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Data for 35 Cl ‐ 1 H heteronuclear correlation MAS NMR experiments for probing pharmaceutical salts
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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 | ||||||||||||||||||||||||
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| Subjects: | Q Science > QD Chemistry | ||||||||||||||||||||||||
| Divisions: | Faculty of Science > Physics | ||||||||||||||||||||||||
| Library of Congress Subject Headings (LCSH): | Chlorides, Hydrochloric acid, Nuclear magnetic resonance spectroscopy, Nuclear magnetic resonance, Pharmaceutical chemistry, Crystallization | ||||||||||||||||||||||||
| Publisher: | Physics, University of Warwick | ||||||||||||||||||||||||
| Official Date: | 8 July 2021 | ||||||||||||||||||||||||
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| Status: | Not Peer Reviewed | ||||||||||||||||||||||||
| Publication Status: | Published | ||||||||||||||||||||||||
| Media of Output: | .txt .dat .cif .magres | ||||||||||||||||||||||||
| Access rights to Published version: | Open Access | ||||||||||||||||||||||||
| Copyright Holders: | University of Warwick | ||||||||||||||||||||||||
| Description: | Dataset of: 1. NMR calculations Detailed description is available in the attached Readme file |
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