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  • Title: New and old NMR experiments for the resonance assignment of complex oligosaccharides--application to a cyclodextrin derivative.
    Author: Plainchont B, Martinez A, Tisse S, Bouillon JP, Pilard F, Wieruszeski JM, Lippens G, Jeannerat D, Nuzillard JM.
    Journal: Magn Reson Chem; 2011 Dec; 49(12):781-7. PubMed ID: 22052381.
    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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