The new vicinal dioxime N,N'-bis(2-benzimidazolylmethyl)diaminoglyoxime (H2L) has been prepared by reacting 2-aminomethylbenzimidazole with cyanogen-di-N-oxide. Reaction of H2L with Cu-II and Co-III salts and appropriate reagents gave mono- and trinuclear complexes, [Cu(HL)(2)], [Cu-3(L)(2)(phen>(2)], [Co(HL)(2)L'CI] (L' = 2,6-lutidine), [Co(LBF2)(2)L " Cl] and [Cu-2(ClO4)(2)-Co(LBF2)(2)L'CI](ClO4)(2), which were characterized by i.r., H-1- and C-13-n.m.r., m.s. and elemental analyses. spectrometer, respectively. Fourier transform i.r. spectroscopy (KBr pellets) was performed on Perkin Elmer 1600 and Mattson 1000 FTIR instruments. H-1- and C-13-n.m.r. spectra were recorded in d(6)-DMSO on Varian XL-300 and Varian 200 n.m.r. spectrometers, respectively. Mass spectra were measured on VG Analytical AutoSpec (Kansas University, USA) and Kratos MS-50 (York University, Canada) spectrometers. Melting points were determined on an Electrothermal apparatus and are uncorrected.