Novel anhydrous solid-state form of Azathioprine: The assessing of crystal structure by powder X-Ray diffraction, Infrared Absorption Spectroscopy and Raman scattering
| Autor: | Daniel Gherca, Lucian Buhalteanu, Adrian Barbatu, Mihaela Baibarac, Monica Daescu, Adelina Matea, Dumitru Samohvalov, Ovidiu Ilie Covaci, Corina Mihaela Manta |
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| Rok vydání: | 2019 |
| Předmět: |
010405 organic chemistry
Rietveld refinement Chemistry Organic Chemistry Crystal structure 010402 general chemistry 01 natural sciences 0104 chemical sciences Analytical Chemistry Inorganic Chemistry Transplantation Crystal Crystallography symbols.namesake Polymorphism (materials science) X-ray crystallography Anhydrous symbols Raman spectroscopy Spectroscopy |
| Zdroj: | Journal of Molecular Structure. 1178:702-710 |
| ISSN: | 0022-2860 |
| DOI: | 10.1016/j.molstruc.2018.10.065 |
| Popis: | Azathioprine (Imuran), one of the oldest immunosuppressants, having been used in transplantation since the early 1960`s, is known to have only two crystal forms: an anhydrous form and a dihydrate phase. We report the crystal structure of a new anhydrous solid-state form of Azathioprine, determined directly form powder X-Ray diffraction data, employing the direct-space genetic algorithm technique for structure solution, followed by Rietveld refinement. The new anhydrous polymorph is accessible only by a solid-state dehydration process of the readily obtained monohydrate form of Azathioprine, the form for which a crystal structure has not previously been reported. The IR and Raman spectra confirmed the results obtained from X-Ray diffraction indicating the presence of all functional groups involved in intermolecular hydrogen bonding which dictates different arrangement of molecules in the structural packing. |
| Databáze: | OpenAIRE |
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