ALBERT

All Library Books, journals and Electronic Records Telegrafenberg

X
feed icon rss

Your email was sent successfully. Check your inbox.

An error occurred while sending the email. Please try again.

Proceed reservation?

Export
Filter
  • American Meteorological Society (AMS)
  • International Union of Crystallography
  • Irkutsk : Ross. Akad. Nauk, Sibirskoe Otd., Inst. Zemnoj Kory
  • Krefeld : Geologischer Dienst Nordhein-Westfalen
Collection
Keywords
Publisher
Language
Years
  • 1
    facet.materialart.
    Unknown
    INSIGHT: in situ heuristic tool for the efficient reduction of grazing‐incidence X‐ray scattering data (2024)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-04-25
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉〈italic〉INSIGHT〈/italic〉 is a Python‐based software tool for processing and reducing 2D grazing‐incidence wide‐ and small‐angle X‐ray scattering (GIWAXS/GISAXS) data. It offers the geometric transformation of the 2D GIWAXS/GISAXS detector image to reciprocal space, including vectorized and parallelized pixel‐wise intensity correction calculations. An explicit focus on efficient data management and batch processing enables full control of large time‐resolved synchrotron and laboratory data sets for a detailed analysis of kinetic GIWAXS/GISAXS studies of thin films. It processes data acquired with arbitrarily rotated detectors and performs vertical, horizontal, azimuthal and radial cuts in reciprocal space. It further allows crystallographic indexing and GIWAXS pattern simulation, and provides various plotting and export functionalities. Customized scripting offers a one‐step solution to reduce, process, analyze and export findings of large 〈italic〉in situ〈/italic〉 and 〈italic〉operando〈/italic〉 data sets.〈/p〉
    Keywords: ddc:548 ; grazing‐incidence X‐ray scattering ; time‐resolved studies ; in situ studies ; operando studies ; computer programs
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 2
    facet.materialart.
    Unknown
    Energy‐dispersive X‐ray stress analysis under geometric constraints: exploiting the material's inherent anisotropy (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-09-12
    Description: Two data evaluation concepts for X‐ray stress analysis based on energy‐dispersive diffraction on polycrystalline materials with cubic crystal structure, almost random crystallographic texture and strong single‐crystal elastic anisotropy are subjected to comparative assessment. The aim is the study of the residual stress state in hard‐to‐reach measurement points, for which the sin2ψ method is not applicable due to beam shadowing at larger sample tilting. This makes the approaches attractive for stress analysis in engineering parts with complex shapes, for example. Both approaches are based on the assumption of a biaxial stress state within the irradiated sample volume. They exploit in different ways the elastic anisotropy of individual crystallites acting at the microscopic scale and the anisotropy imposed on the material by the near‐surface stress state at the macroscopic scale. They therefore complement each other, in terms of both their preconditions and their results. The first approach is based on the evaluation of strain differences, which makes it less sensitive to variations in the strain‐free lattice parameter a0. Since it assumes a homogeneous stress state within the irradiated sample volume, it provides an average value of the in‐plane stresses. The second approach exploits the sensitivity of the lattice strain to changes in a0. Consequently, it assumes a homogeneous chemical composition but provides a stress profile within the information depth. Experimental examples from different fields in materials science, namely shot peening of austenitic steel and in situ stress analysis during welding, are presented to demonstrate the suitability of the proposed methods.
    Description: The single‐crystal elastic anisotropy and the anisotropy of the near‐surface (residual) stress state of polycrystalline materials with random texture are exploited in energy‐dispersive X‐ray stress analysis to study samples under constrained measurement conditions.
    Keywords: ddc:548 ; X‐ray stress analysis ; energy‐dispersive diffraction ; polycrystalline materials ; single‐crystal elastic anisotropy
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 3
    facet.materialart.
    Unknown
    Mapping the 3D position of battery cathode particles in Bragg coherent diffractive imaging (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-12-14
    Description: In Bragg coherent diffractive imaging, the precise location of the measured crystals in the interior of the sample is usually missing. Obtaining this information would help the study of the spatially dependent behavior of particles in the bulk of inhomogeneous samples, such as extra‐thick battery cathodes. This work presents an approach to determine the 3D position of particles by precisely aligning them at the instrument axis of rotation. In the test experiment reported here, with a 60 µm‐thick LiNi0.5Mn1.5O4 battery cathode, the particles were located with a precision of 20 µm in the out‐of‐plane direction, and the in‐plane coordinates were determined with a precision of 1 µm.
    Description: A method to determine the 3D position of particles in Bragg coherent diffractive imaging experiments is proposed. Test measurements demonstrate depth‐resolution with a precision of 20 µm along the beam. image
    Keywords: ddc:548 ; extra‐thick battery cathodes ; Bragg coherent X‐ray diffractive imaging ; battery cathodes ; Bragg diffraction ; sphere of confusion ; 3D mapping
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 4
    facet.materialart.
    Unknown
    The soft X‐ray and XUV split‐and‐delay unit at beamlines FL23/24 at FLASH2 (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-01-12
    Description: A split‐and‐delay unit for the extreme ultraviolet and soft X‐ray spectral regions has been built which enables time‐resolved experiments at beamlines FL23 and FL24 at the Free‐electron LASer in Hamburg (FLASH). Geometric wavefront splitting at a sharp edge of a beam splitting mirror is applied to split the incoming soft X‐ray pulse into two beams. Ni and Pt coatings at grazing incidence angles have been chosen in order to cover the whole spectral range of FLASH2 and beyond, up to hν = 1800 eV. In the variable beam path with a grazing incidence angle of ϑd = 1.8°, the total transmission (T) ranges are of the order of 0.48 〈 T 〈 0.84 for hν 〈 100 eV and T 〉 0.50 for 100 eV 〈 hν 〈 650 eV with the Ni coating, and T 〉 0.06 for hν 〈 1800 eV for the Pt coating. For a fixed beam path with a grazing incidence angle of ϑf = 1.3°, a transmission of T 〉 0.61 with the Ni coating and T 〉 0.23 with a Pt coating is achieved. Soft X‐ray pump/soft X‐ray probe experiments are possible within a delay range of −5 ps 〈 Δt 〈 +18 ps with a nominal time resolution of tr = 66 as and a measured timing jitter of tj = 121 ± 2 as. First experiments with the split‐and‐delay unit determined the averaged coherence time of FLASH2 to be τc = 1.75 fs at λ = 8 nm, measured at a purposely reduced coherence of the free‐electron laser.
    Description: The properties of the recently installed split‐and‐delay unit at beamlines FL23 and FL24 at FLASH2 are presented. Its operational range, performance parameters and results of a first experiment are described. image
    Keywords: ddc:550.724 ; time‐resolved pump–probe ; XUV ; soft X‐rays ; free‐electron laser
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 5
    facet.materialart.
    Unknown
    XDSGUI: a graphical user interface for XDS, SHELX and ARCIMBOLDO (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-01-12
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉〈italic〉XDSGUI〈/italic〉 is a lightweight graphical user interface (GUI) for the 〈italic〉XDS〈/italic〉, 〈italic〉SHELX〈/italic〉 and 〈italic〉ARCIMBOLDO〈/italic〉 program packages that serves both novice and experienced users in obtaining optimal processing and phasing results for X‐ray, neutron and electron diffraction data. The design of the program enables data processing and phasing without command line usage, and supports advanced command flows in a simple user‐modifiable and user‐extensible way. The GUI supplies graphical information based on the tabular log output of the programs, which is more intuitive, comprehensible and efficient than text output can be.〈/p〉
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉A customizable stateless graphical user interface simplifies the processing, analysis and phasing of diffraction data.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005767:jcr2yr5110:jcr2yr5110-fig-0001"〉 〈alt-text〉image〈/alt-text〉 〈/graphic〉〈/boxed-text〉〈/p〉
    Keywords: ddc:548 ; X‐ray diffraction ; neutron diffraction ; electron diffraction ; data processing ; graphical user interfaces ; phasing ; XDS ; ARCIMBOLDO ; SHELX
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 6
    facet.materialart.
    Unknown
    Use of electron backscatter diffraction patterns to determine the crystal lattice. Part 3. Pseudosymmetry (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-20
    Description: A pseudosymmetric description of the crystal lattice derived from a single wide‐angle Kikuchi pattern can have several causes. The small size (〈15%) of the sector covered by an electron backscatter diffraction pattern, the limited precision of the projection centre position and the Kikuchi band definition are crucial. Inherent pseudosymmetries of the crystal lattice and/or structure also pose a challenge in the analysis of Kikuchi patterns. To eliminate experimental errors as much as possible, simulated Kikuchi patterns of 350 phases have been analysed using the software CALM [Nolze et al. (2021). J. Appl. Cryst.54, 1012–1022] in order to estimate the frequency of and reasons for pseudosymmetric crystal lattice descriptions. Misinterpretations occur in particular when the atomic scattering factors of non‐equivalent positions are too similar and reciprocal‐lattice points are systematically missing. As an example, a pseudosymmetry prediction depending on the elements involved is discussed for binary AB compounds with B1 and B2 structure types. However, since this is impossible for more complicated phases, this approach cannot be directly applied to compounds of arbitrary composition and structure.
    Description: Distinguishing between actual and apparent pseudosymmetry in electron backscatter diffraction patterns is nearly impossible, even for simulated patterns. However, the resulting lattice is always a superlattice as long as the signal is not a superposition of multiple patterns.
    Keywords: ddc:548 ; Bravais lattices ; pseudosymmetry ; lattice point density ; ordered/disordered structures ; lattice distortion ; electron backscatter diffraction ; backscattered Kikuchi diffraction patterns ; lattice parameters ; Funk transform
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 7
    facet.materialart.
    Unknown
    Crystal diffraction prediction and partiality estimation using Gaussian basis functions (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-04
    Description: The recent diversification of macromolecular crystallographic experiments including the use of pink beams, convergent electron diffraction and serial snapshot crystallography has shown the limitations of using the Laue equations for diffraction prediction. This article gives a computationally efficient way of calculating approximate crystal diffraction patterns given varying distributions of the incoming beam, crystal shapes and other potentially hidden parameters. This approach models each pixel of a diffraction pattern and improves data processing of integrated peak intensities by enabling the correction of partially recorded reflections. The fundamental idea is to express the distributions as weighted sums of Gaussian functions. The approach is demonstrated on serial femtosecond crystallography data sets, showing a significant decrease in the required number of patterns to refine a structure to a given error.
    Description: Reflection position, size and shape prediction and partiality estimation of crystal diffraction by integrating using a Gaussian basis are described.
    Keywords: ddc:548 ; partiality estimation ; diffraction prediction ; merging ; serial snapshot crystallography
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 8
    facet.materialart.
    Unknown
    Use of electron backscatter diffraction patterns to determine the crystal lattice. Part 2. Offset corrections (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-21
    Description: A band width determination using the first derivative of the band profile systematically underestimates the true Bragg angle. Corrections are proposed to compensate for the resulting offset Δa/a of the mean lattice parameters derived from as many Kikuchi band widths as possible. For dynamically simulated Kikuchi patterns, Δa/a can reach up to 8% for phases with a high mean atomic number Z, whereas for much more common low‐Z materials the offset decreases linearly. A predicted offset Δa/a = f(Z) is therefore proposed, which also includes the unit‐cell volume and thus takes into account the packing density of the scatterers in the material. Since Z is not always available for unknown phases, its substitution by Zmax, i.e. the atomic number of the heaviest element in the compound, is still acceptable for an approximate correction. For simulated Kikuchi patterns the offset‐corrected lattice parameter deviation is Δa/a 〈 1.5%. The lattice parameter ratios, and the angles α, β and γ between the basis vectors, are not affected at all.
    Description: Automatically determined band widths in simulated backscatter Kikuchi patterns exhibit differences from the double Bragg angles that correlate with the scatterer density. Corrections are proposed to compensate for this.
    Keywords: ddc:548 ; mean atomic number ; Kikuchi patterns ; lattice parameters ; automated Bragg angle determination ; lattice parameter determination ; dynamical theory of electron diffraction ; electron backscatter diffraction ; Funk transform
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 9
    facet.materialart.
    Unknown
    POWTEX visits POWGEN (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-21
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉The high‐intensity time‐of‐flight (TOF) neutron diffractometer POWTEX for powder and texture analysis is currently being built prior to operation in the eastern guide hall of the research reactor FRM II at Garching close to Munich, Germany. Because of the world‐wide 〈sup〉3〈/sup〉He crisis in 2009, the authors promptly initiated the development of 〈sup〉3〈/sup〉He‐free detector alternatives that are tailor‐made for the requirements of large‐area diffractometers. Herein is reported the 2017 enterprise to operate one mounting unit of the final POWTEX detector on the neutron powder diffractometer POWGEN at the Spallation Neutron Source located at Oak Ridge National Laboratory, USA. As a result, presented here are the first angular‐ and wavelength‐dependent data from the POWTEX detector, unfortunately damaged by a 50〈italic〉g〈/italic〉 shock but still operating, as well as the efforts made both to characterize the transport damage and to successfully recalibrate the voxel positions in order to yield nonetheless reliable measurements. Also described is the current data reduction process using the 〈italic〉PowderReduceP2D〈/italic〉 algorithm implemented in 〈italic〉Mantid〈/italic〉 [Arnold 〈italic〉et al.〈/italic〉 (2014). 〈italic〉Nucl. Instrum. Methods Phys. Res. A〈/italic〉, 〈bold〉764〈/bold〉, 156–166]. The final part of the data treatment chain, namely a novel multi‐dimensional refinement using a modified version of the 〈italic〉GSAS‐II〈/italic〉 software suite [〈ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/paper?aj5212"〉Toby & Von Dreele (2013). 〈italic〉J. Appl. Cryst.〈/italic〉〈bold〉46〈/bold〉, 544–549〈/ext-link〉], is compared with a standard data treatment of the same event data conventionally reduced as TOF diffraction patterns and refined with the unmodified version of 〈italic〉GSAS‐II〈/italic〉. This involves both determining the instrumental resolution parameters using POWGEN's powdered diamond standard sample and the refinement of a friendly‐user sample, BaZn(NCN)〈sub〉2〈/sub〉. Although each structural parameter on its own looks similar upon comparing the conventional (1D) and multi‐dimensional (2D) treatments, also in terms of precision, a closer view shows small but possibly significant differences. For example, the somewhat suspicious proximity of the 〈italic〉a〈/italic〉 and 〈italic〉b〈/italic〉 lattice parameters of BaZn(NCN)〈sub〉2〈/sub〉 crystallizing in 〈italic〉Pbca〈/italic〉 as resulting from the 1D refinement (0.008 Å) is five times less pronounced in the 2D refinement (0.038 Å). Similar features are found when comparing bond lengths and bond angles, 〈italic〉e.g.〈/italic〉 the two N—C—N units are less differently bent in the 1D results (173 and 175°) than in the 2D results (167 and 173°). The results are of importance not only for POWTEX but also for other neutron TOF diffractometers with large‐area detectors, like POWGEN at the SNS or the future DREAM beamline at the European Spallation Source.〈/p〉
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉The first real‐world neutron diffraction data have been collected with one of the POWTEX detectors (FRM II, Garching, Germany) mounted for testing at the Spallation Neutron Source (Oak Ridge National Laboratory, USA). They allow for angular‐ and wavelength‐dispersive Rietveld refinement using a modified version of 〈italic〉GSAS‐II〈/italic〉.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005767:jcr2tu5033:jcr2tu5033-fig-0001"〉 〈/graphic〉〈/boxed-text〉〈/p〉
    Keywords: ddc:548 ; neutron detectors ; POWGEN beamline ; POWTEX detector ; DREAM beamline ; time‐of‐flight diffraction ; angular‐dispersive refinement ; wavelength‐dispersive refinement ; powder diffraction ; Rietveld refinement ; multi‐dimensional refinement
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 10
    facet.materialart.
    Unknown
    A note on the wedge reversion antisymmetry operation and 51 types of physical quantities in arbitrary dimensions (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-21
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉The paper by Gopalan [〈ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/paper?ib5086"〉(2020). 〈italic〉Acta Cryst.〈/italic〉 A〈bold〉76〈/bold〉, 318–327〈/ext-link〉] presented an enumeration of the 41 physical quantity types in non‐relativistic physics, in arbitrary dimensions, based on the formalism of Clifford algebra. Gopalan considered three antisymmetries: spatial inversion, 〈overline〉1〈/overline〉, time reversal, 1′, and wedge reversion, 1〈sup〉†〈/sup〉. A consideration of the set of all seven antisymmetries (〈overline〉1〈/overline〉, 1′, 1〈sup〉†〈/sup〉, 1′〈sup〉†〈/sup〉, 〈overline〉1〈/overline〉〈sup〉†〈/sup〉, 〈overline〉1〈/overline〉′, 〈overline〉1〈/overline〉′〈sup〉†〈/sup〉) leads to an extension of the results obtained by Gopalan. It is shown that there are 51 types of physical quantities with distinct symmetry properties in total.〈/p〉
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉It is shown that there are 51 types of physical quantities in arbitrary dimensions with distinct transformations by wedge reversion symmetry. In the paper by 〈ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/paper?ib5086"〉Gopalan [(2020). 〈italic〉Acta Cryst.〈/italic〉 A〈bold〉76〈/bold〉, 318–327]〈/ext-link〉 only 41 types were enumerated.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:20532733:aya2ib5117:aya2ib5117-fig-0001"〉 〈alt-text〉image〈/alt-text〉 〈/graphic〉〈/boxed-text〉〈/p〉
    Keywords: ddc:548 ; multivectors ; wedge reversion ; antisymmetry ; Clifford algebra
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 11
    facet.materialart.
    Unknown
    Use of electron backscatter diffraction patterns to determine the crystal lattice. Part 1. Where is the Bragg angle? (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-19
    Description: The derivation of a crystal structure and its phase‐specific parameters from a single wide‐angle backscattered Kikuchi diffraction pattern requires reliable extraction of the Bragg angles. By means of the first derivative of the lattice profile, an attempt is made to determine fully automatically and reproducibly the band widths in simulated Kikuchi patterns. Even under such ideal conditions (projection centre, wavelength and lattice plane traces are perfectly known), this leads to a lattice parameter distribution whose mean shows a linear offset that correlates with the mean atomic number Z of the pattern‐forming phase. The consideration of as many Kikuchi bands as possible reduces the errors that typically occur if only a single band is analysed. On the other hand, the width of the resulting distribution is such that higher image resolution of diffraction patterns, employing longer wavelengths to produce wider bands or the use of higher interference orders is less advantageous than commonly assumed.
    Description: The lattice parameters of more than 350 phases have been determined from simulated backscatter Kikuchi patterns. The deviations correlating with the mean atomic number correspond to those observed previously for experimental electron backscatter diffraction patterns.
    Keywords: ddc:548 ; Bragg angles ; Kikuchi bands ; Kikuchi patterns ; first derivative ; lattice parameters ; lattice parameter determination ; Bravais lattice type ; electron backscatter diffraction ; Radon transform
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 12
    facet.materialart.
    Unknown
    Data reduction for X‐ray serial crystallography using machine learning (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-19
    Description: Serial crystallography experiments produce massive amounts of experimental data. Yet in spite of these large‐scale data sets, only a small percentage of the data are useful for downstream analysis. Thus, it is essential to differentiate reliably between acceptable data (hits) and unacceptable data (misses). To this end, a novel pipeline is proposed to categorize the data, which extracts features from the images, summarizes these features with the `bag of visual words' method and then classifies the images using machine learning. In addition, a novel study of various feature extractors and machine learning classifiers is presented, with the aim of finding the best feature extractor and machine learning classifier for serial crystallography data. The study reveals that the oriented FAST and rotated BRIEF (ORB) feature extractor with a multilayer perceptron classifier gives the best results. Finally, the ORB feature extractor with multilayer perceptron is evaluated on various data sets including both synthetic and experimental data, demonstrating superior performance compared with other feature extractors and classifiers.
    Description: A machine learning method for distinguishing good and bad images in serial crystallography is presented. To reduce the computational cost, this uses the oriented FAST and rotated BRIEF feature extraction method from computer vision to detect image features, followed by a multilayer perceptron (neural network) to classify the images.
    Keywords: ddc:548 ; serial crystallography ; data reduction ; machine learning ; feature extraction
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 13
    facet.materialart.
    Unknown
    Towards joint in situ determination of pressure and temperature in the large volume press exclusively from X‐ray diffraction (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-19
    Description: Since high‐pressure devices have been used at synchrotron facilities, accurate determination of pressure and temperature in the sample has been a crucial objective, particularly for experiments that simulate the Earth's interior. However, in some cases using a thermocouple may have a high likelihood of failure or is incompatible with a high‐pressure assembly. To address these challenges and similar issues, we aim to expand a previously proposed solution: to jointly estimate pressure and temperature (〈italic〉PT〈/italic〉) through 〈italic〉in situ〈/italic〉 X‐ray diffraction, to cover a wider range of internal 〈italic〉PT〈/italic〉 calibrants tested over larger 〈italic〉PT〈/italic〉 ranges. A modifiable Python‐based software is offered to quickly obtain results. To achieve these aims, 〈italic〉in situ〈/italic〉 large volume press experiments are performed on pellets of intimately mixed powders of a halide (NaCl, KCl, KBr, CsCl) or MgO and a metal (Pt, Re, Mo, W, Ni) in the pressure range 3–11 GPa and temperature range 300–1800 K. Although the pressure range was chosen for practical reasons, it also covers an equally important depth range in the Earth (down to 350 km) for geoscience studies. A thermocouple was used to validate the 〈italic〉PT〈/italic〉 conditions in the cell assemblies. The key results show that choosing the appropriate calibrant materials and using a joint 〈italic〉PT〈/italic〉 estimation can yield surprisingly small uncertainties (〈italic〉i.e.〈/italic〉 〈±0.1 GPa and 〈±50 K). This development is expected to benefit current and future research at extreme conditions, as other materials with high compressibility or high thermal pressure, stable over large 〈italic〉PT〈/italic〉 ranges, may be discovered and used as 〈italic〉PT〈/italic〉 calibrants.〈/p〉
    Description: Research in high‐pressure devices, such as the diamond anvil cell and the large volume press, requires knowledge of the pressure and temperature in the sample. Here, a large volume press and an internal resistive heater were used to generate high load and heat to various combinations of intimately mixed powders of materials. X‐ray diffraction and custom software were used to jointly estimate the pressures and temperatures in the samples and establish calibrants for 〈italic〉in situ〈/italic〉 experiments at extreme conditions.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005775:jsy2vl5008:jsy2vl5008-fig-0001"〉
    Description: https://gitlab.desy.de/robert.farla/eoscross
    Keywords: ddc:548 ; equations of state ; X‐ray diffraction ; large volume press ; high pressure ; resistive heating
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 14
    facet.materialart.
    Unknown
    In situ neutron diffraction for analysing complex coarse‐grained functional materials (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-10-24
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉Complex functional materials play a crucial role in a broad range of energy‐related applications and in general for materials science. Revealing the structural mechanisms is challenging due to highly correlated coexisting phases and microstructures, especially for 〈italic〉in situ〈/italic〉 or 〈italic〉operando〈/italic〉 investigations. Since the grain sizes influence the properties, these microstructural features further complicate investigations at synchrotrons due to the limitations of illuminated sample volumes. In this study, it is demonstrated that such complex functional materials with highly correlated coexisting phases can be investigated under 〈italic〉in situ〈/italic〉 conditions with neutron diffraction. For large grain sizes, these experiments are valuable methods to reveal the structural mechanisms. For an example of 〈italic〉in situ〈/italic〉 experiments on barium titanate with an applied electric field, details of the electric‐field‐induced phase transformation depending on grain size and frequency are revealed. The results uncover the strain mechanisms in barium titanate and elucidate the complex interplay of stresses in relation to grain sizes as well as domain‐wall densities and mobilities.〈/p〉
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉This work reports 〈italic〉in situ〈/italic〉 neutron diffraction experiments on a broad range of grain sizes of barium titanate. The study reveals the grain‐size‐dependent strain mechanisms and shows the competitiveness of neutron diffraction with high‐resolution synchrotron diffraction.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005767:jcr2vb5054:jcr2vb5054-fig-0001"〉 〈alt-text〉image〈/alt-text〉 〈/graphic〉〈/boxed-text〉〈/p〉
    Keywords: ddc:550.724 ; ddc:548 ; neutron diffraction ; in situ ; applied electric fields ; barium titanate ; strain mechanisms ; grain sizes ; complex functional materials ; microstructures ; coexisting phases
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 15
    facet.materialart.
    Unknown
    Beam‐induced redox chemistry in iron oxide nanoparticle dispersions at ESRF–EBS (2023)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-02-21
    Description: The storage ring upgrade of the European Synchrotron Radiation Facility makes ESRF–EBS the most brilliant high‐energy fourth‐generation light source, enabling in situ studies with unprecedented time resolution. While radiation damage is commonly associated with degradation of organic matter such as ionic liquids or polymers in the synchrotron beam, this study clearly shows that highly brilliant X‐ray beams readily induce structural changes and beam damage in inorganic matter, too. Here, the reduction of Fe3+ to Fe2+ in iron oxide nanoparticles by radicals in the brilliant ESRF–EBS beam, not observed before the upgrade, is reported. Radicals are created due to radiolysis of an EtOH–H2O mixture with low EtOH concentration (∼6 vol%). In light of extended irradiation times during insitu experiments in, for example, battery and catalysis research, beam‐induced redox chemistry needs to be understood for proper interpretation of insitu data.
    Description: With the increased brilliance at the European Research Facility–Extremely Brilliant Source (ESRF–EBS), a beam‐induced reduction of non‐stochiometric iron oxide nanoparticles (almost maghemite composition) to magnetite was observed in a mixture of ethanol and water with low ethanol concentration.
    Keywords: ddc:548 ; beam‐induced radiolysis ; radiation damage on inorganic materials ; ESRF–EBS
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 16
    facet.materialart.
    Unknown
    Machine learning for scattering data: strategies, perspectives and applications to surface scattering (2023)
    Hinderhofer, Alexander ; Greco, Alessandro ; Starostin, Vladimir ; [et al.]
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-02-14
    Description: Machine learning (ML) has received enormous attention in science and beyond. Discussed here are the status, opportunities, challenges and limitations of ML as applied to X‐ray and neutron scattering techniques, with an emphasis on surface scattering. Typical strategies are outlined, as well as possible pitfalls. Applications to reflectometry and grazing‐incidence scattering are critically discussed. Comment is also given on the availability of training and test data for ML applications, such as neural networks, and a large reflectivity data set is provided as reference data for the community.
    Description: The status, opportunities, challenges and limitations of machine learning are discussed as applied to X‐ray and neutron scattering techniques, with an emphasis on surface scattering.
    Keywords: ddc:548 ; surface scattering ; X‐ray diffraction ; neutron scattering ; machine learning ; data analysis
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 17
    facet.materialart.
    Unknown
    Hard X‐ray full‐field nanoimaging using a direct photon‐counting detector (2023)
    Flenner, Silja ; Hagemann, Johannes ; Wittwer, Felix ; [et al.]
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-03-05
    Description: Full‐field X‐ray nanoimaging is a widely used tool in a broad range of scientific areas. In particular, for low‐absorbing biological or medical samples, phase contrast methods have to be considered. Three well established phase contrast methods at the nanoscale are transmission X‐ray microscopy with Zernike phase contrast, near‐field holography and near‐field ptychography. The high spatial resolution, however, often comes with the drawback of a lower signal‐to‐noise ratio and significantly longer scan times, compared with microimaging. In order to tackle these challenges a single‐photon‐counting detector has been implemented at the nanoimaging endstation of the beamline P05 at PETRA III (DESY, Hamburg) operated by Helmholtz‐Zentrum Hereon. Thanks to the long sample‐to‐detector distance available, spatial resolutions of below 100 nm were reached in all three presented nanoimaging techniques. This work shows that a single‐photon‐counting detector in combination with a long sample‐to‐detector distance allows one to increase the time resolution for in situ nanoimaging, while keeping a high signal‐to‐noise level.
    Description: A direct photon‐counting detector was used for different nanoimaging phase contrast techniques, increasing the temporal resolution.
    Keywords: ddc:548 ; nanotomography ; full‐field X‐ray microscopy ; near‐field holography ; near‐field ptychography ; Zernike phase contrast ; single‐photon‐counting detector ; phase contrast
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 18
    facet.materialart.
    Unknown
    Using diffraction losses of X‐rays in a single crystal for determination of its lattice parameters as well as for monochromator calibration (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-12-04
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉A way has been developed to measure the unit‐cell parameters of a single crystal just from an energy scan with X‐rays, even when the exact energy of the X‐rays is not well defined due to an error in the pitch angle of the monochromator. The precision of this measurement reaches 〈italic〉da〈/italic〉/〈italic〉a〈/italic〉 ∼ 1 × 10〈sup〉−5〈/sup〉. The method is based on the analysis of diffraction losses of the beam, transmitted through a single crystal (the so‐called `glitch effect'). This method can be easily applied to any transmissive X‐ray optical element made of single crystals (for example, X‐ray lenses). The only requirements are the possibility to change the energy of the generated X‐ray beam and some intensity monitor to measure the transmitted intensity. The method is agnostic to the error in the monochromator tuning and it can even be used for determination of the absolute pitch (or 2gθ) angle of the monochromator. Applying the same method to a crystal with well known lattice parameters allows determination of the exact cell parameters of the monochromator at any energy.〈/p〉
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉Diffraction losses (glitches) at certain energies of the X‐ray beam, transmitted through a single crystal, can be used for lattice parameters determination as well as for calibrating the monochromator (absolute pitch angle and the unit‐cell parameter).〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005775:jsy2ay5590:jsy2ay5590-fig-0001"〉 〈alt-text〉image〈/alt-text〉 〈/graphic〉〈/boxed-text〉〈/p〉
    Keywords: ddc:548 ; X‐ray glitches ; diffraction losses ; unit‐cell parameter ; single‐crystal X‐ray optics ; monochromator calibration
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 19
    facet.materialart.
    Unknown
    Quantifying electron cascade size in various irradiated materials for free‐electron laser applications (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-12-12
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉Studying electron‐ and X‐ray‐induced electron cascades in solids is essential for various research areas at free‐electron laser facilities, such as X‐ray imaging, crystallography, pulse diagnostics or X‐ray‐induced damage. To better understand the fundamental factors that define the duration and spatial size of such cascades, this work investigates the electron propagation in ten solids relevant for the applications of X‐ray lasers: Au, B〈sub〉4〈/sub〉C, diamond, Ni, polystyrene, Ru, Si, SiC, Si〈sub〉3〈/sub〉N〈sub〉4〈/sub〉 and W. Using classical Monte Carlo simulation in the atomic approximation, we study the dependence of the cascade size on the incident electron or photon energy and on the target parameters. The results show that an electron‐induced cascade is systematically larger than a photon‐induced cascade. Moreover, in contrast with the common assumption, the maximal cascade size does not necessarily coincide with the electron range. It was found that the cascade size can be controlled by careful selection of the photon energy for a particular material. Photon energy, just above an ionization potential, can essentially split the absorbed energy between two electrons (photo‐ and Auger), reducing their initial energy and thus shrinking the cascade size. This analysis suggests a way of tailoring the electron cascades for applications requiring either small cascades with a high density of excited electrons or large‐spread cascades with lower electron densities.〈/p〉
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉Studying electron‐ and X‐ray‐induced electron cascades in solids is essential for various research areas at free‐electron laser facilities, such as X‐ray imaging, crystallography, pulse diagnostics or X‐ray‐induced damage. To better understand the fundamental factors that define the duration and spatial size of such cascades, this work investigates the electron propagation in ten solids relevant for the applications of X‐ray lasers. Using classical Monte Carlo simulation in the atomic approximation, the dependence of the cascade size on the incident electron or photon energy and on the target parameters is studied.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005775:jsy2gb5123:jsy2gb5123-fig-0001"〉 〈/graphic〉〈/boxed-text〉〈/p〉
    Keywords: ddc:548 ; electron cascades ; X‐ray free‐electron lasers ; Monte Carlo ; photon‐induced cascade ; electron transport
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 20
    facet.materialart.
    Unknown
    Digitization of imaging plates from Guinier powder X‐ray diffraction cameras (2022)
    Nasir, Jamal ; Steinbrück, Nils ; Xu, Ke ; [et al.]
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-01-15
    Description: A Guinier camera equipped with an imaging plate is used to investigate and eliminate the sources of instrumental errors affecting the quality of the obtained scanned Guinier data. A program with a graphical user interface is presented which converts the data of the scanned images into different standard file formats for powder X‐ray patterns containing intensities, their standard deviations and the diffraction angles. The program also allows for manual and automatic correction of the 2gθ scale against a known reference material. It is shown using LaB6 that the exported X‐ray diffraction patterns provide a 2gθ scale reproducible enough to allow for averaging diffractograms obtained from different exposures of the imaging plate for the same sample. As shown on a mixture of NaCl and sodalite, the quality of the produced data is sufficient for Rietveld refinement. The software including source code is made available under a free software license.
    Description: A program for the digitization of Guinier powder diffraction images is described, which works with images from both optical and laser scanners. Thus, processing of data from storage‐phosphor‐based imaging plates and Ag‐based photographic films is possible.
    Keywords: ddc:548 ; IPreader software ; Guinier cameras ; imaging plates (IPs) ; diffraction pattern conversion into data columns ; powder X‐ray diffraction ; data processing ; Guinier method
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 21
    facet.materialart.
    Unknown
    X‐ray diffraction with micrometre spatial resolution for highly absorbing samples (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-01-21
    Description: X‐ray diffraction with high spatial resolution is commonly used to characterize (poly)crystalline samples with, for example, respect to local strain, residual stress, grain boundaries and texture. However, the investigation of highly absorbing samples or the simultaneous assessment of high‐Z materials by X‐ray fluorescence have been limited due to the utilization of low photon energies. Here, a goniometer‐based setup implemented at the P06 beamline of PETRA III that allows for micrometre spatial resolution with a photon energy of 35 keV and above is reported. A highly focused beam was achieved by using compound refractive lenses, and high‐precision sample manipulation was enabled by a goniometer that allows up to 5D scans (three rotations and two translations). As experimental examples, the determination of local strain variations in martensitic steel samples with micrometre spatial resolution, as well as the simultaneous elemental distribution for high‐Z materials in a thin‐film solar cell, are demonstrated. The proposed approach allows users from the materials‐science community to determine micro‐structural properties even in highly absorbing samples.
    Description: A demonstration of high‐resolution micro X‐ray diffraction at high photon energies for highly absorbing samples.
    Keywords: ddc:548 ; X‐ray diffraction ; high spatial resolution ; high photon energy ; X‐ray fluorescence ; goniometers
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 22
    facet.materialart.
    Unknown
    Domain Auto Finder (DAFi) program: the analysis of single‐crystal X‐ray diffraction data from polycrystalline samples (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-01-21
    Description: This paper presents the Domain Auto Finder (DAFi) program and its application to the analysis of single‐crystal X‐ray diffraction (SC‐XRD) data from multiphase mixtures of microcrystalline solids and powders. Superposition of numerous reflections originating from a large number of single‐crystal domains of the same and/or different (especially unknown) phases usually precludes the sorting of reflections coming from individual domains, making their automatic indexing impossible. The DAFi algorithm is designed to quickly find subsets of reflections from individual domains in a whole set of SC‐XRD data. Further indexing of all found subsets can be easily performed using widely accessible crystallographic packages. As the algorithm neither requires a priori crystallographic information nor is limited by the number of phases or individual domains, DAFi is powerful software to be used for studies of multiphase polycrystalline and microcrystalline (powder) materials. The algorithm is validated by testing on X‐ray diffraction data sets obtained from real samples: a multi‐mineral basalt rock at ambient conditions and products of the chemical reaction of yttrium and nitrogen in a laser‐heated diamond anvil cell at 50 GPa. The high performance of the DAFi algorithm means it can be used for processing SC‐XRD data online during experiments at synchrotron facilities.
    Description: This paper presents the Domain Auto Finder (DAFi) program and its application to the analysis of single‐crystal X‐ray diffraction (SC‐XRD) data from multiphase mixtures of microcrystalline solids and powders. The DAFi algorithm is designed to quickly find subsets of reflections from individual domains in a whole set of SC‐XRD data and neither requires a priori crystallographic information nor is limited by the number of phases or individual domains.
    Keywords: ddc:548 ; single‐crystal domain auto finder ; DAFi ; single‐crystal X‐ray diffraction ; polycrystalline samples ; multiphase mixtures
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 23
    facet.materialart.
    Unknown
    High‐resolution XEOL spectroscopy setup at the X‐ray absorption spectroscopy beamline P65 of PETRA III (2022)
    Levcenko, S. ; Biller, R. ; Pfeiffelmann, T. ; [et al.]
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-01-25
    Description: A newly designed setup to perform steady‐state X‐ray excited optical luminescence (XEOL) spectroscopy and simultaneous XEOL and X‐ray absorption spectroscopy characterization at beamline P65 of PETRA III is described. The XEOL setup is equipped with a He‐flow cryostat and state‐of‐the‐art optical detection system, which covers a wide wavelength range of 300–1700 nm with a high spectral resolution of 0.4 nm. To demonstrate the setup functioning, low‐temperature XEOL studies on polycrystalline CuInSe2 thin film, single‐crystalline GaN thin film and single‐crystalline ZnO bulk semiconductor samples are performed.
    Description: X‐ray excited optical luminescence (XEOL) spectroscopy is increasingly important to understand the interplay between the optical properties, structure and chemical composition, providing insights into the mechanism of radiative recombination for a wide range of materials. This study demonstrates a newly implemented setup to perform steady‐state XEOL and simultaneous XEOL and XAFS characterizations at beamline P65 of PETRA III.
    Keywords: ddc:550.2 ; XEOL ; XAS ; CuInSe2 ; ZnO ; GaN
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 24
    facet.materialart.
    Unknown
    Small‐angle neutron scattering of long‐wavelength magnetic modulations in reduced sample dimensions (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-04
    Description: Magnetic small‐angle neutron scattering (SANS) is ideally suited to providing direct reciprocal‐space information on long‐wavelength magnetic modulations, such as helicoids, solitons, merons or skyrmions. SANS of such structures in thin films or micro‐structured bulk materials is strongly limited by the tiny scattering volume vis a vis the prohibitively high background scattering by the substrate and support structures. Considering near‐surface scattering just above the critical angle of reflection, where unwanted signal contributions due to substrate or support structures become very small, it is established that the scattering patterns of the helical, conical, skyrmion lattice and fluctuation‐disordered phases in a polished bulk sample of MnSi are equivalent for conventional transmission and near‐surface SANS geometries. This motivates the prediction of a complete repository of scattering patterns expected for thin films in the near‐surface SANS geometry for each orientation of the magnetic order with respect to the scattering plane.
    Description: Near‐surface SANS is discussed for its potential as a probe of long‐wavelength magnetic modulations in specimens with reduced sample dimensions.
    Keywords: ddc:548 ; small‐angle neutron scattering ; near‐surface SANS ; magnetism ; non‐collinear magnetism ; thin films ; skyrmions ; MnSi
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 25
    facet.materialart.
    Unknown
    Combining reverse Monte Carlo analysis of X‐ray scattering and extended X‐ray absorption fine structure spectra of very small nanoparticles (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2023-07-21
    Description: Finite size effects in partial pair distribution functions generate artefacts in the scattering structure factor and scattering intensity. It is shown how they can be overcome using a binned version of the Debye scattering equation. Accordingly, reverse Monte Carlo simulations are used for very small nanoparticles of LaFeO3 with diameters below 10 nm to simultaneously analyse X‐ray scattering data and extended X‐ray absorption fine structure spectra at the La K and Fe K edges. The structural information obtained is consistent regarding local structure and long‐range order.
    Description: Computing scattering intensity using the Debye scattering equation after binning interatomic distances avoids finite size artefacts and is efficient enough for simultaneous refinement of scattering data and extended X‐ray absorption spectra by reverse Monte Carlo simulations.
    Keywords: ddc:548 ; extended X‐ray absorption fine structure ; EXAFS ; wide‐angle X‐ray scattering ; WAXS ; reverse Monte Carlo ; RMC ; nanocrystals ; LaFeO3
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 26
    facet.materialart.
    Unknown
    Site dependence of the magnetocaloric effect in Mn5−xFexSi3 (2022)
    Ait Haddouch, Mohammed ; Abboushi, Nour ; Sharma, Neetika ; [et al.]
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2022-12-06
    Description: The nuclear and magnetic structures of Mn3Fe2Si3 are investigated in the temperature range from 20 to 300 K. The magnetic properties of Mn3Fe2Si3 were measured on a single crystal. The compound undergoes a paramagnetic to antiferromagnetic transition at TN2 ≃ 120 K and an antiferromagnetic to antiferromagnetic transition at TN1 ≃ 69 K. A similar sequence of magnetic phase transitions is found for the parent compound Mn5Si3 upon temperature variation, but the field‐driven transition observed in Mn5Si3 is not found in Mn3Fe2Si3, resulting in a strongly reduced magnetocaloric effect. Structurally, the hexagonal symmetry found for both compounds under ambient conditions is preserved in Mn3Fe2Si3 through both magnetic transitions, indicating that the crystal structure is only weakly affected by the magnetic phase transition, in contrast to Mn5Si3 where both transitions distort the nuclear structure. Both compounds feature a collinear high‐temperature magnetic phase AF2 and transfer into a non‐collinear phase AF1 at low temperature. While one of the distinct crystallographic sites remains disordered in the AF2 phase in the parent compound, the magnetic structure in the AF2 phase involves all magnetic atoms in Mn3Fe2Si3. These observations imply that the distinct sites occupied by the magnetic atoms play an important role in the magnetocaloric behaviour of the family.
    Description: The nuclear and magnetic structures of Mn3Fe2Si3 are determined and the magnetic properties are compared with those of the parent compound Mn5Si3. The results imply that the distinct magnetic sites play an important role in the magnetocaloric behaviour of the family. image
    Keywords: ddc:548 ; magnetocaloric effect ; magnetic structure ; neutron diffraction ; synchrotron diffraction ; site dependence
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 27
    facet.materialart.
    Unknown
    Sub‐micrometer focusing setup for high‐pressure crystallography at the Extreme Conditions beamline at PETRA III (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2022-06-24
    Description: Scientific tasks aimed at decoding and characterizing complex systems and processes at high pressures set new challenges for modern X‐ray diffraction instrumentation in terms of X‐ray flux, focal spot size and sample positioning. Presented here are new developments at the Extreme Conditions beamline (P02.2, PETRA III, DESY, Germany) that enable considerable improvements in data collection at very high pressures and small scattering volumes. In particular, the focusing of the X‐ray beam to the sub‐micrometer level is described, and control of the aberrations of the focusing compound refractive lenses is made possible with the implementation of a correcting phase plate. This device provides a significant enhancement of the signal‐to‐noise ratio by conditioning the beam shape profile at the focal spot. A new sample alignment system with a small sphere of confusion enables single‐crystal data collection from grains of micrometer to sub‐micrometer dimensions subjected to pressures as high as 200 GPa. The combination of the technical development of the optical path and the sample alignment system contributes to research and gives benefits on various levels, including rapid and accurate diffraction mapping of samples with sub‐micrometer resolution at multimegabar pressures.
    Description: Facing the challenges of X‐ray diffraction from tiny samples subjected to multimegabar pressures, instrumentation developments are presented that enable, among other studies, single‐crystal data collection from micrometer‐ to sub‐micrometer‐sized grains. The developments are based on a sub‐micrometer beam capability employing compound refractive lenses operating with a phase correcting plate and a precise motorization solution.
    Keywords: ddc:548
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 28
    facet.materialart.
    Unknown
    Robust approaches for model‐free small‐angle scattering data analysis (2022)
    Bender, Philipp ; Honecker, Dirk ; Bersweiler, Mathias ; [et al.]
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2022-10-04
    Description: The small‐angle neutron scattering data of nanostructured magnetic samples contain information regarding their chemical and magnetic properties. Often, the first step to access characteristic magnetic and structural length scales is a model‐free investigation. However, due to measurement uncertainties and a restricted q range, a direct Fourier transform usually fails and results in ambiguous distributions. To circumvent these problems, different methods have been introduced to derive regularized, more stable correlation functions, with the indirect Fourier transform being the most prominent approach. Here, the indirect Fourier transform is compared with the singular value decomposition and an iterative algorithm. These approaches are used to determine the correlation function from magnetic small‐angle neutron scattering data of a powder sample of iron oxide nanoparticles; it is shown that with all three methods, in principle, the same correlation function can be derived. Each method has certain advantages and disadvantages, and thus the recommendation is to combine these three approaches to obtain robust results.
    Description: Three different approaches are compared for determination of the correlation function from the small‐angle neutron scattering data of a powder sample of iron oxide nanoparticles.
    Keywords: ddc:548
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 29
    facet.materialart.
    Unknown
    Structure determination from unindexed powder data from scratch by a global optimization approach using pattern comparison based on cross‐correlation functions (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2022-06-16
    Description: A method of ab initio crystal structure determination from powder diffraction data for organic and metal–organic compounds, which does not require prior indexing of the powder pattern, has been developed. Only a reasonable molecular geometry is required, needing knowledge of neither unit‐cell parameters nor space group. The structures are solved from scratch by a global fit to the powder data using the new program FIDEL‐GO (`FIt with DEviating Lattice parameters ‐ Global Optimization'). FIDEL‐GO uses a similarity measure based on cross‐correlation functions, which allows the comparison of simulated and experimental powder data even if the unit‐cell parameters deviate strongly. The optimization starts from large sets of random structures in various space groups. The unit‐cell parameters, molecular position and orientation, and selected internal degrees of freedom are fitted simultaneously to the powder pattern. The optimization proceeds in an elaborate multi‐step procedure with built‐in clustering of duplicate structures and iterative adaptation of parameter ranges. The best structures are selected for an automatic Rietveld refinement. Finally, a user‐controlled Rietveld refinement is performed. The procedure aims for the analysis of a wide range of `problematic' powder patterns, in particular powders of low crystallinity. The method can also be used for the clustering and screening of a large number of possible structure candidates and other application scenarios. Examples are presented for structure determination from unindexed powder data of the previously unknown structures of the nanocrystalline phases of 4,11‐difluoro‐, 2,9‐dichloro‐ and 2,9‐dichloro‐6,13‐dihydro‐quinacridone, which were solved from powder patterns with 14–20 peaks only, and of the coordination polymer dichloro‐bis(pyridine‐N)copper(II).
    Description: A new method for the structure determination of molecular crystals from unindexed powder data has been developed and successfully applied. The method performs a global optimization using pattern comparison based on cross‐correlation functions.
    Keywords: ddc:548
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 30
    facet.materialart.
    Unknown
    HTD2: a single‐crystal X‐ray diffractometer for combined high‐pressure/low‐temperature experiments at laboratory scale (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2022-12-15
    Description: High‐pressure (HP) X‐ray diffraction experiments at low temperature (LT) require dedicated instruments as well as non‐standard sample environments and measuring strategies. This is especially true when helium cryogenic temperatures below 80 K are targeted. Furthermore, only experiments on single‐crystalline samples provide the prerequisites to study subtle structural changes in the p–T phase diagram under extreme LT and HP conditions in greater detail. Due to special hardware requirements, such measurements are usually in the realm of synchrotron beamlines. This contribution describes the design of an LT/HP diffractometer (HTD2) to perform single‐crystal X‐ray diffraction experiments using a laboratory source in the temperature range 400 〉 T 〉 2 K while applying pressures of up to 20 GPa.
    Description: The design and operation of a newly commissioned single‐crystal X‐ray diffractometer (HTD2) are presented. The device enables experiments under simultaneous low‐temperature and high‐pressure conditions using a laboratory X‐ray source.
    Keywords: ddc:548 ; HTD2 ; low temperature ; high pressure ; single crystals ; instrumentation
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 31
    facet.materialart.
    Unknown
    Extending MIEZE spectroscopy towards thermal wavelengths (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-02-05
    Description: A modulation of intensity with zero effort (MIEZE) setup is proposed for high‐resolution neutron spectroscopy at momentum transfers up to 3 Å〈sup〉−1〈/sup〉, energy transfers up to 20 meV and an energy resolution in the microelectronvolt range using both thermal and cold neutrons. MIEZE has two prominent advantages compared with classical neutron spin echo. The first is the possibility to investigate spin‐depolarizing samples or samples in strong magnetic fields without loss of signal amplitude and intensity. This allows for the study of spin fluctuations in ferromagnets, and facilitates the study of samples with strong spin‐incoherent scattering. The second advantage is that multi‐analyzer setups can be implemented with comparatively little effort. The use of thermal neutrons increases the range of validity of the spin‐echo approximation towards shorter spin‐echo times. In turn, the thermal MIEZE option for greater ranges (TIGER) closes the gap between classical neutron spin‐echo spectroscopy and conventional high‐resolution neutron spectroscopy techniques such as triple‐axis, time‐of‐flight and back‐scattering. To illustrate the feasibility of TIGER, this paper presents the details of its implementation at the RESEDA beamline at FRM II by means of an additional velocity selector, polarizer and analyzer.
    Description: A modulation of intensity with zero effort (MIEZE) setup is proposed for high‐resolution neutron spectroscopy at momentum transfers up to 3 Å〈sup〉−1〈/sup〉, energy transfers up to 20 meV and an energy resolution in the microelectronvolt range using both thermal and cold neutrons.
    Keywords: ddc:548 ; neutron resonant spin echo ; MIEZE ; quasielastic scattering ; thermal neutrons
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 32
    facet.materialart.
    Unknown
    Extreme conditions research using the large‐volume press at the P61B endstation, PETRA III (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-02-05
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉Penetrating, high‐energy synchrotron X‐rays are in strong demand, particularly for high‐pressure research in physics, chemistry and geosciences, and for materials engineering research under less extreme conditions. A new high‐energy wiggler beamline P61 has been constructed to meet this need at PETRA III in Hamburg, Germany. The first part of the paper offers an overview of the beamline front‐end components and beam characteristics. The second part describes the performance of the instrumentation and the latest developments at the P61B endstation. Particular attention is given to the unprecedented high‐energy photon flux delivered by the ten wigglers of the PETRA III storage ring and the challenges faced in harnessing this amount of flux and heat load in the beam. Furthermore, the distinctiveness of the world's first six‐ram Hall‐type large‐volume press, Aster‐15, at a synchrotron facility is described for research with synchrotron X‐rays. Additionally, detection schemes, experimental strategies and preliminary data acquired using energy‐dispersive X‐ray diffraction and radiography techniques are presented.〈/p〉
    Description: 〈p xmlns:mml="http://www.w3.org/1998/Math/MathML" xml:lang="en"〉The operation of the P61B endstation large‐volume press and optics of P61 are reviewed. The instrumentation at P61B, including the large‐volume press, detection systems and data acquisition for 〈italic〉in situ〈/italic〉 high‐pressure experiments are described.〈boxed-text position="anchor" content-type="graphic" xml:lang="en"〉〈graphic position="anchor" id="jats-graphic-1" xlink:href="urn:x-wiley:16005775:jsy2ju5040:jsy2ju5040-fig-0001"〉 〈/graphic〉〈/boxed-text〉〈/p〉
    Keywords: ddc:550.724 ; extreme conditions ; high‐pressure ; large‐volume press ; energy‐dispersive X‐ray diffraction ; radiography ; resistive heating ; ultrasonic interferometry ; acoustic emissions detection
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 33
    facet.materialart.
    Unknown
    The PERCIVAL detector: first user experiments (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-03-13
    Description: The PERCIVAL detector is a CMOS imager designed for the soft X‐ray regime at photon sources. Although still in its final development phase, it has recently seen its first user experiments: ptychography at a free‐electron laser, holographic imaging at a storage ring and preliminary tests on X‐ray photon correlation spectroscopy. The detector performed remarkably well in terms of spatial resolution achievable in the sample plane, owing to its small pixel size, large active area and very large dynamic range; but also in terms of its frame rate, which is significantly faster than traditional CCDs. In particular, it is the combination of these features which makes PERCIVAL an attractive option for soft X‐ray science.
    Keywords: ddc:548 ; X‐ray detectors ; soft X‐rays ; ptychography ; holographic imaging ; XPCS ; detectors
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 34
    facet.materialart.
    Unknown
    Automatic bad‐pixel mask maker for X‐ray pixel detectors with application to serial crystallography (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-02-14
    Description: X‐ray crystallography has witnessed a massive development over the past decade, driven by large increases in the intensity and brightness of X‐ray sources and enabled by employing high‐frame‐rate X‐ray detectors. The analysis of large data sets is done via automatic algorithms that are vulnerable to imperfections in the detector and noise inherent with the detection process. By improving the model of the behaviour of the detector, data can be analysed more reliably and data storage costs can be significantly reduced. One major requirement is a software mask that identifies defective pixels in diffraction frames. This paper introduces a methodology and program based upon concepts of machine learning, called robust mask maker (RMM), for the generation of bad‐pixel masks for large‐area X‐ray pixel detectors based on modern robust statistics. It is proposed to discriminate normally behaving pixels from abnormal pixels by analysing routine measurements made with and without X‐ray illumination. Analysis software typically uses a Bragg peak finder to detect Bragg peaks and an indexing method to detect crystal lattices among those peaks. Without proper masking of the bad pixels, peak finding methods often confuse the abnormal values of bad pixels in a pattern with true Bragg peaks and flag such patterns as useful regardless, leading to storage of enormous uninformative data sets. Also, it is computationally very expensive for indexing methods to search for crystal lattices among false peaks and the solution may be biased. This paper shows how RMM vastly improves peak finders and prevents them from labelling bad pixels as Bragg peaks, by demonstrating its effectiveness on several serial crystallography data sets.
    Description: Attention is focused on perhaps the biggest bottleneck in data analysis for serial crystallography at X‐ray free‐electron lasers, which has not received serious enough examination to date. An effective and reliable way is presented to identify anomalies in detectors, using machine learning and recently developed mathematical methods in the field referred to as `robust statistics'. image
    Keywords: ddc:548 ; bad‐pixel masks ; robust mask maker ; machine learning ; robust statistics ; serial crystallography
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 35
    facet.materialart.
    Unknown
    Updates in SASfit for fitting analytical expressions and numerical models to small‐angle scattering patterns (2022)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2024-02-22
    Description: Small‐angle scattering is an increasingly common method for characterizing particle ensembles in a wide variety of sample types and for diverse areas of application. SASfit has been one of the most comprehensive and flexible curve‐fitting programs for decades, with many specialized tools for various fields. Here, a selection of enhancements and additions to the SASfit program are presented that may be of great benefit to interested and advanced users alike: (a) further development of the technical basis of the program, such as new numerical algorithms currently in use, a continuous integration practice for automated building and packaging of the software, and upgrades on the plug‐in system for easier adoption by third‐party developers; (b) a selection of new form factors for anisotropic scattering patterns and updates to existing form factors to account for multiple scattering effects; (c) a new type of a very flexible distribution called metalog [Keelin (2016). Decis. Anal.13, 243–277], and regularization techniques such as the expectation‐maximization method [Dempster et al. (1977). J. R. Stat. Soc. Ser. B (Methodological), 39, 1–22; Richardson (1972) J. Opt. Soc. Am.62, 55; Lucy (1974). Astron. J.79, 745; Lucy (1994). Astron. Astrophys.289, 983–994], which is compared with fits of analytical size distributions via the non‐linear least‐squares method; and (d) new structure factors, especially for ordered nano‐ and meso‐scaled material systems, as well as the Ornstein–Zernike solver for numerical determination of particle interactions and the resulting structure factor when no analytical solution is available, with the aim of incorporating its effects into the small‐angle scattering intensity model used for fitting with SASfit.
    Description: Recent enhancements and additions to the SASfit program are discussed, including anisotropic scattering models, flexible distributions, regularization techniques such as the expectation‐maximization method, and new structure factors, especially for ordered nano‐ and meso‐scaled material. The Ornstein–Zernike solver for numerical structure factors is also introduced. image
    Keywords: ddc:548 ; small‐angle scattering ; SASfit ; numerical models ; structure factors ; form factors ; regularization techniques
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 36
    facet.materialart.
    Unknown
    Facilitated crystal handling using a simple device for evaporation reduction in microtiter plates (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-30
    Description: In the past two decades, most of the steps in a macromolecular crystallography experiment have undergone tremendous development with respect to speed, feasibility and increase of throughput. The part of the experimental workflow that is still a bottleneck, despite significant efforts, involves the manipulation and harvesting of the crystals for the diffraction experiment. Here, a novel low‐cost device is presented that functions as a cover for 96‐well crystallization plates. This device enables access to the individual experiments one at a time by its movable parts, while minimizing evaporation of all other experiments of the plate. In initial tests, drops of many typically used crystallization cocktails could be successfully protected for up to 6 h. Therefore, the manipulation and harvesting of crystals is straightforward for the experimenter, enabling significantly higher throughput. This is useful for many macromolecular crystallography experiments, especially multi‐crystal screening campaigns.
    Description: A simple and low‐cost device has been developed to minimize evaporation in microtiter plates for easy crystal handling and harvesting. image
    Keywords: 548 ; evaporation reduction ; crystal handling ; crystal harvesting ; crystallographic fragment screening
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 37
    facet.materialart.
    Unknown
    Cation distribution in Cu2ZnSnSe4, Cu2FeSnS4 and Cu2ZnSiSe4 by multiple‐edge anomalous diffraction (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-30
    Description: Multiple‐Edge Anomalous Diffraction (MEAD) has been applied to various quaternary sulfosalts belonging to the adamantine compound family in order to validate the distribution of copper, zinc and iron cations in the structure. Semiconductors from this group of materials are promising candidates for photovoltaic applications. Their properties strongly depend on point defects, in particular related to cation order–disorder. However, Cu+, Zn2+ and Fe2+ have very similar scattering factors and are all but indistinguishable in usual X‐ray diffraction experiments. Anomalous diffraction utilizes the dependency of the atomic scattering factors f′ and f′′ of the energy of the radiation, especially close to the element‐specific absorption edges. In the MEAD technique, individual Bragg peaks are tracked over an absorption edge. The intensity changes depending on the structure factor can be highly characteristic for Miller indices selected for a specific structural problem, but require very exact measurements. Beamline KMC‐2 at synchrotron BESSY II, Berlin, has been recently upgraded for this technique. Anomalous X‐ray powder diffraction and XAFS compliment the data. Application of this technique confirmed established cation distribution in Cu2ZnSnSe4 (CZTSe) and Cu2FeSnS4 (CFTS). In contrast to the literature, cation distribution in Cu2ZnSiSe4 (CZSiSe) is shown to adopt a highly ordered wurtz‐kesterite structure type.
    Description: Multiple‐Edge Anomalous Diffraction (MEAD) has been applied to various quaternary sulfosalts belonging to the adamantine compound family in order to validate the distribution of copper, zinc and iron cations in the structure. Application of this technique confirms established cation distribution in Cu2ZnSnSe4 (CZTSe) and Cu2FeSnS4 (CFTS), but in Cu2ZnSiSe4 (CZSiSe) the cation distribution is shown to adopt a highly ordered wurtz‐kesterite structure type in contrast to the literature. image
    Keywords: 548 ; synchrotron ; anomalous diffraction ; semiconductor ; MEAD
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 38
    facet.materialart.
    Unknown
    The copper(II)‐binding tripeptide GHK, a valuable crystallization and phasing tag for macromolecular crystallography (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-27
    Description: The growth of diffraction‐quality crystals and experimental phasing remain two of the main bottlenecks in protein crystallography. Here, the high‐affinity copper(II)‐binding tripeptide GHK was fused to the N‐terminus of a GFP variant and an MBP‐FG peptide fusion. The GHK tag promoted crystallization, with various residues (His, Asp, His/Pro) from symmetry molecules completing the copper(II) square‐pyramidal coordination sphere. Rapid structure determination by copper SAD phasing could be achieved, even at a very low Bijvoet ratio or after significant radiation damage. When collecting highly redundant data at a wavelength close to the copper absorption edge, residual S‐atom positions could also be located in log‐likelihood‐gradient maps and used to improve the phases. The GHK copper SAD method provides a convenient way of both crystallizing and phasing macromolecular structures, and will complement the current trend towards native sulfur SAD and MR‐SAD phasing.
    Description: A novel three‐residue tag containing the residues GHK that can be used to promote crystallization and in SAD phasing experiments using its tightly bound copper ion is described. image
    Keywords: 548 ; phasing ; crystallization ; GHK ; SAD
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 39
    facet.materialart.
    Unknown
    Determining paracrystallinity in mixed‐tacticity polyhydroxybutyrates (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-30
    Description: Recently, the authors reported on the development of crystallinity in mixed‐tacticity polyhydroxybutyrates. Comparable values reported in the literature vary depending on the manner of determination, the discrepancies being partially attributable to scattering from paracrystalline portions of the material. These portions can be qualified by peak profile fitting or quantified by allocation of scattered X‐ray intensities. However, the latter requires a good quality of the former, which in turn must additionally account for peak broadening inherent in the measurement setup, and due to limited crystallite sizes and the possible presence of microstrain. Since broadening due to microstrain and paracrystalline order both scale with scattering vector, they are easily confounded. In this work, a method to directionally discern these two influences on the peak shape in a Rietveld refinement is presented. Allocating intensities to amorphous, bulk and paracrystalline portions with changing tactic disturbance provided internal validations of the obtained directional numbers. In addition, the correlation between obtained thermal factors and Young's moduli, determined in earlier work, is discussed.
    Description: A method to robustly determine paracrystalline contents from Rietveld‐refined powder X‐ray data is presented and discussed for the example of mixed‐tacticity polyhydroxybutyrates. image
    Keywords: 548 ; polyhydroxybutyrates ; mixed tacticity ; paracrystallinity ; Rietveld refinement ; thermal factors
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 40
    facet.materialart.
    Unknown
    Concepts for nondestructive and depth‐resolved X‐ray residual stress analysis in the near‐surface region of nearly single crystalline materials with mosaic structure (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-27
    Description: Two evaluation concepts for nondestructive depth‐resolved X‐ray residual stress analysis in the near‐surface region of materials with cubic symmetry and nearly single crystalline structure are introduced by simulated examples. Both concepts are based on the same data acquisition strategy, which consists in the determination of lattice‐spacing depth profiles along the ⟨hkl⟩ poles by stepwise sample rotation around the scattering vector. Segmentation of these profiles parallel to the sample surface provides the lattice strain state as a function of depth. The first evaluation concept extends the crystallite group method developed for materials with pronounced crystallographic texture by the feature of depth resolution and can be applied to samples with arbitrary orientation. The second evaluation concept, which adapts the linear regression approach of the sin2ψ method for the case of single crystalline materials, is restricted to samples with (001) orientation. The influence of the strain‐free lattice parameter a0 on residual stress analysis using both evaluation concepts is discussed on the basis of explicitly derived relations.
    Description: Two data evaluation concepts are proposed for nondestructive and depth‐resolved X‐ray residual stress analysis by means of energy‐dispersive diffraction on materials featuring cubic symmetry and a nearly single crystalline structure. image
    Keywords: 548 ; residual stress ; X‐ray diffraction ; depth‐resolved analysis ; mosaic crystals
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 41
    facet.materialart.
    Unknown
    X‐ray dichroism in polyimide caused by non‐resonant scattering (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-30
    Description: Dichroism is one of the most important optical effects in both the visible and the X‐ray range. Besides absorption, scattering can also contribute to dichroism. This paper demonstrates that, based on the example of polyimide, materials can show tiny dichroism even far from electronic resonances due to scattering. Although the effect is small, it can lead to a measurable polarization change and might have influence on highly sensitive polarimetric experiments.
    Description: Aligned molecules, for example in polyimide foils, lead to small dichroism even far from resonances, which can be revealed by high‐precision X‐ray polarimetry. image
    Keywords: 548 ; polyimide ; polarization ; X‐ray polarimetry ; wide‐angle scattering ; X‐ray dichroism
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 42
    facet.materialart.
    Unknown
    Elastic stiffness coefficients of thiourea from thermal diffuse scattering (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-27
    Description: The complete elastic stiffness tensor of thiourea has been determined from thermal diffuse scattering (TDS) using high‐energy photons (100 keV). Comparison with earlier data confirms a very good agreement of the tensor coefficients. In contrast with established methods to obtain elastic stiffness coefficients (e.g. Brillouin spectroscopy, inelastic X‐ray or neutron scattering, ultrasound spectroscopy), their determination from TDS is faster, does not require large samples or intricate sample preparation, and is applicable to opaque crystals. Using high‐energy photons extends the applicability of the TDS‐based approach to organic compounds which would suffer from radiation damage at lower photon energies.
    Description: The elastic stiffness coefficients of thiourea are determined from thermal diffuse scattering. image
    Keywords: 548 ; thermal diffuse scattering ; elastic stiffness ; thiourea
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 43
    facet.materialart.
    Unknown
    Fast fitting of reflectivity data of growing thin films using neural networks (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-07-03
    Description: X‐ray reflectivity (XRR) is a powerful and popular scattering technique that can give valuable insight into the growth behavior of thin films. This study shows how a simple artificial neural network model can be used to determine the thickness, roughness and density of thin films of different organic semiconductors [diindenoperylene, copper(II) phthalocyanine and α‐sexithiophene] on silica from their XRR data with millisecond computation time and with minimal user input or a priori knowledge. For a large experimental data set of 372 XRR curves, it is shown that a simple fully connected model can provide good results with a mean absolute percentage error of 8–18% when compared with the results obtained by a genetic least mean squares fit using the classical Parratt formalism. Furthermore, current drawbacks and prospects for improvement are discussed.
    Description: Artificial neural networks trained with simulated data are shown to correctly and quickly determine film parameters from experimental X‐ray reflectivity curves.
    Keywords: 548 ; X‐ray reflectivity ; machine learning ; organic semi‐conductors ; neural networks
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 44
    facet.materialart.
    Unknown
    Numerically stable form factor of any polygon and polyhedron (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-05
    Description: Coordinate‐free expressions for the form factors of arbitrary polygons and polyhedra are derived using the divergence theorem and Stokes's theorem. Apparent singularities, all removable, are discussed in detail. Cancellation near the singularities causes a loss of precision that can be avoided by using series expansions. An important application domain is small‐angle scattering by nanocrystals.
    Description: Coordinate‐free expressions for the form factors of arbitrary polygons and polyhedra are derived using the divergence theorem and Stokes's theorem. Series expansions are used to ensure numeric precision close to apparent singularities. image
    Keywords: 548 ; form factors ; polyhedra ; Fourier shape transform
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 45
    facet.materialart.
    Unknown
    ROBL‐II at ESRF: a synchrotron toolbox for actinide research (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-30
    Description: ROBL‐II provides four different experimental stations to investigate actinide and other alpha‐ and beta‐emitting radionuclides at the new EBS storage ring of ESRF within an energy range of 3 to 35 keV. The XAFS station consists of a highly automatized, high sample throughput installation in a glovebox, to measure EXAFS and conventional XANES of samples routinely at temperatures down to 10 K, and with a detection limit in the sub‐p.p.m. range. The XES station with its five bent‐crystal analyzer, Johann‐type setup with Rowland circles of 1.0 and 0.5 m radii provides high‐energy resolution fluorescence detection (HERFD) for XANES, XES, and RIXS measurements, covering both actinide L and M edges together with other elements accessible in the 3 to 20 keV energy range. The six‐circle heavy duty goniometer of XRD‐1 is equipped for both high‐resolution powder diffraction as well as surface‐sensitive CTR and RAXR techniques. Single crystal diffraction, powder diffraction with high temporal resolution, as well as X‐ray tomography experiments can be performed at a Pilatus 2M detector stage (XRD‐2). Elaborate radioprotection features enable a safe and easy exchange of samples between the four different stations to allow the combination of several methods for an unprecedented level of information on radioactive samples for both fundamental and applied actinide and environmental research.
    Description: ROBL‐II at ESRF provides four experimental stations to investigate actinides with X‐ray absorption and emission spectroscopy, and with surface, high‐resolution powder, and single‐crystal X‐ray diffractometry.
    Keywords: 549 ; actinides ; EXAFS ; XANES ; HERFD‐XANES ; XAS ; XES ; RIXS ; XRD ; CTR ; RAXR ; surface diffraction
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 46
    facet.materialart.
    Unknown
    ATSAS 3.0: expanded functionality and new tools for small‐angle scattering data analysis (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-30
    Description: The ATSAS software suite encompasses a number of programs for the processing, visualization, analysis and modelling of small‐angle scattering data, with a focus on the data measured from biological macromolecules. Here, new developments in the ATSAS 3.0 package are described. They include IMSIM, for simulating isotropic 2D scattering patterns; IMOP, to perform operations on 2D images and masks; DATRESAMPLE, a method for variance estimation of structural invariants through parametric resampling; DATFT, which computes the pair distance distribution function by a direct Fourier transform of the scattering data; PDDFFIT, to compute the scattering data from a pair distance distribution function, allowing comparison with the experimental data; a new module in DATMW for Bayesian consensus‐based concentration‐independent molecular weight estimation; DATMIF, an ab initio shape analysis method that optimizes the search model directly against the scattering data; DAMEMB, an application to set up the initial search volume for multiphase modelling of membrane proteins; ELLLIP, to perform quasi‐atomistic modelling of liposomes with elliptical shapes; NMATOR, which models conformational changes in nucleic acid structures through normal mode analysis in torsion angle space; DAMMIX, which reconstructs the shape of an unknown intermediate in an evolving system; and LIPMIX and BILMIX, for modelling multilamellar and asymmetric lipid vesicles, respectively. In addition, technical updates were deployed to facilitate maintainability of the package, which include porting the PRIMUS graphical interface to Qt5, updating SASpy – a PyMOL plugin to run a subset of ATSAS tools – to be both Python 2 and 3 compatible, and adding utilities to facilitate mmCIF compatibility in future ATSAS releases. All these features are implemented in ATSAS 3.0, freely available for academic users at https://www.embl‐hamburg.de/biosaxs/software.html.
    Description: ATSAS is a comprehensive software suite for the processing, visualization, analysis and modelling of small‐angle scattering data. This article describes developments in the ATSAS 3.0 release, including new programs for data simulation and for the structural modelling of lipids, nucleic acids and polydisperse systems. image
    Keywords: 548 ; small‐angle scattering ; data analysis ; biological macromolecules ; structural modelling ; ATSAS
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 47
    facet.materialart.
    Unknown
    XGANDALF – extended gradient descent algorithm for lattice finding (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-27
    Description: Serial crystallography records still diffraction patterns from single, randomly oriented crystals, then merges data from hundreds or thousands of them to form a complete data set. To process the data, the diffraction patterns must first be indexed, equivalent to determining the orientation of each crystal. A novel automatic indexing algorithm is presented, which in tests usually gives significantly higher indexing rates than alternative programs currently available for this task. The algorithm does not require prior knowledge of the lattice parameters but can make use of that information if provided, and also allows indexing of diffraction patterns generated by several crystals in the beam. Cases with a small number of Bragg spots per pattern appear to particularly benefit from the new approach. The algorithm has been implemented and optimized for fast execution, making it suitable for real‐time feedback during serial crystallography experiments. It is implemented in an open‐source C++ library and distributed under the LGPLv3 licence. An interface to it has been added to the CrystFEL software suite.
    Description: A description and evaluation are given of XGANDALF, extended gradient descent algorithm for lattice finding, an algorithm developed for fast and accurate indexing of snapshot diffraction patterns. image
    Keywords: 548 ; indexing ; XGANDALF ; CrystFEL ; multiple lattices ; serial crystallography
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 48
    facet.materialart.
    Unknown
    pinkIndexer – a universal indexer for pink‐beam X‐ray and electron diffraction snapshots (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-27
    Description: A crystallographic indexing algorithm, pinkIndexer, is presented for the analysis of snapshot diffraction patterns. It can be used in a variety of contexts including measurements made with a monochromatic radiation source, a polychromatic source or with radiation of very short wavelength. As such, the algorithm is particularly suited to automated data processing for two emerging measurement techniques for macromolecular structure determination: serial pink‐beam X‐ray crystallography and serial electron crystallography, which until now lacked reliable programs for analyzing many individual diffraction patterns from crystals of uncorrelated orientation. The algorithm requires approximate knowledge of the unit‐cell parameters of the crystal, but not the wavelengths associated with each Bragg spot. The use of pinkIndexer is demonstrated by obtaining 1005 lattices from a published pink‐beam serial crystallography data set that had previously yielded 140 indexed lattices. Additionally, in tests on experimental serial crystallography diffraction data recorded with quasi‐monochromatic X‐rays and with electrons the algorithm indexed more patterns than other programs tested.
    Description: pinkIndexer, an algorithm developed for indexing of snapshot diffraction patterns recorded with pink‐beam X‐rays, monochromatic X‐rays and electrons, is described and its use evaluated. image
    Keywords: 548 ; indexing ; pinkIndexer ; CrystFEL ; pink X‐ray beam ; serial electron diffraction
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 49
    facet.materialart.
    Unknown
    Crystal structure of human CRM1, covalently modified by 2‐mercaptoethanol on Cys528, in complex with RanGTP (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-17
    Description: CRM1 is a nuclear export receptor that has been intensively targeted over the last decade for the development of antitumor and antiviral drugs. Structural analysis of several inhibitor compounds bound to CRM1 revealed that their mechanism of action relies on the covalent modification of a critical cysteine residue (Cys528 in the human receptor) located in the nuclear export signal‐binding cleft. This study presents the crystal structure of human CRM1, covalently modified by 2‐mercaptoethanol on Cys528, in complex with RanGTP at 2.58 Å resolution. The results demonstrate that buffer components can interfere with the characterization of cysteine‐dependent inhibitor compounds.
    Description: The covalent modification of human CRM1 by 2‐mercaptoethanol interferes with the characterization of cysteine‐dependent inhibitor compounds. image
    Keywords: 548 ; nuclear export ; cancer ; exportin 1 ; cysteine modification
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 50
    facet.materialart.
    Unknown
    Staircase array of inclined refractive multi‐lenses for large field of view pixel super‐resolution scanning transmission hard X‐ray microscopy (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-26
    Description: Owing to the development of X‐ray focusing optics during the past decades, synchrotron‐based X‐ray microscopy techniques allow the study of specimens with unprecedented spatial resolution, down to 10 nm, using soft and medium X‐ray photon energies, though at the expense of the field of view (FOV). One of the approaches to increase the FOV to square millimetres is raster‐scanning of the specimen using a single nanoprobe; however, this results in a long data acquisition time. This work employs an array of inclined biconcave parabolic refractive multi‐lenses (RMLs), fabricated by deep X‐ray lithography and electroplating to generate a large number of long X‐ray foci. Since the FOV is limited by the pattern height if a single RML is used by impinging X‐rays parallel to the substrate, many RMLs at regular intervals in the orthogonal direction were fabricated by tilted exposure. By inclining the substrate correspondingly to the tilted exposure, 378000 X‐ray line foci were generated with a length in the centimetre range and constant intervals in the sub‐micrometre range. The capability of this new X‐ray focusing device was first confirmed using ray‐tracing simulations and then using synchrotron radiation at BL20B2 of SPring‐8, Japan. Taking account of the fact that the refractive lens is effective for focusing high‐energy X‐rays, the experiment was performed with 35 keV X‐rays. Next, by scanning a specimen through the line foci, this device was used to perform large FOV pixel super‐resolution scanning transmission hard X‐ray microscopy (PSR‐STHXM) with a 780 ± 40 nm spatial resolution within an FOV of 1.64 cm × 1.64 cm (limited by the detector area) and a total scanning time of 4 min. Biomedical implant abutments fabricated via selective laser melting using Ti–6Al–4V medical alloy were measured by PSR‐STHXM, suggesting its unique potential for studying extended and thick specimens. Although the super‐resolution function was realized in one dimension in this study, it can be expanded to two dimensions by aligning a pair of presented devices orthogonally.
    Description: A new X‐ray focusing device generates hundreds of thousands of line foci, periodically spaced in the sub‐micrometre range, with centimetre length. It enables to achieve large FOV pixel super‐resolution scanning transmission hard X‐ray microscopy. image
    Keywords: 502.82 ; inclined refractive X‐ray multi‐lens array ; pixel super‐resolution ; scanning transmission hard X‐ray microscopy ; deep X‐ray lithography and electroplating
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 51
    facet.materialart.
    Unknown
    A new concept for temporal gating of synchrotron X‐ray pulses (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-07-02
    Description: A new concept for temporal gating of synchrotron X‐ray pulses based on laser‐induced thermal transient gratings is presented. First experimental tests of the concept yield a diffraction efficiency of 0.18%; however, the calculations indicate a theoretical efficiency and contrast of 〉30% and 10−5, respectively. The full efficiency of the pulse picker has not been reached yet due to a long‐range thermal deformation of the sample after absorption of the excitation laser. This method can be implemented in a broad spectral range (100 eV to 20 keV) and is only minimally invasive to an existing setup.
    Description: A new concept for temporal gating of synchrotron X‐ray pulses based on laser‐induced thermal transient gratings is presented.
    Keywords: 548 ; synchrotron ; time‐resolved ; thermal deformation ; transient grating ; pulse picking
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 52
    facet.materialart.
    Unknown
    The time‐resolved hard X‐ray diffraction endstation KMC‐3 XPP at BESSY II (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-06
    Description: The time‐resolved hard X‐ray diffraction endstation KMC‐3 XPP for optical pump/X‐ray probe experiments at the electron storage ring BESSY II is dedicated to investigating the structural response of thin film samples and heterostructures after their excitation with ultrashort laser pulses and/or electric field pulses. It enables experiments with access to symmetric and asymmetric Bragg reflections via a four‐circle diffractometer and it is possible to keep the sample in high vacuum and vary the sample temperature between ∼15 K and 350 K. The femtosecond laser system permanently installed at the beamline allows for optical excitation of the sample at 1028 nm. A non‐linear optical setup enables the sample excitation also at 514 nm and 343 nm. A time‐resolution of 17 ps is achieved with the `low‐α' operation mode of the storage ring and an electronic variation of the delay between optical pump and hard X‐ray probe pulse conveniently accesses picosecond to microsecond timescales. Direct time‐resolved detection of the diffracted hard X‐ray synchrotron pulses use a gated area pixel detector or a fast point detector in single photon counting mode. The range of experiments that are reliably conducted at the endstation and that detect structural dynamics of samples excited by laser pulses or electric fields are presented.
    Description: The KMC‐3 XPP endstation of the synchrotron BESSY II is dedicated to time‐resolved studies of structural dynamics of matter upon optical and/or electrical excitation using hard X‐ray diffraction with an accessible time range from 17 ps to several microseconds. image
    Keywords: 548 ; beamline instrumentation ; time‐resolved X‐ray diffraction ; optical excitation ; thermal transport ; ferroelectric switching
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 53
    facet.materialart.
    Unknown
    Disordered sodium alkoxides from powder data: crystal structures of sodium ethoxide, propoxide, butoxide and pentoxide, and some of their solvates (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-27
    Description: The crystal structures of sodium ethoxide (sodium ethanolate, NaOEt), sodium n‐propoxide (sodium n‐propanolate, NaOnPr), sodium n‐butoxide (sodium n‐butanolate, NaOnBu) and sodium n‐pentoxide (sodium n‐amylate, NaOnAm) were determined from powder X‐ray diffraction data. NaOEt crystallizes in space group P421m, with Z = 2, and the other alkoxides crystallize in P4/nmm, with Z = 2. To resolve space‐group ambiguities, a Bärnighausen tree was set up, and Rietveld refinements were performed with different models. In all structures, the Na and O atoms form a quadratic net, with the alkyl groups pointing outwards on both sides (anti‐PbO type). The alkyl groups are disordered. The disorder becomes even more pronounced with increasing chain length. Recrystallization from the corresponding alcohols yielded four sodium alkoxide solvates: sodium ethoxide ethanol disolvate (NaOEt·2EtOH), sodium n‐propoxide n‐propanol disolvate (NaOnPr·2nPrOH), sodium isopropoxide isopropanol pentasolvate (NaOiPr·5iPrOH) and sodium tert‐amylate tert‐amyl alcohol monosolvate (NaOtAm·tAmOH, tAm = 2‐methyl‐2‐butyl). Their crystal structures were determined by single‐crystal X‐ray diffraction. All these solvates form chain structures consisting of Na+, –O− and –OH groups, encased by alkyl groups. The hydrogen‐bond networks diverge widely among the solvate structures. The hydrogen‐bond topology of the iPrOH network in NaOiPr·5iPrOH shows branched hydrogen bonds and differs considerably from the networks in pure crystalline iPrOH.
    Description: The crystal structures of NaOEt, NaOPr, NaOBu and NaOAm (Am = amyl = pentyl) were determined from powder data. These compounds crystallize in an anti‐PbO structure in the space groups P21m and P4/nmm. Additionally, solvates with the composition NaOEt·2EtOH, NaOPr·2PrOH, NaOiPr·5iPrOH and NaOtAm·tAmOH were synthesized, and their structures were determined from single crystals. They form interesting chain structures of different compositions and topologies. image
    Keywords: 548 ; sodium alkoxide ; powder data ; solvate ; isopropanol ; Bärnighausen tree ; PXRD
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 54
    facet.materialart.
    Unknown
    Small‐angle X‐ray scattering from GaN nanowires on Si(111): facet truncation rods, facet roughness and Porod's law (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-27
    Description: Small‐angle X‐ray scattering from GaN nanowires grown on Si(111) is measured in the grazing‐incidence geometry and modelled by means of a Monte Carlo simulation that takes into account the orientational distribution of the faceted nanowires and the roughness of their side facets. It is found that the scattering intensity at large wavevectors does not follow Porod's law I(q) ∝ q−4. The intensity depends on the orientation of the side facets with respect to the incident X‐ray beam. It is maximum when the scattering vector is directed along a facet normal, reminiscent of surface truncation rod scattering. At large wavevectors q, the scattering intensity is reduced by surface roughness. A root‐mean‐square roughness of 0.9 nm, which is the height of just 3–4 atomic steps per micrometre‐long facet, already gives rise to a strong intensity reduction.
    Description: The intensity of small‐angle X‐ray scattering from GaN nanowires on Si(111) depends on the orientation of the side facets with respect to the incident beam. This reminiscence of truncation rod scattering gives rise to a deviation from Porod's law. A roughness of just 3–4 atomic steps per micrometre‐long side facet notably changes the intensity curves. image
    Keywords: 548 ; nanowires ; Porod's law ; facet truncation rods ; small‐angle X‐ray scattering ; SAXS ; grazing‐incidence small‐angle X‐ray scattering ; GISAXS
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 55
    facet.materialart.
    Unknown
    The accuracy of protein models automatically built into cryo‐EM maps with ARP/wARP (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-28
    Description: Recent developments in cryogenic electron microscopy (cryo‐EM) have enabled structural studies of large macromolecular complexes at resolutions previously only attainable using macromolecular crystallography. Although a number of methods can already assist in de novo building of models into high‐resolution cryo‐EM maps, automated and reliable map interpretation remains a challenge. Presented here is a systematic study of the accuracy of models built into cryo‐EM maps using ARP/wARP. It is demonstrated that the local resolution is a good indicator of map interpretability, and for the majority of the test cases ARP/wARP correctly builds 90% of main‐chain fragments in regions where the local resolution is 4.0 Å or better. It is also demonstrated that the coordinate accuracy for models built into cryo‐EM maps is comparable to that of X‐ray crystallographic models at similar local cryo‐EM and crystallographic resolutions. The model accuracy also correlates with the refined atomic displacement parameters.
    Keywords: 548 ; ARP/wARP ; model building ; cryo‐EM ; model accuracy ; sequence assignment
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 56
    facet.materialart.
    Unknown
    Synthesis, crystal structure and structure–property relations of strontium orthocarbonate, Sr2CO4 (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-05
    Description: Carbonates containing CO4 groups as building blocks have recently been discovered. A new orthocarbonate, Sr2CO4 is synthesized at 92 GPa and at a temperature of 2500 K. Its crystal structure was determined by in situ synchrotron single‐crystal X‐ray diffraction, selecting a grain from a polycrystalline sample. Strontium orthocarbonate crystallizes in the orthorhombic crystal system (space group Pnma) with CO4, SrO9 and SrO11 polyhedra as the main building blocks. It is isostructural to Ca2CO4. DFT calculations reproduce the experimental findings very well and have, therefore, been used to predict the equation of state, Raman and IR spectra, and to assist in the discussion of bonding in this compound.
    Description: A new orthocarbonate, Sr2CO4, was synthesized under extreme pressure and temperature conditions of 92 GPa and 2500 K, respectively. The crystal structure of the compound s fully characterized in situ by synchrotron single‐crystal X‐ray diffraction and DFT calculations were employed to provide insight into its equation of state, Raman and IR spectra, and bonding. image
    Keywords: 548 ; orthocarbonates ; crystal structure ; single‐crystal X‐ray diffraction ; high pressure ; Sr2CO4
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 57
    facet.materialart.
    Unknown
    Anomalous SAXS at P12 beamline EMBL Hamburg: instrumentation and applications (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-28
    Description: Small‐angle X‐ray scattering (SAXS) is an established method for studying nanostructured systems and in particular biological macromolecules in solution. To obtain element‐specific information about the sample, anomalous SAXS (ASAXS) exploits changes of the scattering properties of selected atoms when the energy of the incident X‐rays is close to the binding energy of their electrons. While ASAXS is widely applied to condensed matter and inorganic systems, its use for biological macromolecules is challenging because of the weak anomalous effect. Biological objects are often only available in small quantities and are prone to radiation damage, which makes biological ASAXS measurements very challenging. The BioSAXS beamline P12 operated by the European Molecular Biology Laboratory (EMBL) at the PETRA III storage ring (DESY, Hamburg) is dedicated to studies of weakly scattering objects. Here, recent developments at P12 allowing for ASAXS measurements are presented. The beamline control, data acquisition and data reduction pipeline of the beamline were adapted to conduct ASAXS experiments. Modelling tools were developed to compute ASAXS patterns from atomic models, which can be used to analyze the data and to help designing appropriate data collection strategies. These developments are illustrated with ASAXS experiments on different model systems performed at the P12 beamline.
    Keywords: 548 ; ASAXS ; biological SAXS ; metalloproteins ; gold nanoparticles ; anomalous scattering ; beamline development
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 58
    facet.materialart.
    Unknown
    Symmetry relations in wurtzite nitrides and oxide nitrides and the curious case of Pmc21 (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-27
    Description: Binary III–V nitrides such as AlN, GaN and InN in the wurtzite‐type structure have long been considered as potent semiconducting materials because of their optoelectronic properties, amongst others. With rising concerns over the utilization of scarce elements, a replacement of the trivalent cations by others in ternary and multinary nitrides has led to the development of different variants of nitrides and oxide nitrides crystallizing in lower‐symmetry variants of wurtzite. This work presents the symmetry relationships between these structural types specific to nitrides and oxide nitrides and updates some prior work on this matter. The non‐existence of compounds crystallizing in Pmc21, formally the highest subgroup of the wurtzite type fulfilling Pauling's rules for 1:1:2 stoichiometries, has been puzzling scientists for a while; a rationalization is given, from a crystallographic basis, of why this space group is unlikely to be adopted.
    Keywords: 548 ; group–subgroup relationships ; nitride materials ; wurtzite type
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 59
    facet.materialart.
    Unknown
    Comparison and evaluation of pair distribution functions, using a similarity measure based on cross‐correlation functions (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-20
    Description: An approach for the comparison of pair distribution functions (PDFs) has been developed using a similarity measure based on cross‐correlation functions. The PDF is very sensitive to changes in the local structure, i.e. small deviations in the structure can cause large signal shifts and significant discrepancies between the PDFs. Therefore, a comparison based on pointwise differences (e.g. R values and difference curves) may lead to the assumption that the investigated PDFs as well as the corresponding structural models are not in agreement at all, whereas a careful visual inspection of the investigated structural models and corresponding PDFs may reveal a relatively good match. To quantify the agreement of different PDFs for those cases an alternative approach is introduced: the similarity measure based on cross‐correlation functions. In this paper, the power of this application of the similarity measure to the analysis of PDFs is highlighted. The similarity measure is compared with the classical Rwp values as representative of the comparison based on pointwise differences as well as with the Pearson product‐moment correlation coefficient, using polymorph IV of barbituric acid as an example.
    Description: A novel approach to the quantification of the agreement between pair distribution functions by a similarity measure based on cross‐correlation functions is introduced and evaluated. image
    Keywords: 548 ; pair distribution functions ; similarity measures ; total scattering techniques ; cross‐correlation functions ; R values
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 60
    facet.materialart.
    Unknown
    Novel experimental setup for megahertz X‐ray diffraction in a diamond anvil cell at the High Energy Density (HED) instrument of the European X‐ray Free‐Electron Laser (EuXFEL) (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-26
    Description: The high‐precision X‐ray diffraction setup for work with diamond anvil cells (DACs) in interaction chamber 2 (IC2) of the High Energy Density instrument of the European X‐ray Free‐Electron Laser is described. This includes beamline optics, sample positioning and detector systems located in the multipurpose vacuum chamber. Concepts for pump–probe X‐ray diffraction experiments in the DAC are described and their implementation demonstrated during the First User Community Assisted Commissioning experiment. X‐ray heating and diffraction of Bi under pressure, obtained using 20 fs X‐ray pulses at 17.8 keV and 2.2 MHz repetition, is illustrated through splitting of diffraction peaks, and interpreted employing finite element modeling of the sample chamber in the DAC.
    Description: The high‐precision X‐ray diffraction (XRD) setup for work with diamond anvil cells (DACs) in Interaction Chamber 2 of the High Energy Density (HED) instrument of the European X‐ray Free‐Electron Laser is described. image
    Keywords: 548 ; diamond anvil cells ; X‐ray free‐electron lasers ; high‐precision X‐ray diffraction ; finite element modeling
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 61
    facet.materialart.
    Unknown
    The anisotropy in the optical constants of quartz crystals for soft X‐rays (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-26
    Description: The refractive index of a y‐cut SiO2 crystal surface is reconstructed from orientation‐dependent soft X‐ray reflectometry measurements in the energy range from 45 to 620 eV. Owing to the anisotropy of the crystal structure in the (100) and (001) directions, a significant deviation of the measured reflectance at the Si L2,3 and O K absorption edges is observed. The anisotropy in the optical constants reconstructed from these data is also confirmed by ab initio Bethe–Salpeter equation calculations for the O K edge. This new experimental data set expands the existing literature data for quartz crystal optical constants significantly, particularly in the near‐edge regions.
    Description: The refractive index of a y‐cut SiO2 crystal surface is reconstructed from polarization‐dependent soft X‐ray reflectometry measurements in the energy range from 45 to 620 eV. The reconstructed anisotropy in the optical constants is also confirmed by ab initio Bethe–Salpeter equation calculations of the O K edge. image
    Keywords: 548 ; optical constants ; quartz ; anisotropy ; soft X‐ray reflectometry
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 62
    facet.materialart.
    Unknown
    Unravelling the crystal structure of Nd5.8WO12−δ and Nd5.7W0.75Mo0.25O12−δ mixed ionic electronic conductors (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-07-05
    Description: Mixed ionic electronic conducting ceramics Nd6−yWO12−δ (δ is the oxygen deficiency) provide excellent stability in harsh environments containing strongly reactive gases such as CO2, CO, H2, H2O or H2S. Due to this chemical stability, they are promising and cost‐efficient candidate materials for gas separation, catalytic membrane reactors and protonic ceramic fuel cell technologies. As in La6−yWO12−δ, the ionic/electronic transport mechanism in Nd6−yWO12−δ is expected to be largely controlled by the crystal structure, the conclusive determination of which is still lacking. This work presents a crystallographic study of Nd5.8WO12−δ and molybdenum‐substituted Nd5.7W0.75Mo0.25O12−δ prepared by the citrate complexation route. High‐resolution synchrotron and neutron powder diffraction data were used in combined Rietveld refinements to unravel the crystal structure of Nd5.8WO12−δ and Nd5.7W0.75Mo0.25O12−δ. Both investigated samples crystallize in a defect fluorite crystal structure with space group Fm3m and doubled unit‐cell parameter due to cation ordering. Mo replaces W at both Wyckoff sites 4a and 48h and is evenly distributed, in contrast with La6−yWO12−δ. X‐ray absorption spectroscopy as a function of partial pressure pO2 in the near‐edge regions excludes oxidation state changes of Nd (Nd3+) and W (W6+) in reducing conditions: the enhanced hydrogen permeation, i.e. ambipolar conduction, observed in Mo‐substituted Nd6−yWO12−δ is therefore explained by the higher Mo reducibility and the creation of additional – disordered – oxygen vacancies.
    Description: The crystal structures of non‐substituted and Mo‐substituted neodymium tungstates are described in detail through neutron diffraction and high‐resolution X‐ray diffraction. Combined X‐ray and neutron diffraction refinements and electron probe micro‐analysis were employed to locate Mo atoms in the crystal structure of Nd6−yW1−zMozO12−δ (z = 0, 0.25), while X‐ray absorption spectroscopy in the near‐edge regions confirmed no changes in the oxidation states of Nd and W.
    Keywords: 548 ; powder diffraction ; mixed conductors ; X‐ray absorption spectroscopy (XAS) ; Nd6−yWO12−δ
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 63
    facet.materialart.
    Unknown
    High‐temperature treatments of niobium under high vacuum, dilute air‐ and nitrogen‐atmospheres as investigated by in situ X‐ray absorption spectroscopy (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-30
    Description: Niobium metal foils were heat‐treated at 900°C under different conditions and in situ investigated with time‐resolved X‐ray absorption fine‐structure (EXAFS and XANES) measurements. The present study aims to mimic the conditions usually applied for heat treatments of Nb materials used for superconducting radiofrequency cavities, in order to better understand the evolving processes during vacuum annealing as well as for heat treatments in controlled dilute gases. Annealing in vacuum in a commercially available cell showed a substantial amount of oxidation, so that a designated new cell was designed and realized, allowing treatments under clean high‐vacuum conditions as well as under well controllable gas atmospheres. The experiments performed under vacuum demonstrated that the original structure of the Nb foils is preserved, while a detailed evaluation of the X‐ray absorption fine‐structure data acquired during treatments in dilute air atmospheres (10−5 mbar to 10−3 mbar) revealed a linear oxidation with the time of the treatment, and an oxidation rate proportional to the oxygen (air) pressure. The structure of the oxide appears to be very similar to that of polycrystalline NbO. The cell also permits controlled exposures to other reactive gases at elevated temperatures; here the Nb foils were exposed to dilute nitrogen atmospheres after a pre‐conditioning of the studied Nb material for one hour under high‐vacuum conditions, in order to imitate typical conditions used for nitrogen doping of cavity materials. Clear structural changes induced by the N2 exposure were found; however, no evidence for the formation of niobium nitride could be derived from the EXAFS and XANES experiments. The presented results establish the feasibility to study the structural changes of the Nb materials in situ during heat treatments in reactive gases with temporal resolution, which are important to better understand the underlaying mechanisms and the dynamics of phase formation during those heat treatments in more detail.
    Keywords: 548 ; in situ EXAFS ; high temperature ; time‐resolved EXAFS ; niobium
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 64
    facet.materialart.
    Unknown
    Pressure‐induced Pb–Pb bonding and phase transition in Pb2SnO4 (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-03-27
    Description: High‐pressure single‐crystal to 20 GPa and powder diffraction measurements to 50 GPa, show that the structure of Pb2SnO4 strongly distorts on compression with an elongation of one axis. A structural phase transition occurs between 10 GPa and 12 GPa, with a change of space group from Pbam to Pnam. The resistivity decreases by more than six orders of magnitude when pressure is increased from ambient conditions to 50 GPa. This insulator‐to‐semiconductor transition is accompanied by a reversible appearance change from transparent to opaque. Density functional theory‐based calculations show that at ambient conditions the channels in the structure host the stereochemically‐active Pb 6s2 lone electron pairs. On compression the lone electron pairs form bonds between Pb2+ ions. Also provided is an assignment of irreducible representations to the experimentally observed Raman bands.
    Description: The structure of Pb2SnO4 is found to strongly distort on compression and a structural phase transition with a change of space group from Pbam to Pnam occurs at ∼11 GPa. Our complementary DFT‐based calculations show that at ambient conditions, the channels in the structure host the stereochemically active Pb 6s2 lone electron pairs which form bonds between the Pb2+ ions with increasing pressure. image
    Keywords: 548 ; lead stannate (Pb2SnO4) ; density functional theory ; high‐pressure X‐ray diffraction ; pressure‐induced phase transition ; insulator–semiconductor transition
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 65
    facet.materialart.
    Unknown
    A discussion on `Domain formation and phase transitions in the wurtzite‐based heterovalent ternaries: a Landau theory analysis' (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-05
    Description: Heterovalent ternary nitrides are considered one of the promising classes of materials for photovoltaics, combining attractive physical properties with low toxicity and element abundance. One of the front‐runner systems under consideration is ZnSnN2. Although it is nominally a ternary compound, no clear crystallographic evidence for cation ordering has been observed so far. An attempt to elucidate this discrepancy [Quayle (2020). Acta Cryst. A76, 410–420] was the trigger for an intensive discussion between the authors, and an agreement was reached to elaborate on some points in order to set things in perspective. Rather than using a conventional comment–answer scheme, this is published in the form of a joint discussion to celebrate constructive criticism and collegiality.
    Description: A scientific exchange on an earlier paper [Quayle (2020). Acta Cryst. A76, 410–420] has led to the clarification of some of the points. image
    Keywords: 548 ; group–subgroup relationships ; nitride materials ; wurtzite type
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 66
    facet.materialart.
    Unknown
    X‐SPEC: a 70 eV to 15 keV undulator beamline for X‐ray and electron spectroscopies (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-26
    Description: X‐SPEC is a high‐flux spectroscopy beamline at the KIT (Karlsruhe Institute of Technology) Synchrotron for electron and X‐ray spectroscopy featuring a wide photon energy range. The beamline is equipped with a permanent magnet undulator with two magnetic structures of different period lengths, a focusing variable‐line‐space plane‐grating monochromator, a double‐crystal monochromator and three Kirkpatrick–Baez mirror pairs. By selectively moving these elements in or out of the beam, X‐SPEC is capable of covering an energy range from 70 eV up to 15 keV. The flux of the beamline is maximized by optimizing the magnetic design of the undulator, minimizing the number of optical elements and optimizing their parameters. The beam can be focused into two experimental stations while maintaining the same spot position throughout the entire energy range. The first experimental station is optimized for measuring solid samples under ultra‐high‐vacuum conditions, while the second experimental station allows in situ and operando studies under ambient conditions. Measurement techniques include X‐ray absorption spectroscopy (XAS), extended X‐ray absorption fine structure (EXAFS), photoelectron spectroscopy (PES) and hard X‐ray PES (HAXPES), as well as X‐ray emission spectroscopy (XES) and resonant inelastic X‐ray scattering (RIXS).
    Description: X‐SPEC is a high‐flux undulator beamline for electron and X‐ray spectroscopy with an energy range from 70 eV to 15 keV. It offers X‐ray absorption spectroscopy (XAS), extended X‐ray absorption fine structure (EXAFS), photoelectron spectroscopy (PES) and hard X‐ray PES (HAXPES), as well as X‐ray emission spectroscopy (XES) and resonant inelastic X‐ray scattering (RIXS) for in vacuo, in situ and operando sample environments. image
    Keywords: 548 ; undulator beamline ; soft X‐ray ; tender X‐ray ; hard X‐ray ; in situ ; operando ; HAXPES ; RIXS ; XAS ; XES
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 67
    facet.materialart.
    Unknown
    On incoherent diffractive imaging (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2022-04-07
    Description: Incoherent diffractive imaging (IDI) promises structural analysis with atomic resolution based on intensity interferometry of pulsed X‐ray fluorescence emission. However, its experimental realization is still pending and a comprehensive theory of contrast formation has not been established to date. Explicit expressions are derived for the equal‐pulse two‐point intensity correlations, as the principal measured quantity of IDI, with full control of the prefactors, based on a simple model of stochastic fluorescence emission. The model considers the photon detection statistics, the finite temporal coherence of the individual emissions, as well as the geometry of the scattering volume. The implications are interpreted in view of the most relevant quantities, including the fluorescence lifetime, the excitation pulse, as well as the extent of the scattering volume and pixel size. Importantly, the spatiotemporal overlap between any two emissions in the sample can be identified as a crucial factor limiting the contrast and its dependency on the sample size can be derived. The paper gives rigorous estimates for the optimum sample size, the maximum photon yield and the expected signal‐to‐noise ratio under optimal conditions. Based on these estimates, the feasibility of IDI experiments for plausible experimental parameters is discussed. It is shown in particular that the mean number of photons per detector pixel which can be achieved with X‐ray fluorescence is severely limited and as a consequence imposes restrictive constraints on possible applications.
    Description: Starting from a simple model of stochastic fluorescence emission, a theory is derived of contrast formation and signal‐to‐noise ratio for incoherent diffractive imaging; its feasibility for plausible experimental parameters is discussed. image
    Keywords: ddc:548
    Language: English
    Type: doc-type:article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 68
    facet.materialart.
    Unknown
    Structure determination of organic compounds by a fit to the pair distribution function from scratch without prior indexing (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-06-26
    Description: A method for the ab initio crystal structure determination of organic compounds by a fit to the pair distribution function (PDF), without prior knowledge of lattice parameters and space group, has been developed. The method is called `PDF‐Global‐Fit' and is implemented by extension of the program FIDEL (fit with deviating lattice parameters). The structure solution is based on a global optimization approach starting from random structural models in selected space groups. No prior indexing of the powder data is needed. The new method requires only the molecular geometry and a carefully determined PDF. The generated random structures are compared with the experimental PDF and ranked by a similarity measure based on cross‐correlation functions. The most promising structure candidates are fitted to the experimental PDF data using a restricted simulated annealing structure solution approach within the program TOPAS, followed by a structure refinement against the PDF to identify the correct crystal structure. With the PDF‐Global‐Fit it is possible to determine the local structure of crystalline and disordered organic materials, as well as to determine the local structure of unindexable powder patterns, such as nanocrystalline samples, by a fit to the PDF. The success of the method is demonstrated using barbituric acid as an example. The crystal structure of barbituric acid form IV solved and refined by the PDF‐Global‐Fit is in excellent agreement with the published crystal structure data.
    Keywords: 548 ; pair distribution function analysis ; structure determination ; total scattering technique ; similarity measures ; PDF‐Global‐Fit
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 69
    facet.materialart.
    Unknown
    Structural basis of chitin utilization by a GH20 β‐N‐acetylglucosaminidase from Vibrio campbellii strain ATCC BAA‐1116 (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-07-01
    Description: Vibrio species play a crucial role in maintaining the carbon and nitrogen balance between the oceans and the land through their ability to employ chitin as a sole source of energy. This study describes the structural basis for the action of the GH20 β‐N‐acetylglucosaminidase (VhGlcNAcase) in chitin metabolism by Vibrio campbellii (formerly V. harveyi) strain ATCC BAA‐1116. Crystal structures of wild‐type VhGlcNAcase in the absence and presence of the sugar ligand, and of the unliganded D437A mutant, were determined. VhGlcNAcase contains three distinct domains: an N‐terminal carbohydrate‐binding domain linked to a small α+β domain and a C‐terminal (β/α)8 catalytic domain. The active site of VhGlcNAcase has a narrow, shallow pocket that is suitable for accommodating a small chitooligosaccharide. VhGlcNAcase is a monomeric enzyme of 74 kDa, but its crystal structures show two molecules of enzyme per asymmetric unit, in which Gln16 at the dimeric interface of the first molecule partially blocks the entrance to the active site of the neighboring molecule. The GlcNAc unit observed in subsite −1 makes exclusive hydrogen bonds to the conserved residues Arg274, Tyr530, Asp532 and Glu584, while Trp487, Trp546, Trp582 and Trp505 form a hydrophobic wall around the −1 GlcNAc. The catalytic mutants D437A/N and E438A/Q exhibited a drastic loss of GlcNAcase activity, confirming the catalytic role of the acidic pair (Asp437–Glu438).
    Description: Crystal structures of a GH20 β‐N‐acetylglucosaminidase from V. campbellii reveal substrate specificity in chitin utilization.
    Keywords: 577.14 ; GH20 β‐N‐acetylglucosaminidase ; chitin recycling ; Vibrio spp ; marine bacteria
    Type: article
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 70
    facet.materialart.
    Unknown
    Resolution of a bent‐crystal spectrometer for X‐ray free‐electron laser pulses: diamond versus silicon (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-09-29
    Description: The resolution function of a spectrometer based on a strongly bent single crystal (bending radius of 10 cm or less) is evaluated. It is shown that the resolution is controlled by two parameters: (i) the ratio of the lattice spacing of the chosen reflection to the crystal thickness and (ii) a single parameter comprising crystal thickness, its bending radius, distance to a detector, and anisotropic elastic constants of the chosen crystal. The results allow the optimization of the parameters of bent‐crystal spectrometers for the hard X‐ray free‐electron laser sources.
    Description: The resolution function of a bent‐crystal spectrometer for pulses of an X‐ray free‐electron laser is evaluated. Under appropriate conditions, the energy resolution reaches the ratio of the lattice spacing to the crystal thickness. image
    Keywords: 548 ; X‐ray free‐electron lasers ; X‐ray spectroscopy ; bent crystals ; diamond crystal optics ; femtosecond X‐ray diffraction
    Type: map
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 71
    facet.materialart.
    Unknown
    Separation of the inelastic and elastic scattering in time‐of‐flight mode on the pinhole small‐angle neutron scattering diffractometer KWS‐2 (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-09-29
    Description: To study and control the incoherent inelastic background in small‐angle neutron scattering, which makes a significant contribution to the detected scattering from hydrocarbon systems, the KWS‐2 small‐angle neutron scattering diffractometer operated by the Jülich Centre for Neutron Science (JCNS) at Heinz‐Maier Leibnitz Zentrum (MLZ), Garching, Germany, was equipped with a secondary single‐disc chopper that is placed in front of the sample stage. This makes it possible to record in time‐of‐flight mode the scattered neutrons in the high‐Q regime of the instrument (i.e. short incoming wavelengths and detection distances) and to discard the inelastic component from the measured data. Examples of measurements on different materials routinely used as standard samples, sample containers and solvents in the experiments at KWS‐2 are presented. When only the elastic region of the spectrum is used in the data‐reduction procedure, a decrease of up to two times in the incoherent background of the experimentally measured scattering cross section may be obtained. The proof of principle is demonstrated on a solution of bovine serum albumin in D2O.
    Description: A new chopper has been installed at the sample position in front of the sample stage at the KWS‐2 small‐angle neutron‐scattering diffractometer of the Jülich Centre for Neutron Science. The pulsed beam and the time‐of‐flight data acquisition enable the separation of elastic and inelastic scattering from hydrogenous samples.
    Keywords: 548 ; TOF‐SANS ; incoherent neutron scattering ; inelastic neutron scattering ; hydrocarbon systems
    Type: map
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 72
    facet.materialart.
    Unknown
    Czochralski growth of mixed cubic sesquioxide crystals in the ternary system Lu2O3–Sc2O3–Y2O3 (2021)
    International Union of Crystallography | 5 Abbey Square, Chester, Cheshire CH1 2HU, England
    Details
    Publication Date: 2021-09-29
    Description: Cubic rare‐earth sesquioxide crystals are strongly demanded host materials for high power lasers, but due to their high melting points investigations on their thermodynamics and the growth of large‐size crystals of high optical quality remain a challenge. Detailed thermal investigations of the ternary system Lu2O3–Sc2O3–Y2O3 revealing a large range of compositions with melting temperatures below 2200°C and a minimum of 2053°C for the composition (Sc0.45Y0.55)2O3 are presented. These reduced temperatures enable for the first time the growth of high optical quality mixed sesquioxide crystals with disordered structure by the conventional Czochralski method from iridium crucibles. An (Er0.07Sc0.50Y0.43)2O3 crystal is successfully grown and characterized with respect to its crystallographic properties as well as its composition, thermal conductivity and optical absorption in the 1 µm range.
    Description: The phase diagram of the ternary system Lu2O3–Sc2O3–Y2O3 is investigated and compositions with melting points below 2200°C are found. This allows for the first successful growth of the mixed cubic sesquioxide crystal (Er0.07Sc0.50Y0.43)2O3 by the Czochralski method from an iridium crucible. image
    Keywords: 548 ; crystal growth ; optical materials ; phase diagrams ; melting points ; rare earth sesquioxides
    Type: map
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    CITATION GEO-LEO
  • 73
    facet.materialart.
    Unknown
    Mathematics for Physicists. Introductory Concepts and Methods. By Alexander Altland and Jan von Delft. Cambridge University Press, 2019. Hardback, Pp. 720. Price GBP 39.99. ISBN 9781108471220. (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-01-01
    Electronic ISSN: 2053-2733
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 74
    facet.materialart.
    Unknown
    A cloud platform for atomic pair distribution function analysis: PDFitc (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-01-01
    Description: A cloud web platform for analysis and interpretation of atomic pair distribution function (PDF) data (PDFitc) is described. The platform is able to host applications for PDF analysis to help researchers study the local and nanoscale structure of nanostructured materials. The applications are designed to be powerful and easy to use and can, and will, be extended over time through community adoption and development. The currently available PDF analysis applications, structureMining, spacegroupMining and similarityMapping, are described. In the first and second the user uploads a single PDF and the application returns a list of best-fit candidate structures, and the most likely space group of the underlying structure, respectively. In the third, the user can upload a set of measured or calculated PDFs and the application returns a matrix of Pearson correlations, allowing assessment of the similarity between different data sets. structureMining is presented here as an example to show the easy-to-use workflow on PDFitc. In the future, as well as using the PDFitc applications for data analysis, it is hoped that the community will contribute their own codes and software to the platform.
    Electronic ISSN: 2053-2733
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 75
    facet.materialart.
    Unknown
    Spiral tetrahedral packing in the β-Mn crystal as symmetry realization of the 8D E 8 lattice (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-01-01
    Description: Experimental values of atomic positions in the β-Mn crystal permit one to distinguish among them a fragment of the helix containing 15 interpenetrating distorted icosahedra, 90 vertices and 225 tetrahedra. This fragment corresponds to the closed helix of 15 icosahedra in the 4D {3, 3, 5} polytope. The primitive cubic lattice of these icosahedral helices envelopes not only all atoms of β-Mn, but also all tetrahedra belonging to the tiling of the β-Mn structure. The 2D projection of all atomic positions in the β-Mn unit cells shows that they are situated (by neglecting small differences) on three circumferences containing 2D projections of 90 vertices of the {3, 3, 5} polytope on the same plane. Non-crystallographic symmetry of the β-Mn crystal is defined by mapping the closed icosahedral helix of the {3, 3, 5} polytope into 3D Euclidean space E 3. This interpretation must be correlated also with the known previous determination of non-crystallographic symmetry of the β-Mn crystal by mapping into the 3D E 3 space system of icosahedra from the 6D cubic B 6 lattice. The recently proposed determination of non-crystallographic symmetry of the β-Mn crystal actually uses the symmetries of the 8D E 8 lattice, in which both the 4D {3, 3, 5} polytope and cubic 6D B 6 lattice can be inserted.
    Electronic ISSN: 2053-2733
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 76
    facet.materialart.
    Unknown
    Crystal structure, Hirshfeld surface analysis, DFT and molecular docking investigation of 2-(2-oxo-1,3-oxazolidin-3-yl)ethyl 2-[2-(2-oxo-1,3-oxazolidin-3-yl)ethoxy]quinoline-4-carboxylate (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-01-01
    Description: In the molecular structure of the title compound, C20H21N3O7, the quinoline ring system is slightly bent, with a dihedral angle between the phenyl and the pyridine rings of 3.47 (7)°. In the crystal, corrugated layers of molecules extending along the ab plane are generated by C—H...O hydrogen bonds. The intermolecular interactions were quantified by Hirshfeld surface analysis and two-dimensional fingerprint plots. The most significant contributions to the crystal packing are from H...H (42.3%), H...O/O...H (34.5%) and H...C/ C...H (17.6%) contacts. Molecular orbital calculations providing electron-density plots of the HOMO and LUMO as well as molecular electrostatic potentials (MEP) were computed, both with the DFT/B3LYP/6–311 G++(d,p) basis set. A molecular docking study between the title molecule and the COVID-19 main protease (PDB ID: 6LU7) was performed, showing that it is a good agent because of its affinity and ability to adhere to the active sites of the protein.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 77
    facet.materialart.
    Unknown
    Synthesis and structural characterization of hexa-μ2-chlorido-μ4-oxido-tetrakis{[4-(phenylethynyl)pyridine-κN]copper(II)} dichloromethane monosolvate (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-01-01
    Description: In the crystal structure of the title compound, [Cu4Cl6O(C13H9N)4]·CH2Cl2, the core molecular structure consists of a Cu4 tetrahedron with a central interstitial O atom. Each edge of the Cu4 tetrahedron is bridged by a chlorido ligand. Each copper(II) cation is coordinated to the central O atom, two chlorido ligands and one N atom of the 4-phenylethynylpyridine ligand. In the crystal, the molecules are linked by intermolecular C—H...Cl interactions. Furthermore, C—H...π and π–π interactions also connect the molecules, forming a three-dimensional network. Hirshfeld surface analysis indicates that the most important contributions for the packing arrangement are from H...H and C...H/H...C interactions.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 78
    facet.materialart.
    Unknown
    Crystal structure, Hirshfeld surface analysis and energy framework study of 6-formyl-7,8,9,11-tetrahydro-5H-pyrido[2,1-b]quinazolin-11-one (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-01-01
    Description: At 100 K, the title compound, C13H12N2O2, crystallizes in the orthorhombic space group Pna21 with two very similar molecules in the asymmetric unit. An intramolecular N—H...O hydrogen bond leads to an S(6) graph-set motif in each of the molecules. Intermolecular π–π stacking and C=O...π interactions involving the aldehyde O atoms link molecules into stacks parallel to [100]. A Hirshfeld surface analysis indicates that the most important contributions to the crystal packing stem from H...H (49.4%) and H...O/O...H (21.5%) interactions. Energy framework calculations reveal a significant contribution of dispersion energy. The crystal studied was refined as a two-component inversion twin.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 79
    facet.materialart.
    Unknown
    Two 3-amino-1H-pyrazol-2-ium salts containing organic anions, and an orthorhombic polymorph of 3-amino-1H-pyrazol-2-ium nitrate (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-01-01
    Description: Co-crystallization from methanol of 3-amino-1H-pyrazole with 3,5-dinitrobenzoic acid produces 3-amino-1H-pyrazol-2-ium 3,5-dinitrobenzoate monohydrate, C3H6N3 +·C7H3N2O6 −·H2O, (I), while similar co-crystallization of this pyrazole with an equimolar quantity of fumaric acid produces bis(3-amino-1H-pyrazol-2-ium) fumarate–fumaric acid (1/1), 2C3H6N3 +·C4H2O4 2−·C4H4O4, (II). The reaction of 3-amino-1H-pyrazole with a dilute solution of nitric acid in methanol yields a second, orthorhombic polymorph of 3-amino-1H-pyrazol-2-ium nitrate, C3H6N3 +·NO3 −, (III). In each of (I)–(III), the bond distances in the cation provide evidence for extensive delocalization of the positive charge. In each of (I) and (II), an extensive series of O—H...O and N—H...O hydrogen bonds links the components into complex sheets, while in the structure of (III), the ions are linked by multiple N—H...O hydrogen bonds into a three-dimensional arrangement. Comparisons are made with the structures of some related compounds.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 80
    facet.materialart.
    Unknown
    Evaluation of the data-collection strategy for room-temperature micro-crystallography studied by serial synchrotron rotation crystallography combined with the humid air and glue-coating method (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-02-25
    Description: Synchrotron serial crystallography (SSX) is an emerging data-collection method for micro-crystallography on synchrotron macromolecular (MX) crystallography beamlines. At SPring-8, the feasibility of the fixed-target approach was examined by collecting data using a 2D raster scan combined with goniometer rotation. Results at cryogenic temperatures demonstrated that rotation is effective for efficient data collection in SSX and the method was named serial synchrotron rotation crystallography (SS-ROX). To use this method for room-temperature (RT) data collection, a humid air and glue-coating (HAG) method was developed in which data were collected from polyvinyl alcohol-coated microcrystals fixed on a loop under humidity-controlled air. The performance and the RT data-collection strategy for micro-crystallography were evaluated using microcrystals of lysozyme. Although a change in unit-cell dimensions of up to 1% was observed during data collection, the impact on data quality was marginal. A comparison of data obtained at various absorbed doses revealed that absorbed doses of up to 210 kGy were tolerable in both global and local damage. Although this limits the number of photons deposited on each crystal, increasing the number of merged images improved the resolution. On the basis of these results, an equation was proposed that relates the achievable resolution to the total photon flux used to obtain a data set.
    Electronic ISSN: 2059-7983
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 81
    facet.materialart.
    Unknown
    Diffraction structural biology – an introductory overview (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-02-25
    Electronic ISSN: 2059-7983
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 82
    facet.materialart.
    Unknown
    Crystal structure of the GTP-binding protein-like domain of AGAP1 (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-31
    Description: AGAP1 is often considered to regulate membrane trafficking, protein transport and actin cytoskeleton dynamics. Recent studies have shown that aberrant expression of AGAP1 is associated with many diseases, including neurodevelopmental disorders and acute lymphoblastic leukemia. It has been proposed that the GTP-binding protein-like domain (GLD) is involved in the binding of cofactors and thus regulates the catalytic activity of AGAP1. To obtain a better understanding of the pathogenic mechanism underpinning AGAP1-related diseases, it is essential to obtain structural information. Here, the GLD (residues 70–235) of AGAP1 was overexpressed in Escherichia coli BL21 (DE3) cells. Affinity and gel-filtration chromatography were used to obtain AGAP1GLD with high purity for crystallization. Using the hanging-drop vapor-diffusion method with the protein at a final concentration of 20 mg ml−1, AGAP1GLD protein crystals of suitable size were obtained. The crystals were found to diffract to 3.0 Å resolution and belonged to space group I4, with unit-cell parameters a = 100.39, b = 100.39, c = 48.08 Å. The structure of AGAP1GLD exhibits the highly conserved functional G1–G5 loops and is generally similar to other characterized ADP-ribosylation factor (Arf) GTPase-activating proteins (GAPs), implying an analogous function to Arf GAPs. Additionally, this study indicates that AGAP1 could be classified as a type of NTPase, the activity of which might be regulated by protein partners or by its other domains. Taken together, these results provide insight into the regulatory mechanisms of AGAP1 in cell signaling.
    Electronic ISSN: 2053-230X
    Topics: Biology , Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 83
    facet.materialart.
    Unknown
    Novel clostridial cell-surface hemicellulose-binding CBM3 proteins (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-31
    Description: A novel member of the family 3 carbohydrate-binding modules (CBM3s) is encoded by a gene (Cthe_0271) in Clostridium thermocellum which is the most highly expressed gene in the bacterium during its growth on several types of biomass substrates. Surprisingly, CtCBM3-0271 binds to at least two different types of xylan, instead of the common binding of CBM3s to cellulosic substrates. CtCBM3-0271 was crystallized and its three-dimensional structure was solved and refined to a resolution of 1.8 Å. In order to learn more about the role of this type of CBM3, a comparative study with its orthologue from Clostridium clariflavum (encoded by the Clocl_1192 gene) was performed, and the three-dimensional structure of CcCBM3-1192 was determined to 1.6 Å resolution. Carbohydrate binding by CcCBM3-1192 was found to be similar to that by CtCBM3-0271; both exhibited binding to xylan rather than to cellulose. Comparative structural analysis of the two CBM3s provided a clear functional correlation of structure and binding, in which the two CBM3s lack the required number of binding residues in their cellulose-binding strips and thus lack cellulose-binding capabilities. This is an enigma, as CtCBM3-0271 was reported to be a highly expressed protein when the bacterium was grown on cellulose. An additional unexpected finding was that CcCBM3-1192 does not contain the calcium ion that was considered to play a structural stabilizing role in the CBM3 family. Despite the lack of calcium, the five residues that form the calcium-binding site are conserved. The absence of calcium results in conformational changes in two loops of the CcCBM3-1192 structure. In this context, superposition of the non-calcium-binding CcCBM3-1192 with CtCBM3-0271 and other calcium-binding CBM3s reveals a much broader two-loop region in the former compared with CtCBM3-0271.
    Electronic ISSN: 2053-230X
    Topics: Biology , Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 84
    facet.materialart.
    Unknown
    Structural differences/similarities of diastereotopic groups in three new chiral phosphoramides (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-29
    Description: The crystal structures of two single-enantiomer amidophosphoesters with an (O)2P(O)(N) skeleton and one single-enantiomer phosphoric triamide with an (N)2P(O)(N) skeleton were studied. The compounds are diphenyl [(R)-(+)-α-4-dimethylbenzylamido]phosphate, (I), and diphenyl [(S)-(−)-α-4-dimethylbenzylamido]phosphate, (II), both C21H22NO3P, and N-(2,6-difluorobenzoyl)-N′,N′′-bis[(R)-(+)-α-ethylbenzyl]phosphoric triamide, C25H28F2N3O2P, (III). The asymmetric units contain two amidophosphoester molecules for (I) and (II), and one phosphoric triamide molecule for (III). In the crystal structures of (I) and (II), molecules are assembled in a similar one-dimensional chiral ribbon architecture, but with almost a mirror-image relationship with respect to each other through N—H...O(P) and C—H...O(P) hydrogen bonds along [010]. In the crystal structure of (III), the chiral tape architecture along [100] is mediated by N—H...O(P) and N—H...O(C) hydrogen bonds, and the tapes are connected into slabs by C—H...O interactions (along the ab plane). The differences/similarities of the two diastereotopic phenoxy groups in (I)/(II) and the two chiral amine fragments in (III) were studied on the grounds of geometry, conformation and contribution to the crystal packing, as well as 1H and 13C signals in a solution NMR study.
    Electronic ISSN: 2053-2296
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 85
    facet.materialart.
    Unknown
    Preliminary results of neutron and X-ray diffraction data collection on a lytic polysaccharide monooxygenase under reduced and acidic conditions (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-31
    Description: Lytic polysaccharide monooxygenases (LPMOs) are copper-center enzymes that are involved in the oxidative cleavage of the glycosidic bond in crystalline cellulose and other polysaccharides. The LPMO reaction is initiated by the addition of a reductant and oxygen to ultimately form an unknown activated copper–oxygen species that is responsible for polysaccharide-substrate H-atom abstraction. Given the sensitivity of metalloproteins to radiation damage, neutron protein crystallography provides a nondestructive technique for structural characterization while also informing on the positions of H atoms. Neutron cryo-crystallography permits the trapping of catalytic intermediates, thereby providing insight into the protonation states and chemical nature of otherwise short-lived species in the reaction mechanism. To characterize the reaction-mechanism intermediates of LPMO9D from Neurospora crassa, a cryo-neutron diffraction data set was collected from an ascorbate-reduced crystal. A second neutron diffraction data set was collected at room temperature from an LPMO9D crystal exposed to low-pH conditions to probe the protonation states of ionizable groups involved in catalysis under acidic conditions.
    Electronic ISSN: 2053-230X
    Topics: Biology , Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 86
    facet.materialart.
    Unknown
    Chloridotetrakis(imidazole)copper(II) chloride. Corrigendum (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-31
    Description: In the article by Li et al. [Acta Cryst. (2007), E63, m2536], four imidazole H atoms are missing in the refinement.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 87
    facet.materialart.
    Unknown
    Structure of Λ(δλλ)-[Co(en)3]I3(I)2 (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-31
    Description: The structure of tris(ethane-1,2-diamine-κ2 N,N')cobalt(III) bis(iodide) triiodide, [Co(C2H8N2)3]I3(I)2, at 120 K has orthorhombic (P212121) symmetry. The diamine nitrogen atoms form N—H...I hydrogen bonds throughout the lattice, resulting in a three-dimensional network, which involves the iodide and all atoms in the triiodide anions.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 88
    facet.materialart.
    Unknown
    Symmetry relations in wurtzite nitrides and oxide nitrides and the curious case of Pmc21 (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-23
    Description: Binary III–V nitrides such as AlN, GaN and InN in the wurtzite-type structure have long been considered as potent semiconducting materials because of their optoelectronic properties, amongst others. With rising concerns over the utilization of scarce elements, a replacement of the trivalent cations by others in ternary and multinary nitrides has led to the development of different variants of nitrides and oxide nitrides crystallizing in lower-symmetry variants of wurtzite. This work presents the symmetry relationships between these structural types specific to nitrides and oxide nitrides and updates some prior work on this matter. The non-existence of compounds crystallizing in Pmc21, formally the highest subgroup of the wurtzite type fulfilling Pauling's rules for 1:1:2 stoichiometries, has been puzzling scientists for a while; a rationalization is given, from a crystallographic basis, of why this space group is unlikely to be adopted.
    Electronic ISSN: 2053-2733
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 89
    facet.materialart.
    Unknown
    A discussion on `Domain formation and phase transitions in the wurtzite-based heterovalent ternaries: a Landau theory analysis' (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-23
    Description: Heterovalent ternary nitrides are considered one of the promising classes of materials for photovoltaics, combining attractive physical properties with low toxicity and element abundance. One of the front-runner systems under consideration is ZnSnN2. Although it is nominally a ternary compound, no clear crystallographic evidence for cation ordering has been observed so far. An attempt to elucidate this discrepancy [Quayle (2020). Acta Cryst. A76, 410–420] was the trigger for an intensive discussion between the authors, and an agreement was reached to elaborate on some points in order to set things in perspective. Rather than using a conventional comment–answer scheme, this is published in the form of a joint discussion to celebrate constructive criticism and collegiality.
    Electronic ISSN: 2053-2733
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 90
    facet.materialart.
    Unknown
    Crystal structure of cis-(1,4,8,11-tetraazacyclotetradecane-κ4 N)bis(thiocyanato-κN)chromium(III) bromide from synchrotron X-ray diffraction data (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-02-02
    Description: The crystal structure of the title complex, cis-[Cr(NCS)2(cyclam)]Br (cyclam = 1,4,8,11-tetraazacyclotetradecane, C10H24N4), has been determined from synchrotron X-ray data. The asymmetric unit contains one [Cr(NCS)2(cyclam)]+ cation and one bromide anion. The CrIII ion of the complex cation is coordinated by the four N atoms of the cyclam ligand and by two N-coordinating NCS groups in a cis arrangement, displaying a distorted octahedral coordination sphere. The Cr—N(cyclam) bond lengths are in the range 2.075 (3) to 2.081 (3) Å while the average Cr—N(NCS) bond length is 1.996 (16) Å. The macrocyclic cyclam moiety adopts the most stable cis-V conformation. The crystal structure is stabilized by intermolecular hydrogen bonds involving the cyclam N—H groups as donor groups, and the bromide anion and the S atom of one of the NCS ligands as acceptor groups.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 91
    facet.materialart.
    Unknown
    Synthesis, crystal structure and Hirshfeld surface analysis of [bis(diphenylphosphanyl)methane-κP]chloridobis[2-(pyridin-2-yl)phenyl-κ2 N,C 1]iridium(III) (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-02-02
    Description: The title IrIII complex, [Ir(C11H8N)2Cl(C25H22P2)], was synthesized from the substitution reaction between the (ppy)2Ir(μ-Cl)2Ir(ppy)2 (ppy = deprotonated 2-phenylpyridine, C11H8N−) dimer and 1,1-bis(diphenylphosphanyl)methane (dppm, C25H22P2) under an argon gas atmosphere for 20 h. The IrIII atom is coordinated by two C,N-bidentate ppy anions, a unidentate dppm ligand and a chloride anion in a distorted octahedral IrC2N2PCl arrangement. The N donor atoms of the ppy ligands are mutually trans while the C atoms are cis. Intramolecular aromatic π–π stacking between the phenyl rings of ppy and dppm, and C—H...Cl interactions are observed. In the crystal, C—H...Cl and C—H...π contacts link the molecules into a three-dimensional network. A Hirshfeld surface analysis was carried out to further quantify the intermolecular interactions, and indicated that H...H contacts (63.9%) dominate the packing.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 92
    facet.materialart.
    Unknown
    Crystal structure of (E)-1-(3-benzyl-5-phenyl-1,3-thiazol-2-ylidene)-2-[(E)-1,2,3,4-tetrahydronaphthalen-1-ylidene]hydrazin-1-ium bromide (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-23
    Description: In the title molecular salt, C26H24N3S+·Br−, the dihedral angles between the thiazole ring and its attached phenyl and benzoyl rings are 54.81 (7) and 85.51 (7)°, respectively. In the crystal, ion pairs are linked by C—H...Br and N—H...Br hydrogen bonds and are connected into helical chains extending along the c-axis direction by weak, electrostatic S...Br− interactions. A Hirshfeld surface analysis was performed, which showed the dominant role of H...H contacts (51.3%).
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 93
    facet.materialart.
    Unknown
    The structure of Prp2 bound to RNA and ADP-BeF3 − reveals structural features important for RNA unwinding by DEAH-box ATPases (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-30
    Description: Noncoding intron sequences present in precursor mRNAs need to be removed prior to translation, and they are excised via the spliceosome, a multimegadalton molecular machine composed of numerous protein and RNA components. The DEAH-box ATPase Prp2 plays a crucial role during pre-mRNA splicing as it ensures the catalytic activation of the spliceosome. Despite high structural similarity to other spliceosomal DEAH-box helicases, Prp2 does not seem to function as an RNA helicase, but rather as an RNA-dependent ribonucleoprotein particle-modifying ATPase. Recent crystal structures of the spliceosomal DEAH-box ATPases Prp43 and Prp22, as well as of the related RNA helicase MLE, in complex with RNA have contributed to a better understanding of how RNA binding and processivity might be achieved in this helicase family. In order to shed light onto the divergent manner of function of Prp2, an N-terminally truncated construct of Chaetomium thermophilum Prp2 was crystallized in the presence of ADP-BeF3 − and a poly-U12 RNA. The refined structure revealed a virtually identical conformation of the helicase core compared with the ADP-BeF3 −- and RNA-bound structure of Prp43, and only a minor shift of the C-terminal domains. However, Prp2 and Prp43 differ in the hook-loop and a loop of the helix-bundle domain, which interacts with the hook-loop and evokes a different RNA conformation immediately after the 3′ stack. On replacing these loop residues in Prp43 by the Prp2 sequence, the unwinding activity of Prp43 was abolished. Furthermore, a putative exit tunnel for the γ-phosphate after ATP hydrolysis could be identified in one of the Prp2 structures.
    Electronic ISSN: 2059-7983
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 94
    facet.materialart.
    Unknown
    Cryo-EM of kinesin-binding protein: challenges and opportunities from protein-surface interactions (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-30
    Description: Kinesin-binding protein (KBP) is an important selective inhibitor of specific kinesin family members and its genetic disruption causes Goldberg–Shprintzen syndrome. Cryo-electron microscopy (cryo-EM) has recently been used to reveal the structure of KBP alone (72 kDa) and in complex with the motor domain of the mitotic kinesin-12 KIF15 (110 kDa). KBP is an α-solenoid, tetratricopeptide-repeat protein that interacts with the microtubule-binding region of the kinesin motor domain and blocks microtubule attachment. Numerous challenges arose relating to the behavior of KBP and KBP–kinesin complexes during cryo-EM sample preparation. These included the partial denaturation of KBP by air–water interfaces, protein aggregation resulting from carbon interaction and preferential orientation. Sample preparation with a graphene oxide substrate enabled the eventual structure determination. Here, experiences with preparing these samples are detailed, bringing attention to some of the challenges and opportunities that are likely to arise from protein-surface interactions.
    Electronic ISSN: 2059-7983
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 95
    facet.materialart.
    Unknown
    Identification of Mg2+ ions next to nucleotides in cryo-EM maps using electrostatic potential maps (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-30
    Description: Cryo electron microscopy (cryo-EM) can produce maps of macromolecules that have resolutions that are sufficiently high that structural details such as chemical modifications, water molecules and bound metal ions can be discerned. However, those accustomed to interpreting the electron-density maps of macromolecules produced by X-ray crystallography need to be careful when assigning features such as these in cryo-EM maps because cations, for example, interact far more strongly with electrons than they do with X-rays. Using simulated electrostatic potential (ESP) maps as a tool led us to re-examine a recent cryo-EM map of the human ribosome, and we realized that some of the ESP peaks originally identified as novel groups covalently bonded to the N7, O6 or O4 atoms of several guanines, adenines or uridines, respectively, in this structure are likely to instead represent Mg2+ ions coordinated to these atoms, which provide only partial charge compensation compared with Mg2+ ions located next to phosphate groups. In addition, direct evidence is provided for a variation in the level of 2′-O ribose methylation of nucleotides in the human ribosome. ESP maps can thus help in identifying ions next to nucleotide bases, i.e. at positions that can be difficult to address in cryo-EM maps due to charge effects, which are specifically encountered in cryo-EM. This work is particularly relevant to nucleoprotein complexes and shows that it is important to consider charge effects when interpreting cryo-EM maps, thus opening possibilities for localizing charges in structures that may be relevant for enzymatic mechanisms and drug interactions.
    Electronic ISSN: 2059-7983
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 96
    facet.materialart.
    Unknown
    Crystal structures of β-1,4-N-acetylglucosaminyltransferase 2: structural basis for inherited muscular dystrophies (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-30
    Description: The canonical O-mannosylation pathway in humans is essential for the functional glycosylation of α-dystroglycan. Disruption of this post-translational modification pathway leads to congenital muscular dystrophies. The first committed step in the construction of a functional matriglycan structure involves the post-translational modification of α-dystroglycan. This is essential for binding extracellular matrix proteins and arenaviruses, and is catalyzed by β-1,4-N-acetylglucosaminyltransferase 2 (POMGNT2). While another glycosyl transferase, β-1,4-N-acetylglucosaminyltransferase 1 (POMGNT1), has been shown to be promiscuous in extending O-mannosylated sites, POMGNT2 has been shown to display significant primary amino-acid selectivity near the site of O-mannosylation. Moreover, several single point mutations in POMGNT2 have been identified in patients with assorted dystroglycanopathies such as Walker–Warburg syndrome and limb girdle muscular dystrophy. To gain insight into POMGNT2 function in humans, the enzyme was expressed as a soluble, secreted fusion protein by transient infection of HEK293 suspension cultures. Here, crystal structures of POMGNT2 (amino-acid residues 25–580) with and without UDP bound are reported. Consistent with a novel fold and a unique domain organization, no molecular-replacement model was available and phases were obtained through crystallization of a selenomethionine variant of the enzyme in the same space group. Tetragonal (space group P4212; unit-cell parameters a = b = 129.8, c = 81.6 Å, α = γ = β = 90°) crystals with UDP bound diffracted to 1.98 Å resolution and contained a single monomer in the asymmetric unit. Orthorhombic (space group P212121; unit-cell parameters a = 142.3, b = 153.9, c = 187.4 Å, α = γ = β = 90°) crystals were also obtained; they diffracted to 2.57 Å resolution and contained four monomers with differential glycosylation patterns and conformations. These structures provide the first rational basis for an explanation of the loss-of-function mutations and offer significant insights into the mechanics of this important human enzyme.
    Electronic ISSN: 2059-7983
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 97
    facet.materialart.
    Unknown
    Protein identification from electron cryomicroscopy maps by automated model building and side-chain matching (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-30
    Description: Using single-particle electron cryo-microscopy (cryo-EM), it is possible to obtain multiple reconstructions showing the 3D structures of proteins imaged as a mixture. Here, it is shown that automatic map interpretation based on such reconstructions can be used to create atomic models of proteins as well as to match the proteins to the correct sequences and thereby to identify them. This procedure was tested using two proteins previously identified from a mixture at resolutions of 3.2 Å, as well as using 91 deposited maps with resolutions between 2 and 4.5 Å. The approach is found to be highly effective for maps obtained at resolutions of 3.5 Å and better, and to have some utility at resolutions as low as 4 Å.
    Electronic ISSN: 2059-7983
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 98
    facet.materialart.
    Unknown
    Polymorphs of phenazine hexacyanoferrate(II) hydrate: supramolecular isomerism in a 2D hydrogen-bonded network (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-10
    Description: The crystal structures of two polymorphs of a phenazine hexacyanoferrate(II) salt/cocrystal, with the formula (Hphen)3[H2Fe(CN)6][H3Fe(CN)6]·2(phen)·2H2O, are reported. The polymorphs are comprised of (Hphen)2[H2Fe(CN)6] trimers and (Hphen)[(phen)2(H2O)2][H3Fe(CN)6] hexamers connected into two-dimensional (2D) hydrogen-bonded networks through strong hydrogen bonds between the [H2Fe(CN)6]2− and [H3Fe(CN)6]− anions. The layers are further connected by hydrogen bonds, as well as through π–π stacking of phenazine moieties. Aside from the identical 2D hydrogen-bonded networks, the two polymorphs share phenazine stacks comprising both protonated and neutral phenazine molecules. On the other hand, the polymorphs differ in the conformation, placement and orientation of the hydrogen-bonded trimers and hexamers within the hydrogen-bonded networks, which leads to different packing of the hydrogen-bonded layers, as well as to different hydrogen bonding between the layers. Thus, aside from an exceptional number of symmetry-independent units (nine in total), these two polymorphs show how robust structural motifs, such as charge-assisted hydrogen bonding or π-stacking, allow for different arrangements of the supramolecular units, resulting in polymorphism.
    Print ISSN: 2052-5192
    Electronic ISSN: 2052-5206
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 99
    facet.materialart.
    Unknown
    Structural and theoretical analysis of 2-chloro-4-nitroaniline and 2-methyl-6-nitroaniline salts (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-02-18
    Description: The crystal structures of five new salts of 2-chloro-4-nitroaniline (2Cl4na) and 2-methyl-6-nitroaniline (2m6na) with inorganic acids, namely, 2-chloro-4-nitroanilinium bromide, C6H6ClN2O2 +·Br− (1), 2-chloro-4-nitroanilinium hydrogen sulfate, C6H6ClN2O2 +·HSO4 − (2), 2-methyl-6-nitroanilinium bromide, C7H9N2O2 +·Br− (3), 2-methyl-6-nitroanilinium triiodide, C7H9N2O2 +·I3 − (4), and 2-methyl-6-nitroanilinium hydrogen sulfate, C7H9N2O2 +·HSO4 − (5), were determined by single-crystal X-ray diffraction. Theoretical calculations of the relaxed potential energy surface (rPES) revealed that the energy barriers for the rotation of the nitro group for isolated H2Cl4na+ and H2m6na+ cations are 4.6 and 11.6 kcal mol−1, respectively. The ammonium group and respective anions form hydrogen bonds which are the most important interactions and are arranged in zero- (in 3), one- (in 1 and 4) or two-dimensional (in 2 and 5) networks. Hydrogen-bonding patterns were analyzed by means of mathematical relationships between graph-set descriptors and compared with previously reported nitroaniline salts. Hirshfeld surface analysis indicates that the nitro group plays a dominant role among the weak interactions, i.e. C—H...O(NO2), NO2...π(Ar) and O(NO2)...π(NO2). The frequency of the νsNO2 vibration is correlated with the type of interaction in which the NO2 group is involved. Analysis of the νsNO2 band observed in the IR and Raman spectra allowed an assessment of its shift in the sequence (H2m6na)I3 (4) 〈 (H2m6na)HSO4 (5) 〈 (H2m6na)Br (3) 〈 (H2Cl4na)Br (1) 〈 (H2Cl4na)HSO4 (2).
    Electronic ISSN: 2053-2296
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
  • 100
    facet.materialart.
    Unknown
    Crystallographic characterization of (C5H4SiMe3)3U(BH4) (2021)
    International Union of Crystallography
    Details
    Publication Date: 2021-03-12
    Description: New syntheses have been developed for the synthesis of (borohydrido-κ3 H)tris[η5-(trimethylsilyl)cyclopentadienyl]uranium(IV), [U(BH4)(C8H13Si)3] or Cp′3U(BH4) (Cp′ = C5H4SiMe3) and its structure has been determined by single-crystal X-ray crystallography. This compound crystallized in the space group Poverline{1} and the structure features three η 5-coordinated Cp′ rings and a κ 3-coordinated (BH4)− ligand.
    Electronic ISSN: 2056-9890
    Topics: Chemistry and Pharmacology , Geosciences
    Published by International Union of Crystallography
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    PAPER CURRENT
Close ⊗
This website uses cookies and the analysis tool Matomo. More information can be found here...