|本期目录/Table of Contents|

[1]董水超,陶亚秋,沈晓冬,等.粉末X线衍射测定间氨基苯甲酸/富马酸(2/1)有机盐晶体结构[J].南京工业大学学报(自然科学版),2014,36(02):83-88.[doi:10.3969/j.issn.1671-7627.2014.02.014]
 DONG Shuichao,TAO Yaqiu,SHEN Xiaodong,et al.Structure determination of an organic salt of 3-aminobenzoic acid/fumaric acid(2/1)from powder X-ray diffraction data[J].Journal of NANJING TECH UNIVERSITY(NATURAL SCIENCE EDITION),2014,36(02):83-88.[doi:10.3969/j.issn.1671-7627.2014.02.014]
点击复制

粉末X线衍射测定间氨基苯甲酸/富马酸(2/1)有机盐晶体结构()
分享到:

《南京工业大学学报(自然科学版)》[ISSN:1671-7627/CN:32-1670/N]

卷:
36
期数:
2014年02期
页码:
83-88
栏目:
出版日期:
2014-03-30

文章信息/Info

Title:
Structure determination of an organic salt of 3-aminobenzoic acid/fumaric acid(2/1)from powder X-ray diffraction data
文章编号:
1671-7627(2014)02-0083-06
作者:
董水超1陶亚秋1沈晓冬1杜峰2潘志刚1
1.南京工业大学 材料科学与工程学院,江苏 南京 210009; 2.江苏瑞丰科技实业有限公司,江苏 南京 210009
Author(s):
DONG Shuichao1TAO Yaqiu1SHEN Xiaodong1DU Feng2PAN Zhigang1
1.College of Materials Science and Engineering, Nanjing Tech University, Nanjing 21009, China; 2.Jiangsu Refontech Industrial Co.Ltd.,Nanjing 210009, China
关键词:
晶体工程 氢键 质子转移 直接空间法 Rietveld 精修
Keywords:
crystal engineering hydrogen bonding proton transfer direct space method Rietveld refinement
分类号:
O641.3
DOI:
10.3969/j.issn.1671-7627.2014.02.014
文献标志码:
A
摘要:
以间氨基苯甲酸和富马酸为原料,采用乙醇溶液结晶法制备间氨基苯甲酸/富马酸(2/1)有机盐粉晶体。利用粉末X线衍射数据,通过指标化确定其晶胞参数并采用直接空间法解析其晶体结构。结合傅里叶红外光谱仪测定羧酸根中H的结合情况,利用Rietveld精修技术对其晶体结构进行精修,最终测定了间氨基苯甲酸/富马酸(2/1)有机盐的晶体结构。该晶体结构中不对称单元中包含1个质子化的间氨基苯甲酸和半个去质子化的富马酸。羧基上和氨基上的H全部参与氢键作用。系统分析了该晶体结构中氢键的形成方式,揭示了氢键在晶体结构中的堆砌作用,并展示了粉末X线衍射技术在有机分子晶体结构测定中应用前景。
Abstract:
An organic salt of 3-aminobenzoic acid/fumaric acid(2/1)was crystallized from a solution of ethanol. The high resolution powder X-ray diffraction(XRD)data were indexed and the crystal structure of the title compound was solved using a direct space method for the structure solution by Rietveld refinement in combination of Fourier transform infrared spectroscopy(FT-IR)analysis. In the crystal structure of the title compound, the asymmetric unit consisted of one protonized 3-aminobenzoic acid and half of the deprotonated fumaric acid. The hydrogen atoms attached to the amino and carboxylic acid groups were involved in hydrogen bonding. The arrangement of the hydrogen bonding was analyzed and its role in crystal packing was investigated. Results demonstrated the relevance and the application with powder XRD techniques in the field of organic crystal determination.

参考文献/References:

[1] Arends I W C E,Sheldo R A,Wallau M,et al.Oxidative transformations of organic compounds medited by redox molecular sieves [J].Angew Chem Int Ed Engl,1997,36(11):1144-1163.
[2] Chen C T,Suslick K S.One-dimensional coordination polymers:applications to material science [J].Coord Chem Rew,1993,128(1/2):293-322.
[3] Lehn J M.Supramolecular chemistry [M].Weinheim:VCH,1995.
[4] Desiraju G R,Parshall G W.Crystal engineering:the design of organic solids [J].Mater Sci Monog,1989,54:312-326.
[5] Desiraju G R.Crystal engineering:solid state supramolecular synthesis [J].Curr Opin Solid State Mater Sci,1997,2(4):451-454.
[6] Sharma C V K,Rogers R D.Perspectives of crystal engineering [J].Mater Today,1998,1(3):27-30.
[7] Steiner T,Desiraju G R.Distinction between the weak hydrogen bond and the van der Waals interaction [J].Chem Commun,1998(8):891-892.
[8] 晏华.超分子液晶 [M].北京:科学出版社,2000.
[9] Etter M C.Encoding and decoding hydrogen-hond patterns of organic compounds [J].Acc Chem Res,1990,23(4):120-126.
[10] Calhorda M J.Weak hydrogen bonds:theoretical studies [J].Chem Commun,2000,10:801-809.
[11] Vangala V R,Chow P S,Tan R B H.Co-crystals and Co-crystal hydrates of the antibiotic nitrofurantoin:structural studies and physicochemical properties [J].Cryst Growth Des,2012,12(12):5925-5938.
[12] Yin H D,Liu H,Hong M.Synthesis,structural characterization and DNA-binding properties of organotin(IV)complexes based on Schiff base ligands derived from 2-hydroxy-1-naphthaldy and 3- or 4-aminobenzoic acid [J].J Organomet Chem,2012,713:11-19.
[13] Kanazawa T,Matsuda Y,Tasaka S.Fabrication of a porous structure of poly(tetrafluoroethylene)from a mixture with fumaric acid [J].Polym J,2010,42:509-513.
[14] Cheney M L,Weyna D R,Shan N,et al.Supramolecular architectures of meloxicam carboxylic acid cocrystals,a crystal engineering case study[J].Cryst Growth Des,2010,10(10):4401-4413.
[15] 李海峰.基于多羧酸超分子配合物的构筑与结构研究 [D].汕头:汕头大学,2006.

相似文献/References:

[1]徐南平,王延儒,时钧.水-二甲亚砜、乙醇——二甲亚砜体系密度数据的测定与关联[J].南京工业大学学报(自然科学版),1992,14(03):62.
[2]居威材,陶亚秋,沈晓冬,等.间硝基苯甲酸/8-羟基喹啉(1/1)共晶体结构解析与Rietveld精修[J].南京工业大学学报(自然科学版),2017,39(03):126.[doi:10.3969/j.issn.1671-7627.2017.03.022]
 JU Weicai,TAO Yaqiu,SHEN Xiaodong,et al.Structure analysis and Rietveld refinement of a cocrystal of m-nitrobenzoic acid/8-hydroxyquinoline(1/1)[J].Journal of NANJING TECH UNIVERSITY(NATURAL SCIENCE EDITION),2017,39(02):126.[doi:10.3969/j.issn.1671-7627.2017.03.022]

备注/Memo

备注/Memo:
收稿日期:2013-04-26
作者简介:董水超(1988—),男,江苏溧阳人,硕士,主要研究方向为粉末X线衍射技术; 潘志刚(联系人),副研究员,E-mail:zg_pan@163.com..
更新日期/Last Update: 2014-03-20