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

Huang, Zhehao; Meng, Guangyao; Carraro, Francesco; Doonan, Christian J.; Falcaro, Paolo; Zou, Xiaodong

doi:10.1039/d0fd00015a

Cited by 42 publications

(37 citation statements)

References 68 publications

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“…This has been a key concern in the eld of electron crystallography. Nevertheless, recently studies on zeolites 39 and MOFs 40 have proved that the structural models obtained from 3DED are similar to those obtained by SCXRD, with average deviations of atomic positions by less than 0.10Å. Moreover, structure determination by 3DED also shows high reproducibility.…”

Section: Three-dimensional Electron Diffraction (3ded)mentioning

confidence: 68%

“…Therefore, it is much easier to perform ab initio structure determination on nano-and submicron-sized MOFs nowadays. 40,41,[73][74][75][76][77][78][79][80][81][82][83][84][85] The revealed structural details provide an enhanced understanding of their properties as well as fundamental knowledge to promote the discovery of new materials.…”

Section: Application Of 3ded To Mofsmentioning

confidence: 99%

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

2021

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Section: Three-dimensional Electron Diffraction (3ded)mentioning

confidence: 68%

Section: Application Of 3ded To Mofsmentioning

confidence: 99%

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

2021

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“…U14) [41] . Only after our investigations of ZIF-CO3-1 by cRED [34] , could we identify ZIF-CO3-1 as the major phase in the sample (Figure 1a). Yet, there are many peaks in the PXRD pattern that cannot be identified.…”

Section: Resultsmentioning

confidence: 92%

“…For MOFs, structural studies are even more difficult due to their relatively large unit cells that intensify the drawback of peak overlapping in PXRD patterns. These challenges are well tackled with the recent development of three-dimensional electron diffraction (3DED) [32][33][34] . Benefited from the strong interaction between electrons and matter, 3DED allows single crystal structural analysis even when the crystal sizes are down to the range of nanometers [35][36][37][38] .…”

Section: Introductionmentioning

confidence: 99%

High‐Throughput Electron Diffraction Reveals a Hidden Novel Metal–Organic Framework for Electrocatalysis

et al. 2021

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Metal-organic frameworks (MOFs) are known for their versatile combination of inorganic building units and organic linkers, which offers immense opportunities in a wide range of applications. However, many MOFs are typically synthesized as multiphasic polycrystalline powders, which are challenging for studies by X-ray diffraction. Therefore, developing new structural characterization techniques is highly desired in order to accelerate discoveries of new materials. Here, we report a high-throughput approach for structural analysis of MOF nano-and sub-microcrystals by three-dimensional electron diffraction (3DED). A new zeolitic-imidazolate framework (ZIF), denoted ZIF-EC1, was first discovered in a trace amount during the study of a known ZIF-CO3-1 material by 3DED. The structures of both ZIFs were solved and refined using 3DED data. ZIF-EC1 has a dense 3D framework structure, which is built by linking mono-and bi-nuclear Zn clusters and 2-methylimidazolates (mIm -). With a composition of Zn3(mIm)5(OH), ZIF-EC1 exhibits high N and Zn densities. We show that the N-doped carbon material derived from ZIF-EC1 is a promising electrocatalysis for oxygen reduction reaction (ORR). The discovery of this new MOF and its conversion to an efficient electrocatalyst highlights the power of 3DED in developing new materials and their applications.

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“…Recent developments of fast 3D electron diffraction (3DED) or microcrystal electron diffraction (MicroED) data collection techniques (<5 min) using continuous rotation (denoted cRED here) have made it possible for studying beam sensitive nano-and micrometer-sized crystals 18,[36][37][38][39][40] . Here, we demonstrate the ab initio structure determination of PST-5 using cRED data collected under low-dose condition.…”

mentioning

confidence: 99%

3D-3D topotactic transformation in aluminophosphate molecular sieves and its implication in new zeolite structure generation

et al. 2020

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Zeolites have unique pore structures of molecular dimensions and tunable compositions, making them ideal for shape selective catalysis and separation. However, targeted synthesis of zeolites with new pore structures and compositions remains a key challenge. Here, we propose an approach based on a unique 3D-3D topotactic transformation, which takes advantage of weak bonding in zeolites. This is inspired by the structure transformation of PST-5, a new aluminophosphate molecular sieve, to PST-6 by calcination. The structure of nano-sized PST-5 crystals is determined by 3D electron diffraction. We find that the 3D-3D topotactic transformation involves two types of building units where penta-or hexacoordinated Al is present. We apply this approach to several other zeolite systems and predict a series of new zeolite structures that would be synthetically feasible. This method provides a concept for the synthesis of targeted zeolites, especially those which may not be feasible by conventional methods.

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

Abstract: Many framework materials such as metal-organic frameworks (MOF) or porous coordination polymers (PCPs) are synthesized as polycrystalline powders, which are too small for structure determination by single crystal X-ray diffraction...

Cited by 42 publications

References 68 publications

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

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

High‐Throughput Electron Diffraction Reveals a Hidden Novel Metal–Organic Framework for Electrocatalysis

3D-3D topotactic transformation in aluminophosphate molecular sieves and its implication in new zeolite structure generation

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