Synthesis and Characterization of Three Vanadium(Ⅴ) Complexes Incorporating Tridentate Hydrazone Ligands of Thiophene-2-carboxylic Hydrazide and 2-Furoic Acid Hydrazide  

作　　者：耿磊珍 邢婧 魏玮 周荫庄 

机构地区：[1]Department of Chemistry,Capital Normal University

出　　处：《Chinese Journal of Structural Chemistry》2012年第4期562-568,共7页结构化学（英文）

基　　金：supported by the Scientific Research Common Program of Beijing Municipal Commission of Education,PRC (KM200910028011)

摘　　要：Divanadium（Ⅴ） complex [VO（aptch）（μ-OCH3）]2（1） and two monovanadium（Ⅴ） complexes [VO（apfah））（OEt）]（2a and 2b,H2aptch = 2-hydroxyacetophenone thiophene-2-car-boxylic hydrazone,H2apfah = 2-hydroxyacetophenone 2-furoic acid hydrazone） have been synthesized and characterized.Single-crystal X-ray diffraction studies reveal that 1 is a cen-trosymmetric dimer bridged by two methoxido O-atoms.Complex 1 crystallizes in the monoclinic crystal system,space groups P21/c with a = 7.4825（4）,b = 17.0928（11）,c = 11.6961（7） ,β = 98.172（4）o,Z = 2,F（000） = 728,μ = 0.829 mm-1,the final R = 0.0457 and wR = 0.1137 for 2654 observed reflections with I 〉 2（I）.The vanadium（V） is coordinated to the tridentate ligand,ethanol molecule to form a distorted square-pyramidal geometry,complexes 2a and 2b.Although 2a and 2b have the same asymmetric unit,they belong to different space groups.Complex 2a crystallizes in the monoclinic crystal system,space groups P21/n with a = 10.2293（2）,b = 15.6660（3）,c = 10.6298（2） ,β = 116.259（1）o,Z = 4,μ = 0.676 mm-1;complex 2b crystallizes in the triclinic crystal system,space groups P with a = 8.2808（4）,b = 9.4704（5）,c = 10.0819（5） ,α = 86.133（3）,= 81.956（3）,γ = 80.248（3）o,Z = 2 and μ = 0.670 mm-1.The hydrogen bonds are found to exist in 2b only.The crystal structure is stabilized by intermolecular hydrogen bonds of C-H···O.Divanadium（Ⅴ） complex [VO（aptch）（μ-OCH3）]2（1） and two monovanadium（Ⅴ） complexes [VO（apfah））（OEt）]（2a and 2b,H2aptch = 2-hydroxyacetophenone thiophene-2-car-boxylic hydrazone,H2apfah = 2-hydroxyacetophenone 2-furoic acid hydrazone） have been synthesized and characterized.Single-crystal X-ray diffraction studies reveal that 1 is a cen-trosymmetric dimer bridged by two methoxido O-atoms.Complex 1 crystallizes in the monoclinic crystal system,space groups P21/c with a = 7.4825（4）,b = 17.0928（11）,c = 11.6961（7） ,β = 98.172（4）o,Z = 2,F（000） = 728,μ = 0.829 mm-1,the final R = 0.0457 and wR = 0.1137 for 2654 observed reflections with I 〉 2（I）.The vanadium（V） is coordinated to the tridentate ligand,ethanol molecule to form a distorted square-pyramidal geometry,complexes 2a and 2b.Although 2a and 2b have the same asymmetric unit,they belong to different space groups.Complex 2a crystallizes in the monoclinic crystal system,space groups P21/n with a = 10.2293（2）,b = 15.6660（3）,c = 10.6298（2） ,β = 116.259（1）o,Z = 4,μ = 0.676 mm-1;complex 2b crystallizes in the triclinic crystal system,space groups P with a = 8.2808（4）,b = 9.4704（5）,c = 10.0819（5） ,α = 86.133（3）,= 81.956（3）,γ = 80.248（3）o,Z = 2 and μ = 0.670 mm-1.The hydrogen bonds are found to exist in 2b only.The crystal structure is stabilized by intermolecular hydrogen bonds of C-H···O.

关 键 词：vanadium（Ⅴ） complex hydrazone synthesis crystal structure 

分 类 号：O627.2[理学—有机化学]