Journal of Applied Crystallography最新文献

{"title":"A cryogenic probe for <i>in situ</i> delivery of gaseous samples for neutron scattering.","authors":"Chris Baldwin, Larissa Lopes Cavalcante, Nicholas D Stapleton, Tait Francis, Tim D'Adam, Helen E Maynard-Casely","doi":"10.1107/S1600576726000543","DOIUrl":"https://doi.org/10.1107/S1600576726000543","url":null,"abstract":"<p><p>This laboratory note describes an optimized solution for the delivery of gaseous samples for neutron scattering measurements. The original design to accomplish this, though effective, was not ideal from a use and maintenance perspective - especially in view of the time-constrained nature of neutron scattering experiments. In response to user demand and a need for a more reliable solution the gas-delivery sticks have been significantly redesigned, with a number of innovations applied. Here we describe the resulting equipment and the operation of the gas sticks for condensation experiments, and we present results using this equipment and methodology.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 2","pages":"700-704"},"PeriodicalIF":2.8,"publicationDate":"2026-02-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13060611/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147645142","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Non-reciprocal spin excitations across the skyrmion-paramagnetic phase transition in MnSi.","authors":"T Weber, K Schmalzl, J Waizner, A Bauer, M Garst, C Pfleiderer","doi":"10.1107/S1600576725011537","DOIUrl":"https://doi.org/10.1107/S1600576725011537","url":null,"abstract":"<p><p>The magnetic excitations of the skyrmion lattice in MnSi comprise a multitude of individual modes, which are non-reciprocal and thereby propagate unidirectionally. We report inelastic neutron scattering experiments for temperatures near and above the skyrmion-paramagnetic phase transition in the chiral magnet MnSi, tracking the evolution from the skyrmion lattice towards the high-temperature paramagnetic state. Within the resolution of the triple-axis measurements the excitations vary smoothly across the skyrmion-paramagnetic boundary, and the quasi-elastic paramagnetic signal under applied field retains the non-reciprocal character seen in the skyrmion phase even far above the critical temperature. Using a resolution convolution, our results are consistent with linear spin-wave theory.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 2","pages":"326-333"},"PeriodicalIF":2.8,"publicationDate":"2026-02-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13060468/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147645184","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A user-friendly goniometer-compatible fixed-target platform for macromolecular crystallography at synchrotrons.","authors":"Swagatha Ghosh, Analia Banacore, Per Norder, Monica Bjelčić, Arpitha Kabbinale, Padmini Nileshwar, Gabrielle Wehlander, Daniele de Sanctis, Shibom Basu, Julien Orlans, Adams Vallejos, Leonard M G Chavas, Richard Neutze, Gisela Brändén","doi":"10.1107/S1600576725011513","DOIUrl":"https://doi.org/10.1107/S1600576725011513","url":null,"abstract":"<p><p>Fixed-target platforms provide convenient support for microcrystals during serial X-ray crystallography studies using synchrotron radiation. Here, we describe a simple user-friendly 3D-printed support where the crystals are sandwiched between two layers of thin X-ray-transparent membrane resulting in very low scattering background. The platform is compatible with magnetic mounting onto the standard goniometer of macromolecular crystallography beamlines. Our design utilizes a 96-well frame that facilitates hanging-drop experiments directly on the membrane using conventional crystallization plates, thereby eliminating multiple pipetting and crystal handling steps. Crystals can be enclosed in a sandwich and packed into 'cassettes', preventing the risk of the sample drying out during room-temperature transportation to synchrotron sources. The versatility of the platform is demonstrated by five structures solved using different crystallization and data-collection strategies. Lysozyme single-crystal rotational crystallography at room temperature is shown, as well as microcrystal serial data collection under cryogenic conditions. On-chip microcrystallization is illustrated by use of a photosynthetic reaction center as an example. Finally, serial crystallography data collection at room temperature from microcrystals of the membrane protein cytochrome <i>c</i> oxidase crystallized in lipidic cubic phase is presented.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 2","pages":"303-315"},"PeriodicalIF":2.8,"publicationDate":"2026-02-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13060402/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147645177","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Neutron reflectometry instrumentation at the ISIS source: current state.","authors":"Mario Campana, Andrew Caruana, Luke Clifton, Stephen Hall, Arwel Hughes, Christy Kinane, Maximilian Skoda, Oleksandr Tomchuk, John Webster","doi":"10.1107/S1600576726000397","DOIUrl":"https://doi.org/10.1107/S1600576726000397","url":null,"abstract":"<p><p>Neutron reflectometry (NR) at the ISIS Neutron and Muon Source has evolved into a mature, versatile technique for investigating the structure and dynamics of interfaces across a wide range of scientific disciplines, including soft matter, magnetism, quantum materials and environmental systems. This article provides a comprehensive overview of the current instrumentation available at ISIS, detailing the capabilities of the four operational reflectometers - OFFSPEC, INTER, POLREF and SURF - including their time-of-flight configurations, scattering geometries, polarization options and range of accessible sample environments. Special emphasis is placed on the integration of advanced sample environments, automated control software and data analysis tools, including <i>IBEX</i>, <i>MANTID</i> and the <i>ISIS Data Analysis as a Service</i> (<i>IDAaaS</i>) platform, which collectively facilitate efficient, reproducible and high-quality NR measurements. Representative scientific highlights demonstrate the unique potential of NR to resolve sub-nanometre structural and kinetic information in biological membranes, thin functional films, quantum fluids and environmental interfaces. By consolidating detailed technical information, operational characteristics and examples of cutting-edge research, this article serves as a practical guide for new and experienced users, helping them design experiments, select suitable instruments and sample environments, and fully exploit the capabilities of ISIS neutron reflectometers.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 2","pages":"381-391"},"PeriodicalIF":2.8,"publicationDate":"2026-02-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13060407/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147645229","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Compact tape-driven sample delivery system for serial femtosecond crystallography.","authors":"Jungmin Kang, Yoshiaki Shimazu, Fangjia Luo, Ayumi Yamashita, Tomoyuki Tanaka, Yuichi Inubushi, Kensuke Tono, Nipawan Nuemket, Allen M Orville, So Iwata, Eriko Nango, Makina Yabashi","doi":"10.1107/S1600576726000063","DOIUrl":"https://doi.org/10.1107/S1600576726000063","url":null,"abstract":"<p><p>We have developed a compact tape drive (CoT) with on-demand sample delivery for time-resolved serial femtosecond crystallography (SFX) experiments, which can deliver sample droplets and/or initiate reactions with a drop-on-drop strategy. Two disposable piezoelectric injectors are positioned in tandem along the tape to produce a queue of nanolitre-scale droplets. X-ray free-electron laser pulses arrive perpendicular to and pass through the broad face of the tape. The pulse is synchronized and aligned to the droplets, thereby enabling highly efficient SFX data collection. The tape transport speed and the delivery distance can be varied to control the mixing time from approximately 130 ms to tens of seconds. We conducted time-resolved SFX experiments utilizing a basic enzymatic reaction model of hen egg white lysozyme (HEWL) and <i>N</i>-acetyl-<i>D</i>-glucosamine (GlcNAc) to demonstrate the drop-on-drop capabilities of the CoT, and the full binding process of GlcNAc to HEWL was observed at 1.3-9.7 s.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 2","pages":"291-302"},"PeriodicalIF":2.8,"publicationDate":"2026-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13060467/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147645155","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Quantum refinement with electron diffraction and X-ray free-electron laser data: comparative study of ribonucleotide reductase dimetal site.","authors":"Kristoffer J M Lundgren, Xiaoli Sun, Laura Pacoste, Rohit Kumar, Gerhard Hofer, Hongyi Xu, Xiaodong Zou, Martin Högbom, Esko Oksanen, Ulf Ryde","doi":"10.1107/S1600576725011264","DOIUrl":"https://doi.org/10.1107/S1600576725011264","url":null,"abstract":"<p><p>Quantum refinement (QR) is an approach in which the empirical restraints used in standard structural refinement to ensure that the details of the structure, <i>e.g.</i> bond lengths and angles, make chemical sense are replaced by more accurate quantum mechanical calculations for a small but interesting part of the structure. QR has previously been used for X-ray and neutron crystallography, cryogenic electron microscopy, nuclear magnetic resonance, and extended X-ray absorption fine structure. Here, QR is used for the first time for X-ray free-electron laser (XFEL) crystallography and microcrystal electron diffraction (MicroED). As a test case, we use six structures of the R2a protein of ribonucleotide reductase, concentrating on the binuclear Fe₂ site in either the oxidized (Fe₂ ^III) or reduced (Fe₂ ^II) state, two each from single-crystal X-ray (SCX) crystallography, XFEL crystallography or MicroED. The results show that QR works well for data from all three radiation sources, even though scattering factors for neutral atoms had to be used for MicroED. QR corrects unrealistically short Fe-O distances in the reduced SCX structure and gives improved real-space <i>Z</i> scores for the reduced MicroED structure. The three methods give similar structures, apart from variation in the weak water ligands and in the binding of carboxylate groups (monodentate, bidentate or a mixture). By performing QR for three protonation states of the bridging solvent molecule, we could show that it is undoubtedly a water molecule in the reduced XFEL and MicroED structures (it is not present in the SCX structure) and that it is not water in the oxidized structures. The XFEL data indicate that it is O^2- in the oxidized XFEL structure, in agreement with the spectroscopic results. However, for the SCX structure, O^2- and OH^- give comparable results, whereas OH^- is slightly preferred in the MicroED structure. This indicates that the SCX and MicroED structures may be partly photoreduced during data collection.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 2","pages":"277-290"},"PeriodicalIF":2.8,"publicationDate":"2026-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13060455/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147645246","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Software for small-angle neutron scattering contrast variation experiment planning and data analysis.","authors":"Susan Krueger, Kathryn L Sarachan, Emre Brookes, Joseph E Curtis","doi":"10.1107/S1600576725011677","DOIUrl":"https://doi.org/10.1107/S1600576725011677","url":null,"abstract":"<p><p>Contrast variation (CV) small-angle neutron scattering (SANS) enables the determination of structural parameters from individual components in multi-component biological complexes in solution. Researchers can selectively highlight different parts of a multi-component system by varying the contrast between the components, typically through adjusting the deuteration level of solvents or specific molecular constituents. While this approach provides unique insights into component shapes, spatial arrangements and interactions, SANS CV experiments require substantial resources, specialized facilities and, often, a steep learning curve. To address these challenges and improve the likelihood of a successful experiment, a new contrast software suite has been developed within the <i>SASSIE-web</i> framework, allowing researchers to plan and simulate experiments <i>in silico</i>, integrate structural modeling, and streamline both experiment design and CV data analysis into a unified platform.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 2","pages":"631-639"},"PeriodicalIF":2.8,"publicationDate":"2026-02-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13060616/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147645327","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Evolution of crystallographic texture and material anisotropy effects resulting from uniaxial deformation for high-strength steels with high manganese content.","authors":"Michael Zuern, Morteza Dadkhah, Thomas Nitschke-Pagel, Jens Gibmeier","doi":"10.1107/S1600576725010350","DOIUrl":"10.1107/S1600576725010350","url":null,"abstract":"<p><p>Steels used in the automotive industry have seen significant improvements within the past few decades, as economic and environmental efficiency play major and increasing roles in current individual transportation. In particular, it has been possible to combine high formability with high strength, which contributes to passenger safety, vehicle performance and efficiency. Deep-drawing steels with higher manganese content play a special role in the class of automotive body sheet materials, in which the final mechanical properties are achieved, for example, through twinning-induced plasticity and/or transformation-induced plasticity effects. In this study, the deformation behavior of steels X40MnCrAlV-19-2.5-2, HCT690T and S355MC was investigated using laboratory X-ray diffraction analyses. The investigations cover the evolution of crystallographic texture and material anisotropy resulting from uniaxial deformation, as well as their influence on diffraction data, especially in the context of stress analyses. In contrast to the situation in the initial as-rolled state, the induced deformations up to the limit of uniform elongation lead to the formation of strong textures and a considerable impairment of the diffraction data due to material anisotropy. However, the formed crystallographic textures do not suffice to describe this impairment. Rather, this effect is mainly attributable to intergranular strains, which are caused by different degrees of deformation of individual crystallites within the elasto-plastic regime. These phenomena need to be considered, and this is demonstrated using the application example of a welded metal sheet. Correction approaches are proposed and their application is illustrated, with a focus on how readily the residual stresses can be evaluated.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 1","pages":"163-178"},"PeriodicalIF":2.8,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12871490/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146124988","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Scattering from 'Babinet' particles (or not…): spherical particles made up of spheres and spherical particles with spherical voids.","authors":"Jan Skov Pedersen, Thea Lykkegaard Møller, Milena Corredig","doi":"10.1107/S1600576725010143","DOIUrl":"10.1107/S1600576725010143","url":null,"abstract":"<p><p>The small-angle scattering form factors of two classes of composite particles with contrasting internal architectures have been studied: one consisting of inclusions of smaller spheres embedded within a larger sphere, and the other comprising a solid sphere with randomly distributed spherical voids. These systems serve as material- and void-based analogues, providing a model framework for examining how internal material distribution in porous particles influences scattering signatures. Monte Carlo simulations were used to generate scattering curves across a range of volume fractions and polydispersities, which were then employed to benchmark analytically derived form factor expressions. Steric repulsion between, respectively, spheres and voids was taken as hard-sphere interactions. The results reveal that internal structural asymmetries, especially in spatial correlations and contrast topology, significantly affect scattering patterns, despite the particles having similar overall structures and volume fractions. In particular, spheres-of-spheres structures exhibit features in the scattering signal from internal modulations, while void-based particles display smoother shell-like scattering features. The analytical models show excellent agreement with the simulated data, capturing both the global shape and fine structural characteristics. These findings demonstrate that relatively simple analytical approaches, validated against numerical simulations, can reliably describe complex heterogeneous particles. This methodology provides a robust basis for interpreting scattering data from porous and composite materials across a wide range of applications.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 1","pages":"59-68"},"PeriodicalIF":2.8,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12871482/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146125095","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Machine learning approaches for crystallographic classification from synthetic 2D X-ray diffraction data.","authors":"Ayoub Shahnazari, Zeliang Zhang, Sachith E Dissanayake, Chenliang Xu, Niaz Abdolrahim","doi":"10.1107/S1600576726000099","DOIUrl":"10.1107/S1600576726000099","url":null,"abstract":"<p><p>Crystallographic structure identification is crucial for understanding material properties; however, current methodologies often depend on labor-intensive and time-consuming analyses of 2D X-ray diffraction (XRD) patterns. To address these limitations, this study employs synthetic 2D XRD patterns combined with deep learning (DL) techniques to enable automated and high-throughput classification of the seven crystal systems and 230 space groups. We introduce the novel Auto Diffraction Pipeline, designed to generate synthetic 2D XRD spot patterns from crystallographic information files under diverse conditions, including varying zone axes, atomic substitution, atomic depletion and mechanical loading. These conditions enhance the realism of synthetic data, mitigating the scarcity of experimental datasets and enabling the creation of large representative training sets. Convolutional neural networks were trained and validated on these synthetic datasets to classify crystallographic structures across multiple scenarios. Our results demonstrate that integrating synthetic 2D XRD patterns with DL facilitates rapid, accurate and automated crystallographic classification, promoting the wider adoption of data-driven approaches in materials science.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"59 Pt 1","pages":"206-224"},"PeriodicalIF":2.8,"publicationDate":"2026-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12871478/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"146125120","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}