Measurement of 14N quadrupole couplings in biomolecular solids using indirect-detection 14N solid-state NMR with DNP

Chemical Communications : Chem Comm
James A JarvisPhilip T F Williamson

Abstract

The quadrupolar interaction experienced by the spin-1 14N nucleus is known to be extremely sensitive to local structure and dynamics. Furthermore, the 14N isotope is 99.6% naturally abundant, making it an attractive target for characterisation of nitrogen-rich biological molecules by solid-state NMR. In this study, dynamic nuclear polarization (DNP) is used in conjunction with indirect 14N detected solid-state NMR experiments to simultaneously characterise the quadrupolar interaction at multiple 14N sites in the backbone of the microcrystalline protein, GB3. Considerable variation in the quadrupolar interaction (>700 kHz) is observed throughout the protein backbone. The distribution in quadrupolar interactions observed reports on the variation in local backbone conformation and subtle differences in hydrogen-bonding; demonstrating a new route to the structural and dynamic analysis of biomolecules.

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Citations

Feb 28, 2019·Physical Chemistry Chemical Physics : PCCP·James A JarvisPhilip T F Williamson
Mar 20, 2020·Chemphyschem : a European Journal of Chemical Physics and Physical Chemistry·Diego CarnevaleGeoffrey Bodenhausen
Aug 23, 2020·Chemistry : a European Journal·Maria ConcistréPhilip T F Williamson
Jan 23, 2019·Solid State Nuclear Magnetic Resonance·Frédéric A PerrasMarek Pruski

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Methods Mentioned

BETA
NMR
ssNMR
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