Crystallization, spectral, crystallographical, and thermoanalytical studies of succinobucol polymorphism |
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Authors: | Jur?ek Ond?ej Lahtinen Manu Wimmer Zdeněk Dra?ar Pavel Kolehmainen Erkki |
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Institution: | 1. Department of Chemistry, University of Jyväskylä, 40014 Jyväskylä, Finland;2. Institute of Chemical Technology, 16628 Prague 6, Czech Republic;3. Isotope Laboratory, Institute of Experimental Botany, Academy of Sciences of the Czech Republic, 14220 Prague 4, Czech Republic |
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Abstract: | Four different polymorphs, A, C, D, and E, of succinobucol were isolated and characterized by means of solid-state nuclear magnetic resonance spectroscopy, single crystal and powder X-ray diffraction, differential scanning calorimetry, thermogravimetry, and attenuated total reflection-infrared spectroscopy. From a number of experiments, the same polymorphs (C, D, and E) and an equilibrium phase mixture B consisting of polymorphs C and D were repeatedly gained using different solvents or their mixtures. Although polymorph A was obtained directly from recrystallization only on few occasions, polymorphs C, D, and E proved to be metastable kinetic polymorphs, which slowly transform to a thermodynamically more stable form A during long-term storage. The single-crystal structures of polymorph C and D were determined by X-ray single-crystal diffraction. |
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