Three different Ge environments in a new Sr5CuGe9O24phase synthesized at high pressure and high temperature

Klein, Holger; Kodjikian, Stéphanie; Philippe, Rémy; Ding, Lei; Colin, Claire; Darie, Céline; Bordet, Pierre

doi:10.1107/s2052520620008914

Cited by 3 publications

(3 citation statements)

References 19 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The first compound, Sr 5 CuGe 9 O 24 , is not beam sensitive and a lowdose technique is not really necessary for diffraction experiments on this crystal. Its rather complex structure for an oxide with 22 independent atom positions [20] and good crystalline quality makes it a good test structure for our method in order to determine the minimal dose necessary for structure solution and refinement.…”

Section: Resultsmentioning

confidence: 99%

See 1 more Smart Citation

Low-Dose Electron Crystallography: Structure Solution and Refinement

et al. 2022

Self Cite

View full text Add to dashboard Cite

There is a wealth of materials that are beam sensitive and only exist in nanometric crystals, because the growth of bigger crystals is either impossible or so complicated that it is not reasonable to spend enough time and resources to grow big crystals before knowing their potential for research or applications. This difficulty is encountered in minerals, zeolites, metal-organic frameworks or molecular crystals, including pharmaceuticals and biological crystals. In order to study these crystals a structure determination method for beam sensitive crystals of nanometric size is needed. The nanometric size makes them destined for electron diffraction, since electrons interact much more strongly with matter than X-rays or neutrons. In addition, for the same amount of beam damage, electron diffraction yields more information than X-rays. The recently developed low-dose electron diffraction tomography (LD-EDT) not only combines the advantages inherent in electron diffraction, but is also optimized for minimizing the electron dose used for the data collection. The data quality is high, allowing not only the solution of complex unknown structures, but also their refinement taking into account the dynamical diffraction effects. Here we present several examples of crystals solved and refined by this method. The range of the crystals presented includes two synthetic oxides, Sr5CuGe9O24 and (Na2/3Mn1/3)3Ge5O12, a natural mineral (bulachite), and a metal organic framework (Mn-formiate). The dynamical refinement can be successfully performed on data sets that needed less than 0.1 e−/Å2 for the entire data set.

show abstract

Section: Resultsmentioning

confidence: 99%

“…Structure solution of Sr 5 CuGe 9 O 24 obtained by electron diffraction and comparison to the positions obtained by X-ray diffraction[20].…”

mentioning

confidence: 99%

Low-Dose Electron Crystallography: Structure Solution and Refinement

et al. 2022

Self Cite

View full text Add to dashboard Cite

show abstract

“…This data collection procedure is often referred to as precession or precession‐assisted electron diffraction tomography (PEDT; Boullay et al, 2013). The ED data collected in this way have a large reciprocal space coverage and have been successfully used for ab initio structure solution by direct methods with a fully kinematical approximation (Andrusenko et al, 2019; Jiang et al, 2011; Klein et al, 2020).…”

Section: Ed For the Structure Analysis Of Small‐molecule Organicsmentioning

confidence: 99%

3Delectron diffraction for structure determination of small‐molecule nanocrystals: A possible breakthrough for the pharmaceutical industry

Andrusenko

Gemmi

2022

WIREs Nanomed Nanobiotechnol

View full text Add to dashboard Cite

Nanomedicine is among the most fascinating areas of research. Most of the newly discovered pharmaceutical polymorphs, as well as many new synthesized or isolated natural products, appear only in form of nanocrystals. The development of techniques that allow investigating the atomic structure of nanocrystalline materials is therefore one of the most important frontiers of crystallography. Some unique features of electrons, like their non‐neutral charge and their strong interaction with matter, make this radiation suitable for imaging and detecting individual atoms, molecules, or nanoscale objects down to sub‐angstrom resolution. In the recent years the development of three‐dimensional (3D) electron diffraction (3D ED) has shown that electron diffraction can be successfully used to solve the crystal structure of nanocrystals and most of its limiting factors like dynamical scattering or limited completeness can be easily overcome. This article is a review of the state of the art of this method with a specific focus on how it can be applied to beam sensitive samples like small‐molecule organic nanocrystals. This article is categorized under: Therapeutic Approaches and Drug Discovery > Emerging Technologies

show abstract

Electron crystallography and dedicated electron-diffraction instrumentation

Simoncic¹,

Romeijn²,

Hovestreydt³

et al. 2023

Acta Crystallogr E Cryst Commun

View full text Add to dashboard Cite

Electron diffraction (known also as ED, 3D ED or microED) is gaining momentum in science and industry. The application of electron diffraction in performing nano-crystallography on crystals smaller than 1 µm is a disruptive technology that is opening up fascinating new perspectives for a wide variety of compounds required in the fields of chemical, pharmaceutical and advanced materials research. Electron diffraction enables the characterization of solid compounds complementary to neutron, powder X-ray and single-crystal X-ray diffraction, as it has the unique capability to measure nanometre-sized crystals. The recent introduction of dedicated instrumentation to perform ED experiments is a key aspect of the continued growth and success of this technology. In addition to the ultra-high-speed hybrid-pixel detectors enabling ED data collection in continuous rotation mode, a high-precision goniometer and horizontal layout have been determined as essential features of an electron diffractometer, both of which are embodied in the Eldico ED-1. Four examples of data collected on an Eldico ED-1 are showcased to demonstrate the potential and advantages of a dedicated electron diffractometer, covering selected applications and challenges of electron diffraction: (i) multiple reciprocal lattices, (ii) absolute structure of a chiral compound, and (iii) R-values achieved by kinematic refinement comparable to X-ray data.

show abstract

Three different Ge environments in a new Sr₅CuGe₉O₂₄phase synthesized at high pressure and high temperature

Cited by 3 publications

References 19 publications

Low-Dose Electron Crystallography: Structure Solution and Refinement

Low-Dose Electron Crystallography: Structure Solution and Refinement

3Delectron diffraction for structure determination of small‐molecule nanocrystals: A possible breakthrough for the pharmaceutical industry

Electron crystallography and dedicated electron-diffraction instrumentation

Contact Info

Product

Resources

About