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NMR spectra and dynamics of the sodium salt of per(6‐thiobenzoic acid)‐γ‐cyclodextrin
Author(s) -
Cameron K. S.,
Fielding L.,
Palin R.,
Uhrin D.
Publication year - 2005
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.1599
Subject(s) - chemistry , heteronuclear single quantum coherence spectroscopy , cyclodextrin , two dimensional nuclear magnetic resonance spectroscopy , spectral line , nuclear magnetic resonance spectroscopy , nmr spectra database , dispersion (optics) , proton nmr , carbon 13 nmr satellite , molecular dynamics , salt (chemistry) , spectroscopy , carbon 13 nmr , crystallography , stereochemistry , computational chemistry , fluorine 19 nmr , organic chemistry , physics , quantum mechanics , astronomy , optics
The solution‐state NMR spectra of a per‐6‐substituted γ‐cyclodextrin show some interesting dynamic properties. At high temperature (353 K), the 1 H NMR spectrum shows dynamic averaging of the different conformations. This averaging is no longer observed on cooling of the cyclodextrin solution to 278 K, resulting in NMR spectra with a large 1 H and 13 C chemical shift dispersion. The complete assignment of the eight unique glucosyl residues was achieved using COSY, HSQC and exchange spectroscopy. A ROESY spectrum, with a short mixing time to reduce the effects of exchange, gives correlations that lead to the determination of the connectivity of all eight glucosyl residues. On the NMR time‐scale, the cyclodextrin is highly dynamic; the lower temperature minimum energy conformation has one of the aromatic rings self‐complexed and a distorted cyclodextrin torus. Copyright © 2005 John Wiley & Sons, Ltd.