Acta Physico-Chimica Sinica ›› 2020, Vol. 36 ›› Issue (1): 1907052.doi: 10.3866/PKU.WHXB201907052
Special Issue: Special Issue in Honor of Academician Youqi Tang on the Occasion of His 100th Birthday
• Review • Previous Articles Next Articles
Jian Li,Cong Lin,Jianhua Lin,Junliang Sun*()
Received:
2019-07-18
Accepted:
2019-09-17
Published:
2019-09-24
Contact:
Junliang Sun
E-mail:junliang.sun@pku.edu.cn
Supported by:
MSC2000:
Jian Li,Cong Lin,Jianhua Lin,Junliang Sun. Application of Combining X-ray Diffraction and Electron Crystallography for Determination of Complex Inorganic Crystal Structure[J].Acta Physico-Chimica Sinica, 2020, 36(1): 1907052.
Table 1
Comparison of SCXRD, PXRD, HRTEM and ED."
SCXRD | PXRD | ED (2D/3D) | HRTEM | |
Unit cell | Easy | Difficult | Require expertise /Easy | Difficult |
Space group | Easy | Difficult | Require expertise /Easy | Difficult |
Peak overlapping | No | Yes | No/No | No |
Completeness | High | High | Low/High | Low |
Beam damage | Low | Low | Medium/Medium | Strong |
Phase | No | No | No/No | Yes |
Information of sample | Single crystal | over | Single crystal | Single crystal |
Intensities | Kinematic | Kinematic | Dynamic/Dynamic | Dynamic |
Data collection | Easy | Easy | Difficult /Difficult | Difficult |
Structure solution | Easy | Difficult | Difficult/easy | Difficult |
Refinement | Accurate | Accurate | Less accurate/ Less accurate | Less accurate/ Less accurate |
Crystal size | > 1 μm | > 50 nm | > 50 nm | > 5 nm |
Fig 1
The structure determination of microporous aluminoborates with large channels14, 15. (a) Rietveld refinement on powder X-ray diffraction of PKU-2; (b) HRTEM image along the [001] direction of PKU-2. Insets are the corresponding ED pattern (right) and a simulated image based on the structure model (left); (c) Projected structure views of both PKU-1 and PKU-2 along the c axis. Adapted with permission from Ref. 15. Copyright 2011 Wiley. "
Fig 2
The structure model of ITQ-37和PKU-332, 33. (a) Electron density map of ITQ-37 derived by charge flipping algorithm; (b) The obtained structure model of ITQ 37 along the c axis; (c) The model of PKU-3. Adapted with permission from Ref. 32, 33. Copyright 2009 Nature Publishing Group and copyright 2015 American Chemical Society."
Fig 4
PKU-16: A germanosilicate structure with 11 × 11 × 12-ring channels solved by electron crystallography 21. (a) SEM of PKU-16; (b) Reconstructed three-dimensional RED data of PKU-16. Overview of the data. (c) The 3D channels systems in PKU-16. Adapted with permission from Ref. 21. Copyright 2014 Wiley."
Fig 5
Intergrown new zeolite beta polymorphs with interconnected 12-ring channels solved by combining electron crystallography and single-crystal X-ray diffraction 35. (a) Structure of SU-78 viewing along a axis; (b, c) SCXRD along [100] (b) and HRTEM image along [010] (c) of SU 78; (d) SU 78 viewing along b axis, which is an intergrowth of polymorph D and E of zeolite beta. Adapted with permission from Ref. 35. Copyright 2012 American Chemical Society. "
Fig 6
The structure of a complex open-framework germanate obtained by combining powder charge-flipping and simulated annealing 13. The cavity in SU-74 and the location of the guest species in the cavity. (a) A single cavity with the face symbol [312.43.62.72.83.10.12]. Oxygen atoms are excluded for clarity. The pockets formed by the Ge10 clusters in the Ge10 layer are shown in green, while the part in the pillared region is in gray. (b) H2MPMD2+ and NH4+ cations, and water molecules found in SU-74-MPMD. (c) H2AEP2+ cation with 82% occupancy and NH4+ cations in SU-74-AEP. (d) H2AEP2+ cation with 18% occupancy and NH4+ cations in SU-74-AEP. (e) A cross-section in parallel to the bc-plane cut in the middle of the cavity showing the position of the H2MPMD2+ cation in SU-74-MPMD. (f) A cross-section in parallel to the bc-plane cut in the middle of the cavity showing the position of the H2AEP2+ cation in SU-74-AEP. Adapted with permission from Ref. 13. Copyright 2012 American Chemical Society. "
Fig 7
Locating carbon dioxide and sulfur dioxide in a decorated porous host by PXRD and inelastic neutron scattering 43. (a) View of the structure of NOTT-300·3.2CO2 obtained using PXRD analysis. (b) Detailed view of the roles of the -OH and -CH groups in binding CO2 molecules in a pocket-like cavity. (c) View of the crystal structure of NOTT-300·4.0 SO2. (d) Detailed view of the role of the -OH and -CH groups in binding SO2 molecules into a distorted pocket-like cavity. Adapted with permission from Ref. 43. Copyright 2012 Nature Publishing Group."
Fig 8
The model of PKU-14 with a 3D 12-ring zeolite 45. (a) The SEM image of PKU 14 with twinning. The twinning grain boundaries are indicated by white arrows. (b) Rietveld refinement of PXRD for as synthesized PKU-14. (c) The framework structure of as synthesized PKU 14 along the [010] direction. (d) The tiling of PKU-14. Adapted with permission from Ref. 45. Copyright 2014 Wiley."
Fig 9
Unusual long-range ordering incommensurate structural modulations in an organic molecular ferroelectric 54. (a) (0hk) plane diffraction patterns for 1 at 100, 150 and 240 K (above), and dielectric properties of N-isopropylbenzylaminium trichloroacetate measured on the single crystals along the b-axis direction (blow). (b, c) Superlattice approximants of 1 at 150 K 1a × 1b × 7c modulated approximant along its a-axis (c) and c-axis (b). Adapted with permission from Ref. 54. Copyright 2017 American Chemical Society."
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