A new vic-dioxime ligand (1), bearing pendant an azacrown ether moiety and its soluble mononuclear cadmium(II), zinc(II), nickel(II), copper(II) and cobalt(II) complexes were obtained with the metal: ligand ratios of 1:2 and 1:1. The structures of the ligand and its complexes were verified using Fourier transform infrared (FT-IR), ultraviolet-visible (UV-Vis), mass spectrometry (MS), 1H and 13C NMR techniques. More detailed information about the structure of the 1 was provided by the two-dimensional (2D) heteronuclear single quantum coherence and heteronuclear multiple bond correlation techniques. The complexation properties of the ligand 1 were studied in the presence of different cations such as Pb2+, Zn2+,Cu2+, Cr3+, Hg2+, Zn2+, Fe3+ and Al3+ by UV-Vis spectroscopy and 1H NMR titration methods. All experimental results indicated that the new ligand acts as a selective compound only for Hg+2 cation. The redox behaviour of the complexes, were investigated by cyclic voltammetry at the glassy carbon electrode in 0.1 M tetrabutylamoniumtetrafluoroborate in dimethyl sulfoxide.