Three novel vic-dioxime compounds and their transition metal complexes were synthesized for the first time. These ligands are anti-glyoximehydrazine (GH(2)),:.,anti-2-pyridinealdehydeglyoxime hydrazone (PyGH(2)) and anti-2-furanearboxaldehydeglyoxime h hydrazone (FGH(2)). The synthesized antiglyoximehydrazine was reacted with 2-pyridinealdehyde or 2-furancarboxaldehyde to obtain the PyGH2 and FGH(2)ligands. Mononuclear complexes of these ligands with a metal-ligand ratio of 1:2 were prepared with Ni(II), Co(II) and Cu(II) ions. The structures of the ligands and complexes were determined by H-1 n.m.r, i.r spectroscopy and elemental analytical techniques.