Aliev, Abil E., Mann, Sam E., Iuga, Dinu, Hughes, Colan E. and Harris, Kenneth D. M. (2011) Natural-abundance solid-state 2H NMR spectroscopy at high magnetic field. The Journal of Physical Chemistry A, Vol.115 (No.22). 5568-5578 . doi:10.1021/jp202810k

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Abstract

High-resolution solid-state (2)H NMR spectroscopy provides a method for measuring (1)H NMR chemical shifts in solids and is advantageous over the direct measurement of high-resolution solid-state (1)H NMR spectra, as it requires only the application of routine magic angle sample spinning (MAS) and routine (1)H decoupling methods, in contrast to the requirement for complex pulse sequences for homonuclear (1)H decoupling and ultrafast MAS in the case of high-resolution solid-state (1)H NMR. However, a significant obstacle to the routine application of high-resolution solid-state (2)H NMR is the very low natural abundance of (2)H, with the consequent problem of inherently low sensitivity. Here, we explore the feasibility of measuring (2)H MAS NMR spectra of various solids with natural isotopic abundances at high magnetic field (850 MHz), focusing on samples of amino acids, peptides, collagen, and various organic solids. The results show that high-resolution solid-state (2)H NMR can be used successfully to measure isotropic (1)H chemical shifts in favorable cases, particularly for mobile functional groups, such as methyl and -N(+)H(3) groups, and in some cases phenyl groups. Furthermore, we demonstrate that routine (2)H MAS NMR measurements can be exploited for assessing the relative dynamics of different functional groups in a molecule and for assessing whole-molecule motions in the solid state. The magnitude and field-dependence of second-order shifts due to the (2)H quadrupole interaction are also investigated, on the basis of analysis of simulated and experimental (1)H and (2)H MAS NMR spectra of fully deuterated and selectively deuterated samples of the alpha polymorph of glycine at two different magnetic field strengths.

Item Type:	Journal Article
Subjects:	Q Science > QC Physics Q Science > QD Chemistry
Divisions:	Faculty of Science > Physics
Library of Congress Subject Headings (LCSH):	Nuclear magnetic resonance spectroscopy, Solid state chemistry, Magnetic fields
Journal or Publication Title:	The Journal of Physical Chemistry A
Publisher:	American Chemical Society
ISSN:	1089-5639
Official Date:	2011
Dates:	Date Event 2011 Published
Volume:	Vol.115
Number:	No.22
Page Range:	5568-5578
DOI:	10.1021/jp202810k
Status:	Peer Reviewed
Publication Status:	Published
Funder:	Engineering and Physical Sciences Research Council (EPSRC) , Biotechnology and Biological Sciences Research Council (BBSRC), University of Warwick , European Regional Development Fund (ERDF), Advantage West Midlands (AWM)

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