Insights into the Crystallization and Structural Evolution of Glycine Dihydrate by In Situ Solid‐State NMR Spectroscopy. Issue 22 (8th May 2018)

• Record Type: Journal Article
• Authors: Cerreia Vioglio, Paolo; Mollica, Giulia; Juramy, Marie; Hughes, Colan E.; Williams, P. Andrew; Ziarelli, Fabio; Viel, Stéphane; Thureau, Pierre; Harris, Kenneth D. M.
• Is Part Of: Angewandte Chemie international edition. Volume 57:Issue 22(2018)
• Page Start: 6619
• Page End: 6623
• Publication Date: 2018-05-08
• Subjects: crystallization -- glycine -- polymorphism -- solid-state NMR spectroscopy -- structural transformation; Chemistry -- Periodicals; 540
• DOI: 10.1002/anie.201801114
• Languages: English
• ISSNs: 1433-7851

Abstract

Abstract: In situ solid‐state NMR spectroscopy is exploited to monitor the structural evolution of a glycine/water glass phase formed on flash cooling an aqueous solution of glycine, with a range of modern solid‐state NMR methods applied to elucidate structural properties of the solid phases present. The glycine/water glass is shown to crystallize into an intermediate phase, which then transforms to the β polymorph of glycine. Our in situ NMR results fully corroborate the identity of the intermediate crystalline phase as glycine dihydrate, which was first proposed only very recently. Abstract : Phase transitions : Following flash cooling of an aqueous solution of glycine, in situ solid‐state NMR spectroscopy is exploited to study the structural evolution from a glycine/water glass phase to crystalline glycine dihydrate and then to the β polymorph of anhydrous glycine. By using this strategy, the formation and structural properties of the crystalline dihydrate phase of glycine, which was first reported only very recently, are explored.