4,4'-Bis(cliloroacetyl)diphenyl thioether (HL) was synthesized from chloroacetyl chloride and diphenyl thioether in the presence of AlCl3 as catalyst in a Friedel-Crafts reaction. Subsequently, its keto oxime (H2L) and glyoxime (H4L) derivatives were also prepared. Then 3 new substituted 4,4'-thiobis(aminophenylglyoxime) (H4L1-3) were synthesized from 4,4'-thiobis(chlorophenylglyoxime) and the corresponding amines. The Ni(II), Cu(II) and Co(II) complexes of these ligands were prepared. The structures of these ligands and their complexes were identifed by FT-IR, H-1 NMR and ICP-AES spectral data, elemental analyses and magnetic measurements.