Experimental 13C and 1H Solid-State NMR Response in Weakly Tetrel-Bonded Methyl Groups

2021 ◽  
Vol 125 (3) ◽  
pp. 2111-2123
Author(s):  
Scott A. Southern ◽  
Michael S. West ◽  
Maressa J. Z. Bradshaw ◽  
David L. Bryce
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Methyl Groups

Investigation of Methyl Reorientations in 1,4-Dimethoxy- 2,6-dimethylbenzene by NMR and Inelastic Neutron Scattering

1979 ◽  
Vol 34 (5) ◽  
pp. 631-645 ◽  
Author(s):  
R. A. Wind ◽  
W. M. M. J. Bovée ◽  
J. C. F. Kupers ◽  
J. Smidt ◽  
Chr. Steenbergen
Keyword(s):  
Solid State ◽  
Neutron Scattering ◽  
Liquid State ◽  
Solid State Nmr ◽  
Inelastic Neutron Scattering ◽  
Nmr Relaxation ◽  
Inelastic Neutron ◽  
Methyl Groups ◽  
Methyl Group ◽  
Nmr Study

Abstract In this paper a solid state NMR relaxation study and inelastic neutron scattering (INS) experiments (the latter in the solid and liquid phase) are reported for a molecule containing methyl groups in different surroundings, namely 1,4-dimethoxy-2,6-dimethylbenzene. The results are compared with each other and with those of a liquid state NMR study reported earlier. It is found that in this way both the shapes and magnitudes of the various hindering potentials can be determined. The result is that the methyl groups 1, 2 and 4 possess a threefold cosine-shaped potential with heights given by 7.7, 9.0 and 15.0 kJ/mol according to the solid state NMR measurements (from the INS study the values 7.5, 7.5 and 16.0 kJ/mol were obtained). For methyl group 6 a mixture of a three-and six-fold symmetry had to be taken into account in order to explain the experiments. Except for methyl group 4 the liquid state NMR results deviate from those obtained with the other two techniques. A possible cause for this discrepancy is discussed. For the molecular structure it is concluded that the reorientations of the methyl groups 1 and 2 are influenced by mutual hindering and that the angle between the plane through the C4-O-C bond and the aromatic plane is small, whereas for the C1-O-C bond this angle is estimated to be about 70°.

scholarly journals Accessing Methyl Groups in Proteins via 1H-detected MAS Solid-state NMR Spectroscopy Employing Random Protonation

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Sam Asami ◽  
Bernd Reif
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Cost Effective ◽  
Order Parameters ◽  
Side Chain ◽  
Methyl Groups ◽  
Glucose Carbon ◽  
Distance Restraints ◽  
Asymmetry Parameters ◽  
Labelling Scheme

Abstract We recently introduced RAP (reduced adjoining protonation) labelling as an easy to implement and cost-effective strategy to yield selectively methyl protonated protein samples. We show here that even though the amount of H2O employed in the bacterial growth medium is rather low, the intensities obtained in MAS solid-state NMR 1H,13C correlation spectra are comparable to spectra obtained for samples in which α-ketoisovalerate was employed as precursor. In addition to correlations for Leu and Val residues, RAP labelled samples yield also resonances for all methyl containing side chains. The labelling scheme has been employed to quantify order parameters, together with the respective asymmetry parameters. We obtain a very good correlation between the order parameters measured using a GlcRAP (glucose carbon source) and a α-ketoisovalerate labelled sample. The labelling scheme holds the potential to be very useful for the collection of long-range distance restraints among side chain atoms. Experiments are demonstrated using RAP and α-ketoisovalerate labelled samples of the α-spectrin SH3 domain, and are applied to fibrils formed from the Alzheimer’s disease Aβ1-40 peptide.

scholarly journals Dynamics of Methyl Groups in Membrane Proteins Studied by Deterium Solid State NMR Relaxation

2016 ◽  
Vol 110 (3) ◽  
pp. 73a
Author(s):  
Xiaolin Xu ◽  
Andrey V. Struts ◽  
Aswini Kumar Giri ◽  
Trivikram R. Molugu ◽  
Charitha Guruge ◽  
...  
Keyword(s):  
Solid State ◽  
Membrane Proteins ◽  
Solid State Nmr ◽  
Nmr Relaxation ◽  
Methyl Groups

scholarly journals Specific 13C labeling of leucine, valine and isoleucine methyl groups for unambiguous detection of long-range restraints in protein solid-state NMR studies

2015 ◽  
Vol 252 ◽  
pp. 10-19 ◽  
Author(s):  
Hannes Klaus Fasshuber ◽  
Jean-Philippe Demers ◽  
Veniamin Chevelkov ◽  
Karin Giller ◽  
Stefan Becker ◽  
...  
Keyword(s):  
Solid State ◽  
Long Range ◽  
Solid State Nmr ◽  
Methyl Groups ◽  
Nmr Studies ◽  
13C Labeling ◽  
Unambiguous Detection
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