scholarly journals On the Completeness of Three-Dimensional Electron Diffraction Data for Structural Analysis of Metal-Organic Frameworks

2021 ◽  
Author(s):  
Meng Ge ◽  
Taimin Yang ◽  
Yanzhi Wang ◽  
Francesco Carraro ◽  
Weibin Liang ◽  
...  
Keyword(s):  
Structural Analysis ◽  
Electron Diffraction ◽  
Metal Organic Frameworks ◽  
Three Dimensional ◽  
Accurate Method ◽  
Electron Diffraction Data ◽  
Dimensional Electron ◽  
The Past ◽  
Metal Organic

Three-dimensional electron diffraction (3DED) has been proven as an effective and accurate method for structure determination of nano-sized crystals. In the past decade, the crystal structures of various new complex...

scholarly journals On the Completeness of Three-Dimensional Electron Diffraction Data for Structural Analysis of Metal-Organic Frameworks

2021 ◽  
Author(s):  
Meng Ge ◽  
Taimin Yang ◽  
Yanzhi Wang ◽  
Francesco Carraro ◽  
Weibin Liang ◽  
...  
Keyword(s):  
Structural Analysis ◽  
Electron Diffraction ◽  
Structural Model ◽  
Metal Organic Frameworks ◽  
Three Dimensional ◽  
Electron Diffraction Data ◽  
Dimensional Electron ◽  
Data Completeness ◽  
Continuous Rotation ◽  
Metal Organic

<p>Three-dimensional electron diffraction (3DED) has been proven as an effective and accurate method for structure determination of nano-sized crystals. In the past decade, the crystal structures of various new complex metal-organic frameworks (MOFs) have been revealed by 3DED, which has been the key to understand their properties. However, due to the design of transmission electron microscopes (TEMs), one drawback of 3DED experiments is the limited tilt range of goniometer, which often leads to incomplete 3DED data, particularly when the crystal symmetry is low. This drawback can be overcome by high throughput data collection using continuous rotation electron diffraction (cRED), where data from a large number of crystals can be collected and merged. Here, we investigate the effects of improving completeness on structural analysis of MOFs. We use ZIF-EC1, a zeolitic imidazolate framework (ZIF), as an example. ZIF-EC1 crystallizes in a monoclinic system with a plate-like morphology. cRED data of ZIF-EC1 with different completeness and resolution were analyzed. The data completeness increased to 92.0% by merging ten datasets. Although the structures could be solved from individual datasets with a completeness as low as 44.5% and refined to a high precession (better than 0.04 Å), we demonstrate that a high data completeness could improve the structural model, especially on the electrostatic potential map. We further discuss the strategy adopted during data merging. We also show that ZIF-EC1 doped with cobalt can act as an efficient electrocatalyst for oxygen reduction reaction. </p>

scholarly journals On the Completeness of Three-Dimensional Electron Diffraction Data for Structural Analysis of Metal-Organic Frameworks

2021 ◽  
Author(s):  
Meng Ge ◽  
Taimin Yang ◽  
Yanzhi Wang ◽  
Francesco Carraro ◽  
Weibin Liang ◽  
...  
Keyword(s):  
Structural Analysis ◽  
Electron Diffraction ◽  
Structural Model ◽  
Metal Organic Frameworks ◽  
Three Dimensional ◽  
Electron Diffraction Data ◽  
Dimensional Electron ◽  
Data Completeness ◽  
Continuous Rotation ◽  
Metal Organic

<p>Three-dimensional electron diffraction (3DED) has been proven as an effective and accurate method for structure determination of nano-sized crystals. In the past decade, the crystal structures of various new complex metal-organic frameworks (MOFs) have been revealed by 3DED, which has been the key to understand their properties. However, due to the design of transmission electron microscopes (TEMs), one drawback of 3DED experiments is the limited tilt range of goniometer, which often leads to incomplete 3DED data, particularly when the crystal symmetry is low. This drawback can be overcome by high throughput data collection using continuous rotation electron diffraction (cRED), where data from a large number of crystals can be collected and merged. Here, we investigate the effects of improving completeness on structural analysis of MOFs. We use ZIF-EC1, a zeolitic imidazolate framework (ZIF), as an example. ZIF-EC1 crystallizes in a monoclinic system with a plate-like morphology. cRED data of ZIF-EC1 with different completeness and resolution were analyzed. The data completeness increased to 92.0% by merging ten datasets. Although the structures could be solved from individual datasets with a completeness as low as 44.5% and refined to a high precession (better than 0.04 Å), we demonstrate that a high data completeness could improve the structural model, especially on the electrostatic potential map. We further discuss the strategy adopted during data merging. We also show that ZIF-EC1 doped with cobalt can act as an efficient electrocatalyst for oxygen reduction reaction. </p>

scholarly journals Three-Dimensional Electron Diffraction for Structural Analysis of Beam-Sensitive Metal-Organic Frameworks

Crystals ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 263
Author(s):  
Meng Ge ◽  
Xiaodong Zou ◽  
Zhehao Huang
Keyword(s):  
High Resolution ◽  
Electron Diffraction ◽  
Data Quality ◽  
Metal Organic Frameworks ◽  
Three Dimensional ◽  
Electron Diffraction Data ◽  
X Rays ◽  
Dimensional Electron ◽  
Continuous Rotation ◽  
Metal Organic

Electrons interact strongly with matter, which makes it possible to obtain high-resolution electron diffraction data from nano- and submicron-sized crystals. Using electron beam as a radiation source in a transmission electron microscope (TEM), ab initio structure determination can be conducted from crystals that are 6–7 orders of magnitude smaller than using X-rays. The rapid development of three-dimensional electron diffraction (3DED) techniques has attracted increasing interests in the field of metal-organic frameworks (MOFs), where it is often difficult to obtain large and high-quality crystals for single-crystal X-ray diffraction. Nowadays, a 3DED dataset can be acquired in 15–250 s by applying continuous crystal rotation, and the required electron dose rate can be very low (<0.1 e s−1 Å−2). In this review, we describe the evolution of 3DED data collection techniques and how the recent development of continuous rotation electron diffraction techniques improves data quality. We further describe the structure elucidation of MOFs using 3DED techniques, showing examples of using both low- and high-resolution 3DED data. With an improved data quality, 3DED can achieve a high accuracy, and reveal more structural details of MOFs. Because the physical and chemical properties of MOFs are closely associated with their crystal structures, we believe 3DED will only increase its importance in developing MOF materials.

scholarly journals Probing Molecular Motions in Metal–Organic Frameworks by Three-Dimensional Electron Diffraction

2021 ◽  
Author(s):  
Laura Samperisi ◽  
Aleksander Jaworski ◽  
Gurpreet Kaur ◽  
Karl Petter Lillerud ◽  
Xiaodong Zou ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Metal Organic Frameworks ◽  
Three Dimensional ◽  
Molecular Motions ◽  
Dimensional Electron ◽  
Metal Organic

A complex pseudo-decagonal quasicrystal approximant, Al37(Co,Ni)15.5, solved by rotation electron diffraction

2014 ◽  
Vol 47 (1) ◽  
pp. 215-221 ◽  
Author(s):  
Devinder Singh ◽  
Yifeng Yun ◽  
Wei Wan ◽  
Benjamin Grushko ◽  
Xiaodong Zou ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Single Crystal ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Basic Structure ◽  
Electron Diffraction Data ◽  
Dimensional Electron ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Patterns

Electron diffraction is a complementary technique to single-crystal X-ray diffraction and powder X-ray diffraction for structure solution of unknown crystals. Crystals too small to be studied by single-crystal X-ray diffraction or too complex to be solved by powder X-ray diffraction can be studied by electron diffraction. The main drawbacks of electron diffraction have been the difficulties in collecting complete three-dimensional electron diffraction data by conventional electron diffraction methods and the very time-consuming data collection. In addition, the intensities of electron diffraction suffer from dynamical scattering. Recently, a new electron diffraction method, rotation electron diffraction (RED), was developed, which can overcome the drawbacks and reduce dynamical effects. A complete three-dimensional electron diffraction data set can be collected from a sub-micrometre-sized single crystal in less than 2 h. Here the RED method is applied forab initiostructure determination of an unknown complex intermetallic phase, the pseudo-decagonal (PD) quasicrystal approximant Al37.0(Co,Ni)15.5, denoted as PD2. RED shows that the crystal is F-centered, witha= 46.4,b= 64.6,c= 8.2 Å. However, as with other approximants in the PD series, the reflections with oddlindices are much weaker than those withleven, so it was decided to first solve the PD2 structure in the smaller, primitive unit cell. The basic structure of PD2 with unit-cell parametersa= 23.2,b= 32.3,c= 4.1 Å and space groupPnmmhas been solved in the present study. The structure withc= 8.2 Å will be taken up in the near future. The basic structure contains 55 unique atoms (17 Co/Ni and 38 Al) and is one of the most complex structures solved by electron diffraction. PD2 is built of characteristic 2 nm wheel clusters with fivefold rotational symmetry, which agrees with results from high-resolution electron microscopy images. Simulated electron diffraction patterns for the structure model are in good agreement with the experimental electron diffraction patterns obtained by RED.

scholarly journals Three-dimensional electron diffraction for porous crystalline materials: structural determination and beyond

2021 ◽  
Author(s):  
Zhehao Huang ◽  
Tom Willhammar ◽  
Xiaodong Zou
Keyword(s):  
Electron Diffraction ◽  
Three Dimensional ◽  
Structural Determination ◽  
New Materials ◽  
Dimensional Electron ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Structural Details

Three-dimensional electron diffraction is a powerful tool for accurate structure determination of zeolite, MOF, and COF crystals that are too small for X-ray diffraction. By revealing the structural details, the properties of the materials can be understood, and new materials and applications can be designed.

EDIFF: a program for automated unit-cell determination and indexing of electron diffraction data

2011 ◽  
Vol 44 (5) ◽  
pp. 1132-1136 ◽  
Author(s):  
Linhua Jiang ◽  
Dilyana Georgieva ◽  
Jan Pieter Abrahams
Keyword(s):  
Electron Diffraction ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Unit Cell ◽  
Electron Diffraction Data ◽  
Cell Determination ◽  
Diffraction Patterns ◽  
Inorganic Molecules ◽  
User Friendly

EDIFFis a new user-friendly software suite for unit-cell determination of three-dimensional nanocrystals from randomly oriented electron diffraction patterns with unknown independent orientations. It can also be used for three-dimensional cell reconstruction from diffraction tilt series. In neither case is exact knowledge of the angular relationship between the patterns required. The unit cell can be validated and the crystal system assigned.EDIFFcan index the reflections in electron diffraction patterns. Thus,EDIFFcan be employed as a first step in reconstructing the three-dimensional atomic structure of organic and inorganic molecules and of proteins from diffraction data. An example illustrates the viability of theEDIFFapproach.

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