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New and old NMR experiments for the resonance assignment of complex oligosaccharides-application to a cyclodextrin derivative |
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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 | |
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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. doi: 10.1002/mrc.2828 https://archive-ouverte.unige.ch/unige:17801 |