Cryocrystallography in capillaries: critical glycerol concentrations and cooling rates

Capillary tubes have many advantages over multi-well plates for macromolecular crystal growth and handling, including the possibility ofin situstructure determination. To obtain complete high-resolution X-ray data sets, cryopreservation protocols must be developed to prevent crystalline ice formation and preserve macromolecular crystal order. The minimum glycerol concentrations required to vitrify aqueous solutions during plunging into liquid nitrogen and liquid propane have been determined for capillary diameters from 3.3 mm to 150 µm. For the smallest diameter, the required glycerol concentrations are 30%(w/v) in nitrogen and 20%(w/v) in propane, corresponding to cooling rates of ∼800 and ∼7000 K s−1, respectively. These concentrations are much larger than are required in current best practice using crystals in loops or on microfabricated mounts. In additon, the relation between the minimum cooling rate for vitrification and glycerol concentration has been estimated; this relation is of fundamental importance in developing rational cryopreservation protocols.

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High resolution in-situ interferometric studies of lysozyme crystal growth morphology and kinetics

10.2514/6.1995-3579 ◽

1995 ◽

Author(s):

Peter Vekilov ◽

Franz Rosenberger

Keyword(s):

Crystal Growth ◽

High Resolution ◽

Growth Morphology ◽

Lysozyme Crystal

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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

10.26434/chemrxiv.11345063.v2 ◽

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.

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Texture Evolution Under Fast Heating and Cooling Rates of Zirconium Alloys Studied In-Situ by Synchrotron X-Ray Diffraction

SSRN Electronic Journal ◽

10.2139/ssrn.3680386 ◽

2020 ◽

Author(s):

Chi-Toan Nguyen ◽

Alistair Garner ◽

Javier Romero ◽

Antoine Ambard ◽

Michael Preuss ◽

...

Keyword(s):

Texture Evolution ◽

Zirconium Alloys ◽

X Ray Diffraction ◽

Fast Heating ◽

Cooling Rates ◽

X Ray ◽

Heating And Cooling

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Insights into Microscopic Crystal Growth Dynamics of CH3NH3PbI3 under a Laser Deposition Process Revealed by In Situ X-ray Diffraction

ACS Applied Materials & Interfaces ◽

10.1021/acsami.1c04488 ◽

2021 ◽

Author(s):

Tetsuhiko Miyadera ◽

Yuto Auchi ◽

Kohei Yamamoto ◽

Noboru Ohashi ◽

Tomoyuki Koganezawa ◽

...

Keyword(s):

Crystal Growth ◽

Growth Dynamics ◽

Deposition Process ◽

Laser Deposition ◽

X Ray Diffraction ◽

X Ray

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Dynamic observation of dislocation evolution and interaction with twin boundaries in silicon crystal growth using in – situ synchrotron X-ray diffraction imaging

Acta Materialia ◽

10.1016/j.actamat.2021.116819 ◽

2021 ◽

Vol 210 ◽

pp. 116819

Author(s):

M.G. Tsoutsouva ◽

G. Regula ◽

B. Ryningen ◽

P.E. Vullum ◽

N. Mangelinck-Noël ◽

...

Keyword(s):

Crystal Growth ◽

Silicon Crystal ◽

X Ray Diffraction ◽

Twin Boundaries ◽

X Ray ◽

Dynamic Observation ◽

Diffraction Imaging

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In-situ diffraction experiments at the Photon Factory MX beamlines

Acta Crystallographica Section A Foundations and Advances ◽

10.1107/s2053273314094996 ◽

2014 ◽

Vol 70 (a1) ◽

pp. C500-C500

Author(s):

Yusuke Yamada ◽

Naohiro Matsugaki ◽

Masahiko Hiraki ◽

Ryuichi Kato ◽

Toshiya Senda

Keyword(s):

Gas Flow ◽

Active Area ◽

Array Detector ◽

Data Sets ◽

Diffraction Experiment ◽

X Ray ◽

Photon Factory ◽

Large Active Area ◽

In Situ Diffraction

Crystallization trial is one of the most important but time-consuming steps in macromolecular crystallography. Once a crystal appears in a certain crystallization condition, the crystal is typically harvested from the crystallization drop, soaked into a cryoprotection buffer, flash-cooled with a liquid nitrogen or cold gas flow and finally evaluated its diffraction quality by an X-ray beam. During these long process, crystal may be damaged and the result from the diffraction experiment does not necessarily reflect a nature of the crystal. On in-situ diffraction experiment, where a crystal in a crystallization drop is directly irradiated to an X-ray beam, a diffraction image from a crystal without any external factors such as harvesting and cryoprotection and, as a result, a nature of crystal can be evaluated quickly. In the Photon Factory, a new table-top diffractometer for in-situ diffraction experiments has been developed. It consists of XYZ translation stages with a plate handler, on-axis viewing system with a large numeric aperture and a plate rack where ten crystallization plates can be placed. These components sit on a common plate and it is placed on the existing diffractometer table in the beamline endstation. The CCD detector with a large active area and a pixel array detector with a small active area are used for acquiring diffraction images from crystals. Dedicated control software and user interface were also developed. Since 2014, user operation of the new diffractometer was started and in-situ diffraction experiments were mainly performed for evaluations of crystallization plates from a large crystallization screening project in our facility. BL-17A [1], one of micro-focus beamlines at the Photon Factory, is planned to be upgraded in March 2015. With this upgrade, a new diffractometer, which has a capability to handle a crystallization plate, will be installed so that diffraction data sets from crystals in crystallization drop can be collected.

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Applications of High-Resolution Powder X-Ray Diffraction

Solid State Phenomena ◽

10.4028/www.scientific.net/ssp.130.7 ◽

2007 ◽

Vol 130 ◽

pp. 7-14 ◽

Cited By ~ 4

Author(s):

Andrew N. Fitch

Keyword(s):

High Resolution ◽

Synchrotron Radiation ◽

Powder Diffraction ◽

X Rays ◽

X Ray Diffraction ◽

Crystalline Materials ◽

X Ray ◽

Structural Characterisation ◽

Pdf Analysis

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.

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