| Reference Type | Journal (article/letter/editorial) |
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| Title | Towards clathrates. 2. The frozen states of hydration of tert-butanol |
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| Journal | Zeitschrift für Kristallographie - Crystalline Materials |
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| Authors | Dobrzycki, Lukasz | Author |
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| Year | 2018 (January 26) | Volume | 233 |
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| Issue | 1 |
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| Publisher | Walter de Gruyter GmbH |
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| DOI | doi:10.1515/zkri-2017-2074Search in ResearchGate |
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| Generate Citation Formats |
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| Mindat Ref. ID | 118059 | Long-form Identifier | mindat:1:5:118059:0 |
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| GUID | 0 |
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| Full Reference | Dobrzycki, Lukasz (2018) Towards clathrates. 2. The frozen states of hydration of tert-butanol. Zeitschrift für Kristallographie - Crystalline Materials, 233 (1) 41-49 doi:10.1515/zkri-2017-2074 |
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| Plain Text | Dobrzycki, Lukasz (2018) Towards clathrates. 2. The frozen states of hydration of tert-butanol. Zeitschrift für Kristallographie - Crystalline Materials, 233 (1) 41-49 doi:10.1515/zkri-2017-2074 |
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| In | (2018, January) Zeitschrift für Kristallographie - Crystalline Materials Vol. 233 (1) Walter de Gruyter GmbH |
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| Abstract/Notes | AbstractA new crystal structure oftert-butanol and water crystallizing as the decahydrate is reported. The crystallization of the mixture in the desired molar ratio was performed in a capillary placed directly on a goniometer of a single crystal diffractometer at 200 K and ambient pressure using focused IR laser radiation. The crystals were grown while the melting zone formed by the IR laser was moved along the capillary. Usually the crystallization process should be long enough (hours) in order to obtain a good quality single crystal. However, in the case oftert-butanol decahydrate, such a long process led to separation of the ice and alcohol. Only fast crystallization taking tens of seconds allowed crystallization of the desired crystalline phase. In the decahydratetert-butanol molecules are located in channels formed by water molecules. Hydroxyl groups are anchored to the water framework via hydrogen bonds. All water molecules in the structure have hydrogen atoms disordered equally over two sites; the hydroxyl group is likewise disordered. This effect is observed at both, 200 K and 100 K. Raman spectra recorded for the crystalline phase suggest dynamic disorder at higher temperature, converting to static at lowerT. The decahydrate oftert-butanol, together with already known itsdi- andhepta-hydrates, display similar features to those observed for series oftert-butylamine hydrates. The latter structures behave as frozen steps of amine hydration observed as crystal structures leading, at maximum dilution, to hexagonal ice. Hydrates oftert-butanol nicely follow this tendency completing the relationship found for thetert-butylamine: water system. |
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