Two new soluble phenylaminoglyoxime ligands, 4- isopropylanilinephenylglyoxime (L1H2), 4-benzylpiperidinephenylglyoxime (L2H2), were prepared by reacting 4-isopropylaniline and 4-benzylpiperidine with chlorophenylglyoxime. Mononuclear nickel(II), cobalt(II), copper(II), zinc(II), and cadmium(II) complexes with these ligands were synthesized. On the basis of the magnetic and spectral evidence a square-planar geometry for Ni(II) and Cu(II) complexes, a tedrahedral geometry for Cd(II) and Zn(II) complexes and octahedral geometry for Co(II) complexes are proposed. These compounds were elucidated by elemental analysis, IR, UV-Vis, and magnetic moments. The ligands were additionally characterized by 1H NMR and 13C NMR spectra. © 2008 Taylor & Francis.