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New and old NMR experiments for the resonance assignment of complex oligosaccharides--application to a cyclodextrin derivative
Authors:Plainchont B  Martinez A  Tisse S  Bouillon J-P  Pilard F  Wieruszeski J-M  Lippens G  Jeannerat D  Nuzillard J-M
Institution:Institut de Chimie Moléculaire de Reims, Université de Reims Champagne-Ardenne, CNRS UMR 6229, Reims, France.
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.
Keywords:NMR  1H  13C  cyclodextrin  assignment  selective pulses  resolution enhancement  aliasing  sequential assignment
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