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3D MAS NMR Experiment Utilizing Through-Space 15N-15N Correlations

Donovan, Kevin J.; Silvers, Robert; Linse, Sara LU and Griffin, Robert G (2017) In Journal of the American Chemical Society 139(19). p.6518-6521
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 M01-42 fibril sample that yields high-quality data that is readily assigned and interpreted. The 3D NNC experiment... (More)

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 M01-42 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.

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author
organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Journal of the American Chemical Society
volume
139
issue
19
pages
4 pages
publisher
The American Chemical Society
external identifiers
  • scopus:85019615815
  • wos:000401781900002
ISSN
0002-7863
DOI
10.1021/jacs.7b01159
language
English
LU publication?
yes
id
5f20e7c1-78cb-4002-840d-b0018a8d76f0
date added to LUP
2017-06-13 08:52:01
date last changed
2018-01-07 12:07:12
@article{5f20e7c1-78cb-4002-840d-b0018a8d76f0,
  abstract     = {<p>We demonstrate a novel 3D NNC magic angle spinning NMR experiment that generates <sup>15</sup>N-<sup>15</sup>N internuclear contacts in protein systems using an optimized <sup>15</sup>N-<sup>15</sup>N proton assisted recoupling (PAR) mixing period and a <sup>13</sup>C 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 M<sub>0</sub>Aβ<sub>1-42</sub> 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.</p>},
  author       = {Donovan, Kevin J. and Silvers, Robert and Linse, Sara and Griffin, Robert G},
  issn         = {0002-7863},
  language     = {eng},
  month        = {05},
  number       = {19},
  pages        = {6518--6521},
  publisher    = {The American Chemical Society},
  series       = {Journal of the American Chemical Society},
  title        = {3D MAS NMR Experiment Utilizing Through-Space <sup>15</sup>N-<sup>15</sup>N Correlations},
  url          = {http://dx.doi.org/10.1021/jacs.7b01159},
  volume       = {139},
  year         = {2017},
}