In situX-ray crystallography

2000 ◽  
Vol 33 (2) ◽  
pp. 397-400 ◽  
Author(s):  
Alexander McPherson
Keyword(s):  
Data Collection ◽  
Single Crystals ◽  
Room Temperature ◽  
Automated Data Collection ◽  
Vapor Diffusion ◽  
X Ray

A method is proposed, and preliminary experiments are described, for collection of X-ray data from macromolecular crystalsin situ. The usual processes of mounting for either room-temperature or cryogenic X-ray data collection are eliminated by growing crystals, using vapor diffusion, on small supports or films that can be either frozen or treated before transfer directly to the X-ray beam. The approach has the advantage that individual crystals are never manipulated and it is not necessary to isolate single crystals. Furthermore, crystals fixed to the surface on which they grow provides a positive advantage, small and otherwise problematic crystals become serviceable, and robotic or automated data collection becomes simplified.

Texture Evolution of Magnesium Single Crystals Deformed by High-Pressure Torsion

2008 ◽  
Vol 584-586 ◽  
pp. 263-268 ◽  
Author(s):  
Bartlomiej J. Bonarski ◽  
Erhard Schafler ◽  
Borys Mikułowski ◽  
Michael Zehetbauer
Keyword(s):  
High Pressure ◽  
Single Crystals ◽  
Room Temperature ◽  
High Pressure Torsion ◽  
Texture Evolution ◽  
In Situ Stress ◽  
Higher Symmetry ◽  
Strain Measurements ◽  
X Ray

Single crystals of technical purity Magnesium (99.8 wt.%) of initial orientations [ ] 2 1 10 and [ ] 2 2 11 were subjected to HPT deformation at room temperature up to strains of 10. The microstructural evolution has been analyzed by X-ray microtexture investigations and by in-situ stress-strain measurements. The results can be described in terms of shear arising from HPT deformation and - with higher strains - in terms of recrystallization. In crystals with hard orientation[ ] 2 2 11 , these features occur at smaller strains than in crystals with soft orientation [ ] 2 1 10 , i.e. with higher symmetry. In general, the observed textures and strength variations are much stronger than those reported for fcc HPT deformed metals.

scholarly journals Attaining atomic resolution from in situ data collection at room temperature using counter-diffusion-based low-cost microchips

2020 ◽  
Vol 76 (8) ◽  
pp. 751-758
Author(s):  
Jose A. Gavira ◽  
Isaac Rodriguez-Ruiz ◽  
Sergio Martinez-Rodriguez ◽  
Shibom Basu ◽  
Sébastien Teychené ◽  
...  
Keyword(s):  
Data Collection ◽  
Diffraction Data ◽  
Room Temperature ◽  
Low Cost ◽  
Atomic Resolution ◽  
Microfluidic Channels ◽  
High Symmetry ◽  
X Ray ◽  
Counter Diffusion

Sample handling and manipulation for cryoprotection currently remain critical factors in X-ray structural determination. While several microchips for macromolecular crystallization have been proposed during the last two decades to partially overcome crystal-manipulation issues, increased background noise originating from the scattering of chip-fabrication materials has so far limited the attainable resolution of diffraction data. Here, the conception and use of low-cost, X-ray-transparent microchips for in situ crystallization and direct data collection, and structure determination at atomic resolution close to 1.0 Å, is presented. The chips are fabricated by a combination of either OSTEMER and Kapton or OSTEMER and Mylar materials for the implementation of counter-diffusion crystallization experiments. Both materials produce a sufficiently low scattering background to permit atomic resolution diffraction data collection at room temperature and the generation of 3D structural models of the tested model proteins lysozyme, thaumatin and glucose isomerase. Although the high symmetry of the three model protein crystals produced almost complete data sets at high resolution, the potential of in-line data merging and scaling of the multiple crystals grown along the microfluidic channels is also presented and discussed.

scholarly journals An automated platform for in situ serial crystallography at room temperature

IUCrJ ◽  
2020 ◽  
Vol 7 (6) ◽  
pp. 1009-1018
Author(s):  
Zhong Ren ◽  
Cong Wang ◽  
Heewhan Shin ◽  
Sepalika Bandara ◽  
Indika Kumarapperuma ◽  
...  
Keyword(s):  
Data Collection ◽  
Room Temperature ◽  
Protein Structures ◽  
Routine Data ◽  
Protein Crystals ◽  
X Ray Diffraction ◽  
X Ray ◽  
Serial Crystallography ◽  
Routine Data Collection

Direct observation of functional motions in protein structures is highly desirable for understanding how these nanomachineries of life operate at the molecular level. Because cryogenic temperatures are non-physiological and may prohibit or even alter protein structural dynamics, it is necessary to develop robust X-ray diffraction methods that enable routine data collection at room temperature. We recently reported a crystal-on-crystal device to facilitate in situ diffraction of protein crystals at room temperature devoid of any sample manipulation. Here an automated serial crystallography platform based on this crystal-on-crystal technology is presented. A hardware and software prototype has been implemented, and protocols have been established that allow users to image, recognize and rank hundreds to thousands of protein crystals grown on a chip in optical scanning mode prior to serial introduction of these crystals to an X-ray beam in a programmable and high-throughput manner. This platform has been tested extensively using fragile protein crystals. We demonstrate that with affordable sample consumption, this in situ serial crystallography technology could give rise to room-temperature protein structures of higher resolution and superior map quality for those protein crystals that encounter difficulties during freezing. This serial data collection platform is compatible with both monochromatic oscillation and Laue methods for X-ray diffraction and presents a widely applicable approach for static and dynamic crystallographic studies at room temperature.

scholarly journals High-throughput in situ X-ray screening of and data collection from protein crystals at room temperature and under cryogenic conditions

2018 ◽  
Vol 13 (2) ◽  
pp. 260-292 ◽  
Author(s):  
Jana Broecker ◽  
Takefumi Morizumi ◽  
Wei-Lin Ou ◽  
Viviane Klingel ◽  
Anling Kuo ◽  
...  
Keyword(s):  
Data Collection ◽  
High Throughput ◽  
Room Temperature ◽  
Protein Crystals ◽  
X Ray ◽  
Cryogenic Conditions

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.

Effect of trytophan as dopant on potassium acid phthalate single crystals

2019 ◽  
Author(s):  
Chem Int
Keyword(s):  
Single Crystals ◽  
Room Temperature ◽  
Visible Region ◽  
X Ray Diffraction ◽  
X Ray ◽  
Slow Evaporation Technique ◽  
Absorption Studies ◽  
Evaporation Technique ◽  
Potassium Acid Phthalate ◽  
Acid Phthalate

Optically transparent single crystals of potassium acid phthalate (KAP, 0.5 g) 0.05 g and 0.1 g (1 and 2 mol %) trytophan were grown in aqueous solution by slow evaporation technique at room temperature. Single crystal X- ray diffraction analysis confirmed the changes in the lattice parameters of the doped crystals. The presence of functional groups in the crystal lattice has been determined qualitatively by FTIR analysis. Optical absorption studies revealed that the doped crystals possess very low absorption in the entire visible region. The dielectric constant has been studied as a function of frequency for the doped crystals. The thermal stability was evaluated by TG-DSC analysis.

Evolution of Pore Ordering during Anodizing of Aluminum Single Crystals: In Situ Small-Angle X-ray Scattering Study

2021 ◽  
Author(s):  
Ilya V. Roslyakov ◽  
Andrei P. Chumakov ◽  
Andrei A. Eliseev ◽  
Alexey P. Leontiev ◽  
Oleg V. Konovalov ◽  
...  
Keyword(s):  
Single Crystals ◽  
Small Angle ◽  
X Ray ◽  
X Ray Scattering ◽  
Scattering Study ◽  
Ray Scattering

Photoluminescence Enhancement of CdS Nanocrystals Fabricated on Dithiocarbamate Functionalized PET Substrates

2012 ◽  
Vol 512-515 ◽  
pp. 1511-1515
Author(s):  
Chun Lin Zhao ◽  
Li Xing ◽  
Xiao Hong Liang ◽  
Jun Hui Xiang ◽  
Fu Shi Zhang ◽  
...  
Keyword(s):  
Room Temperature ◽  
Hexagonal Structure ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Visible Absorption ◽  
X Ray ◽  
Cds Nanocrystals ◽  
Morphological Studies ◽  
Transmission Electron

Cadmium sulfide (CdS) nanocrystals (NCs) were self-assembled and in-situ immobilized on the dithiocarbamate (DTCs)-functionalized polyethylene glycol terephthalate (PET) substrates between the organic (carbon disulfide diffused in n-hexane) –aqueous (ethylenediamine and Cd2+ dissolved in water) interface at room temperature. Powder X-ray diffraction measurement revealed the hexagonal structure of CdS nanocrystals. Morphological studies performed by scanning electron microscopy (SEM) and high-resolution transmission electron microscope (HRTEM) showed the island-like structure of CdS nanocrystals on PET substrates, as well as energy-dispersive X-ray spectroscopy (EDS) confirmed the stoichiometries of CdS nanocrystals. The optical properties of DTCs modified CdS nanocrystals were thoroughly investigated by ultraviolet-visible absorption spectroscopy (UV-vis) and fluorescence spectroscopy. The as-prepared DTCs present intrinsic hydrophobicity and strong affinity for CdS nanocrystals.

In Situ Synchrotron X-Ray Diffraction Study of a Deformed Cu-Fe-P Alloy during Heating

2016 ◽  
Vol 850 ◽  
pp. 191-196 ◽  
Author(s):  
Wei Wang ◽  
Cun Lei Zou ◽  
Ren Geng Li ◽  
Wen Wen ◽  
Hui Jun Kang ◽  
...  
Keyword(s):  
Room Temperature ◽  
Lattice Distortion ◽  
Copper Matrix ◽  
Heating Process ◽  
Recrystallization Process ◽  
Full Width ◽  
X Ray Diffraction ◽  
Dramatic Decrease ◽  
X Ray

In situ synchrotron X-ray diffraction was used to study a deformed Cu-0.88 Fe-0.24 P alloy during heating process. The measurements were performed at room temperature and also at high temperatures up to 893 K in order to determine the recovery, ageing and recrystallization process. With the increase of temperature, the angles of copper matrix peaks moved left and the FWHM (full width at half maximum) decreased slightly. Fe3P precipitates were first detected at 533 K, reached the maximum at 673 K, and re-dissolved into matrix at 853 K. A dramatic decrease in FWHM was observed accompanied by the precipitation of Fe3P phases, indicating the reduction of lattice distortion of copper matrix.

scholarly journals Insertion of Phosphenium Ions into a Bicyclo[1.1.0]Tetraphosphabutane Iron Complex

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3920
Author(s):  
Martin Weber ◽  
Gábor Balázs ◽  
Alexander V. Virovets ◽  
Eugenia Peresypkina ◽  
Manfred Scheer
Keyword(s):  
Diffraction Analysis ◽  
Room Temperature ◽  
31P Nmr ◽  
Spectroscopic Studies ◽  
Iron Complex ◽  
The Novel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Phosphenium Ions

By reacting [{Cp‴Fe(CO)2}2(µ,η1:1-P4)] (1) with in situ generated phosphenium ions [Ph2P][A] ([A]− = [OTf]− = [O3SCF3]−, [PF6]−), a mixture of two main products of the composition [{Cp‴Fe(CO)2}2(µ,η1:1-P5(C6H5)2)][PF6] (2a and 3a) could be identified by extensive 31P NMR spectroscopic studies at 193 K. Compound 3a was also characterized by X-ray diffraction analysis, showing the rarely observed bicyclo[2.1.0]pentaphosphapentane unit. At room temperature, the novel compound [{Cp‴Fe}(µ,η4:1-P5Ph2){Cp‴(CO)2Fe}][PF6] (4) is formed by decarbonylation. Reacting 1 with in situ generated diphenyl arsenium ions gives short-lived intermediates at 193 K which disproportionate at room temperature into tetraphenyldiarsine and [{Cp‴Fe(CO)2}4(µ4,η1:1:1:1-P8)][OTf]2 (5) containing a tetracyclo[3.3.0.02,7.03,6]octaphosphaoctane ligand.

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