform infrared (FT-IR), 1 H nuclear magnetic resonance (NMR), 13 C NMR. The crystal structure was determined by single-crystal X-ray diffraction tool, indicating that the compound belongs to the orthorhombic crystal system of the Fdd2 space group, where