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Data for A combined NMR crystallographic and PXRD investigation of the structure-directing role of water molecules in orotic acid and its lithium and magnesium salts
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Poeppler, Ann-Christin, Walker, David and Brown, Steven P. (2016) Data for A combined NMR crystallographic and PXRD investigation of the structure-directing role of water molecules in orotic acid and its lithium and magnesium salts. [Dataset]
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Official URL: http://wrap.warwick.ac.uk/83544
Abstract
Despite the abundance of hydrates, their multifaceted nature and hydration/dehydration behaviour is still not fully understood. For the example of orotic acid monohydrate and its lithium and magnesium hydrate salts, we show how NMR crystallography, namely a combination of solid-state NMR with a focus here on 1H Magic Angle Spinning (MAS) NMR experiments and first-principles DFT GIPAW (gauge-including projector augmented wave) calculations, can play a valuable role in the characterization of hydrate systems. Starting from lithium orotate monohydrate, a rigid system with a limited number of tightly bound water molecules, the general feasibility of this approach was demonstrated. Moving onto more complex hydrate structures, mobility in the orotic acid monohydrate was observed, while for the most complex hydrate, magnesium orotate octahydrate, a loss of associated water molecules was observed after an overnight MAS NMR experiment. A combined study by experimental MAS NMR, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA) revealed changes after vacuum drying as well as after storage of a vacuum dried sample under ambient conditions. Specifically, TGA showed the vacuum dried sample to correspond to a dihydrate, for which no structure has yet been determined by single-crystal diffraction. An NMR crystallography analysis showed that a combination of putative symmetric and asymmetric dihydrate structures explains the observed changes in the experimental MAS NMR spectra.
Item Type: | Dataset | |||||||||||||||||||||||||||
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Subjects: | Q Science > QD Chemistry Q Science > QP Physiology |
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | |||||||||||||||||||||||||||
Type of Data: | NMR data | |||||||||||||||||||||||||||
Library of Congress Subject Headings (LCSH): | Orotic acid, Magnesium salts, Lithium compounds | |||||||||||||||||||||||||||
Journal or Publication Title: | CrystEngComm | |||||||||||||||||||||||||||
Publisher: | University of Warwick, Department of Physics | |||||||||||||||||||||||||||
ISSN: | 1466-8033 | |||||||||||||||||||||||||||
Official Date: | 2 November 2016 | |||||||||||||||||||||||||||
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DOI: | 10.1039/C6CE02101H | |||||||||||||||||||||||||||
Status: | Not Peer Reviewed | |||||||||||||||||||||||||||
Publication Status: | Published | |||||||||||||||||||||||||||
Media of Output (format): | .asc .cif .magres .par .txt .xy | |||||||||||||||||||||||||||
Access rights to Published version: | Open Access (Creative Commons) | |||||||||||||||||||||||||||
Description: | 1.Magres-files for the different calculation including initial CIF files as well as those obtained directly after geometry optimization, single molecule calculations and the files for the symmetric and asymmetric magnesium orotate dehydrate. All calculations were run and analyzed by Ann-Christin Pöppler. a)Orotic Acid Monohydrate (1): The following data was used in Figures 4 and 6. 2.TGA: raw files (.txt) with both values of the mass [mg] and the heatflow [mW] at certain times/temperatures. The first two datasets are shown in the ESI, while the two magnesium orotate datasets were used in Figure 8. The TGA measurements were carried out by Ann-Christin Pöppler with the help of David Hammond. 3.PXRD experiments: raw files as recorded under a) ambient condition or b) vacuum. All experiments were recorded by Ann-Christin Pöppler and David Walker. a)Ambient condition: The first two datasets are shown in the ESI; the two mg_orotate datasets are shown in the ESI as well as Figure 9. All diffraction experiments were recorded on 14.04.2015. 4.NMR experiments: raw files as recorded for the three compounds by Ann-Christin Pöppler a)Orotic Acid Monohydrate |
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Date of first compliant deposit: | 4 November 2016 | |||||||||||||||||||||||||||
Date of first compliant Open Access: | 11 November 2016 | |||||||||||||||||||||||||||
RIOXX Funder/Project Grant: |
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