Synthesis and Structural Characterization of [(C_2H_5)_4N][V~((V))O_2(OC_6H_3(OCH_3)CHNNCSNH_2)]·H_2

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The reaction of tetraethylammonium metavanadate, (Et4N)VO3, with isovanillin semithiocarbazone(VSTC), HOC_6H_3(OCH_3)CH=NNHCSNH2, in a mixed solvent of ethanol, water and DMSO yields the mononuclear dioxovanadate(V) complex, [(C_2H_5)_4N][V~((V))O_2 (OC6H3- (OCH3)CHNNCSNH2)](H_2O (C17H31N4O5SV, Mr = 454.5) and its single-crystal structure has been determined by X-ray diffraction. The crystal belongs to orthorhombic space group P212121 with unit cell parameters a = 12.940(3), b= 15.414(3), c = 10.703(2) ?, V = 2134.8(11) ?3, Z=4, Dcalc = 1.414 Kg/m3, ( = 0.597 mm-1, and F(000) = 960. The final agreement factors are R = 0.076 and Rw=0.096 for 1600 observed independent reflections with F ≥4.0((F). The structure revealed that the vanadium atom is bound to two terminal oxygen atoms and one tridentate donor ligand in a distorted square pyramidal 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 (-nitrogen and the hydroxylate oxygen. The reaction of tetraethylammonium metavanadate (Et4N) VO3 with isovanillin semithiocarbazone (VSTC), HOC_6H_3 (OCH_3) CH = NNHCSNH2 in a mixed solvent of ethanol, water and DMSO yields the mononuclear dioxovanadate (V) complex, [(C_2H_5) The crystal belongs to the orthorhombic space group (C17H31N4O5SV, Mr = 454.5) and its single-crystal structure has been determined by X-ray diffraction P212121 with unit cell parameters a = 12.940 (3), b = 15.414 (3), c = 10.703 (2) ?, V = 2134.8 (11)? 3, Z = 4, Dcalc = 1.414 Kg / mm-1, and F (000) = 960. The final agreement factors are R = 0.076 and Rw = 0.096 for 1600. Observed with independent reflections with F ≥ 4.0 ((F). The structure revealed that the vanadium atom is bound to two terminals oxygen atoms and one tridentate donor ligand in a distorted square pyramidal 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 sulfur, the (-nitrogen and the hydroxylate oxygen.
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