原位脱羧制备的配合物(HP2W18O62)(C6H6NO2)5·2H2O:结构、光谱及电化学性能 |
Complex (HP2W18O62)(C6H6NO2)5·2H2O via in-situ Decarboxylation: Crystal Structure, Spectroscopy and Electrochemistry |
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摘要: 采用水热法将钨酸钠和浓磷酸与有机配体吡啶-2,6-二羧酸通过原位脱羧制得配合物(HP2W18O62)(C6H6NO2)5·2H2O (1), 并用红外光谱、紫外光谱、循环伏安(CV)和X射线单晶衍射等方法进行了表征。分子中的2-吡啶甲酸来源于吡啶-2,6-二羧酸的脱羧反应。化合物1属于单斜晶系,空间群P21/n,晶胞参数分别为:a=1.553 3(2) nm,b=2.006 3(3) nm,c=2.759 9(4) nm,β=103.981(2)°,Z=4,F(000)=8 816。分子间氢键和2-吡啶甲酸与杂多化合物间的弱相互作用使该化合物具有3D超分子结构。CV结果表明,化合物1有四步氧化还原反应。 |
关键词: 多酸 吡啶-2,6-二羧酸 2-吡啶甲酸 电化学 晶体结构 |
基金项目: 国家自然科学基金(No.21201061),湖北省自然科学基金(No.2012FFB00205)资助项目。 |
Abstract: Heteropolyacid complex (HP2W18O62)(C6H6NO2)5·2H2O (1) with 2-picolinic acid in deionized water has been synthesized and characterized by IR, UV, cyclic voltammetry (CV) and X-ray single-crystal diffraction methods. The 2-picolinic acid was obtained by decarboxylation of pyridine-2,6-dicarboxylicacid(H2PDA). The results show that the crystal of the complex 1 belongs to monoclinic system, space group P21/n with: a=1.553 3(2)nm, b=2.006 3(3) nm, c=2.759 9(4) nm, β=103.981(2)°, Z=4, F(000)=8 816. Intermolecular hydrogen-bond and weak interactions from polyanions and 2-picolinic acid lead the complex to a 3D supramolecular architecture. CV study reveals that compound 1 exhibits four chemical processes. CCDC: 905785. |
Keywords: polyoxometallate pyridine-2,6-dicarboxylic 2-picolinic acid electrochemistry crystal structure |
投稿时间:2013-01-17 修订日期:2013-03-15 |
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魏振,朱鹏飞,张雅琴,郭枫晚,祁晓婷,王娟.原位脱羧制备的配合物(HP2W18O62)(C6H6NO2)5·2H2O:结构、光谱及电化学性能[J].无机化学学报,2013,29(5):1089-1095. |
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