A vicinal dioxime ligand with two 2-benzimidazolylmethyl groups, namely S,S'-bis(2-benzimidazolylmethyl) dithioglyoxine (H2L) and its axially pyridine and 2,6-dimethyl pyridine bonded Co(III) complexes were prepared according to prior literature [Y. Gok, S.Z. Yildiz, Synth. React. Inorg. Met-Org. Chem. 22 (9) (1992) 1327]. BF2+ bridged Co(111) complexes have been synthesized via the hydrogen-bridged Co(111) complexes by using borontrifloride ethyl ether complex. Heterotrinuclear complexes have been prepared by the reaction of these more soluble BF2-capped Co(III) complexes with stoichiometric amount of CdCl2 center dot H2O and NiCl2 center dot 6H(2)O salts. Using H-1, C-13 NMR, IR and MS spectral data and elemental analysis, the structures of the complexes were identified. Qualitative and quantitative determination of Co, Ni and Cd contents of the heterotrinuclear complexes have been investigated by energy dispersive X-ray fluorescence (EDXRF) method. An annular 50 mCi(241) Am radioactive source emitting 59.543 keV photons was used for excitation and Si(Li) detector having 157 eV FWHM at 5.9 keV was used for intensity measurements. (C) 2007 Elsevier B.V. All rights reserved.