How to get maximum structure information from anisotropic displacement parameters obtained by three-dimensional electron diffraction: an experimental study on metal–organic frameworks
Three-dimensional electron diffraction (3D ED) has been used for ab initio structure determination of various types of nanocrystals, such as metal–organic frameworks (MOFs), zeolites, metal oxides and organic crystals. These crystals are often obtained as polycrystalline powders, which are too small...
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| Format: | Article |
| Language: | English |
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International Union of Crystallography
2022-07-01
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| Series: | IUCrJ |
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| Online Access: | http://scripts.iucr.org/cgi-bin/paper?S2052252522005632 |
| _version_ | 1818466934776135680 |
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| author | Laura Samperisi Xiaodong Zou Zhehao Huang |
| author_facet | Laura Samperisi Xiaodong Zou Zhehao Huang |
| author_sort | Laura Samperisi |
| collection | DOAJ |
| description | Three-dimensional electron diffraction (3D ED) has been used for ab initio structure determination of various types of nanocrystals, such as metal–organic frameworks (MOFs), zeolites, metal oxides and organic crystals. These crystals are often obtained as polycrystalline powders, which are too small for single-crystal X-ray diffraction (SCXRD). While it is now possible to obtain accurate atomic positions of nanocrystals by adopting kinematical refinement against 3D ED data, most new structures are refined with isotropic displacement parameters (Ueq), which limits the detection of possible structure disorders and atomic motions. Anisotropic displacement parameters (ADPs, Uij) obtained by anisotropic structure refinement, on the other hand, provide information about the average displacements of atoms from their mean positions in a crystal, which can provide insights with respect to displacive disorder and flexibility. Although ADPs have been obtained from some 3D ED studies of MOFs, they are seldom mentioned or discussed in detail. We report here a detailed study and interpretation of structure models refined anisotropically against 3D ED data. Three MOF samples with different structural complexity and symmetry, namely ZIF-EC1, MIL-140C and Ga(OH)(1,4-ndc) (1,4-ndcH2 is naphthalene-1,4-dicarboxylic acid), were chosen for the studies. We compare the ADPs refined against individual data sets and how they are affected by different data-merging strategies. Based on our results and analysis, we propose strategies for obtaining accurate structure models with interpretable ADPs based on kinematical refinement against 3D ED data. The ADPs of the obtained structure models provide clear and unambiguous information about linker motions in the MOFs. |
| first_indexed | 2024-04-13T21:03:20Z |
| format | Article |
| id | doaj.art-1060892d737748c4a09be4360e75c663 |
| institution | Directory Open Access Journal |
| issn | 2052-2525 |
| language | English |
| last_indexed | 2024-04-13T21:03:20Z |
| publishDate | 2022-07-01 |
| publisher | International Union of Crystallography |
| record_format | Article |
| series | IUCrJ |
| spelling | doaj.art-1060892d737748c4a09be4360e75c6632022-12-22T02:30:04ZengInternational Union of CrystallographyIUCrJ2052-25252022-07-019448049110.1107/S2052252522005632vq5001How to get maximum structure information from anisotropic displacement parameters obtained by three-dimensional electron diffraction: an experimental study on metal–organic frameworksLaura Samperisi0Xiaodong Zou1Zhehao Huang2Department of Materials and Environmental Chemistry, Stockholm University, Stockholm, Sweden 106 91, SwedenDepartment of Materials and Environmental Chemistry, Stockholm University, Stockholm, Sweden 106 91, SwedenDepartment of Materials and Environmental Chemistry, Stockholm University, Stockholm, Sweden 106 91, SwedenThree-dimensional electron diffraction (3D ED) has been used for ab initio structure determination of various types of nanocrystals, such as metal–organic frameworks (MOFs), zeolites, metal oxides and organic crystals. These crystals are often obtained as polycrystalline powders, which are too small for single-crystal X-ray diffraction (SCXRD). While it is now possible to obtain accurate atomic positions of nanocrystals by adopting kinematical refinement against 3D ED data, most new structures are refined with isotropic displacement parameters (Ueq), which limits the detection of possible structure disorders and atomic motions. Anisotropic displacement parameters (ADPs, Uij) obtained by anisotropic structure refinement, on the other hand, provide information about the average displacements of atoms from their mean positions in a crystal, which can provide insights with respect to displacive disorder and flexibility. Although ADPs have been obtained from some 3D ED studies of MOFs, they are seldom mentioned or discussed in detail. We report here a detailed study and interpretation of structure models refined anisotropically against 3D ED data. Three MOF samples with different structural complexity and symmetry, namely ZIF-EC1, MIL-140C and Ga(OH)(1,4-ndc) (1,4-ndcH2 is naphthalene-1,4-dicarboxylic acid), were chosen for the studies. We compare the ADPs refined against individual data sets and how they are affected by different data-merging strategies. Based on our results and analysis, we propose strategies for obtaining accurate structure models with interpretable ADPs based on kinematical refinement against 3D ED data. The ADPs of the obtained structure models provide clear and unambiguous information about linker motions in the MOFs.http://scripts.iucr.org/cgi-bin/paper?S2052252522005632anisotropic displacement parametersadpsthree-dimensional electron diffraction3d edcontinuous rotation electron diffractionmetal-organic frameworks |
| spellingShingle | Laura Samperisi Xiaodong Zou Zhehao Huang How to get maximum structure information from anisotropic displacement parameters obtained by three-dimensional electron diffraction: an experimental study on metal–organic frameworks IUCrJ anisotropic displacement parameters adps three-dimensional electron diffraction 3d ed continuous rotation electron diffraction metal-organic frameworks |
| title | How to get maximum structure information from anisotropic displacement parameters obtained by three-dimensional electron diffraction: an experimental study on metal–organic frameworks |
| title_full | How to get maximum structure information from anisotropic displacement parameters obtained by three-dimensional electron diffraction: an experimental study on metal–organic frameworks |
| title_fullStr | How to get maximum structure information from anisotropic displacement parameters obtained by three-dimensional electron diffraction: an experimental study on metal–organic frameworks |
| title_full_unstemmed | How to get maximum structure information from anisotropic displacement parameters obtained by three-dimensional electron diffraction: an experimental study on metal–organic frameworks |
| title_short | How to get maximum structure information from anisotropic displacement parameters obtained by three-dimensional electron diffraction: an experimental study on metal–organic frameworks |
| title_sort | how to get maximum structure information from anisotropic displacement parameters obtained by three dimensional electron diffraction an experimental study on metal organic frameworks |
| topic | anisotropic displacement parameters adps three-dimensional electron diffraction 3d ed continuous rotation electron diffraction metal-organic frameworks |
| url | http://scripts.iucr.org/cgi-bin/paper?S2052252522005632 |
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