In this study, the novel vic-dioxime ligand (3) and its Ni(II), Cu(II), Co(II), Cd(II) and Zn(II) complexes (4-8) were synthesized for the first time by condensation reactions of N-(4-aminophenyl)aza-15-crown-5 (1) and anti-chlorophenylchloroglyoxime (2). All of these new compounds were characterized by the elemental analysis, Fourier transform infrared, ultraviolet-visible, mass spectrometry, 1H NMR, 13C NMR and magnetic susceptibility measurements. The electrochemical properties of the ligand and its complexes have been investigated by cyclic voltammetry at the glassy carbon electrode in 0.1 M TBATFB in DMSO. © Springer Science+Business Media B.V. 2012.