Three new vic-dioximes, [L1H2], N-(4-ethylphenyl)amino-1-acetyl-1- cyclohexenylglyoxime, [L2H2], N-(4-butylphenyl)amino-1-acetyl-1- cyclohexenylglyoxime, and [L3H2], N-(4-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. These new compounds (ligands and complexes) were characterized with FT-IR, magnetic susceptibility measurement, molar conductivity measurements, mass spectrometry measurements, thermal methods (e.g. thermal gravimetric analysis), 1H NMR (Nuclear Magnetic Resonance) and 13C NMR spectral data and elemental analyses. © 2009 Taylor & Francis.