Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinement
Water is an essential chemical compound for living organisms, and twenty of its different crystal solid forms (ices) are known. Still, there are many fundamental problems with these structures such as establishing the correct positions and thermal motions of hydrogen atoms. The list of ice structure...
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International Union of Crystallography
2022-09-01
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| Online Access: | http://scripts.iucr.org/cgi-bin/paper?S2052252522006662 |
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| author | Michal L. Chodkiewicz Roman Gajda Barbara Lavina Sergey Tkachev Vitali B. Prakapenka Przemyslaw Dera Krzysztof Wozniak |
| author_facet | Michal L. Chodkiewicz Roman Gajda Barbara Lavina Sergey Tkachev Vitali B. Prakapenka Przemyslaw Dera Krzysztof Wozniak |
| author_sort | Michal L. Chodkiewicz |
| collection | DOAJ |
| description | Water is an essential chemical compound for living organisms, and twenty of its different crystal solid forms (ices) are known. Still, there are many fundamental problems with these structures such as establishing the correct positions and thermal motions of hydrogen atoms. The list of ice structures is not yet complete as DFT calculations have suggested the existence of additional and – to date – unknown phases. In many ice structures, neither neutron diffraction nor DFT calculations nor X-ray diffraction methods can easily solve the problem of hydrogen atom disorder or accurately determine their anisotropic displacement parameters (ADPs). Here, accurate crystal structures of H2O, D2O and mixed (50%H2O/50%D2O) ice VI obtained by Hirshfeld atom refinement (HAR) of high-pressure single-crystal synchrotron and laboratory X-ray diffraction data are presented. It was possible to obtain O—H/D bond lengths and ADPs for disordered hydrogen atoms which are in good agreement with the corresponding single-crystal neutron diffraction data. These results show that HAR combined with X-ray diffraction can compete with neutron diffraction in detailed studies of polymorphic forms of ice and crystals of other hydrogen-rich compounds. As neutron diffraction is relatively expensive, requires larger crystals which can be difficult to obtain and access to neutron facilities is restricted, cheaper and more accessible X-ray measurements combined with HAR can facilitate the verification of the existing ice polymorphs and the quest for new ones. |
| first_indexed | 2024-12-10T07:40:45Z |
| format | Article |
| id | doaj.art-107bff11c12b473f8d469d163a701d1d |
| institution | Directory Open Access Journal |
| issn | 2052-2525 |
| language | English |
| last_indexed | 2024-12-10T07:40:45Z |
| publishDate | 2022-09-01 |
| publisher | International Union of Crystallography |
| record_format | Article |
| series | IUCrJ |
| spelling | doaj.art-107bff11c12b473f8d469d163a701d1d2022-12-22T01:57:18ZengInternational Union of CrystallographyIUCrJ2052-25252022-09-019557357910.1107/S2052252522006662lt5051Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinementMichal L. Chodkiewicz0Roman Gajda1Barbara Lavina2Sergey Tkachev3Vitali B. Prakapenka4Przemyslaw Dera5Krzysztof Wozniak6Biological and Chemical Research Centre, Department of Chemistry, University of Warsaw, Żwirki i Wigury, Warszawa 02-089, PolandBiological and Chemical Research Centre, Department of Chemistry, University of Warsaw, Żwirki i Wigury, Warszawa 02-089, PolandAdvanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Lemont, IL 60439, USAAdvanced Photon Source, Argonne National Laboratory, 9700 South Cass Avenue, Lemont, IL 60439, USAHawai'i Institute of Geophysics and Planetology, Université d'hawaï à mānoa, 1680 East-West Road, Honolulu, HI 96822, USAHawai'i Institute of Geophysics and Planetology, Université d'hawaï à mānoa, 1680 East-West Road, Honolulu, HI 96822, USABiological and Chemical Research Centre, Department of Chemistry, University of Warsaw, Żwirki i Wigury, Warszawa 02-089, PolandWater is an essential chemical compound for living organisms, and twenty of its different crystal solid forms (ices) are known. Still, there are many fundamental problems with these structures such as establishing the correct positions and thermal motions of hydrogen atoms. The list of ice structures is not yet complete as DFT calculations have suggested the existence of additional and – to date – unknown phases. In many ice structures, neither neutron diffraction nor DFT calculations nor X-ray diffraction methods can easily solve the problem of hydrogen atom disorder or accurately determine their anisotropic displacement parameters (ADPs). Here, accurate crystal structures of H2O, D2O and mixed (50%H2O/50%D2O) ice VI obtained by Hirshfeld atom refinement (HAR) of high-pressure single-crystal synchrotron and laboratory X-ray diffraction data are presented. It was possible to obtain O—H/D bond lengths and ADPs for disordered hydrogen atoms which are in good agreement with the corresponding single-crystal neutron diffraction data. These results show that HAR combined with X-ray diffraction can compete with neutron diffraction in detailed studies of polymorphic forms of ice and crystals of other hydrogen-rich compounds. As neutron diffraction is relatively expensive, requires larger crystals which can be difficult to obtain and access to neutron facilities is restricted, cheaper and more accessible X-ray measurements combined with HAR can facilitate the verification of the existing ice polymorphs and the quest for new ones.http://scripts.iucr.org/cgi-bin/paper?S2052252522006662deuterated icehirshfeld atom refinementquantum crystallography |
| spellingShingle | Michal L. Chodkiewicz Roman Gajda Barbara Lavina Sergey Tkachev Vitali B. Prakapenka Przemyslaw Dera Krzysztof Wozniak Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinement IUCrJ deuterated ice hirshfeld atom refinement quantum crystallography |
| title | Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinement |
| title_full | Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinement |
| title_fullStr | Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinement |
| title_full_unstemmed | Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinement |
| title_short | Accurate crystal structure of ice VI from X-ray diffraction with Hirshfeld atom refinement |
| title_sort | accurate crystal structure of ice vi from x ray diffraction with hirshfeld atom refinement |
| topic | deuterated ice hirshfeld atom refinement quantum crystallography |
| url | http://scripts.iucr.org/cgi-bin/paper?S2052252522006662 |
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