Abstract: KEYWORDSNickel and copper metal complexes of N-(R-carbamothioyl)-4-nitrobenzamide (R = diphenyl and ethylbutyl) were synthesized and characterized by IR, 1 H NMR, mass spectrometry and elemental analysis. The spectroscopic data are consistent with the ligand and the metal complexes containing two O and S chelated ligands. N-(diphenylcarbamothioyl)-4nitrobenzamide, HL 1 , was characterized by a single crystal X-ray diffraction study. It crystallizes in the triclinic space group P1 with unit cell dimensions of …