Iuga, Dinu, Corlett, Emily K. and Brown, Steven P. (2021) Data for 35 Cl ‐ 1 H heteronuclear correlation MAS NMR experiments for probing pharmaceutical salts. [Dataset]

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Abstract

Heteronuclear multiple-quantum coherence (HMQC) pulse sequences for establishing heteronuclear correlation in solid-state NMR between 35Cl and 1H atoms in chloride salts under fast (60 kHz) magic-angle spinning (MAS) and at high magnetic field (a 1H Larmor frequency of 850 MHz) are investigated. Specifically, recoupling of the 35Cl - 1H dipolar interaction using rotary resonance recoupling with phase inversion every rotor period or the symmetry based SR421 pulse sequence are compared. In our implementation of the PT (population-transfer)-D-HMQC experiment, the satellite transitions of the 35Cl nuclei are saturated with an off-resonance WURST sweep, at a low nutation frequency, over the second spinning sideband, whereby the WURST pulse must be of the same duration as the recoupling time. Numerical simulations of the 35Cl - 1H MAS D-HMQC experiment performed separately for each crystallite orientation in a powder provide insight into the orientation dependence of changes in the second-order quadrupolar broadened 35Cl MAS NMR lineshape under the application of dipolar recoupling. Two-dimensional 35Cl - 1H PT-D-HMQC MAS NMR spectra are presented for the amino acids glycine·HCl and L-tyrosine·HCl and the pharmaceuticals cimetidine·HCl, amitriptyline·HCl and lidocaine·HCl·H2O. Experimentally observed 35Cl lineshapes are compared with those simulated for 35Cl chemical shift and quadrupolar parameters as calculated using the gauge-including projector-augmented wave (GIPAW) method: the calculated quadrupolar product (PQ) values exceed those measured experimentally by a factor of between 1.3 and 1.9.

Item Type:	Dataset
Subjects:	Q Science > QD Chemistry
Divisions:	Faculty of Science, Engineering and Medicine > Science > Physics
Library of Congress Subject Headings (LCSH):	Chlorides, Hydrochloric acid, Nuclear magnetic resonance spectroscopy, Nuclear magnetic resonance, Pharmaceutical chemistry, Crystallization
Publisher:	University of Warwick, Department of Physics
Official Date:	8 July 2021
Dates:	Date Event 8 July 2021 Published 8 July 2021 Created
Status:	Not Peer Reviewed
Publication Status:	Published
Media of Output (format):	.txt .dat .cif .magres
Access rights to Published version:	Open Access (Creative Commons)
Copyright Holders:	University of Warwick
Description:	Dataset of: 1. NMR calculations 2. Raw files from NMR experiments 3. Simpson simulation files Detailed description is available in the attached Readme file
Date of first compliant deposit:	8 July 2021
Date of first compliant Open Access:	8 July 2021
RIOXX Funder/Project Grant:	Project/Grant ID RIOXX Funder Name Funder ID EP/T015063/1 [EPSRC] Engineering and Physical Sciences Research Council http://dx.doi.org/10.13039/501100000266 PR140003 [BBSRC] Biotechnology and Biological Sciences Research Council http://dx.doi.org/10.13039/501100000268 EP/L015307/1 [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 Advantage West Midlands http://dx.doi.org/10.13039/100014381 UNSPECIFIED Science City Research Alliance UNSPECIFIED UNSPECIFIED [ERDF] European Regional Development Fund http://dx.doi.org/10.13039/501100008530
Related URLs:	Other Related item in WRAP
Contributors:	Contribution Name Contributor ID Depositor Iuga, Dinu 29875

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