The work described in this paper involves the synthesis and structural characterization of Ni(II) complexes derived from dihydroxybenzaldehyde thiosemicarbazones (H 3 L 1 , H 3 L 2 , H 3 L 3 , H 3 L 4 ) and 1,2-bis(diphenylphosphino)ethane (dppe). Ligands and their Ni(II) complexes were characterized by elemental analysis, IR, UV-Vis, ( 1 H, 13 C, 31 P) NMR, as well as magnetic moment and X-ray structure analysis. The results so obtained suggest that the thiosemicarbazone ligands behave as a tridentate ligand which were coordinated with Ni(II) ion through O, N and S atoms. Furthermore, the dppe ligand was coordinated with Ni(II) ion through the P atom. It is concluded that all Ni(II) complexes have a Square-planar geometry.
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