A new (E,E)-dioxime, (6Z,7Z)-15,16-dihydro-14H-dibenzo[b,h][1,10,4, 7]dithiadiazacyclotride-cine-6,7(5H,8H)-dionedioxime (H (2) L) has been synthesized by reacting cyanogen-di-N-oxide (2) with 2,2'-[propane-1,3-diylbis(thio)]dianiline (1). Mononuclear complexes (4) and (5) of this ligand have been synthesized by reacting the vic-dioxime (H(2)L) with NiCl(2) center dot 6H(2)O and CoCl(2) center dot 6H(2)O, respectively. The BF(2)(+) capped Ni(II) and Co(III) complexes (6) and (7) of the dioxime have been synthesized from (4) and (5). The new compounds were characterized by a combination of elemental analysis, (1)H- and (13)C-n.m.r, i.r. and m.s. spectral data.