In this study, three new vic-dioximes, [L1H2], N-(5-chloro-2-methoxyphenyl)amino-1-acetyl-1-yclohexenylglyoxime, [L 2H2],N-(3-chloro-4-methoxyphenyl)amino-1-acetyl-1- cyclohexenylgly-oxime and [L3H2], N-(3-chloro-2- methoxyphenyl)amino-1-acetyl-1-cyclohexenylglyoxime were synthesized from 1-acetyl-1-cyclohexeneglyoxime and the corresponding substituted aromatic amines. Metal complexes of these ligands were also synthesized with Ni(II), Cu(II) and Co(II) salts. The structures of these new compounds (ligands and complexes) were characterized with FT-IR, magnetic susceptibility measurement, molar conductivity measurements, mass spectrophotometer measurements, thermal methods (TGA), 1H NMR and 13C NMR spectral data and elemental analyses. © 2008 Springer Science+Business Media B.V.