1-(4-Chlorophenyl)-3-(4-methylbenzoyl)thiourea was synthesized and characterized by IR, 1 H and 13 C NMR, mass spectroscopy and the elemental analysis. The crystal structure was confirmed from single crystal X-ray diffraction data. It crystallizes in the monoclinic space group P2 1 /c with unit cell dimensions a = 12.038(3), b = 6.330(6), c = 18.912(5)Å and β = 100.32(3) • . There is a strong intramolecular hydrogen bond of the type N-H. . . O, with distance N1. . . O1 = 2.659(3)Å. The structure is composed of dimers related by inversion centers. The dimers are formed by intermolecular interactions of the type N-H. . . S with N. . . S separation of 3.440(2)Å. The mass fragmentation pattern has also been discussed.