N-(R-carbamothioyl)cyclohexanecarboxamides (R: diethyl, di-n-propyl, di-n-butyl, diphenyl and morpholine-4) and their Ni(II) and Cu(II) complexes have been synthesized and characterized by elemental analyses, FT-IR and NMR methods. N-(diethylcarbamothioyl) cyclohexanecarboxamide, HL 1 , C 12 H 22 N 2 OS, crystallizes in the orthorhombic space group P2 1 2 1 2 1 , with Z ¼ 4, and unit cell parameters, a ¼ 6.6925(13) Å , b ¼ 9.0457(18) Å , c ¼ 22.728(5) Å . The conformation of the HL 1 molecule with respect to the thiocarbonyl and carbonyl moieties is twisted, as reflected by the torsion angles O1-C6-N2-C5, C6-N2-C5-N1 and S1-C5-N2-C6 of 1.68 , À67.47 and 115.50 , respectively. The structure of HL 1 also shows a delocalization of the electrons of the thiocarbonyl group over the C-N bonds. The ring puckering analysis shows that the cyclohexane ring has a chair conformation. The bis(N-(morpholine-4-carbonothioyl)cyclohexane carboxamido)nickel(II) complex, Ni(L 5 ) 2 , C 24 H 38 N 4 NiO 4 S 2 , crystallizes in the monoclinic space group P2 1 /c, with Z ¼ 4, and unit cell parameters, a ¼ 16.919(3) Å , b ¼ 8.3659(17) Å , c ¼ 19.654(4) Å , ¼ 107.43(3) . Ni(L 5 ) 2 is a cis-complex with a slightly distorted square-planar coordination of the central nickel by two oxygen and two sulfur atoms.