原位脱羧制备的配合物(HP2W18O62)(C6H6NO2)5·2H2O:结构、光谱及电化学性能

引用本文: 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. doi: 10.3969/j.issn.1001-4861.2013.00.182 shu

Citation: WEI Zhen, ZHU Peng-Fei, ZHANG Ya-Qin, GUO Feng-Wan, QI Xiao-Ting, WANG Juan. Complex (HP₂W₁₈O₆₂)(C₆H₆NO₂)₅·2H₂O via in-situ Decarboxylation: Crystal Structure, Spectroscopy and Electrochemistry[J]. Chinese Journal of Inorganic Chemistry, 2013, 29(5): 1089-1095. doi: 10.3969/j.issn.1001-4861.2013.00.182 shu

原位脱羧制备的配合物(HP₂W₁₈O₆₂)(C₆H₆NO₂)₅·2H₂O:结构、光谱及电化学性能

魏振 ^1, ,
朱鹏飞 ^1, ,
张雅琴 ^1, ,
郭枫晚 ^2, ,
祁晓婷 ^1, ,
王娟 ^{1,
,}

通讯作者: 王娟,E-mail:wangjuan_hd@163.com;会员登记号:S06N3916M1012,

基金项目:
国家自然科学基金(No.21201061) (No.21201061)

湖北省自然科学基金(No.2012FFB00205)资助项目。 (No.2012FFB00205)

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

English

Complex (HP₂W₁₈O₆₂)(C₆H₆NO₂)₅·2H₂O via in-situ Decarboxylation: Crystal Structure, Spectroscopy and Electrochemistry

1.
1. College of Chemistry and Chemical Engineering, Hubei University, Wuhan 430062, China;

Corresponding author: 王娟,E-mail:wangjuan_hd@163.com;会员登记号:S06N3916M1012,

Received Date: 17 January 2013
Fund Project:
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.

Key words:

polyoxometallate;pyridine-2,6-dicarboxylic;2-picolinic acid;electrochemistry;crystal structure

1. [1] Fan L L, Xiao D R, Wang E B, et al. Crystal Growth & Design, 2007,7(4):592-954[1] Fan L L, Xiao D R, Wang E B, et al. Crystal Growth & Design, 2007,7(4):592-954
2. [2] Pope M T. Heteropoly and Isopolyoxometalates: Vol.8. Berlin: Springer-Verlag, 1983.[2] Pope M T. Heteropoly and Isopolyoxometalates: Vol.8. Berlin: Springer-Verlag, 1983.
3. [3] Upreti S, Ramanan A. Crystal Growth & Design, 2006,6(9): 2066-2071[3] Upreti S, Ramanan A. Crystal Growth & Design, 2006,6(9): 2066-2071
4. [4] Santiago R, Pablo V, Luis L, et al. Inorg. Chem., 2003,42: 3709-3711[4] Santiago R, Pablo V, Luis L, et al. Inorg. Chem., 2003,42: 3709-3711
5. [5] Ednéia C, José A D, Sílvia C L, et al. Microporous Mesoporous Mater., 2010,132(1/2):103-111[5] Ednéia C, José A D, Sílvia C L, et al. Microporous Mesoporous Mater., 2010,132(1/2):103-111
6. [6] Sun C Y, Liu S X, Liang D D, et al. J. Am. Chem. Soc., 2009,131(5):1883-1888[6] Sun C Y, Liu S X, Liang D D, et al. J. Am. Chem. Soc., 2009,131(5):1883-1888
7. [7] Vanpelt C E, Crooks W J, Choppin G R. Inorg. Chim. Acta, 2003,346:215-222[7] Vanpelt C E, Crooks W J, Choppin G R. Inorg. Chim. Acta, 2003,346:215-222
8. [8] Wang J P, Wei M L, Niu J Y. Trans. Met. Chem., 2004,29: 81-85[8] Wang J P, Wei M L, Niu J Y. Trans. Met. Chem., 2004,29: 81-85
9. [9] Raghuraman K, Katti K K, Barbour L J, et al. J. Am. Chem. Soc., 2003,125(23):6955-6961[9] Raghuraman K, Katti K K, Barbour L J, et al. J. Am. Chem. Soc., 2003,125(23):6955-6961
10. [10] Liu M S, Yu Q Y, Cai Y P, et al. Crystal Growth & Design, 2008,8(11):4083-4091[10] Liu M S, Yu Q Y, Cai Y P, et al. Crystal Growth & Design, 2008,8(11):4083-4091
11. [11] Liu J Z, Zhang Z, Yin X Hong, et al. J. Chem. Crystallogr., 2012,42:1001-1006[11] Liu J Z, Zhang Z, Yin X Hong, et al. J. Chem. Crystallogr., 2012,42:1001-1006
12. [12] Zafar A S, Mohd K, Sarvendra K, et al. Eur. J. Med. Chem., 2010,45:264-269[12] Zafar A S, Mohd K, Sarvendra K, et al. Eur. J. Med. Chem., 2010,45:264-269
13. [13] Liu L F. J. Inorg. Organomet Polym., 2012,22:1308-1313[13] Liu L F. J. Inorg. Organomet Polym., 2012,22:1308-1313
14. [14] Wang J, He F L, Wang X Y, et al. J. Coord. Chem., 2011, 64(13):2312-2320[14] Wang J, He F L, Wang X Y, et al. J. Coord. Chem., 2011, 64(13):2312-2320
15. [15] SMART, Version 5.624; Brüker AXS, Inc.: Madison, WI, 2000.[15] SMART, Version 5.624; Brüker AXS, Inc.: Madison, WI, 2000.
16. [16] SAINT, Version 6.36A; Brüker AXS, Inc.: Madison, WI, 2000.[16] SAINT, Version 6.36A; Brüker AXS, Inc.: Madison, WI, 2000.
17. [17] Sheldrick G. SADABS, Version 2.10, University of Göttingen: Göttingen, Germany, 2003.[17] Sheldrick G. SADABS, Version 2.10, University of Göttingen: Göttingen, Germany, 2003.
18. [18] Sheldrick G. SHELXTL SHELXTL-97: Program for Crystal Structure Refinement, University of Göttingen, Germany, 1997.[18] Sheldrick G. SHELXTL SHELXTL-97: Program for Crystal Structure Refinement, University of Göttingen, Germany, 1997.
19. [19] Niu J Y, Wang Z L, Wang J P. Inorg. Chem. Commun., 2003,6:1272-1274[19] Niu J Y, Wang Z L, Wang J P. Inorg. Chem. Commun., 2003,6:1272-1274
20. [20] Zhao J W, Yu L, Wang J P, et al. Chin. J. Appl. Chem., 2005,12:1324-1328[20] Zhao J W, Yu L, Wang J P, et al. Chin. J. Appl. Chem., 2005,12:1324-1328
21. [21] Huang J, Xu Y H, Chen X K, et al. J. Rare Earths, 2012,30 (6):586-591[21] Huang J, Xu Y H, Chen X K, et al. J. Rare Earths, 2012,30 (6):586-591
22. [22] Moreira A B, Oliveira H P M, Atvars T D Z, et al. Anal. Chim. Acta, 2005,539:257-261[22] Moreira A B, Oliveira H P M, Atvars T D Z, et al. Anal. Chim. Acta, 2005,539:257-261
23. [23] Sadakane M, Steckhan E. Chem. Rev., 1998,98:219-237[23] Sadakane M, Steckhan E. Chem. Rev., 1998,98:219-237
24. [24] WANG Chong-Tai(王崇太), HUA Ying-Jie(华英杰), SUN Zhen-Fan(孙振范), et al. Acta Phys.-Chim. Sin.(Wuli Huaxue Xuebao), 2011,27(2):473-478[24] WANG Chong-Tai(王崇太), HUA Ying-Jie(华英杰), SUN Zhen-Fan(孙振范), et al. Acta Phys.-Chim. Sin.(Wuli Huaxue Xuebao), 2011,27(2):473-478

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 960
HTML全文浏览量: 65

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

原位脱羧制备的配合物(HP₂W₁₈O₆₂)(C₆H₆NO₂)₅·2H₂O:结构、光谱及电化学性能

通讯作者: 王娟,E-mail:wangjuan_hd@163.com;会员登记号:S06N3916M1012,

English

Complex (HP₂W₁₈O₆₂)(C₆H₆NO₂)₅·2H₂O via in-situ Decarboxylation: Crystal Structure, Spectroscopy and Electrochemistry

Corresponding author: 王娟,E-mail:wangjuan_hd@163.com;会员登记号:S06N3916M1012,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处