3D MAS NMR Experiment Utilizing Through-Space
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Author(s) • • •
Linse, Sara
Donovan, Kevin J
Silvers, Robert Paul Georg
Griffin, Robert Guy
Date Issued
May 2017
Journal
Journal of the American Chemical Society
Publisher
American Chemical Society (ACS)
Citation
Donovan, Kevin J. et al. “3D MAS NMR Experiment Utilizing Through-Space 15N–15N Correlations.” Journal of the American Chemical Society 139, 19 (May 2017): 6518–6521 © 2017 American Chemical Society
Version
Author's final manuscript
Abstract
We demonstrate a novel 3D NNC magic angle spinning NMR experiment that generates ¹⁵N–¹⁵N internuclear contacts in protein systems using an optimized ¹⁵N–¹⁵N proton assisted recoupling (PAR) mixing period and a ¹³C dimension for improved resolution. The optimized PAR condition permits the acquisition of high signal-to-noise 3D data that enables backbone chemical shift assignments using a strategy that is complementary to current schemes. The spectra can also provide distance constraints. The utility of the experiment is demonstrated on an M₀Aβ₁₋₄₂ fibril sample that yields high-quality data that is readily assigned and interpreted. The 3D NNC experiment therefore provides a powerful platform for solid-state protein studies and is broadly applicable to a variety of systems and experimental conditions.
MIT Department
Massachusetts Institute of Technology. Department of Chemistry
Francis Bitter Magnet Laboratory (Massachusetts Institute of Technology)
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Article is made available in accordance with the publisher's policy and may be subject to US copyright law. Please refer to the publisher's site for terms of use.
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DOI of Published Version
https://doi.org/10.1021/jacs.7b01159