<p>The synthesis, X-ray crystallographic, and spectroscopic studies of <i>N</i>-(4-chlorophenyl)-6-[(4-chlorophenyl)carbamothioyl]pyridine-2-carboxamide (Cl-pcta) grown from EtOAc/ hexane (1:8) is reported. The compound crystallized in a monoclinic space group P 2₁/c with a = 9.8905(4) Å, b = 21.5491(9) Å, c = 8.9818(4) Å, β = 111.1277(13)° and <i>V</i> = 1785.62(13) ų with <i>Z</i> = 4. The structure of Cl-pcta is pseudo-planar with the Cl-aryl rings twisted in opposite directions out of the plane of the pyridyl ring. The packing of the molecules were stabilized by classical hydrogen bonding between NH and C = O/C = S groups. In the ¹H NMR the NH(C = O) and the NH(C = S) where observed at 9.44 and 11.19&#xa0;ppm, respectively. In the IR spectrum, the NH(C = O) and the NH(C = S) were also resolved and observed at 3216 and 3302&#xa0;cm^–1, respectively; coherent with the asymmetrical nature of the molecule.</p> Graphical abstract <p></p>