Handling the influence of chemical shift in amplitude-modulated heteronuclear dipolar recoupling solid-state NMR

2016 ◽  
Vol 145 (9) ◽  
pp. 094202 ◽  
Author(s):  
Kristoffer Basse ◽  
Ravi Shankar ◽  
Morten Bjerring ◽  
Thomas Vosegaard ◽  
Niels Chr. Nielsen ◽  
...  
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Dipolar Recoupling

scholarly journals A general theoretical description of the influence of isotropic chemical shift in dipolar recoupling experiments for solid-state NMR

2017 ◽  
Vol 146 (13) ◽  
pp. 134105 ◽  
Author(s):  
Ravi Shankar ◽  
Matthias Ernst ◽  
P. K. Madhu ◽  
Thomas Vosegaard ◽  
Niels Chr. Nielsen ◽  
...  
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Theoretical Description ◽  
Isotropic Chemical Shift ◽  
Dipolar Recoupling

Low-power homonuclear dipolar recoupling in solid-state NMR developed using optimal control theory

2005 ◽  
Vol 414 (1-3) ◽  
pp. 204-209 ◽  
Author(s):  
Cindie Kehlet ◽  
Thomas Vosegaard ◽  
Navin Khaneja ◽  
Steffen J. Glaser ◽  
Niels Chr. Nielsen
Keyword(s):  
Optimal Control ◽  
Solid State ◽  
Control Theory ◽  
Low Power ◽  
Optimal Control Theory ◽  
Solid State Nmr ◽  
Dipolar Recoupling

scholarly journals Temperature-Dependent Solid-State NMR Proton Chemical-Shift Values and Hydrogen Bonding

2021 ◽  
Author(s):  
Alexander A. Malär ◽  
Laura A. Völker ◽  
Riccardo Cadalbert ◽  
Lauriane Lecoq ◽  
Matthias Ernst ◽  
...  
Keyword(s):  
Magnetic Field ◽  
Hydrogen Bonding ◽  
Solid State ◽  
Chemical Shift ◽  
Hydrogen Bonds ◽  
Solid State Nmr ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Proton Chemical Shift ◽  
Temperature Dependent

Temperature-dependent NMR experiments are often complicated by rather long magnetic-field equilibration times, for example occurring upon a change of sample temperature. We demonstrate that the fast temporal stabilization of the magnetic field can be achieved by actively stabilizing the temperature which allows to quantify the weak temperature dependence of the proton chemical shift which can be diagnostic for the presence of hydrogen bonds. Hydrogen bonding plays a central role in molecular recognition events from both fields, chemistry and biology. Their direct detection by standard structure determination techniques, such as X-ray crystallography or cryo-electron microscopy, remains challenging due to the difficulties of approaching the required resolution, on the order of 1 Å. We herein explore a spectroscopic approach using solid-state NMR to identify protons engaged in hydrogen bonds and explore the measurement of proton chemical-shift temperature coefficients. Using the examples of a phosphorylated amino acid and the protein ubiquitin, we show that fast Magic-Angle Spinning (MAS) experiments at 100 kHz yield sufficient resolution in proton-detected spectra to quantify the rather small chemical-shift changes upon temperature variations.<br>

Symmetry-based dipolar recoupling by optimal control: Band-selective experiments for assignment of solid-state NMR spectra of proteins

2009 ◽  
Vol 131 (2) ◽  
pp. 025101 ◽  
Author(s):  
Anders Bodholt Nielsen ◽  
Morten Bjerring ◽  
Jakob Toudahl Nielsen ◽  
Niels Chr. Nielsen
Keyword(s):  
Optimal Control ◽  
Solid State ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
Dipolar Recoupling

Probing solid iminobis(diorganophosphine chalcogenide) systems with multinuclear magnetic resonance

2009 ◽  
Vol 87 (1) ◽  
pp. 348-360 ◽  
Author(s):  
Bryan A Demko ◽  
Roderick E Wasylishen
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Magnetic Shielding ◽  
Chemical Shift Tensors ◽  
X Ray ◽  
X Ray Crystallography ◽  
Shielding Tensor ◽  
Nuclear Magnetic Shielding Tensors ◽  
Nuclear Magnetic

A 31P and 77Se solid-state NMR investigation of the iminobis(diorganophosphine chalcogenide) HN(R2PE)2 (R = Ph,iPr; E = O, S, Se) systems is presented. The NMR results are discussed in terms of the known HN(R2PE)2 structures available from X-ray crystallography. The phosphorus chemical shift tensors are found to be sensitive to the nature of the alkyl and chalcogen substituents. The nature of the R group also influences the selenium chemical shift tensors of HN(R2PSe)2 (R = Ph, iPr), which are shown to be sensitive to hydrogen bonding in the dimer structure of HN(Ph2PSe)2 and to the presence of disorder in the case of HN(iPr2PSe)2. Scalar relativistic ZORA DFT nuclear magnetic shielding tensor calculations were performed yielding the orientations of the corresponding chemical shift tensors. A theoretical investigation into the effect of the E-P···P-E “torsion” angle on the phosphorus and selenium chemical shift tensors of a truncated HN(Me2PSe)2 system indicates that the electronic effect of the alkyl group on the respective nuclear magnetic shielding tensors are more important than the steric effect of the E-P···P-E torsion angle.Key words: iminobis(diorganophosphine chalcogenide), solid-state NMR, 31P NMR, 77Se NMR, ZORA DFT.

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