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Synthesis, Crystal Structure and Properties of Complex VO(C10H9NO3) (C13H10NO2)
作者姓名:MA Dong-sheng  GAO Shan **  HUO Li-hua  GAO Jin-sheng and ZHAO Jin-gui College of Chemistry and Chemical Engineering  Heilongjiang University  Harbin  P. R. China
作者单位:MA Dong-sheng,GAO Shan **,HUO Li-hua,GAO Jin-sheng and ZHAO Jin-gui College of Chemistry and Chemical Engineering,Heilongjiang University,Harbin 150080,P. R. China
基金项目:黑龙江省自然科学基金,the Fund of Education Commission of Heilongjiang Province and the Scientific Fund of Remarkable Younths of Heilongjiang University
摘    要:Complex VO(C10H9NO3)(C13H10NO2)(C10H9NO2-3=N-salicylidene-L-alaninate, C13H10NO-2=N-phenylbenzohydroxamate) was synthesized and characterized by means of elemental analysis, IR, UV, 1H NMR spectroscopies, cyclic voltammetry and single crystal X-ray diffraction. The complex crystallized in a monoclinic system with space group P21 and crystal cell parameters a=0.9720(1) nm, b=1.8274(2) nm, c=1.2542(1) nm, β=104.868(9)°, V=2.1532(4) nm3, Mr=470.34, Z=2. The two oxygen atoms and the one nitrogen atom of the tridentate Schiff base ligand and the one oxime oxygen atom of the hydroxamate ligand coordinate to the vanadium atom, forming an equatorial plane, the two axial positions are respectively occupied by the oxygen atom of the oxovanadium and the carbonyl oxygen atom of the hydroxamate and the vanadium atom exhibits a distorted octahedral VO(ONO)(OO) coordination sphere. The 1H NMR spectrum suggests that the two isomers, endo and exo in a molar ratio of 1/1.7, coexist in the solution of the title complex in CDCl3. There exists a quasi-reversible one-electron redox reaction corresponding to VⅤ/VⅥ couple in the three non-aqueous solvents, and the redox potential E1/2 of the title complex substantially shifts in the direction of the positive voltage increase in the order: CH2Cl2<CH3CN<DMF.

关 键 词:合成  晶体结构  VO(C10H9NO3)(C13H10NO2)  氧化钒配合物  光谱性质
收稿时间:2004-02-28

Synthesis, Crystal Structure and Properties of Complex VO(C10H9NO3)(C13H10NO2)
MA Dong-sheng,GAO Shan **,HUO Li-hua,GAO Jin-sheng and ZHAO Jin-gui College of Chemistry and Chemical Engineering,Heilongjiang University,Harbin ,P. R. China.Synthesis, Crystal Structure and Properties of Complex VO(C10H9NO3)(C13H10NO2)[J].Chemical Research in Chinese University,2005,21(1):104-108.
Authors:MA Dong-sheng  GAO Shan  HUO Li-Hua  GAO Jin-sheng  ZHAO Jin-gui
Institution:College of Chemistry and Chemical Engineering, Heilongjiang University,Harbin 150080, P. R. China
Abstract:Complex VO(C10H9NO3)(C13H10NO2)(C10H9NO32-=N-salicylidene-L-alaninate, C13H10NO2-=N-phenylbenzohydroxamate) was synthesized and characterized by means of elemental analysis, IR, UV, 1H NMR spectroscopies, cyclic voltammetry and single crystal X-ray diffraction.The complex crystallized in a monoclinic system with space group P21 and crystal cell parameters a=0.9720(1) nm, b=1.8274(2) nm, c=1.2542(1) nm, β=104.868(9)°, V=2.1532(4) nm3, Mr=470.34, Z=2.The two oxygen atoms and the one nitrogen atom of the tridentate Schiff base ligand and the one oxime oxygen atom of the hydroxamate ligand coordinate to the vanadium atom, forming an equatorial plane, the two axial positions are respectively occupied by the oxygen atom of the oxovanadium and the carbonyl oxygen atom of the hydroxamate and the vanadium atom exhibits a distorted octahedral VO(ONO)(OO) coordination sphere.The 1H NMR spectrum suggests that the two isomers, endo and exo in a molar ratio of 1/1.7, coexist in the solution of the title complex in CDCl3.There exists a quasi-reversible one-electron redox reaction corresponding to V/V couple in the three non-aqueous solvents, and the redox potential E1/2 of the title complex substantially shifts in the direction of the positive voltage increase in the order: CH2Cl2<CH3CN<DMF.
Keywords:Oxovanadium complex  Hydroxamate complex  Crystal structure  Spectral property
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