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Synthesis, Crystal Structure and Properties of Complex VO(C_(10)H_9NO_3)(C_(13)H_(10)NO_2)

Synthesis, Crystal Structure and Properties of Complex VO(C_(10)H_9NO_3)(C_(13)H_(10)NO_2)
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摘要 Complex VO(C 10H 9NO 3)(C 13H 10NO 2)(C 10H 9NO 2- 3=N-salicylidene-L-alaninate, C 13H 10NO- 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 P2 1 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, M r=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 CDCl 3. There exists a quasi-reversible one-electron redox reaction corresponding to VⅤ/VⅥ couple in the three non-aqueous solvents, and the redox potential E 1/2 of the title complex substantially shifts in the direction of the positive voltage increase in the order: CH 2Cl 2<CH 3CN<DMF. Complex VO(C 10H 9NO 3)(C 13H 10NO 2)(C 10H 9NO 2- 3=N-salicylidene-L-alaninate, C 13H 10NO- 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 P2 1 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, M r=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 CDCl 3. There exists a quasi-reversible one-electron redox reaction corresponding to VⅤ/VⅥ couple in the three non-aqueous solvents, and the redox potential E 1/2 of the title complex substantially shifts in the direction of the positive voltage increase in the order: CH 2Cl 2<CH 3CN<DMF.
出处 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2005年第1期104-108,共5页 高等学校化学研究(英文版)
基金 SupportedbytheNaturalScienceFundofHeilongjiangProvince(No.B00-07),theFundofEducationCommissionofHeilongjiangProvinceandtheScientificFundofRemarkableYounthsofHeilongjiangUniversity.
关键词 Oxovanadium complex Hydroxamate complex Crystal structure Spectral property Oxovanadium complex, Hydroxamate complex, Crystal structure, Spectral property
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参考文献16

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