New and old NMR experiments for the resonance assignment of complex oligosaccharides--application to a cyclodextrin derivative |
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Authors: | Plainchont B Martinez A Tisse S Bouillon J-P Pilard F Wieruszeski J-M Lippens G Jeannerat D Nuzillard J-M |
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Institution: | Institut de Chimie Moléculaire de Reims, Université de Reims Champagne-Ardenne, CNRS UMR 6229, Reims, France. |
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Abstract: | The complete assignment of the (1)H and (13)C sugar resonances in mono-3,6-anhydro-heptakis(2,3-O-methyl)-hexakis(6-O-methyl)-β-cyclodextrin, an asymmetrically functionalized β-cyclodextrin, was carried out by means of 2D NMR experiments. The TOCSY and the homonuclear multiple relay COSY spectra provided most of the (1)H assignments. The multiplicity edited HSQC and a set of F(1) selective HSQC-TOCSY and multiple relay HSQC-COSY spectra gave access to most of the (13)C chemical shifts. The latter were fully and accurately determined by means of a pair of complementary, highly folded HSQC-TOCSY spectra. The TOCSY-ROESY and ROESY-TOCSY spectra yielded the sequential assignment of the sugar units. A high resolution F(1) selective F(1) decoupled version of the TOCSY-ROESY experiment was recorded. |
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Keywords: | NMR 1H 13C cyclodextrin assignment selective pulses resolution enhancement aliasing sequential assignment |
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