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Preparation and Spectroscopic Study of Different Stoichiometric Solid Supramolecular Inclusion Complexes of β-Cyclodextrin with Short Chain Aliphatic Amines
Le-xin Song*,Chuan-feng Teng,Hai-ming Wang,Lei Bai
Author NameAffiliationE-mail
Le-xin Song* Department of Chemistry, University of Science and Technology of China, Hefei 230026, China solexin@ustc.edu.cn 
Chuan-feng Teng Department of Chemistry, University of Science and Technology of China, Hefei 230026, China  
Hai-ming Wang Department of Chemistry, University of Science and Technology of China, Hefei 230026, China  
Lei Bai Department of Chemistry, University of Science and Technology of China, Hefei 230026, China  
Abstract:
The solid Supramolecular complexes of β-cyclodextrin (β-CD) with ethylenediamine 1, diethylenetriamine 2 and triethylamine 3 were obtained and characterized using elemental analysis, powder X-ray diffraction, infrared spectroscopy, thermogravimetric analysis, and 1H nuclear magnetic resonance spectroscopy. Based on the results of elemental analysis and 1H NMR, the guest-host stoichiometries of the three solid complexes were determined to be 5:2 for 1-β-CD, 1:1 for 2-β-CD, and 1:3 for 3-β-CD. The yields were relative to the molar volume ratio of guest toβ-CD cavity, and increased in the order: 1-β-CD<2-β-CD<3-β-CD. X-ray diffraction patterns of the inclusion complexes gave very good exhibitions not only in location of diffraction peaks but also in shape and diffraction intensity of the peaks due to the intermolecular complexations betweenβ-CD and the guests. The formation of host-guest inclusion complexes exhibited obviously enhanced phase change temperatures of the complexed guests such as 1 and 3. The H-5 protons located at the narrower rim inside the CD cavity experienced a higher shift upon inclusion while all other protons experienced lower shifts.
Key words:  β-cyclodextrin, Inclusion complex, Ethylenediamine, Supramolecular
FundProject:其它
Preparation and Spectroscopic Study of Different Stoichiometric Solid Supramolecular Inclusion Complexes of β-Cyclodextrin with Short Chain Aliphatic Amines
宋乐新*,滕传峰,王海名,柏雷
摘要:
选择β-CD为主体,制备了它与乙二胺1、二乙烯三胺2和三乙胺3形成的固体包合物,并通过元素分析、X射线衍射、红外光谱、热重和1H核磁共振等物理手段对制备的包合物进行了表征.基于元素分析和1H核磁共振的结果,在1-β-CD、2-β-CD和3-fi-CD三个固体包合物中,主体、客体的化学计量比分别确定为2:5、1:1和3:1.包合物的产率与客体分子对β-CD空腔的体积比有关,提升顺序为1-β-CD<2-β-CD<3-β-CD.X射线衍射表明,由于β-CD与客体存在分子间相互作用,原本归属于主、客体的衍射峰不仅在峰的位置,而且在峰的形状和衍射强度上都发生了明显的变化.并且主、客体包合物的形成明显提高了被包合的客体分子1和3的相变温度.此外,位于β-CD空腔小口端的H-5质子由于包合作用而显示更大的化学位移变化,而所有腔外质子均具有相对较低的化学位移变化值.
关键词:  β-环糊精,包合物,乙二胺,超分子
DOI:10.1088/1674-0068/21/02/174-180
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