Synthesis, Structure and Spectroscopic Properties of Oxovanadium Tris(3,5-dimethylpyrazolyl)borate Aroylthiourea Complexes

被引：2

作者：

Tahir, Syahidah Mohd ^{[1
]}

Al-Abbasi, Aisha ^{[1
]}

Ghazali, Qurnisha ^{[1
]}

Arifin, Khuzaimah ^{[2
]}

Kassim, Mohammad B. ^{[1
,2
]}

机构：

[1] Univ Kebangsaan Malaysia, Fac Sci & Technol, Sch Chem Sci & Food Technol, Ukm Bangi 43600, Selangor Darul, Malaysia

[2] Univ Kebangsaan Malaysia, Fuel Cell Inst, Ukm Bangi 43600, Selangor Darul, Malaysia

来源：

SAINS MALAYSIANA | 2018年 / 47卷 / 08期

关键词：

Aroylthiourea; chelate; oxovanadium(IV); tris(pyrazolyl)borate; vanadyl; CRYSTAL-STRUCTURE; THIOUREA DERIVATIVES; LIGAND; SERIES;

D O I：

10.17576/jsm-2018-4708-16

中图分类号：

O [数理科学和化学]; P [天文学、地球科学]; Q [生物科学]; N [自然科学总论];

学科分类号：

07 ; 0710 ; 09 ;

摘要：

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-cyclohexl-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, to-Cl and p-CI, fully characterized by CHNS micro elemental analysis, infrared spectroscopy, uv-visible, nuclear magnetic resonance (H-1, C-13) 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) angstrom, beta=98.461(7)degrees, Z= 4 and V=1588.5(6) angstrom with space group P2(1)/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( 1)H and C-13 NMR spectra shows the resonances for N-H and -CO groups at range 83-8.5 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 Tp*VOL1,Tp*VOL2 ,Tp*VOL3 and Tp*VOL4 and all complexes were characterized accordingly. X-ray study showed that Tp*VOL1 adopted a monoclinic crystal, a=3.415(2), b=19.463( 3), c=14.22(3) angstrom, beta=107.411(4)* Z= 4 and V=3542.7( 11) angstrom with P2(1)/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*C(3v )symmetry adds stabilization to the VO2+ through its protective tripodal geometry.

引用

页码：1775 / 1785

页数：11