The reaction of anti-chloro(p-nitrophenyl)glyoxime (CPN-PGH(2)) with thiophenol, 4-methylthiophenol and 4-methoxythiophenol in ethanol between -5 degrees and 10 degreesC gives unsymmetrical vic-dioximes, designated as thiophenolo-p-nitrophenylglyoxime [(LH2)-H-1], 4-methyl-thiophenolo-p-nitrophenylglyoxime [(LH2)-H-2], and 4-methoxythiophenolo-p-nitro-phenylglyoxime [(LH2)-H-3]. The Ni(II) and Cu(II) complexes of these ligands were prepared and are proposed to be square-planar, while the also prepared Co(II) complexes are proposed to be octahedral with water molecules as axial ligands. The structural assignments are supported by H-1 NMR, IR, and elemental analyses.