TY - JOUR
T1 - Synthesis, NMR spectral and single crystal X-ray structural studies on Ni(II) dithiocarbamates. Fabrication of nickel sulfide nanospheres by the solvothermal method
AU - Arul Prakasam, Balasubramaniam
AU - Lahtinen, Manu
AU - Peuronen, Anssi
AU - Muruganandham, Manickavachagam
AU - Kolehmainen, Erkki
AU - Haapaniemi, Esa
AU - Sillanpää, Mika
PY - 2014/10/15
Y1 - 2014/10/15
N2 - 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 PPh 3 = triphenylphosphine), were prepared. All three complexes were analyzed by UV-Vis, IR and NMR (1H, 13C and 31P) spectra. The 13C NMR spectra of complexes 1-3 show the most crucial thioureide signal at around 200 ppm. A significant deshielding observed for the 31P 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.
AB - 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 PPh 3 = triphenylphosphine), were prepared. All three complexes were analyzed by UV-Vis, IR and NMR (1H, 13C and 31P) spectra. The 13C NMR spectra of complexes 1-3 show the most crucial thioureide signal at around 200 ppm. A significant deshielding observed for the 31P 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.
KW - Dithiocarbamate
KW - Nanospheres
KW - Solvothermal
KW - Synthesis
KW - X-ray diffraction
UR - http://www.scopus.com/inward/record.url?scp=84905583207&partnerID=8YFLogxK
U2 - 10.1016/j.poly.2014.06.059
DO - 10.1016/j.poly.2014.06.059
M3 - Article
AN - SCOPUS:84905583207
SN - 0277-5387
VL - 81
SP - 588
EP - 596
JO - Polyhedron
JF - Polyhedron
ER -