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Partially-deuterated samples of HET-s(218–289) fibrils: assignment and deuterium isotope effect

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Abstract

Fast magic-angle spinning and partial sample deuteration allows direct detection of 1H in solid-state NMR, yielding significant gains in mass sensitivity. In order to further analyze the spectra, 1H detection requires assignment of the 1H resonances. In this work, resonance assignments of backbone HN and 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.

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Acknowledgements

This work has been supported by the Swiss National Science Foundation (Grants 200020_146757 and 200020_159707) and by the French ANR (ANR-14-CE09-0024B).

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Authors and Affiliations

  1. ETH Zürich, Physical Chemistry, Vladimir-Prelog-Weg 2, 8093, Zürich, Switzerland

    Albert A. Smith, Francesco Ravotti, Emilie Testori, Riccardo Cadalbert, Matthias Ernst & Beat H. Meier

  2. 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

    Anja Böckmann

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  1. Albert A. Smith
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  2. Francesco Ravotti
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  3. Emilie Testori
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  4. Riccardo Cadalbert
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  5. Matthias Ernst
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  7. Beat H. Meier
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Correspondence to Matthias Ernst, Anja Böckmann or Beat H. Meier.

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Smith, A.A., Ravotti, F., Testori, E. et al. Partially-deuterated samples of HET-s(218–289) fibrils: assignment and deuterium isotope effect. J Biomol NMR 67, 109–119 (2017). https://doi.org/10.1007/s10858-016-0087-0

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  • DOI: https://doi.org/10.1007/s10858-016-0087-0

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