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Recent progress in heteronuclear long-range NMR of complex carbohydrates: 3D H2BC and clean HMBC
Authors:Sebastian Meier, Bent O. Petersen, Jens   . Duus,Ole W. S  rensen
Affiliation:aCarlsberg Laboratory, Gamle Carlsberg Vej 10, DK-2500 Valby, Denmark;bDepartment of Chemistry, Technical University of Denmark, Kemitorvet 207, DK-2800 Kgs., Lyngby, Denmark
Abstract:The new NMR experiments 3D H2BC and clean HMBC are explored for challenging applications to a complex carbohydrate at natural abundance of 13C. The 3D H2BC experiment is crucial for sequential assignment as it yields heteronuclear one- and two-bond together with COSY correlations for the 1H spins, all in a single spectrum with good resolution and non-informative diagonal-type peaks suppressed. Clean HMBC is a remedy for the ubiquitous problem of strong coupling induced one-bond correlation artifacts in HMBC spectra of carbohydrates. Both experiments work well for one of the largest carbohydrates whose structure has been determined by NMR, not least due to the enhanced resolution offered by the third dimension in 3D H2BC and the improved spectral quality due to artifact suppression in clean HMBC. Hence these new experiments set the scene to take advantage of the sensitivity boost achieved by the latest generation of cold probes for NMR structure determination of even larger and more complex carbohydrates in solution.
Keywords:3D NMR   H2BC   Heteronuclear NMR   HMBC   NMR assignment
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