anti-Chlorophenylchloroglyoxime, 4-ClC6H4C=NOH)CCl(=NOH), has been synthesized by chlorination of anti-p-cholorophenylglyoxime. The reaction. of 4-ClC6H4C(=NOH)CCl(=NOH) with thiophenol, 4-methylthiophenol and 4-methoxythiophenol in ethanol between -5 and -10degreesC gives the unsymmetrical vic-dioximes, designated as thiophenolo-p-chlorophenylglyoxime, 4-ClC6H4C(=NOH)C(SC6H5)(=NOH), 4-methylthiophenolo-p-chlorophenylglyoxime, 4-ClC6H4C(=NOH)C(SC6H4-CH3-p)(=NOH), and 4-methoxylthiophenolo-p-chlorophenylglyoxime, 4-ClC6H4C(=NOH)C(SC6H4-OCH3-p)(=NOH). The Cu(II) and Ni(II) complexes of these ligands were prepared and are proposed to be square-planar, while the corresponding Co(II) complexes are proposed to be octahedral with water molecules as axial ligands. The structural assiguments are supported by H-1 NMR, IR and elemental analyses.