A new vic-dioxime ligand, [5.6;11,12-di(cyclohexyl)2,3-bis(hydroxyimino)8,9-diimino-1,4-diazzicyclododecanenickel(II)]chloride, [NiDHDD]Cl-2 (2), has been synthesized by the template condensation reaction of [N,N'-bis(2-aminocyclohexyl)-ethanedialdiminenickel(II)]chloride, [NiBAED]Cl-2 (1) with anti-dichloroglyoxime in methanol solution at -10degreesC. A homotrinuclear complex of [NiDHDD]Cl-2 (2), is formed with Ni(H) chloride and a heterotrinuclear complex of this ligand with Cu(II) chloride has been synthesized. The complexes [M(NiDHDD)(2)]Cl-4 have been characterized on the basis of elemental analyses, magnetic susceptibility measurements, conductivity measurements, IR and electronic spectral Studies. The trinuclear Ni(II) and Cu(II) complexes of the vic-dioxime ligand [NiDHDD]Cl-2 (2), have a M: ligand ratio of I : 2 and the ligand coordinates only through the N,N atoms, as do most vicinal dioximes. The molar conductivities in DMF solution indicate the electrolytic nature for the complexes.