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NMR spectra and dynamics of the sodium salt of per(6-thiobenzoic acid)-γ-cyclodextrin

✍ Scribed by K. S. Cameron; L. Fielding; R. Palin; D. Uhrin

Publisher
John Wiley and Sons
Year
2005
Tongue
English
Weight
208 KB
Volume
43
Category
Article
ISSN
0749-1581

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✦ Synopsis

The solution-state NMR spectra of a per-6-substituted gamma-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.

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