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Bulletin of the Korean Chemical Society (BKCS)

ISSN 0253-2964(Print)
ISSN 1229-5949(Online)
Volume 25, Number 5
BKCSDE 25(5)
May 20, 2004 

An NMR Study on Complexation of Cesium Ion by p-tert-Butylcalix[6]arene Ethyl Ester
Kee-Choo Chung, Hyun Namgoong, Jo Woong Lee*
NMR, Calix[6]arene, Cesium, Chemical exchange
Complexation of cesium ion by p-tert-butylcalix[6]arene ethyl ester was studied by NMR spectroscopy in nonpolar CDCl3 and polar acetone-d6 and the results were compared with each other. Analysis of temperature dependent 1H spectra and titration curves reveals that both solvents result in a 1 : 1 cone-form complex with nonpolar CDCl3 yielding a more tightly bound one than acetone-d6. Unexpectedly, at very low temperature, we have found that two phenyl ring proton peaks of equal intensity appear both in CDCl3 and in acetone-d6 solution which gradually collapse and eventually coalesce into a single line as temperature is raised. This observation could be interpreted in terms of the chemical exchange through direct and/or indirect interconversion between two equivalent conformations possible the complex in both solvents over the temperature range observed. And broadening of 133Cs (I = 7/2) nmr line with increasing temperature has also been observed, indicating the exchange of 133Cs ion between the complex and the solvent. From numerical fitting of lineshape changes for one-dimensional 1H and 133Cs spectra, the exchange rate constants and other relevant parameters for this conformational interconversion and the complex-solvent exchange were deduced.
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