scholarly journals Can 3D electron diffraction provide accurate atomic structures of metal–organic frameworks?

2020 ◽  
Vol 76 (a1) ◽  
pp. a52-a52
Author(s):  
Meng Ge ◽  
Zhehao Huang ◽  
Xiaodong Zou
Keyword(s):  
Electron Diffraction ◽  
Metal Organic Frameworks ◽  
Atomic Structures ◽  
Metal Organic ◽  
3D Electron

scholarly journals Can 3D electron diffraction provide accurate atomic structures of metal–organic frameworks?

2021 ◽  
Author(s):  
Zhehao Huang ◽  
Meng Ge ◽  
Francesco Carraro ◽  
Christian Doonan ◽  
Paolo Falcaro ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Single Crystal ◽  
Structure Determination ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Atomic Structures ◽  
Continuous Rotation ◽  
Metal Organic ◽  
3D Electron

Structure determination by continuous rotation electron diffraction can be as feasible and accurate as single crystal X-ray diffraction without the need for large crystals.

scholarly journals Can 3D Electron Diffraction Provide Accurate Atomic Structures of Metal-Organic Frameworks?

2020 ◽  
Author(s):  
Zhehao Huang ◽  
meng ge ◽  
Francesco Carraro ◽  
Christian Doonan ◽  
paolo falcaro ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Data Collection ◽  
Single Crystal ◽  
Structure Determination ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Continuous Rotation ◽  
Metal Organic ◽  
3D Electron

Many framework materials such as metal-organic frameworks (MOFs) or porous coordination polymers (PCPs) are synthesized as polycrystalline powders, which are too small for structure determination by single crystal X-ray diffraction (SCXRD). Here, we show that a three-dimensional (3D) electron diffraction method, namely continuous rotation electron diffraction (cRED), can be used for <i>ab initio</i> structure determination of such materials. As an example, we present a complete structural analysis of a biocomposite, denoted BSA@ZIF-C, where Bovin Serum Albumin (BSA) was encapsulated in a zeolitic imidazolate framework (ZIF). Low electron dose was combined with ultrafast cRED data collection to minimize electron beam damage of the sample. We demonstrate that the atomic structure obtained by cRED is as reliable and accurate as that obtained by single crystal X-ray diffraction. The high accuracy and fast data collection open new opportunities for investigation of cooperative phenomena in framework structures at atomic level.

scholarly journals Can 3D Electron Diffraction Provide Accurate Atomic Structures of Metal-Organic Frameworks?

2020 ◽  
Author(s):  
Zhehao Huang ◽  
meng ge ◽  
Francesco Carraro ◽  
Christian Doonan ◽  
paolo falcaro ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Data Collection ◽  
Single Crystal ◽  
Structure Determination ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Continuous Rotation ◽  
Metal Organic ◽  
3D Electron

Many framework materials such as metal-organic frameworks (MOFs) or porous coordination polymers (PCPs) are synthesized as polycrystalline powders, which are too small for structure determination by single crystal X-ray diffraction (SCXRD). Here, we show that a three-dimensional (3D) electron diffraction method, namely continuous rotation electron diffraction (cRED), can be used for <i>ab initio</i> structure determination of such materials. As an example, we present a complete structural analysis of a biocomposite, denoted BSA@ZIF-C, where Bovin Serum Albumin (BSA) was encapsulated in a zeolitic imidazolate framework (ZIF). Low electron dose was combined with ultrafast cRED data collection to minimize electron beam damage of the sample. We demonstrate that the atomic structure obtained by cRED is as reliable and accurate as that obtained by single crystal X-ray diffraction. The high accuracy and fast data collection open new opportunities for investigation of cooperative phenomena in framework structures at atomic level.

scholarly journals Direct Imaging of Correlated Defect Nanodomains in a Metal-Organic Framework

2020 ◽  
Author(s):  
Duncan Johnstone ◽  
Francesca Firth ◽  
Clare P. Grey ◽  
Paul A. Midgley ◽  
Matthew Cliffe ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Electron Diffraction ◽  
Metal Organic Framework ◽  
Metal Organic Frameworks ◽  
Synthetic Control ◽  
Defect Engineering ◽  
Nanoscale Characterization ◽  
Metal Organic ◽  
Image Defect ◽  
Scanning Electron

<p>Defect engineering can enhance key properties of metal-organic frameworks (MOFs). Tailoring the distribution of defects, for example in correlated nanodomains, requires characterization across length scales. However, a critical nanoscale characterization gap has emerged between the bulk diffraction techniques used to detect defect nanodomains and the sub-nanometre imaging used to observe individual defects. Here, we demonstrate that the emerging technique of scanning electron diffraction (SED) can bridge this gap. We directly image defect nanodomains in the MOF UiO-66(Hf) over an area of ca. 1 000 nm and with a spatial resolution ca. 5 nm to reveal domain morphology and distribution. Based on these observations, we suggest possible crystal growth processes underpinning synthetic control of defect nanodomains. We also identify likely dislocations and small angle grain boundaries, illustrating that SED could be a key technique in developing the potential for engineering the distribution of defects, or “microstructure”, in functional MOF design.</p>

scholarly journals Direct Imaging of Correlated Defect Nanodomains in a Metal-Organic Framework

2020 ◽  
Author(s):  
Duncan Johnstone ◽  
Francesca Firth ◽  
Clare P. Grey ◽  
Paul A. Midgley ◽  
Matthew Cliffe ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Electron Diffraction ◽  
Metal Organic Framework ◽  
Metal Organic Frameworks ◽  
Synthetic Control ◽  
Defect Engineering ◽  
Nanoscale Characterization ◽  
Metal Organic ◽  
Image Defect ◽  
Scanning Electron

<p>Defect engineering can enhance key properties of metal-organic frameworks (MOFs). Tailoring the distribution of defects, for example in correlated nanodomains, requires characterization across length scales. However, a critical nanoscale characterization gap has emerged between the bulk diffraction techniques used to detect defect nanodomains and the sub-nanometre imaging used to observe individual defects. Here, we demonstrate that the emerging technique of scanning electron diffraction (SED) can bridge this gap. We directly image defect nanodomains in the MOF UiO-66(Hf) over an area of ca. 1 000 nm and with a spatial resolution ca. 5 nm to reveal domain morphology and distribution. Based on these observations, we suggest possible crystal growth processes underpinning synthetic control of defect nanodomains. We also identify likely dislocations and small angle grain boundaries, illustrating that SED could be a key technique in developing the potential for engineering the distribution of defects, or “microstructure”, in functional MOF design.</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 Phosphinate MOF formed from tetratopic ligands as proton conductive materials

2021 ◽  
Author(s):  
Matouš Kloda ◽  
Tomáš Plecháček ◽  
Soňa Ondrušová ◽  
Petr Brázda ◽  
Petr Chalupský ◽  
...  
Keyword(s):  
Electron Diffraction ◽  
Proton Transfer ◽  
Rational Design ◽  
Metal Organic Frameworks ◽  
Adsorbed Water ◽  
Proton Conductors ◽  
Water Molecules ◽  
Conductive Materials ◽  
Grotthuss Mechanism ◽  
Metal Organic

Metal organic frameworks (MOFs) are attracting attention as potential proton conductors. There are two main advantages of MOFs in this application: the possibility of rational design and tuning of the properties, and clear conduction pathways given by their crystalline structure. We hereby present two new MOF structures, ICR-10 and ICR-11, based on tetratopic phosphinate ligands. The structures of both MOFs were determined by 3D electron diffraction. They both crystallize in the P-3 space group and contain arrays of parallel linear pores lined with hydrophilic non-coordinated phosphinate groups. This, together with the adsorbed water molecules, facilitates proton transfer via the Grotthuss mechanism, leading to the proton conductivity up to 4.26∙10-4 S cm-1 for ICR-11.

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...

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