A1 Refereed original research article in a scientific journal
Synthesis, NMR spectral and single crystal X-ray structural studies on Ni(II) dithiocarbamates. Fabrication of nickel sulfide nanospheres by the solvothermal method
Authors: Prakasam BA, Lahtinen M, Peuronen A, Muruganandham M, Kolehmainen E, Haapaniemi E, Sillanpaa M
Publisher: PERGAMON-ELSEVIER SCIENCE LTD
Publication year: 2014
Journal: Polyhedron
Journal name in source: POLYHEDRON
Journal acronym: POLYHEDRON
Volume: 81
First page : 588
Last page: 596
Number of pages: 9
ISSN: 0277-5387
DOI: https://doi.org/10.1016/j.poly.2014.06.059
Abstract
Three dithiocarbamatonickel(II) complexes, [Ni(bzbudtc)(2)] (1), [Ni(bzbudtc)(PPh3)(NCS)] (2) and [Ni(bzbudtc)(PPh3)(CN)] (3) (where, bzbudtc = the N-benzyl-N-butyldithiocarbamato anion and PPh3 = triphenylphosphine), were prepared. All three complexes were analyzed by UV-Vis, IR and NMR (H-1, C-13 and P-31) spectra. The C-13 NMR spectra of complexes 1-3 show the most crucial thioureide signal at around 200 ppm. A significant deshielding observed for the P-31 signals in 2 and 3 reveals the effective bonding of phosphorus to the metal center. Single crystal X-ray analysis of crystals of 1-3 show that all the described complexes exhibit a distorted square planar coordination geometry in the solid state as a result of the small bite angle of the dithiocarbamato ligand. The observed magnitude of deviation out of the mean plane of nickel is in the following order: 1 < 3 < 2. A decrease in the thioureide bond distances in 2 and 3, in contrast to 1, could be accounted for by the difference in the steric effect induced by the triphenylphosphine (PPh3) group. In the case of compound 1, solvothermal experiments were performed in order to produce nickel sulfide nanoparticles. The morphological and structural properties of the resultant particles indicate that the average size of the crystals is about 22 nm and the main component of the product is in the form of cubic face-centered NiS2 (vaesite) with a minor fraction of hexagonal NiS. (C) 2014 Elsevier Ltd. All rights reserved.
Three dithiocarbamatonickel(II) complexes, [Ni(bzbudtc)(2)] (1), [Ni(bzbudtc)(PPh3)(NCS)] (2) and [Ni(bzbudtc)(PPh3)(CN)] (3) (where, bzbudtc = the N-benzyl-N-butyldithiocarbamato anion and PPh3 = triphenylphosphine), were prepared. All three complexes were analyzed by UV-Vis, IR and NMR (H-1, C-13 and P-31) spectra. The C-13 NMR spectra of complexes 1-3 show the most crucial thioureide signal at around 200 ppm. A significant deshielding observed for the P-31 signals in 2 and 3 reveals the effective bonding of phosphorus to the metal center. Single crystal X-ray analysis of crystals of 1-3 show that all the described complexes exhibit a distorted square planar coordination geometry in the solid state as a result of the small bite angle of the dithiocarbamato ligand. The observed magnitude of deviation out of the mean plane of nickel is in the following order: 1 < 3 < 2. A decrease in the thioureide bond distances in 2 and 3, in contrast to 1, could be accounted for by the difference in the steric effect induced by the triphenylphosphine (PPh3) group. In the case of compound 1, solvothermal experiments were performed in order to produce nickel sulfide nanoparticles. The morphological and structural properties of the resultant particles indicate that the average size of the crystals is about 22 nm and the main component of the product is in the form of cubic face-centered NiS2 (vaesite) with a minor fraction of hexagonal NiS. (C) 2014 Elsevier Ltd. All rights reserved.
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