New and old NMR experiments for the resonance assignment of complex oligosaccharides-application to a cyclodextrin derivative

Plainchont, B.; Martinez, Alexandre; Tisse, S.; Bouillon, J.-P.; Pilard, F.; Wieruszeski, J.-M.; Lippens, G.; Jeannerat, Damien; Nuzillard, J.-M.

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Title		New and old NMR experiments for the resonance assignment of complex oligosaccharides-application to a cyclodextrin derivative
Authors		Plainchont, B. Martinez, Alexandre Tisse, S. Bouillon, J.-P. Pilard, F. Wieruszeski, J.-M. Lippens, G. Jeannerat, Damien Nuzillard, J.-M. show all authors [1 - 9]
Published in		Magnetic Resonance in Chemistry. 2011, vol. 49, no. 12, p. 781-787
Abstract		The complete assignment of the 1H and 13C 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 1H assignments. The multiplicity edited HSQC and a set of F1 selective HSQC-TOCSY and multiple relay HSQC-COSY spectra gave access to most of the 13C 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 F1 selective F1 decoupled version of the TOCSY-ROESY experiment was recorded.
Keywords		NMR — 1H — 13C — Cyclodextrin — Assignment — Selective pulses — Resolution enhancement — Aliasing — Sequential assignment
Identifiers		DOI: 10.1002/mrc.2828
Full text		Article (Published version) (448 Kb) - Limited access to UNIGE
Structures		Faculté des sciences / Section de chimie et biochimie / Département de chimie organique
Citation (ISO format)		PLAINCHONT, B. et al. New and old NMR experiments for the resonance assignment of complex oligosaccharides-application to a cyclodextrin derivative. In: Magnetic Resonance in Chemistry, 2011, vol. 49, n° 12, p. 781-787. https://archive-ouverte.unige.ch/unige:17801