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Synthesis, spectroscopic characterization of thiosemicarbazone complexes of nickel(II) and X-ray structures of anisaldehyde thiosemicarbazone (ATSZH) and bis(tolualdehyde thiosemicarbazonato)nickel(II)

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Abstract

Complexes of nickel(II) with anisaldehyde (ATSZH), tolualdehyde (TTSZH), and vanillin (VTSZH) thiosemicarbazones have been synthesized and characterized by means of UV-Visible, I.R., Raman,1H and13C NMR spectroscopy. The thiosemicarbazones have been found to exist in the thione form.1H and13C NMR as well as electronic spectral data support a square planar structure for Ni(ATSZ)2 and Ni(TTSZ)2 complexes.1H and13C NMR spectra indicate that the structure of Ni(VTSZ)2 complex differs from the other two nickel(II) complexes and it may possibly consist of mixtures of isomers. The X-ray structures of Ni(TTSZ)2 and ATSZH were determined: the nickel complex is monoclinic witha=26.412(6),b=12.135(3),c=6.888(1)Å,β=95.41(5)°,Z=4,R=0.0647, space groupC2/c. The structure consists of discrete Ni(TTSZ)2 molecules in which the metal, located on a symmetry centre, is N,S-chelated by two ligands forming two five-term chelate rings. The structure of ATSZH is also monoclinic:a=7.859(1),b=13.481(3),c=10.028(3) Å,β=106.32(4)°,Z=4,R=0.0412, space groupP21/c. The molecules, connected by N⋯O hydrogen bonds, reveal a considerable tilting of the aromatic ring in respect to the thiourea moiety if compared with the nickel structure.

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Authors and Affiliations

  1. Department of Chemistry, University of Calabar, Calabar, Nigeria

    N. T. Akinchan, R. Akinchan & U. J. Ibok

  2. Istituto di Chimica Generale ed Inorganica, Centro di Studio per la Strutturistica Diffrattometrica del C.N.R., University of Parma, Viale delle Scienze, 43100, Parma, Italy

    L. P. Battaglia & A. Bonamartini Corradi

  3. Technical University, I-5, Wyb. Wyspiańskiego 27, 50-370, Wroclaw, Poland

    P. Drożdżewski

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  1. N. T. Akinchan
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  2. R. Akinchan
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  3. U. J. Ibok
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  4. L. P. Battaglia
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  5. A. Bonamartini Corradi
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Akinchan, N.T., Akinchan, R., Ibok, U.J. et al. Synthesis, spectroscopic characterization of thiosemicarbazone complexes of nickel(II) and X-ray structures of anisaldehyde thiosemicarbazone (ATSZH) and bis(tolualdehyde thiosemicarbazonato)nickel(II). Journal of Crystallographic and Spectroscopic Research 22, 741–753 (1992). https://doi.org/10.1007/BF01160996

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  • DOI: https://doi.org/10.1007/BF01160996

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