A novel (E, E)-dioxime 5, 6:14,15-dibenzo-9,11-pyrido-2,3-bis(hydroxyimino)-1,4-diaza-7, 13-dithiacyclopentadecane (H(2)L) has been synthesized from the reaction of cyanogendi-N-oxide and 2,6-bis(2-aminothiophenoxymethyl)pyridine (3), which has hen prepared from 2,6-bis(chloromethyl)pyridine (1) and 2-amino thiophenol. The cobalt (III) complex [Co(HL)(2)L'Cl] of H(2)L has been obtained with L' = 2,6-lutidine together with chloride as axial ligands. In addition the synthesis of a new cobalt complex containing BF2+ bridges is achieved with the hydrogen bridged cobalt(III) complex. Three new mono-, tri- and pentanuclear copper(II) complexes of formula [Cu-3(HL)(2)], [CU5(HL)(2)(bipy)(2)] and [Cu-5(HL)(2)(phen)(2)] have been synthesized. The structures of the oxime and its complexes were identified by elemental analysis, H-1, C-13 NMR, IR and MS data.