Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes

Aroylthiourea ligands, 1-aroyl-3-cyclohexyl-3-methylthiourea (HL1), 1-(2-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL2), 1-(3-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL3) and 1-(4-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL4) were synthesized through a condensation reaction of methylcyclohe...

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Main Authors:	Syahidah Mohd Tahir, Aisha Al-Abbasi, Qurnisha Ghazali, Khuzaimah Arifin, Mohammad Kassim
Format:	Article
Language:	English
Published:	Penerbit Universiti Kebangsaan Malaysia 2018
Online Access:	http://journalarticle.ukm.my/12199/ http://journalarticle.ukm.my/12199/ http://journalarticle.ukm.my/12199/1/16%20Syahidah%20Mohd%20Tahir.pdf

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spelling	ukm-121992018-10-16T13:37:53Z http://journalarticle.ukm.my/12199/ Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes Syahidah Mohd Tahir, Aisha Al-Abbasi, Qurnisha Ghazali, Khuzaimah Arifin, Mohammad Kassim, Aroylthiourea ligands, 1-aroyl-3-cyclohexyl-3-methylthiourea (HL1), 1-(2-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL2), 1-(3-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL3) and 1-(4-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL4) were synthesized through a condensation reaction of methylcyclohexylamine and aroylisothiocyanate with a general formula (X-Ph)(CO)NH(CS)N(C6H5)(CH3) where X = H, o-Cl, m-Cl and p-Cl, fully characterized by CHNS micro elemental analysis, infrared spectroscopy, UV-visible, nuclear magnetic resonance (1H, 13C) and X-ray crystallography. 1-(3-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL3) crystallized in the monoclinic system, a=14.504(3), b=4.9599(11), c=22.325(5) Å, β=98.461(7)°, Z= 4 and V=1588.5(6) Å with space group P21/c. The IR spectra of the ligands exhibits the characteristic v(CO) and v(N-H) at range 1701-1640 cm-1 and 3317-3144 cm-1, respectively. Whereas the 1H and 13C NMR spectra shows the resonances for N-H and -CO groups at range 8.3-8.5 and 160-163 ppm, respectively. A one-pot reaction involving the aroylthiourea ligand, oxovanadium(IV) ion and potassium hydrotris(3,5-dimethylpyrazolyl)borate (KTp) complex gave the desired [oxovanadium(IV)(tris(pyrazolyl)borate)(aroylthiourea)] complexes namely TpVOL1, TpVOL2, TpVOL3 and TpVOL4 and all complexes were characterized accordingly. X-ray study showed that TpVOL1 adopted a monoclinic crystal, a=3.415(2), b=19.463(3), c=14.22(3) Å, β=107.411(4)°, Z= 4 and V=3542.7(11) Å with P21/c space group. The VO2+ center adopted a pseudo-octahedral geometry O2N3S, with the oxovanadium(IV) coordinated to the bidentate ligand (X-Ph)(CO)NH(CS)N(C6H5)(CH3) and tridentate Tp* ligands. The results showed that aroylthiourea ligands behave as bidentate chelate through O and S atom and the Tp* C3v symmetry adds stabilization to the VO2+ through its protective tripodal geometry. Penerbit Universiti Kebangsaan Malaysia 2018-08 Article PeerReviewed application/pdf en http://journalarticle.ukm.my/12199/1/16%20Syahidah%20Mohd%20Tahir.pdf Syahidah Mohd Tahir, and Aisha Al-Abbasi, and Qurnisha Ghazali, and Khuzaimah Arifin, and Mohammad Kassim, (2018) Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes. Sains Malaysiana, 47 (8). pp. 1775-1785. ISSN 0126-6039 http://www.ukm.my/jsm/english_journals/vol47num8_2018/contentsVol47num8_2018.html
repository_type	Digital Repository
institution_category	Local University
institution	Universiti Kebangasaan Malaysia
building	UKM Institutional Repository
collection	Online Access
language	English
description	Aroylthiourea ligands, 1-aroyl-3-cyclohexyl-3-methylthiourea (HL1), 1-(2-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL2), 1-(3-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL3) and 1-(4-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL4) were synthesized through a condensation reaction of methylcyclohexylamine and aroylisothiocyanate with a general formula (X-Ph)(CO)NH(CS)N(C6H5)(CH3) where X = H, o-Cl, m-Cl and p-Cl, fully characterized by CHNS micro elemental analysis, infrared spectroscopy, UV-visible, nuclear magnetic resonance (1H, 13C) and X-ray crystallography. 1-(3-chloroaroyl)-3-cyclohexyl-3-methylthiourea (HL3) crystallized in the monoclinic system, a=14.504(3), b=4.9599(11), c=22.325(5) Å, β=98.461(7)°, Z= 4 and V=1588.5(6) Å with space group P21/c. The IR spectra of the ligands exhibits the characteristic v(CO) and v(N-H) at range 1701-1640 cm-1 and 3317-3144 cm-1, respectively. Whereas the 1H and 13C NMR spectra shows the resonances for N-H and -CO groups at range 8.3-8.5 and 160-163 ppm, respectively. A one-pot reaction involving the aroylthiourea ligand, oxovanadium(IV) ion and potassium hydrotris(3,5-dimethylpyrazolyl)borate (KTp) complex gave the desired [oxovanadium(IV)(tris(pyrazolyl)borate)(aroylthiourea)] complexes namely TpVOL1, TpVOL2, TpVOL3 and TpVOL4 and all complexes were characterized accordingly. X-ray study showed that TpVOL1 adopted a monoclinic crystal, a=3.415(2), b=19.463(3), c=14.22(3) Å, β=107.411(4)°, Z= 4 and V=3542.7(11) Å with P21/c space group. The VO2+ center adopted a pseudo-octahedral geometry O2N3S, with the oxovanadium(IV) coordinated to the bidentate ligand (X-Ph)(CO)NH(CS)N(C6H5)(CH3) and tridentate Tp* ligands. The results showed that aroylthiourea ligands behave as bidentate chelate through O and S atom and the Tp* C3v symmetry adds stabilization to the VO2+ through its protective tripodal geometry.
format	Article
author	Syahidah Mohd Tahir, Aisha Al-Abbasi, Qurnisha Ghazali, Khuzaimah Arifin, Mohammad Kassim,
spellingShingle	Syahidah Mohd Tahir, Aisha Al-Abbasi, Qurnisha Ghazali, Khuzaimah Arifin, Mohammad Kassim, Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes
author_facet	Syahidah Mohd Tahir, Aisha Al-Abbasi, Qurnisha Ghazali, Khuzaimah Arifin, Mohammad Kassim,
author_sort	Syahidah Mohd Tahir,
title	Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes
title_short	Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes
title_full	Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes
title_fullStr	Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes
title_full_unstemmed	Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes
title_sort	synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes
publisher	Penerbit Universiti Kebangsaan Malaysia
publishDate	2018
url	http://journalarticle.ukm.my/12199/ http://journalarticle.ukm.my/12199/ http://journalarticle.ukm.my/12199/1/16%20Syahidah%20Mohd%20Tahir.pdf
first_indexed	2023-09-18T20:02:05Z
last_indexed	2023-09-18T20:02:05Z
_version_	1777406915622469632

Synthesis, structure and spectroscopic properties of oxovanadium tris(3,5-dimethylpyrazolyl)borate aroylthiourea complexes

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