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.

Pitfalls in metal–organic framework crystallography: towards more accurate crystal structures

2017 ◽  
Vol 46 (16) ◽  
pp. 4867-4876 ◽  
Author(s):  
S. Øien-Ødegaard ◽  
G. C. Shearer ◽  
D. S. Wragg ◽  
K. P. Lillerud
Keyword(s):  
Single Crystal ◽  
Structure Determination ◽  
Metal Organic Framework ◽  
Metal Organic Frameworks ◽  
Porous Metal ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
Crystal Twinning

Proper handling of pore-occupying species and crystal twinning in structure determination of porous metal–organic frameworks by single crystal X-ray diffraction.

A series of microporous and robust Ln-MOFs showing luminescent properties and catalytic performances towards Knoevenagel reactions

2021 ◽  
Author(s):  
Qing-Xia Yao ◽  
Miaomiao Tian ◽  
Jun Zheng ◽  
Jintang Xue ◽  
Xuze Pan ◽  
...  
Keyword(s):  
Single Crystal ◽  
Metal Organic Frameworks ◽  
Luminescent Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
Catalytic Performances

A series of microporous Ln(III)-based metal-organic frameworks (1-Ln) have been hydrothermally synthesized by using 4,4',4''-nitrilotribenzoic acid (H3NTB). Single crystal X-ray diffraction analyses show 1-Ln are isostructural and have 3D porous...

scholarly journals Coordination Polymers of Scandium(III) and Thiophenedicarboxylic Acid

2021 ◽  
Vol 47 (9) ◽  
pp. 593-600
Author(s):  
A. A. Lysova ◽  
V. A. Dubskikh ◽  
K. D. Abasheeva ◽  
A. A. Vasileva ◽  
D. G. Samsonenko ◽  
...  
Keyword(s):  
Ir Spectroscopy ◽  
Single Crystal ◽  
Diffraction Analysis ◽  
Coordination Polymers ◽  
Elemental Analysis ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
Phase Purity ◽  
X Ray ◽  
Metal Organic

Abstract Three new metal−organic frameworks based on scandium(III) cations and 2,5-thiophenedicarboxylic acid (H2Tdc) are synthesized: [Sc(Tdc)(OH)]·1.2DMF (I), [Sc(Tdc)(OH)]·2/3DMF (II), and (Me2NH2)[Sc3(Tdc)4(OH)2]·DMF (III) (DMF is N,N-dimethylformamide). The structures of the compounds are determined by single-crystal X-ray structure analysis (CIF file CCDC nos. 2067819 (I), 2067820 (II), and 2067821 (III)). The chemical and phase purity of compound I is proved by elemental analysis, thermogravimetry, X-ray diffraction analysis, and IR spectroscopy.

scholarly journals Remodelling a Shp: Transmetallation in a Rare-Earth Cluster-Based Metal–Organic Framework

2021 ◽  
Author(s):  
Hudson de Aguiar Bicalho ◽  
P. Rafael Donnarumma ◽  
Victor Quezada-Novoa ◽  
Hatem M. Titi ◽  
Ashlee J Howarth
Keyword(s):  
Rare Earth ◽  
Single Crystal ◽  
Surface Area ◽  
De Novo ◽  
Metal Organic Framework ◽  
Metal Organic Frameworks ◽  
Metal Exchange ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic

<div> <p>Post-synthetic modification (PSM) of metal–organic frameworks (MOFs) is an important strategy for accessing MOF analogues that cannot be easily synthesized <i>de novo</i>. In this work, the rare-earth (RE) cluster-based MOF, Y-CU-10, with <b>shp</b> topology was modified through transmetallation using a series of RE ions, including: La(III), Nd(III), Eu(III), Tb(III), Er(III), Tm(III), and Yb(III). In all cases, metal-exchange higher than 70 % was observed, with reproducible results. All transmetallated materials were fully characterized and compared to the parent MOF, Y-CU-10, in regards to crystallinity, surface area, and morphology. Additionally, single-crystal X-ray diffraction (SCXRD) measurements were performed to provide further evidence of transmetallation occurring in the nonanuclear cluster nodes of the MOF. </p> </div>

scholarly journals Two metal–organic frameworks based on Sr2+ and 1,2,4,5-tetrakis(4-carboxyphenyl)benzene linkers

2021 ◽  
Vol 77 (12) ◽  
Author(s):  
Muhammad Usman ◽  
Lydia Ogebule ◽  
Raúl Castañeda ◽  
Evgenii Oskolkov ◽  
Tatiana Timofeeva
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structural Control ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
Solvent Systems ◽  
Semiconductor Properties

Two structurally different metal–organic frameworks based on Sr2+ ions and 1,2,4,5-tetrakis(4-carboxyphenyl)benzene linkers have been synthesized solvothermally in different solvent systems and studied with single-crystal X-ray diffraction technique. These are poly[[μ12-4,4′,4′′,4′′′-(benzene-1,2,4,5-tetrayl)tetrabenzoato](dimethylformamide)distrontium(II)], [Sr2(C34H18O8)(C3H7NO)2] n , and poly[tetraaqua{μ2-4,4′-[4,5-bis(4-carboxyphenyl)benzene-1,2-diyl]dibenzoato}tristrontium(II)], [Sr3(C34H20O8)2(H2O)4]. The differences are noted between the crystal structures and coordination modes of these two MOFs, which are responsible for their semiconductor properties, where structural control over the bandgap is desirable. Hydrogen bonding is present in only one of the compounds, suggesting it has a slightly higher structural stability.

Triazole-directed Fabrication of Polyoxovanadate-based Metal-organic Frameworks as Efficient Multifunctional Heterogeneous Catalysts for Knoevenagel Condensation and Oxidation of Alcohols

2021 ◽  
Author(s):  
Jikun Li ◽  
Chuanping Wei ◽  
Yinfeng Han ◽  
Yu Mei ◽  
Xueli Cheng ◽  
...  
Keyword(s):  
Single Crystal ◽  
Heterogeneous Catalysts ◽  
Knoevenagel Condensation ◽  
Metal Organic Frameworks ◽  
X Ray Diffraction ◽  
X Ray ◽  
Oxidation Of Alcohols ◽  
Metal Organic

By introducing 4-amino-1,2,4-triazole (4-NH2-trz), three new polyoxovanadate-based metal-organic frameworks (PMOFs) [Ni3(4-NH2-trz)6][V6O18]•3H2O (1), [Co3(4-NH2-trz)6][V6O18]•3H2O (2) and [Cu3OH(4-NH2-trz)3H2O][VO3]5•H2O (3) have been synthesized and thoroughly characterized by single-crystal X-ray diffraction (SXRD), powder X-ray...

On the quality of the continuous rotation electron diffraction data for accurate atomic structure determination of inorganic compounds

2018 ◽  
Vol 51 (4) ◽  
pp. 1094-1101 ◽  
Author(s):  
Yunchen Wang ◽  
Taimin Yang ◽  
Hongyi Xu ◽  
Xiaodong Zou ◽  
Wei Wan
Keyword(s):  
Electron Diffraction ◽  
Single Crystal ◽  
Diffraction Data ◽  
Structural Models ◽  
Electron Diffraction Data ◽  
Data Sets ◽  
X Ray Diffraction ◽  
X Ray ◽  
Continuous Rotation

The continuous rotation electron diffraction (cRED) method has the capability of providing fast three-dimensional electron diffraction data collection on existing and future transmission electron microscopes; unknown structures could be potentially solved and refined using cRED data collected from nano- and submicrometre-sized crystals. However, structure refinements of cRED data using SHELXL often lead to relatively high R1 values when compared with those refined against single-crystal X-ray diffraction data. It is therefore necessary to analyse the quality of the structural models refined against cRED data. In this work, multiple cRED data sets collected from different crystals of an oxofluoride (FeSeO3F) and a zeolite (ZSM-5) with known structures are used to assess the data consistency and quality and, more importantly, the accuracy of the structural models refined against these data sets. An evaluation of the precision and consistency of the cRED data by examination of the statistics obtained from the data processing software DIALS is presented. It is shown that, despite the high R1 values caused by dynamical scattering and other factors, the refined atomic positions obtained from the cRED data collected for different crystals are consistent with those of the reference models refined against single-crystal X-ray diffraction data. The results serve as a reference for the quality of the cRED data and the achievable accuracy of the structural parameters.

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