Chlorophenylglyoxime and Ligand Complexes ([M(Salen/Salophen)](2)O, [M(Saldeta/Salpy)Cl] shortened as LC, M = Fe(III) or Cr(III)) have been synthesized. 3,5-dicarboxyanilinophenylglyoxime (5) and 4-carboxyphenylhydrazinophenylglyoxime (6) have been synthesized with the reaction of chlorophenylglyoxime and 5-aminoisophtalalic acid or 4-hydrazinobenzoic acid. [M(Salen/Salophen/Saldeta/ Salpy)-3,5-dicarboxyanilinophenyl-glyoxime)] (7-14) or [M(Salen/Salophen)-4-carboxyphenylhydrazinophenylglyoxime)] (15-22) have been synthesized from (5) or (6) and LCs. The new heterotrinuclear and pentanuclear complexes (23-38) have been obtained from (7-22) and Ni(II) salt. Then, heteronuclear and BF2+ capped vic-dioxime complexes (39-54) have been synthesized. The complexes have been characterized as low-spin (S=1/2) distorted octahedral [Fe-III(Salen/Salophen)], high-spin (S = 5/2) distorted octahedral [Fe-III(Saldeta/Salpy)] and (S = 3/2) distorted octahedral [Cr-III(Salen/Salophen/Saldeta/Salpy)] bridged by COO- groups. The structure of all ligand and complexes were identified by using elemental analysis, thermal analyses, magnetic susceptibility, LC-MS, ICP-AES, H-1-NMR and FT-IR spectral data. (C) 2018 Elsevier B.V. All rights reserved.