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):  
Hydrogen Bonding ◽  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Proton Chemical Shift ◽  
Temperature Dependent

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>

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>

scholarly journals 17O NMR spectroscopy as a tool to study hydrogen bonding of cholesterol in lipid bilayers

2020 ◽  
Vol 56 (92) ◽  
pp. 14499-14502
Author(s):  
Lucy J. Rowlands ◽  
Adam Marks ◽  
John M. Sanderson ◽  
Robert V. Law
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Chemical Shift ◽  
Lipid Bilayers ◽  
Solid State Nmr ◽  
17O Nmr ◽  
17O Nmr Spectroscopy

Solid state NMR of 17O enriched cholesterol in bilayers reveals the chemical shift depends on extent of hydrogen bonding.

Carbon−Proton Chemical Shift Correlation in Solid-State NMR by Through-Bond Multiple-Quantum Spectroscopy

1998 ◽  
Vol 120 (50) ◽  
pp. 13194-13201 ◽  
Author(s):  
Anne Lesage ◽  
Dimitris Sakellariou ◽  
Stefan Steuernagel ◽  
Lyndon Emsley
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Multiple Quantum ◽  
Proton Chemical Shift ◽  
Chemical Shift Correlation

Hydrogen bonding and chemical shift assignments in carbazole functionalized isocyanides from solid-state NMR and first-principles calculations

2011 ◽  
Vol 13 (28) ◽  
pp. 13082 ◽  
Author(s):  
Chandrakala M. Gowda ◽  
Filipe Vasconcelos ◽  
Erik Schwartz ◽  
Ernst R. H. van Eck ◽  
Martijn Marsman ◽  
...  
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Chemical Shift ◽  
First Principles ◽  
Solid State Nmr ◽  
Chemical Shift Assignments ◽  
First Principles Calculations
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