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Characterization of a polymorphic system exhibiting substantial variation of solubility in a fluorinated solvent

Cote, M., Hughes, C. E., Austin, T. K., Rogueda, P. G. A., Pan, Z. G., Harris, Kenneth David Maclean and Griffiths, Peter Charles 2008. Characterization of a polymorphic system exhibiting substantial variation of solubility in a fluorinated solvent. Journal of Physical Chemistry C 112 (37) , pp. 14570-14578. 10.1021/jp800848w

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Abstract

We report several aspects of the characterization of a material (triacetylated-β-cyclodextrin) that exists in two crystalline polymorphic forms (denoted I and II). A striking feature of this polymorphic system is that polymorph I (MPt 194 °C) and polymorph II (MPt 219 °C) exhibit remarkably different solubility in the fluorinated solvent 2H,3H-decafluoropentane, with the solubility higher by a factor of ca. eight for polymorph I at ambient temperature. Structural information established from powder X-ray diffraction and high-resolution solid-state 13C NMR spectroscopy for polymorphs I and II is reported, including crystal structure determination of polymorph II from the powder X-ray diffraction data. Differential scanning calorimetry and high-temperature powder X-ray diffraction demonstrate that the metastable polymorph I converts to the stable polymorph II over a range of elevated temperatures. The combined evidence of these and other techniques suggests that there is a monotropic relationship between polymorphs I and II.

Item Type: Article
Date Type: Publication
Status: Published
Schools: Advanced Research Computing @ Cardiff (ARCCA)
Chemistry
Subjects: Q Science > QD Chemistry
Publisher: ACS Publications
ISSN: 1932-7447
Last Modified: 04 Jun 2017 01:55
URI: http://orca.cf.ac.uk/id/eprint/5903

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