Synthesis, crystal structure, chromatographic seperation, and thermogravimetric investigation of a ONNO type asymmetric Schiff base and its trinuclear complexes

Oz S., Ergun U., Yakut M., Svoboda I., Atakol A., İNAL E. K., ...Daha Fazla

Russian Journal of Coordination Chemistry/Koordinatsionnaya Khimiya, cilt.40, sa.8, ss.571-582, 2014 (SCI-Expanded, Scopus)

Özet

1,3-Propanediamine was put to react with 2-hydroxybenzaldehyde and 2-hydroxyacetophenone sequentially in aprotic medium. The crystalline product was examined by high performance liquid chromatography. The composition was 66% asymmetric Schiff base N(2-hydroxybenzylidene)-N'(2-hydroxyacetophenone)-1,3- propanediamine (SALLACH2) and 33% bis-N,N'(2-hydroxyacetophenylidene) -1,3-propanediamine (LACH2). As the crystals were uniform and of appropriate size, the molecular model of the material was revealed by X-ray diffraction. It was seen that two molecules of SALLACH2 and one molecule of LACH 2 formed the mixed crystals. The substance was separated to its components and the asymmetric Schiff base was purified with a silica column. The substance was characterized with elemental analysis, FT-IR, MS, 1HNMR, and 13C NMR. In addition, six tri-nuclear complex with the nuclear structure of NiII-NiII-NiII, NiII-CuII-NiII, NiII-Mn II-NiII were prepared from this Schiff base and stoichiometry was determined by elemental analysis, FT-IR and thermogravimetry. Finally, the molecular structures of two complexes were brought to light by XRD which highlights the asymmetry of the ligand more clearly. © 2014 Pleiades Publishing, Ltd.