Reddy, G. N. Manjunatha , Malon, Michal, Marsh, Andrew, Nishiyama, Yusuke and Brown, Steven P. (2016) Date for A fast magic-angle spinning three-dimensional NMR experiment for simultaneously probing H-H and N-H proximities in solids. [Dataset]

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Abstract

A fast magic-angle spinning (MAS) solid-state NMR experiment is presented that combines 1H Double-Quantum (DQ) and 14N-1H HMQC (Heteronuclear Multiple-Quantum Coherence) pulse-sequence elements, so as to simultaneously probe H-H and N-H proximities in molecular solids. The proposed experiment can be employed in both two-dimensional (2D) and three-dimensional (3D) versions: firstly, a 2D 14N HMQC-filtered 1H-DQ experiment provides specific DQ-SQ correlation peaks for proton pairs that are in close proximities to the nitrogen sites, thereby achieving spectral filtration. Secondly, a proton-detected three-dimensional (3D) 1H(DQ)-14N(SQ)-1H(SQ) experiment correlates 1H(SQ)-1H(DQ) chemical shifts with 14N shifts such that longer range N…H-H correlations are observed between protons and nitrogen atoms with internuclear NH distances exceeding 3 Å. Both 2D and 3D versions of the proposed experiment are demonstrated for an amino acid hydrochloride salt, L-histidine.HCl.H2O, and a DNA nucleoside, guanosine.2H2O. In the latter case, the achieved spectral filtration ensures that DQ cross peaks are only observed for guanine NH and CH8 1H resonances and not ribose and water 1H resonances, thus providing insight into the changes in the solid-state structure of this hydrate that occur over time – significant changes are observed in the NH and NH2 1H chemical shifts as compared to the freshly recrystallized sample previously studied by Reddy et al, Cryst. Growth Des. 15, 5945, 2015.

Item Type:	Dataset
Subjects:	Q Science > QD Chemistry
Divisions:	Faculty of Science, Engineering and Medicine > Science > Chemistry Faculty of Science, Engineering and Medicine > Science > Physics
Type of Data:	JEOL NMR data
Library of Congress Subject Headings (LCSH):	Nuclear magnetic resonance spectroscopy, Self-assembly (Chemistry)
Publisher:	University of Warwick, Department of Physics
Official Date:	31 October 2016
Dates:	Date Event 31 October 2016 Completion
Collection date:	Date from Date to 29 July 2014 21 July 2016
Status:	Not Peer Reviewed
Publication Status:	Published
Media of Output (format):	.jdf .pdf .excel
Access rights to Published version:	Open Access (Creative Commons)
Description:	L-Histidine.HCl Figure 2 1D Single pulse NMR data (recorded on 05/10/2015) 2D 1H DQ-SQ Correlation NMR data (recorded on 05/10/2015) 2D 1H(DQ)- 14N(SQ)-1H(SQ) Correlation NMR data (recorded on 05/10/2015) Figure 3 2D 1H(DQ)- 14N(SQ) HMQC Correlation NMR data (recorded on 07/10/2015) 3D 1H(DQ)- 14N(SQ)-1H(SQ) Correlation NMR data (recorded on 13/10/2015) Figure S3 DFT refined crystallography information file (cif) (performed on 02/10/2015) NMR shielding calculations in .Magres format (performed on 02/10/2015) Experimental powder X-ray diffraction data (recorded on 01/01/2016) Guanosine.2H2O Figure 5 TGA-DSC data in .xls format (recorded on 29/07/2014 and 09/02/2016) Figure 6 1D Single pulse NMR data (recorded on 05/10/2015) 2D 1H DQ-SQ Correlation NMR data (recorded on 05/10/2015) 2D 1H(DQ)- 14N(SQ)-1H(SQ) Correlation NMR data (recorded on 05/10/2015) Figure 7 2D 1H(DQ)- 14N(SQ) HMQC Correlation NMR data (recorded on 05/10/2015) 3D 1H(DQ)- 14N(SQ)-1H(SQ) Correlation NMR data (recorded on 05/10/2015) Figure S4 1D 13C CPMAS NMR data (recorded on 13/02/2015, 16/04/2015 and 06/04/2016) Experimental powder X-ray diffraction data (recorded on 22/07/2016)
Date of first compliant deposit:	2 November 2016
Date of first compliant Open Access:	2 November 2016
RIOXX Funder/Project Grant:	Project/Grant ID RIOXX Funder Name Funder ID EP/K003674/1 [EPSRC] Engineering and Physical Sciences Research Council http://dx.doi.org/10.13039/501100000266 UNSPECIFIED University of Warwick http://dx.doi.org/10.13039/501100000741 UNSPECIFIED European Regional Development Fund http://dx.doi.org/10.13039/501100008530 UNSPECIFIED Birmingham Science City UNSPECIFIED UNSPECIFIED Advantage West Midlands (AWM) UNSPECIFIED
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