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A combined NMR crystallographic and PXRD investigation of the structure-directing role of water molecules in orotic acid and its lithium and magnesium salts

Content Provider	Royal Society of Chemistry (RSC)
Author	Pöppler, Ann-Christin Walker, David Brown, Steven P.
Copyright Year	2017
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 X-ray 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.
Starting Page	224
Ending Page	236
Page Count	13
File Format	HTM / HTML PDF
ISSN	14668033
Volume Number	19
Issue Number	2
Journal	CrystEngComm
DOI	10.1039/c6ce02101h
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Subscribed
Subject Keyword	Lithium orotate Acid Hydrate Magic angle spinning Thermogravimetric analysis Solid-state nuclear magnetic resonance Magnesium orotate Lithium Nuclear magnetic resonance spectroscopy Dehydration TGA X-ray crystallography Magnesium
Content Type	Text
Resource Type	Article
Subject	Chemistry Condensed Matter Physics Materials Science

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