Novel vic-dioxime ligands and their poly-metal complexes bearing 1,8-diamino-3,6-dioxaoctane: synthesis, characterization, spectroscopy and electrochemistry Abstract Three novel vic-dioxime ligands containing the 1, 2 and 3), where M = Cu II , Co II , and Ni II , have been obtained with 1:1 metal/ ligand ratio. The Cu II and Ni II poly-metal complexes of these ligands are proposed to be square planar, while also the prepared Co II complexes are proposed to be octahedral with two water molecules as axial ligands. The detection of Hbonding in the [Ni(L 1 SL 1 )] n , [Ni(L 2 SL 2 )] n and [M(L 3 SL 3 )(H 2 O)] n metal complexes by FT i.r. spectra revealed the square planar or octahedral [MN 4 ÁH 2 O)] n coordination of poly-nuclear metal complexes. [MN 4 ] n coordination of the [Ni(L 1 SL 1 )] n and [Ni(L 2 SL 2 )] n complexes were also determined by 1 H-n.m.r. spectroscopy. The ligands and poly-metal complexes were characterized by elemental analyses, FT-i.r., u.v.-vis., 1 H and 13 C-n.m.r. spectra, magnetic susceptibility measurements, molar conductivity, cyclic voltammetry, and differential pulse voltammetric (DPV) techniques.