We report linewidth and proton T1, T1Ï? and T2â?² relaxation data of the model protein ubiquitin acquired at MAS frequencies up to 126Â*kHz. We find a predominantly linear improvement in linewidths and coherence decay times of protons with increasing spinning frequency in the range from 93 to 126Â*kHz. We further attempt to gain insight into the different contributions to the linewidth at fast MAS using site-specific analysis of proton relaxation parameters and present bulk relaxation times as a function of the MAS frequency. For microcrystalline fully-protonated ubiquitin, inhomogeneous contributions are only a minor part of the proton linewidth, and at 126Â*kHz MAS coherent effects are still dominating. We furthermore present site-specific proton relaxation rate constants during a spinlock at 126Â*kHz MAS, as well as MAS-dependent bulk T1Ï? (1HN).
[NMR paper] Expanding the horizons for structural analysis of fully protonated protein assemblies by NMR spectroscopy at MAS frequencies above 100*kHz.
Expanding the horizons for structural analysis of fully protonated protein assemblies by NMR spectroscopy at MAS frequencies above 100*kHz.
Related Articles Expanding the horizons for structural analysis of fully protonated protein assemblies by NMR spectroscopy at MAS frequencies above 100*kHz.
Solid State Nucl Magn Reson. 2017 Jul 03;:
Authors: Struppe J, Quinn CM, Lu M, Wang M, Hou G, Lu X, Kraus J, Andreas LB, Stanek J, Lalli D, Lesage A, Pintacuda G, Maas W, Gronenborn AM, Polenova T
Abstract
The recent breakthroughs in NMR...
nmrlearner
Journal club
0
07-24-2017 10:10 AM
Expanding the horizons for structural analysis of fully protonated protein assemblies by NMR spectroscopy at MAS frequencies above 100*kHz
Expanding the horizons for structural analysis of fully protonated protein assemblies by NMR spectroscopy at MAS frequencies above 100*kHz
Publication date: Available online 3 July 2017
Source:Solid State Nuclear Magnetic Resonance</br>
Author(s): Jochem Struppe, Caitlin M. Quinn, Manman Lu, Mingzhang Wang, Guangjin Hou, Xingyu Lu, Jodi Kraus, Loren B. Andreas, Jan Stanek, Daniela Lalli, Anne Lesage, Guido Pintacuda, Werner Maas, Angela M. Gronenborn, Tatyana Polenova</br>
The recent breakthroughs in NMR probe technologies resulted in...
nmrlearner
Journal club
0
07-04-2017 04:57 AM
Structural biology Faster spinning for better structure resolution - Nature.com
<img alt="" height="1" width="1">
Structural biology Faster spinning for better structure resolution
Nature.com
Magic angle spinning (MAS) solid-state nuclear magnetic resonance (ssNMR) spectroscopy is a useful technique for structure determination, especially of membrane proteins. This method typically requires that protons in proteins be largely replaced with ...
Structural biology Faster spinning for better structure resolution - Nature.com
More...
nmrlearner
Online News
0
09-29-2016 07:20 PM
[NMR paper] Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies.
Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies.
Related Articles Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies.
J Magn Reson. 2015 Nov 9;261:149-156
Authors: Mote KR, Madhu PK
Abstract
(1)H-detection offers a substitute to the sensitivity-starved experiments often used to characterize biomolecular samples using magic-angle spinning solid-state NMR spectroscopy...
nmrlearner
Journal club
0
11-19-2015 05:22 PM
Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies
Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies
Publication date: Available online 9 November 2015
Source:Journal of Magnetic Resonance</br>
Author(s): Kaustubh R. Mote, Perunthiruthy K. Madhu</br>
1 H-detection offers a substitute to the sensitivity-starved experiments often used to characterize biomolecular samples using magic-angle spinning solid-state NMR spectroscopy (MAS-ssNMR). To mitigate the effects of the strong 1 H- 1 H dipolar coupled network that...
nmrlearner
Journal club
0
11-10-2015 09:10 AM
Protein resonance assignment at MAS frequencies approaching 100Â*kHz: a quantitative comparison of J-coupling and dipolar-coupling-based transfer methods
Protein resonance assignment at MAS frequencies approaching 100Â*kHz: a quantitative comparison of J-coupling and dipolar-coupling-based transfer methods
Abstract
We discuss the optimum experimental conditions to obtain assignment spectra for solid proteins at magic-angle spinning (MAS) frequencies around 100Â*kHz. We present a systematic examination of the MAS dependence of the amide proton T 2â?² times and a site-specific comparison of T 2â?² at 93Â*kHz versus 60Â*kHz MAS frequency. A...
nmrlearner
Journal club
0
08-13-2015 02:00 PM
[NMR paper] Spinning proteins, the faster, the better?
Spinning proteins, the faster, the better?
Publication date: April 2015
Source:Journal of Magnetic Resonance, Volume 253</br>
Author(s): Anja Böckmann , Matthias Ernst , Beat H. Meier</br>
Magic-angle spinning (MAS) is a technique that is a prerequisite for high-resolution solid-state NMR spectroscopy of proteins and other biomolecules. Recently, the 100kHz limit for the rotation frequency has been broken, arguably making MAS rotors the man-made objects with the highest rotation frequency. This development is expected to have a significant impact on biomolecular...
nmrlearner
Journal club
0
03-22-2015 06:36 PM
Sensitive 13Câ??13C correlation spectra of amyloid fibrils at very high spinning frequencies and magnetic fields
Sensitive 13Câ??13C correlation spectra of amyloid fibrils at very high spinning frequencies and magnetic fields
Abstract Sensitive 2D solid-state 13Câ??13C correlation spectra of amyloid β fibrils have been recorded at very fast spinning frequencies and very high magnetic fields. It is demonstrated that PARIS-xy recoupling using moderate rf amplitudes can provide structural information by promoting efficient magnetization transfer even under such challenging experimental conditions. Furthermore, it has been shown both experimentally and by numerical simulations that the method is not...