Reduction of 2,3:9,10-dibenzo-5,12-diaza-1,8-dioxa-cylotetradecane-5,11-diene(1) with sodium borohydride in ethanol generates 2,3:9,10-dibenzo-5,12-diaza-1,8-dioxacyclotetradecane(2) in high yield. The macrocyclic ligand 2,3:9,10-dibenzo-5,12-diaza-1,8-dioxacyclotetradecane-N,N'-diacetic acid (3) has been synthesized and characerized. In addition, reaction of (2) with an excess of acrylonitrile gives 2,3:9,10-dibenzo-5,12-diaza-1,8-dioxacyclotetradecane-N,N'-di(2-cyanoethyl) (4). Several new complexes of these ligands with nickel(II), copper(II) and cobalt(II) have been prepared and identified. The structures of these complexes are proposed on the basis of elemental analysis, H-1, C-13-NMR, IR, UV-VIS spectra, magnetic susceptibility and conductivity data.