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Pinning down the solid-state polymorphism of the ionic liquid [bmim][PF6]

Saouane, Sofiane
Norman, Sarah E.
Hardacre, Christopher
Fabbiani, Francesca P. A.
Journal: Chemical Science, 2012
4, 3: 1270 - 1280
DOI: https://doi.org/10.1039/c2sc21959j
Persistent URL: http://resolver.sub.uni-goettingen.de/purl?gldocs-11858/6983
Saouane, Sofiane; Norman, Sarah E.; Hardacre, Christopher; Fabbiani, Francesca P. A., 2012: Pinning down the solid-state polymorphism of the ionic liquid [bmim][PF6]. In: Chemical Science, Band 4, 3: 1270 - 1280, DOI: 10.1039/c2sc21959j.
 
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  • Abstract
The solid-state polymorphism of the ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate, [bmim][PF6], has been investigated via low-temperature and high-pressure crystallisation experiments. The samples have been characterised by single-crystal X-ray diffraction, optical microscopy and Raman spectroscopy. The solid-state phase behaviour of the compound is confirmed and clarified with respect to previous phase diagrams. The structures of the previously reported g-form, which essentially exhibits a G0T cation conformation, as well as those of the elusive b- and a-forms, are reported. Crystals of the bphase are twinned and the structure is heavily disordered; the cation conformation in this form is predominantly TT, though significant contributions from other less frequently encountered conformers are also observed at low temperature and high pressure. The cation conformation in the a-form is GT; the presence of the G0T conformer at 193 K in this phase can be eliminated on cooling to 100 K. Whilst X-ray structural data are overall in good agreement with previous interpretations based on Raman and NMR studies, they also reveal a more subtle interplay of intermolecular interactions, which give rise to a wider range of conformers than previously considered.
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