Two new vic-dioxime ligands and their complexes with Co+2, Ni+2, Cu+2, Cd+2, and Zn+2 ions were synthesized. Primer amines (3,4-methylenedioxaaniline and 4-methylbenzylamine) reacted with antichloroglyoxime to give 3,4-methylenedioxaphenylaminoglyoxime (H2L1) and N-(4-methylbenzyl)aminoglyoxime (H 2L2) ligands. Structures of the ligands and their complexes are proposed based on elemental analyses, IR, UV-Vis, and 1H NMR spectra, magnetic susceptibility measurements, and thermogravimetric analyses (TGA). © 2007 Pleiades Publishing, Ltd.