The novel quinoxaline substituted (E,E)-dioxime (H2L) containing a hexaoxadiaza macrobicycle [2.2.2(B)] has been synthesized from the reaction of 4,7,13,16,21,24-hexaoxa-5,6-(2',3'-diaminobenzo)- 1,10-diazabicyclo[8.8.8]hexacosane (4) prepared from 4,7,13,16,21,24-hexaoxa-5,6-(2',3'-dinitrobenzo)-1,10-diazabicyclo[ 8.8.8] hexacosane (3) andcyanogendi-N-oxide (5). Only the mononuclear nickel(II) complex with a metal:ligand ratio of 1:2 was prepared. This hydrogen-bridged complex was converted into its BF2+ capped analogue by reaction with BF3 . Et2O. The reaction of the BF2+ bridged complex with KPF6 gave a heterotrinuclear complex. Structures for the dioxime and its complexes are proposed in accordance with elemental analysis, H-1 and C-13 NMR, IR and MS spectral data.