The (E, E)-dioxime containing a dithia-dioxa-diaza macrocyclic moiety 5,6:11,12:17.18-tribenzo-2,3-bis(hydroxyimino)-1,4-diaza-7,16-dithia-10,12-dioxacyclooctadecane (H2L) has been synthesized in high yield by a 1 + 1 addition of cyanogendi-N-oxide with 2,3:8,9: 14,15-tribenzo-1,16-di-amino-4,13-dithia-7,10-dioxahexadecane (3) which was obtained from condensation reaction with 2-amino thiophenol and 1,2-bis(2-bromoethoxy)benzene. in dichloromethane at -10 degreesC. Two vic-Dioxime ligands coordinate with Ni(II), Cu(II) and Co(III) through its hydroxyimino nitrogen donor atoms by the loss of the oxime protons. Home and heterotrinuclear Cu-3(II) and (CoPd2II)-Pd-III complexes of this ligand have been prepared; their two ligand molecules are connected via hydroxyimino or BF2+-bridging groups and two of the metal ions are coordinated by a diaza-dithia mixed donor macrocyclic moiety. The macrocyclic ligand and its transition metal complexes have been characterized on the basis of H-1-, C-13-NMR, IR and MS spectroscopy and elemental analysis data.