Three-dimensional electron diffraction: a powerful structural characterization technique for crystal engineering

Samperisi, Laura; Zou, Xiaodong; Huang, Zhehao

doi:10.1039/d2ce00051b

Cited by 8 publications

(3 citation statements)

References 110 publications

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“…In this regard, high-resolution powder X-ray diffraction (PXRD) becomes very important as a method of structural determination of breathing MOFs [29][30][31]. Since the quality of data, available on laboratory powder diffractometers, often appears to be not enough for the direct structure solution, in the most difficult cases this method is appended by theoretical modeling, DFT computations, electron diffraction [32][33][34][35], or other advanced techniques which allow finding an initial structural model to be further refined for polycrystalline samples on the basis of PXRD data. However, even if PXRD structure refinement is impossible or unnecessary, the qualitative analysis of powder data represents an easy and express method for the observation of breathing behavior and elucidation of the driving factors, such as solvent, temperature, and pressure.…”

Section: Breathing Of Glutaratesmentioning

confidence: 99%

Properties of Aliphatic Ligand-Based Metal–Organic Frameworks

Demakov

2023

Polymers

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Ligands with a purely aliphatic backbone are receiving rising attention in the chemistry of coordination polymers and metal–organic frameworks. Such unique features inherent to the aliphatic bridges as increased conformational freedom, non-polarizable core, and low light absorption provide rare and valuable properties for their derived MOFs. Applications of such compounds in stimuli–responsive materials, gas, and vapor adsorbents with high and unusual selectivity, light-emitting, and optical materials have extensively emerged in recent years. These properties, as well as other specific features of aliphatic-based metal–organic frameworks are summarized and analyzed in this short critical review. Advanced characterization techniques, which have been applied in the reported works to obtain important data on the crystal and molecular structures, dynamics, and functionalities, are also reviewed within a general discussion. In total, 132 references are included.

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Section: Breathing Of Glutaratesmentioning

confidence: 99%

Properties of Aliphatic Ligand-Based Metal–Organic Frameworks

Demakov

2023

Polymers

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“…To address this, emerging techniques like precession electron diffraction (PED) [17,18], automated diffraction tomography (ADT) [19], rotation electron diffraction (RED) [20], continuous rotation electron diffraction (cRED), and serial rotation electron diffraction (SerialRED) [21] aim to reduce the dynamic effects on observed intensities. Several reviews describe these 3D ED methods and their recent evolutions [21][22][23][24][25][26][27]. These methods have proved highly effective in resolving the structures of many zeolites.…”

Section: Introductionmentioning

confidence: 99%

Determination of Na+ Cation Locations in Nanozeolite ECR-1 Using a 3D ED Method

Örs,

Deroche,

Chatelard

et al. 2024

Symmetry

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Until now, the comprehensive structural analysis of single crystals of zeolite ECR-1, an aluminosilicate with the EON topology, has been hindered owing to the submicron dimensions of the obtained crystals. Additionally, this zeolite, which is characterized by a topology comprising alternating periodic building units of MAZ and MOR layers, exhibits stacking faults that impede accurate refinement through the Rietveld method. In this report, we present, for the first time, the structure of ECR-1 elucidated by studying a nanocrystal with a significantly reduced number of stacking faults. The sample used was synthesized hydrothermally using trioxane as the organic structure-directing agent. The structure determination was conducted using precession electron diffraction (PED) at 103 K. Partial dehydration occurred owing to the high vacuum conditions in the TEM sample chamber. From the dynamical refinement (Robs = 0.097), 8.16 Na+ compensating cations were localized on six distinct crystallographic sites, along with approximately four water molecules per unit cell. Furthermore, a canonical Monte Carlo computational study was conducted to compare the experimental cationic distribution and location of water molecules with the simulation.

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“…Compared to single-crystal X-ray diffraction (SC-XRD), 3D-ED has advantages for studying small-sized crystals [8,9] (<5 × 5 × 5 µm 3 ) and polyphasic mixtures [10]. In recent years, with the rapid development of 3D-ED technology, researchers have developed a variety of data collection methods [11], such as automated diffraction tomography (ADT) [5], rotation electron diffraction (RED) [12], precession-assisted electron diffraction tomography (PEDT) [13], continuous rotation electron diffraction (cRED) [14], electron diffraction tomography (EDT) [15], fast electron diffraction tomography (fast-EDT) [16], fast automated diffraction tomography (fast-ADT) [17], low-dose electron diffraction tomography (LD-EDT) [18], and microcrystal electron diffraction (MicroED) [19]. These collection methods are similar in concept, where a series of electron diffraction patterns are recorded from a crystal tilted around the goniometer axis.…”

Section: Introductionmentioning

confidence: 99%

The Application of 3D-ED to Distinguish the Superstructure of Sr1.2Ca0.8Nb2O7 Ignored in SC-XRD

Mei

Zhang

et al. 2023

Crystals

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Compared to X-rays, electrons have stronger interactions with matter. In electron diffraction, the low-order structure factors are sensitive to subtle changes in the arrangement of valence electrons around atoms when the scattering vector is smaller than the critical scattering vector. Therefore, electron diffraction is more advantageous for studying the distribution of atoms in the structure with atomic numbers smaller than that of sulfur. In this work, the crystal structure of Sr1.2Ca0.8Nb2O7 (SCNO-0.8) was analyzed using single-crystal X-ray diffraction (SC-XRD) and three-dimensional electron diffraction (3D-ED) techniques, respectively. Interestingly, the superstructure could only be identified by the 3D-ED technique, while no signal corresponding to the superstructure was detected from the SC-XRD data. The superstructure in SCNO-0.8 was disclosed to be caused by different tilting of NbO6 octahedra and the displacements of Sr/Ca atoms in the different atomic layers perpendicular to the a-axis. Therefore, the application of 3D-ED provides an effective method for studying superstructures caused by ordered arrangements of light atoms.

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Three-dimensional electron diffraction: a powerful structural characterization technique for crystal engineering

Abstract: Understanding crystal structures and behaviors is crucial for constructing and engineering crystalline materials with various properties and functions. Recent advancement in three-dimensional electron diffraction (3D ED) and its application on...

Cited by 8 publications

References 110 publications

Properties of Aliphatic Ligand-Based Metal–Organic Frameworks

Properties of Aliphatic Ligand-Based Metal–Organic Frameworks

Determination of Na+ Cation Locations in Nanozeolite ECR-1 Using a 3D ED Method

The Application of 3D-ED to Distinguish the Superstructure of Sr1.2Ca0.8Nb2O7 Ignored in SC-XRD

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