Magic-angle spinning (MAS) nuclear magnetic resonance (NMR) is establishing itself as a powerful method for the characterization of protein dynamics at the atomic scale. We discuss here how R(1?) MAS relaxation dispersion NMR can explore microsecond-to-millisecond motions. Progress in instrumentation, isotope labeling, and pulse sequence design has paved the way for quantitative analyses of even rare structural fluctuations. In addition to isotropic chemical-shift fluctuations exploited in...
[NMR paper] 1H-Detected Biomolecular NMR under Fast Magic-Angle Spinning
1H-Detected Biomolecular NMR under Fast Magic-Angle Spinning
Since the first pioneering studies on small deuterated peptides dating more than 20 years ago, ¹H detection has evolved into the most efficient approach for investigation of biomolecular structure, dynamics, and interactions by solid-state NMR. The development of faster and faster magic-angle spinning (MAS) rates (up to 150 kHz today) at ultrahigh magnetic fields has triggered a real revolution in the field. This new spinning regime reduces the ¹H-¹H dipolar couplings, so that a direct detection...
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05-11-2022 05:44 AM
[NMR paper] Protein structural dynamics by Magic-Angle Spinning NMR
Protein structural dynamics by Magic-Angle Spinning NMR
Magic-Angle Spinning (MAS) Nuclear Magnetic Resonance (NMR) is a fast-developing technique, capable of complementing solution NMR, X-ray crystallography, and electron microscopy for the biophysical characterization of microcrystalline, poorly crystalline or disordered protein samples, such as enzymes, biomolecular assemblies, membrane-embedded systems or fibrils. Beyond structures, MAS NMR is an ideal tool for the investigation of dynamics, since it is unique in its ability to distinguish static...
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04-30-2021 10:13 PM
[NMR paper] Strategies for 1H-detected dynamic nuclear polarisation magic-angle spinning NMR.
Strategies for 1H-detected dynamic nuclear polarisation magic-angle spinning NMR.
Related Articles Strategies for 1H-detected dynamic nuclear polarisation magic-angle spinning NMR.
Chemistry. 2020 Aug 22;:
Authors: Concistré M, Paul S, Carravetta M, Kuprov I, Williamson PTF
Abstract
Combining dynamic nuclear polarization with proton detection significantly enhances the sensitivity of magic-angle spinning NMR. Here we demonstrate the feasibility of proton- detected experiments with slow (10 kHz) magic angle spinning. The...
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08-23-2020 10:50 AM
[NMR paper] Is protein deuteration beneficial for proton detected solid-state NMR at and above 100*kHz magic-angle spinning?
Is protein deuteration beneficial for proton detected solid-state NMR at and above 100*kHz magic-angle spinning?
Related Articles Is protein deuteration beneficial for proton detected solid-state NMR at and above 100*kHz magic-angle spinning?
Solid State Nucl Magn Reson. 2017 Jul 25;:
Authors: Cala-De Paepe D, Stanek J, Jaudzems K, Tars K, Andreas LB, Pintacuda G
Abstract
(1)H-detection in solid-state NMR of proteins has been traditionally combined with deuteration for both resolution and sensitivity reasons, with the optimal...
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08-15-2017 05:43 PM
Is protein deuteration beneficial for proton detected solid-state NMR at and above 100*kHz magic-angle spinning?
Is protein deuteration beneficial for proton detected solid-state NMR at and above 100*kHz magic-angle spinning?
Publication date: Available online 25 July 2017
Source:Solid State Nuclear Magnetic Resonance</br>
Author(s): Diane Cala-De Paepe, Jan Stanek, Kristaps Jaudzems, Kaspars Tars, Loren B. Andreas, Guido Pintacuda</br>
1H-detection in solid-state NMR of proteins has been traditionally combined with deuteration for both resolution and sensitivity reasons, with the optimal level of proton dilution being dependent on MAS rate. Here we present...
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07-26-2017 10:20 AM
[NMR paper] Peptide and Protein Dynamics and Low-Temperature/DNP Magic Angle Spinning NMR.
Peptide and Protein Dynamics and Low-Temperature/DNP Magic Angle Spinning NMR.
Related Articles Peptide and Protein Dynamics and Low-Temperature/DNP Magic Angle Spinning NMR.
J Phys Chem B. 2017 Apr 24;:
Authors: Ni QZ, Markhasin E, Can TV, Corzilius B, Tan KO, Barnes AB, Daviso E, Su Y, Herzfeld J, Griffin RG
Abstract
In DNP MAS NMR experiments at ~80-110 K, the structurally important -13CH3 and -15NH3+ signals in MAS spectra of biological samples disappear due to the interference of the molecular motions with the 1H...
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04-25-2017 11:48 AM
[NMR paper] Cross-Correlated Relaxation of Dipolar Coupling and Chemical-Shift Anisotropy in Magic-Angle Spinning R1? NMR Measurements: Application to Protein Backbone Dynamics Measurements.
Cross-Correlated Relaxation of Dipolar Coupling and Chemical-Shift Anisotropy in Magic-Angle Spinning R1? NMR Measurements: Application to Protein Backbone Dynamics Measurements.
Cross-Correlated Relaxation of Dipolar Coupling and Chemical-Shift Anisotropy in Magic-Angle Spinning R1? NMR Measurements: Application to Protein Backbone Dynamics Measurements.
J Phys Chem B. 2016 Aug 8;
Authors: Kurauskas V, Weber E, Hessel A, Ayala I, Marion D, Schanda P
Abstract
Transverse relaxation rate measurements in MAS solid-state NMR...
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08-09-2016 02:42 PM
Sensitivity and resolution of proton detected spectra of a deuterated protein at 40 and 60Â*kHz magic-angle-spinning
Sensitivity and resolution of proton detected spectra of a deuterated protein at 40 and 60Â*kHz magic-angle-spinning
Abstract
The use of small rotors capable of very fast magic-angle spinning (MAS) in conjunction with proton dilution by perdeuteration and partial reprotonation at exchangeable sites has enabled the acquisition of resolved, proton detected, solid-state NMR spectra on samples of biological macromolecules. The ability to detect the high-gamma protons, instead of carbons or nitrogens, increases sensitivity. In order to achieve...