title: Partially-deuterated samples of HET-s(218-289) fibrils: assignment and deuterium isotope effect.
abstract: Fast magic-angle spinning and partial sample deuteration allows direct detection of1H in solid-state NMR, yielding significant gains in mass sensitivity. In order to further analyze the spectra,1H detection requires assignment of the1H resonances. In this work, resonance assignments of backbone HNand Hα are presented for HET-s(218-289) fibrils, based on the existing assignment of Cα, Cβ, C', and N resonances. The samples used are partially deuterated for higher spectral resolution, and the shifts in resonance frequencies of Cα and Cβ due to the deuterium isotope effect are investigated. It is shown that the deuterium isotope effect can be estimated and used for assigning resonances of deuterated samples in solid-state NMR, based on known resonances of the protonated protein.
authors.affiliation: ETH Zürich, Physical Chemistry, Vladimir-Prelog-Weg 2, 8093, Zürich, Switzerland.
authors.forename: Albert A
authors.initials: AA
authors.lastname: Smith
authors.affiliation: ETH Zürich, Physical Chemistry, Vladimir-Prelog-Weg 2, 8093, Zürich, Switzerland.
authors.forename: Francesco
authors.initials: F
authors.lastname: Ravotti
authors.affiliation: ETH Zürich, Physical Chemistry, Vladimir-Prelog-Weg 2, 8093, Zürich, Switzerland.
authors.forename: Emilie
authors.initials: E
authors.lastname: Testori
authors.affiliation: ETH Zürich, Physical Chemistry, Vladimir-Prelog-Weg 2, 8093, Zürich, Switzerland.
authors.forename: Riccardo
authors.initials: R
authors.lastname: Cadalbert
authors.affiliation: ETH Zürich, Physical Chemistry, Vladimir-Prelog-Weg 2, 8093, Zürich, Switzerland. maer@ethz.ch.
authors.forename: Matthias
authors.initials: M
authors.lastname: Ernst
authors.affiliation: Institut de Biologie et Chimie des Protéines, Bases Moléculaires et Structurales des Systèmes Infectieux, Labex Ecofect, UMR 5086 CNRS, Université de Lyon, 7 passage du Vercors, 69367, Lyon, France. a.bockmann@ibcp.fr.
authors.forename: Anja
authors.initials: A
authors.lastname: Böckmann
authors.affiliation: ETH Zürich, Physical Chemistry, Vladimir-Prelog-Weg 2, 8093, Zürich, Switzerland. beme@ethz.ch.
authors.forename: Beat H
authors.initials: BH
authors.lastname: Meier
mesh_terms: D003903:Deuterium / Q000737:chemistry*; D005656:Fungal Proteins / Q000737:chemistry*; D007553:Isotope Labeling; D009682:Magnetic Resonance Spectroscopy / Q000379:methods; D066329:Protein Aggregates
chemical_list: D005656:Fungal Proteins; C083891:HET-S protein, Podospora anserina; D066329:Protein Aggregates; D003903:Deuterium
keywords: Chemical shift assignment; Deuterated proteins; Deuterium isotope effect; Fibrils; Proton detection; Solid-state NMR