title: Three-dimensional heteronuclear NMR techniques for assignment and conformational analysis using exchangeable protons in uniformly 13C-enriched oligosaccharides.
abstract: We present heteronuclear three-dimensional gradient-NMR techniques for the resonanceassignment of exchangeable (-OH and -NH) protons in uniformly 13C isotopically enrichedoligosaccharides and for the measurement of 1H-1H nuclear Overhauser enhancementsinvolving these protons. These techniques are derived from conventional HOHAHA-HSQCand NOESY(ROESY)-HSQC experiments, and are illustrated in application to a sample ofuniformly 13C-enriched Galbeta1-4GlcNAc, and demonstrate that a total of 35 ROEs involvingexchangeable protons can be detected and assigned. We present a quantitative analysis ofthese ROEs that can only be accommodated in a model of the solution behaviour of theoligosaccharide that involves considerable internal motion.
authors.affiliation: Centre for Biomolecular Sciences, University of St. Andrews, The Purdie Building, St. Andrews, KY16 9ST, U.K.
authors.forename: R
authors.initials: R
authors.lastname: Harris
authors.forename: T J
authors.initials: TJ
authors.lastname: Rutherford
authors.forename: M J
authors.initials: MJ
authors.lastname: Milton
authors.forename: S W
authors.initials: SW
authors.lastname: Homans