THE SYNTHESIS AND CHARACTERIZATION OF NEW (E,E)-DIOXIME AND ITS MONO AND HETERONUCLEAR COMPLEXES CONTAINING 14-MEMBERED TETRAAZA MACROCYCLIC MOIETY

A new macrocyclic vicinal dioxime, 5,6:9,10:13, 14-tribenzo-2,3-bis(hy droxyimino)- 1,4,8,11-tetraazacyclodecane (H2L) has been synthesized b y the reaction of (E,E)-dichloroglyoxime with 2,3:6,7:10,11-tribenzo-1 ,5,8,11-tetraazadodecane (4), which was prepared by the reduction of 1 ,2-bis(o-nitrophenylaldimino) benzene (3). The mononuclear cobalt(III) complex (5) of the dioxime has been isolated with L' = pyridine, toge ther with chlorine as axial ligand. In addition, cobalt(III) complex c ontaining the BF2+ bridge macrocycle (6) was synthesized using a precu rsor hydrogen-bridged cobalt(III) complex via the template effect. The heterotrinuclear complex of the BF2+-capped cobalt(III) complex (7) h as also been prepared by the reaction of this complex with CdCl2 .sati sfies H2O. The structure of dioxime and its complexes were identified by using elemental analysis, H-1, C-13 NMR, IR and MS spectral data. ( C) 1997 Elsevier Science Ltd.