Synthesis and structural characterization of [(C2H5)(4)N][(VO2)-O-(V)(OC6H3(OCH3)CHNNCSNH2)]center dot H2O

Citation
Yz. Zhou et al., Synthesis and structural characterization of [(C2H5)(4)N][(VO2)-O-(V)(OC6H3(OCH3)CHNNCSNH2)]center dot H2O, CHIN J ST C, 20(4), 2001, pp. 249-252
Citations number
9
Language
INGLESE
art.tipo
Article
Categorie Soggetti
Inorganic & Nuclear Chemistry
Journal title
CHINESE JOURNAL OF STRUCTURAL CHEMISTRY
ISSN journal
0254-5861 → ACNP
Volume
20
Issue
4
Year of publication
2001
Pages
249 - 252
Database
ISI
SICI code
0254-5861(2001)20:4<249:SASCO[>2.0.ZU;2-1
Abstract
The reaction of tetraethylammonium metavanadate, (Et4N)VO3, with isovanilli n semithiocarbazone(VSTC), HOC6H3(OCH3)CH=NNHCSNH2, in a mixed solvent of e thanol, water and DMSO yields the mononuclear dioxovanadate((V)) complex, [ (C2H5)(4)N] [(VO2)-O-(V) (OC6H3(OCH3)CHNNCSNH2)].H2O (C17H31N4O5SV, M-r = 4 54.5) and its single-crystal structure has been determined by X-ray diffrac tion. The crystal belongs to orthorhombic space group P2(1)2(1)2(1) with un it cell parameters a = 12.940(3), b= 15.414(3), c = 10.703(2) Angstrom, V= 2134.8(11) Angstrom (3), Z=4, D-calc 1.414 Kg/m(3), mu = 0.597 mm(-1), and F(000) = 960. The final agreement factors are R = 0.076 and R-w=0.096 for 1 600 observed independent reflections with F greater than or equal to 4.0 si gma (F). The structure revealed that the vanadium atom is bound to two term inal oxygen atoms and one tridentate donor ligand in a distorted square pyr amidal arrangement. The sulphur-nitrogen-oxygen donor Schiff-base ligand in the thiol form rather than the thione form is coordinated to the vanadium via the mercapto sulphur, the beta -nitrogen and the hydroxylate oxygen.