In this study, anti-chloro(p-nitrophenyl)glyoxime (CPNPGH(2)) has been synthesized by chlorination of anti-p-nitrophenylglyoxime. The reaction of CPNPGH(2) with suitable aryl or arylkalyamines in ethanol between -5 degrees C and 15 degrees C gives unsymmetrical dioximes, namely, o-toluidino-p-nitrophenylglyoxime (C15H14N4O4), l-naphthylamino-p-nitrophenylglyoxime (C18H14N4O4), biphenyl-4-amino-4'-amino-p-nitrophenylglyoxime (C20H17N5O4) and N-(2-methylpyridyl) amino-p-nitrophenylglyoxime (C14H13N5O4) The Cu(II) and Ni(II) complexes of these ligands are square-planar while the Co(II) complexes are octahedral with water molecules as axial ligands. H-1 NMR, IR spectra and elemental analyses data are given.