(E, E)S, S′-bis(2-benzimidazolylmethyl) dithioglyoxime, synthesis and characterization of heterotrinuclear complexes of and determination of their metal contents by EDXRF analysis

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. Gök, S.Z. Yıldız, Synth. React. Inorg. Met-Org. Chem. 22 (9) (1992) 1327]. BF2+ bridged Co(III) complexes have been synthesized via the hydrogen-bridged Co(III) 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 · H2O and NiCl2 · 6H2O salts. Using 1H, 13C 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 241Am 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.