Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies

In this study, 4-(diphenylamino)benzaldehyde-4-(2-fluorophenyl)thiosemicarbazone (LH) ligand was synthesized from the reaction of 4-diphenylaminobenzaldehyde and 2-fluorophenyl thiosemicarbazide. The NiL2 complex containing LH ligand were synthesized and characterized using elemental analysis, infra...

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Main Authors: M. Osman, Uwaisulqarni, Silvarajoo, Sharmili, Kamarudin, Khadijah H., Mohamed Tahir, Mohamed Ibrahim, Kwong, Huey Chong
Format: Article
Published: Elsevier 2021
Online Access:http://psasir.upm.edu.my/id/eprint/94358/
https://www.sciencedirect.com/science/article/pii/S002228602031317X?via%3Dihub
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spelling my.upm.eprints.943582023-05-03T08:35:30Z http://psasir.upm.edu.my/id/eprint/94358/ Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies M. Osman, Uwaisulqarni Silvarajoo, Sharmili Kamarudin, Khadijah H. Mohamed Tahir, Mohamed Ibrahim Kwong, Huey Chong In this study, 4-(diphenylamino)benzaldehyde-4-(2-fluorophenyl)thiosemicarbazone (LH) ligand was synthesized from the reaction of 4-diphenylaminobenzaldehyde and 2-fluorophenyl thiosemicarbazide. The NiL2 complex containing LH ligand were synthesized and characterized using elemental analysis, infrared spectroscopy, magnetic susceptibility, molar conductivity and UV-Vis spectroscopy. X-ray structure was determined for both the LH ligand and the NiL2 complex. LH ligand was also characterised via 1H NMR and 13C NMR spectroscopy. FTIR data determined the coordination mode of the ligand with Ni(II) metal ion. The FTIR spectra shows that the LH ligand behave as mononegative bidentate through azomethine (N=C) and (C-S) groups with Ni(II) metal ion. The electronic spectra and magnetic measurements agreed well with a square planar geometry for NiL2 complex with the value of 0.00 B.M. Further confirmation of NiL2 complex was determined through single X-ray Crystallography which indicated a distorted square planar geometry which the angles deviated from 90° with a maximum value of 7°. In addition, the structure of LH ligand presented a thione form and the molecule has crystallized in triclinic crystal system with Pī space group. Conductivity studies of polymer electrolyte (PE) films composed of carboxymethyl cellulose (CMC) polymer, propylene carbonate as a plasticizer and LH/NiL2 compound as a dopant were prepared by a solution casting technique. The conductivity of the prepared PE films was studied using Electrochemical Impedance Spectroscopy (EIS). The conductivity was observed for LH ligand and NiL2 complex at 3.73 × 10−9 Scm−1 and 9.81 Scm−1, respectively. Elsevier 2021-01-05 Article PeerReviewed M. Osman, Uwaisulqarni and Silvarajoo, Sharmili and Kamarudin, Khadijah H. and Mohamed Tahir, Mohamed Ibrahim and Kwong, Huey Chong (2021) Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies. Journal of Molecular Structure, 1223. art. no. 128994. pp. 1-9. ISSN 0022-2860; ESSN: 1872-8014 https://www.sciencedirect.com/science/article/pii/S002228602031317X?via%3Dihub 10.1016/j.molstruc.2020.128994
institution Universiti Putra Malaysia
building UPM Library
collection Institutional Repository
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country Malaysia
content_provider Universiti Putra Malaysia
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description In this study, 4-(diphenylamino)benzaldehyde-4-(2-fluorophenyl)thiosemicarbazone (LH) ligand was synthesized from the reaction of 4-diphenylaminobenzaldehyde and 2-fluorophenyl thiosemicarbazide. The NiL2 complex containing LH ligand were synthesized and characterized using elemental analysis, infrared spectroscopy, magnetic susceptibility, molar conductivity and UV-Vis spectroscopy. X-ray structure was determined for both the LH ligand and the NiL2 complex. LH ligand was also characterised via 1H NMR and 13C NMR spectroscopy. FTIR data determined the coordination mode of the ligand with Ni(II) metal ion. The FTIR spectra shows that the LH ligand behave as mononegative bidentate through azomethine (N=C) and (C-S) groups with Ni(II) metal ion. The electronic spectra and magnetic measurements agreed well with a square planar geometry for NiL2 complex with the value of 0.00 B.M. Further confirmation of NiL2 complex was determined through single X-ray Crystallography which indicated a distorted square planar geometry which the angles deviated from 90° with a maximum value of 7°. In addition, the structure of LH ligand presented a thione form and the molecule has crystallized in triclinic crystal system with Pī space group. Conductivity studies of polymer electrolyte (PE) films composed of carboxymethyl cellulose (CMC) polymer, propylene carbonate as a plasticizer and LH/NiL2 compound as a dopant were prepared by a solution casting technique. The conductivity of the prepared PE films was studied using Electrochemical Impedance Spectroscopy (EIS). The conductivity was observed for LH ligand and NiL2 complex at 3.73 × 10−9 Scm−1 and 9.81 Scm−1, respectively.
format Article
author M. Osman, Uwaisulqarni
Silvarajoo, Sharmili
Kamarudin, Khadijah H.
Mohamed Tahir, Mohamed Ibrahim
Kwong, Huey Chong
spellingShingle M. Osman, Uwaisulqarni
Silvarajoo, Sharmili
Kamarudin, Khadijah H.
Mohamed Tahir, Mohamed Ibrahim
Kwong, Huey Chong
Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies
author_facet M. Osman, Uwaisulqarni
Silvarajoo, Sharmili
Kamarudin, Khadijah H.
Mohamed Tahir, Mohamed Ibrahim
Kwong, Huey Chong
author_sort M. Osman, Uwaisulqarni
title Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies
title_short Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies
title_full Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies
title_fullStr Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies
title_full_unstemmed Ni(II) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal X-ray crystallographic and conductivity studies
title_sort ni(ii) complex containing a thiosemicarbazone ligand: synthesis, spectroscopy, single-crystal x-ray crystallographic and conductivity studies
publisher Elsevier
publishDate 2021
url http://psasir.upm.edu.my/id/eprint/94358/
https://www.sciencedirect.com/science/article/pii/S002228602031317X?via%3Dihub
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score 13.211869