Dinu Iuga1
1University of Warwick, Coventry, United Kingdom
Synopsis
The UK High Field Solid State NMR National Research Facility
provides access to 20 T (850 MHz) and 23 T (1 GHz) spectrometers and probes
capable of spinning samples at the Magic Angle at very high spinning frequencies
(100 kHz). Under very fast MAS, the 1H spin echo life time becomes
considerably longer opening up the possibility to investigate 1H-1H
proximities or to detect other atoms in vicinity to 1H. Enhanced
sensitivity and enhanced resolution provided by the high magnetic fields allows
for structural insights not possible at lower magnetic fields, like
understanding cell wall architecture.
The UK High Field Solid State NMR National Research Facility
provides access to 20 T (850 MHz) and 23 T (1 GHz) spectrometers and probes
capable of spinning samples at the Magic Angle at very high spinning frequencies
(100 kHz). Under very fast MAS, the 1H spin echo life time becomes
considerably longer opening up the possibility to investigate 1H-1H
proximities or to detect other atoms in vicinity to 1H. For
biological solids, the Facility has E-free (low-electric field, loop-gap
loaded) coil MAS probes that allow efficient 1H decoupling with
minimal heating for the sample. The presentation showcases examples of enhanced
resolution and sensitivity enabled by the 1 GHz NMR spectrometer and provides a
basic description of some selected Solid-State NMR experiments performed at
very fast Magic Angle spinning: for example, how sensitivity is enhanced for
half-integer quadrupolar nuclei, and how 1H resolution is enhanced
using Lee-Goldburg homonuclear decoupling. Acknowledgements
The UK High-Field Solid-State NMR Facility used in this
research was funded by EPSRC and BBSRC (EP/T015063/1)References
Solid-State
NMR of a Protein in a Precipitated Complex with a Full-Length AntibodyJonathan
M. Lamley, Dinu Iuga, Carl Öster, Hans-Juergen Sass, Marco Rogowski, Andres
Oss, Jaan Past, Andres Reinhold, Stephan Grzesiek, Ago Samoson, and Józef R.
Lewandowski; J. Am. Chem. Soc., 136, (2014), 16800–16806
Ionothermal 17O Enrichment of Oxides using Microlitre Quantities of Labelled
WaterJohn M. Griffin, Lucy Clark, Valerie R. Seymour, David W. Aldous, Daniel
M. Dawson, Dinu Iuga, Russell E. Morris, and Sharon E. Ashbrook; Chemical
Science, 3 (7), 2293, (2012)
Pushing
the limits of sensitivity and resolution for natural abundance 43Ca NMR using ultra-high magnetic field (35.2 T) Christian
Bonhomme, Xiaoling Wang, Ivan Hung, Zhehong Gan, Christel Gervais, Capucine Sassoye,
Jessica Rimsza, Jincheng Du, Mark E. Smith,John V. Hanna, Stephanie Sarda,
Pierre Gras, Christele Combes and Danielle Laurencin; Chem. Commun.,2018, 54,
9591--9594
1H Line Width Dependence
on MAS Speed in Solid State NMR - Comparison of Experiment and Simulation; U.
Sternberg, R. Witter, I. Kuprov, J.M. Lamley, A. Oss, J.R. Lewandowski and A.
Samoson; J. Magn. Reson. 2018, 219, 32-39
An
even pattern of xylan substitution is critical for interaction with cellulose
in plant cell walls; Nicholas J. Grantham, Joel Wurman-Rodrich, Oliver M.
Terrett, Jan J. Lyczakowski, Katherine Stott, Dinu Iuga, Thomas J. Simmons,
Mylene Durand-Tardif, Steven. P. Brown, Ray Dupree, Marta Busse-Wicher, Paul
Dupree; Nature Plants, 3, (2017), 859–865