Microsecond motions probed by near-rotary-resonance R1ρ15N MAS NMR experiments: the model case of protein overall-rocking in crystals.

Journal of Biomolecular NMR
Alexey KrushelnitskyKay Saalwächter

Abstract

Solid-state near-rotary-resonance measurements of the spin-lattice relaxation rate in the rotating frame (R1ρ) is a powerful NMR technique for studying molecular dynamics in the microsecond time scale. The small difference between the spin-lock (SL) and magic-angle-spinning (MAS) frequencies allows sampling very slow motions, at the same time it brings up some methodological challenges. In this work, several issues affecting correct measurements and analysis of 15N R1ρ data are considered in detail. Among them are signal amplitude as a function of the difference between SL and MAS frequencies, "dead time" in the initial part of the relaxation decay caused by transient spin-dynamic oscillations, measurements under HORROR condition and proper treatment of the multi-exponential relaxation decays. The multiple 15N R1ρ measurements at different SL fields and temperatures have been conducted in 1D mode (i.e. without site-specific resolution) for a set of four different microcrystalline protein samples (GB1, SH3, MPD-ubiquitin and cubic-PEG-ubiquitin) to study the overall protein rocking in a crystal. While the amplitude of this motion varies very significantly, its correlation time for all four sample is practically the same, 30-50 μ...Continue Reading

References

Oct 31, 2001·Nature Structural Biology·F A MulderL E Kay
Jan 31, 2002·Proceedings of the National Academy of Sciences of the United States of America·Bertil Halle
Aug 31, 2002·Journal of Magnetic Resonance·Kay Saalwächter, Ingrid Fischbach
Dec 22, 2005·Journal of the American Chemical Society·Nicolas GiraudLyndon Emsley
Apr 29, 2006·Angewandte Chemie·Veniamin ChevelkovBernd Reif
Sep 12, 2009·Journal of the American Chemical Society·Veniamin ChevelkovBernd Reif
Aug 10, 2010·Journal of the American Chemical Society·Alexey KrushelnitskyBernd Reif
Sep 21, 2013·Journal of Biomolecular NMR·Tatiana ZinkevichAlexey Krushelnitsky
Jan 29, 2014·Journal of the American Chemical Society·Daryl B GoodVladimir Ladizhansky
Oct 6, 2014·Journal of Magnetic Resonance·Alexey KrushelnitskyKay Saalwächter
Aug 4, 2015·Physical Chemistry Chemical Physics : PCCP·Jonathan M LamleyJózef R Lewandowski
Dec 6, 2012·The Journal of Physical Chemistry Letters·Luca MollicaMartin Blackledge
Oct 6, 2015·Nature Communications·Peixiang MaPaul Schanda
Nov 6, 2015·Angewandte Chemie·Jonathan M LamleyJózef R Lewandowski
Apr 26, 2016·Progress in Nuclear Magnetic Resonance Spectroscopy·Paul Schanda, Matthias Ernst
Jul 18, 2016·Journal of Biomolecular NMR·Albert A SmithMatthias Ernst
Jun 15, 2017·Journal of the American Chemical Society·Daryl GoodVladimir Ladizhansky
Jul 28, 2017·Nature Communications·Vilius KurauskasPaul Schanda
Sep 5, 2017·Solid State Nuclear Magnetic Resonance·Hiroki NagashimaJean-Paul Amoureux
Sep 26, 2017·Journal of Magnetic Resonance·Zdeněk TošnerBernd Reif
Mar 10, 2018·Journal of Biomolecular NMR·Albert A SmithMatthias Ernst

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Citations

Oct 3, 2018·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Matthew D ShannonChristopher P Jaroniec
Nov 18, 2018·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Dominique MarionPaul Schanda
Jul 22, 2019·The Journal of Chemical Physics·Albert A SmithFabien Ferrage
May 16, 2019·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Liliya VugmeysterRiqiang Fu
Jan 16, 2021·Solid State Nuclear Magnetic Resonance·Liliya Vugmeyster
Aug 14, 2021·Frontiers in Molecular Biosciences·Liliya VugmeysterRiqiang Fu
Nov 12, 2021·Frontiers in Molecular Biosciences·Kai Zumpfe, Albert A Smith

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