title: An Efficient Labelling Approach to Harness Backbone and Side-Chain Protons in (1) H-Detected Solid-State NMR Spectroscopy.
abstract: (1) H-detection can greatly improve spectral sensitivity in biological solid-state NMR (ssNMR), thus allowing the study of larger and more complex proteins. However, the general requirement to perdeuterate proteins critically curtails the potential of (1) H-detection by the loss of aliphatic side-chain protons, which are important probes for protein structure and function. Introduced herein is a labelling scheme for (1) H-detected ssNMR, and it gives high quality spectra for both side-chain and backbone protons, and allows quantitative assignments and aids in probing interresidual contacts. Excellent (1) H resolution in membrane proteins is obtained, the topology and dynamics of an ion channel were studied. This labelling scheme will open new avenues for the study of challenging proteins by ssNMR.
authors.affiliation: NMR Spectroscopy, Bijvoet Center for Biomolecular Research, Department of Chemistry, Faculty of Science, Utrecht University, Padualaan 8, 3584 CH Utrecht (The Netherlands).
authors.forename: Deni
authors.initials: D
authors.lastname: Mance
authors.affiliation: NMR Spectroscopy, Bijvoet Center for Biomolecular Research, Department of Chemistry, Faculty of Science, Utrecht University, Padualaan 8, 3584 CH Utrecht (The Netherlands).|Present address: Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW (UK).
authors.forename: Tessa
authors.initials: T
authors.lastname: Sinnige
authors.affiliation: NMR Spectroscopy, Bijvoet Center for Biomolecular Research, Department of Chemistry, Faculty of Science, Utrecht University, Padualaan 8, 3584 CH Utrecht (The Netherlands).
authors.forename: Mohammed
authors.initials: M
authors.lastname: Kaplan
authors.affiliation: NMR Spectroscopy, Bijvoet Center for Biomolecular Research, Department of Chemistry, Faculty of Science, Utrecht University, Padualaan 8, 3584 CH Utrecht (The Netherlands).
authors.forename: Siddarth
authors.initials: S
authors.lastname: Narasimhan
authors.affiliation: NMR Spectroscopy, Bijvoet Center for Biomolecular Research, Department of Chemistry, Faculty of Science, Utrecht University, Padualaan 8, 3584 CH Utrecht (The Netherlands).
authors.forename: Mark
authors.initials: M
authors.lastname: Daniëls
authors.affiliation: NMR Spectroscopy, Bijvoet Center for Biomolecular Research, Department of Chemistry, Faculty of Science, Utrecht University, Padualaan 8, 3584 CH Utrecht (The Netherlands).
authors.forename: Klaartje
authors.initials: K
authors.lastname: Houben
authors.affiliation: NMR Spectroscopy, Bijvoet Center for Biomolecular Research, Department of Chemistry, Faculty of Science, Utrecht University, Padualaan 8, 3584 CH Utrecht (The Netherlands). M.Baldus@uu.nl.
authors.forename: Marc
authors.initials: M
authors.lastname: Baldus
authors.affiliation: NMR Spectroscopy, Bijvoet Center for Biomolecular Research, Department of Chemistry, Faculty of Science, Utrecht University, Padualaan 8, 3584 CH Utrecht (The Netherlands). M.H.Weingarth@uu.nl.
authors.forename: Markus
authors.initials: M
authors.lastname: Weingarth
keywords: ion channels; membrane proteins; proton detection; side-chain protons; solid-state NMR spectroscopy