Microplates for Crystal Growth and in situ Data Collection at a Synchrotron Beamline

An efficient data collection method is important for microcrystals, because microcrystals are sensitive to radiation damage. Moreover, microcrystals are difficult to harvest and locate owing to refraction effects from the surface of the liquid drop or optically invisible, owing to their small size. Collecting X-ray diffraction data directly from the crystallization devices to completely eliminate the crystal harvesting step is of particular interest. To address these needs, novel microplates combining crystal growth and data collection have been designed for efficient in situ data collection and fully tested at Shanghai Synchrotron Radiation Facility (SSRF) crystallography beamlines. The design of the novel microplates fully adapts the advantage of in situ technology. Thin Kapton membranes were selected to seal the microplate for crystal growth, the crystallization plates can support hanging drop and setting drop vapor diffusion crystallization experiments. Then, the microplate was fixed on a magnetic base and mounted on the goniometer head for in situ data collection. Automatic grid scanning was applied for crystal location with a Blu-Ice data collection system and then in situ data collection was performed. The microcrystals of lysozyme were selected as the testing samples for diffraction data collection using the novel microplates. The results show that this method can achieve comparable data quality to that of the traditional method using the nylon loop. In addition, our method can efficiently and diversely perform data acquisition experiments, and be especially suitable for solving structures of multiple crystals at room temperature or cryogenic temperature.

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Novel combined crystallization plate for high-throughput crystal screening and in situ data collection at a crystallography beamline

Acta Crystallographica Section F Structural Biology Communications ◽

10.1107/s2053230x21008104 ◽

2021 ◽

Vol 77 (9) ◽

pp. 319-327

Author(s):

Miao Liang ◽

Li Yu ◽

Zhijun Wang ◽

Huan Zhou ◽

Yi Zhang ◽

...

Keyword(s):

Data Collection ◽

High Throughput ◽

Diffraction Data ◽

Large Scale ◽

Liquid Drop ◽

In Situ Data ◽

Combined Crystallization ◽

Manual Manipulation ◽

Large Scale Screening

In situ microplates are small in size, crystal cultivation and operation are difficult, and the efficiency of crystal screening is relatively low. To solve this problem, a novel combined crystallization plate was designed for high-throughput crystal cultivation and in situ data collection. A frame was used to hold 48 in situ microplates, and the in situ microplates were sealed on one side with an ultralow background-scattering Kapton film. An automatic liquid handler (Mosquito) was used to add a liquid drop to the in situ microplates in the frame, and CrystalClear HD tape was used to seal the frame. A sealed frame holding 48 microplates was developed as a novel combined crystallization plate and was used for crystal cultivation under different conditions and in situ data collection at the synchrotron beamline. Moreover, individual microplates can be separated from the combined crystal plate and then fixed on a magnetic base or loaded onto a UniPuck for in situ data collection. Automatic grid scanning was used to locate crystals. The efficiency of the combined crystallization plate for crystal screening was verified. This method avoids the manual manipulation of crystals during crystal screening and diffraction data collection; therefore, the combined crystallization plate is suitable for large-scale screening of microcrystals.

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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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Transient phase fraction and dislocation density estimation from in-situ X-ray diffraction data with a low signal-to-noise ratio using a Bayesian approach to the Rietveld analysis

Materials Characterization ◽

10.1016/j.matchar.2020.110860 ◽

2020 ◽

pp. 110860

Author(s):

Manfred Wiessner ◽

Paul Angerer ◽

Sybrand van der Zwaag ◽

Ernst Gamsjäger

Keyword(s):

Dislocation Density ◽

Density Estimation ◽

Diffraction Data ◽

Signal To Noise Ratio ◽

Rietveld Analysis ◽

Transient Phase ◽

X Ray Diffraction ◽

Signal To Noise ◽

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

Molecules ◽

10.3390/molecules26133920 ◽

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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In situ X-ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)-based Metal-Organic Frameworks with UiO-66 and MIL-140 architectures

10.26434/chemrxiv.13252544 ◽

2020 ◽

Author(s):

Stephen Shearan ◽

Jannick Jacobsen ◽

Ferdinando Costantino ◽

Roberto D’Amato ◽

Dmitri Novikov ◽

...

Keyword(s):

Crystal Growth ◽

Metal Organic Frameworks ◽

Building Blocks ◽

Nucleation And Growth ◽

X Ray Diffraction ◽

X Ray ◽

Rate Determining Step ◽

Wide Range ◽

Metal Organic

We report on the results of a thorough in situ synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds in situ in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO3) and amount of the coordination modulator acetic acid (AcOH). When only HNO3 is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO3, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO3 slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO3 favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO3. Based on these in situ results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

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Iterative diffraction pattern retrieval from a single focal construct geometry image

Journal of Applied Crystallography ◽

10.1107/s1600576721009626 ◽

2021 ◽

Vol 54 (6) ◽

Author(s):

Xiao-Hui Chen ◽

Tao Xue ◽

Bo-Zhong Tan ◽

Xiao-Ya Li ◽

Jun Li

Keyword(s):

Crystal Structure ◽

Diffraction Pattern ◽

Diffraction Data ◽

Laser Energy ◽

Dynamic Compression ◽

Neutron Energy Spectrum ◽

X Ray Diffraction ◽

Successful Recovery ◽

Pattern Retrieval

Understanding the crystal structure of materials under extreme conditions of pressure and temperature has been revolutionized by major advances in laser-driven dynamic compression and in situ X-ray diffraction (XRD) technology. Instead of the well known Debye–Scherrer configuration, the focal construct geometry (FCG) was introduced to produce high-intensity diffraction data from laser-based in situ XRD experiments without increasing the amount of laser energy, but the resulting reflections suffered from profoundly asymmetrical broadening, leading to inaccuracy in determination of the crystal structure. Inspired by fast-neutron energy spectrum measurements, proposed here is an iterative retrieval method for recovering diffraction data from a single FCG image. This iterative algorithm restores both the peak shape and relative intensity with rapid convergence and requires no prior knowledge about the expected diffraction pattern, allowing the FCG to increase the in situ XRD intensity while simultaneously preserving the angular resolution. The feasibility and validity of the method are shown by successful recovery of the diffraction pattern from both a single simulated FCG image and a single laser-based nanosecond XRD measurement.

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