IUCrJ最新文献

{"title":"Enhancing hydrogen positions in X-ray structures of transition metal hydride complexes with dynamic quantum crystallography","authors":"Magdalena Woińska ,&nbsp;Anna A. Hoser ,&nbsp;Michał L. Chodkiewicz ,&nbsp;Krzysztof Woźniak ,&nbsp;A. Fitch (Editor)","doi":"10.1107/S205225252300951X","DOIUrl":"10.1107/S205225252300951X","url":null,"abstract":"<div><p>Hirshfeld atom refinement with anisotropic hydrogen thermal motions estimated using sophisticated methods, such as NoMoRe and SHADE3, was applied to X-ray data collected for transition metal hydride complexes.</p></div><div><p>Hirshfeld atom refinement (HAR) is a method which enables the user to obtain more accurate positions of hydrogen atoms bonded to light chemical elements using X-ray data. When data quality permits, this method can be extended to hydrogen-bonded transition metals (TMs), as in hydride complexes. However, addressing hydrogen thermal motions with HAR, particularly in TM hydrides, presents a challenge. At the same time, proper description of thermal vibrations can be vital for determining hydrogen positions correctly. In this study, we employ tools such as SHADE3 and Normal Mode Refinement (NoMoRe) to estimate anisotropic displacement parameters (ADPs) for hydrogen atoms during HAR and IAM refinements performed for seven structures of TM (Fe, Ni, Cr, Nb, Rh and Os) and metalloid (Sb) hydride complexes for which both the neutron and the X-ray structures have been determined. A direct comparison between neutron and HAR/SHADE3/NoMoRe ADPs reveals that the similarity between neutron hydrogen ADPs and those estimated with NoMoRe or SHADE3 is significantly higher than when hydrogen ADPs are refined with HAR. Regarding TM—H bond lengths, traditional HAR exhibits a slight advantage over the other methods. However, combining NoMoRe/SHADE3 with HAR results in a minor decrease in agreement with neutron TM—H bond lengths. For the Cr complex, for which high-resolution X-ray data were collected, an investigation of resolution-related effects was possible.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 45-56"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833390/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138291037","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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":"What is isostructurality? Questions on the definition","authors":"Petra Bombicz ,&nbsp;L. R. MacGillivray (Editor)","doi":"10.1107/S2052252523010436","DOIUrl":"10.1107/S2052252523010436","url":null,"abstract":"<div><p>The phenomenon and definition of isostructurality are discussed. It deserves reconsideration regarding the aspects of symmetry, measure of similarity and formation of supramolecular interactions.</p></div><div><p>Investigation of isostructurality leads to a deeper understanding of close-packing principles and contributes to the ability of crystal engineering. A given packing motif may tolerate small molecular changes within a limit. Slight alterations of a crystal packing arrangement are carried out in order to fine-tune the structural and macroscopic properties, keeping the balance of the spatial requirements and electrostatic effects of the altered molecules in the crystals, preserving their isostructurality. Even so, the definition of isostructurality is not explicit about several issues. Are the corresponding structures required to have the same stoichiometry, <em>Z</em>′, symmetry elements and the same space group? Because it is not obvious in the definition, studies on structure analysis and software calculating various numerical descriptors developed for the quantitative comparison of the degree of similarity of isostructural crystals self-define their criteria. The extent of the difference between corresponding crystal structures referred to as isostructural is not limited. Should it be determined numerically? There is nothing in the definition about a demand for similar supramolecular arrangements in isostructural crystals. Should the similarity of supramolecular interactions be a criterion of isostructurality? The definition of isostructurality deserves reconsideration regarding symmetry, measure of similarity and formation of supramolecular interactions.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 3-6"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833389/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138804104","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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":"Conformation–aggregation interplay in the simplest aliphatic ethers probed under high pressure","authors":"Natalia Sacharczuk ,&nbsp;Anna Olejniczak ,&nbsp;Maciej Bujak ,&nbsp;Kamil Filip Dziubek ,&nbsp;Andrzej Katrusiak ,&nbsp;Marcin Podsiadło ,&nbsp;L. R. MacGillivray (Editor)","doi":"10.1107/S2052252523009995","DOIUrl":"10.1107/S2052252523009995","url":null,"abstract":"<div><p>The most stable <em>trans</em>–<em>trans</em> conformation of the di­ethyl ether molecule hinders its aggregation due to restricted access to the oxygen atom. This hindrance can be removed by conformational transformation under high pressure.</p></div><div><p>The structures of the simplest symmetric primary ethers [(C<em>n</em>H₂<em>n</em>₊₁)₂O, <em>n</em> = 1–3] determined under high pressure revealed their conformational preferences and intermolecular interactions. In three new polymorphs of di­ethyl ether (C₂H₅)₂O, high pressure promotes intermolecular CH⋯O contacts and enforces a conversion from the <em>trans</em>–<em>trans</em> conformer present in the α, β and γ phases to the <em>trans</em>–<em>gauche</em> conformer, which is higher in energy by 6.4 kJ mol⁻¹, in the δ phase. Two new polymorphs of di­methyl ether (CH₃)₂O display analogous transformations of the CH⋯O bonds. The crystal structure of di-<em>n</em>-propyl ether (C₃H₇)₂O, determined for the first time, is remarkably stable over the whole pressure range investigated from 1.70 up to 5.30 GPa.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 57-61"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833391/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138451542","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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":"Structure determination using high-order spatial correlations in single-particle X-ray scattering","authors":"Wenyang Zhao ,&nbsp;Osamu Miyashita ,&nbsp;Miki Nakano ,&nbsp;Florence Tama ,&nbsp;F. Maia (Editor)","doi":"10.1107/S2052252523009831","DOIUrl":"10.1107/S2052252523009831","url":null,"abstract":"<div><p>A method is described for determining the 3D structure of a sample from X-ray free-electron laser single-particle diffraction patterns by analyzing different orders of spatial correlations of diffraction intensities.</p></div><div><p>Single-particle imaging using X-ray free-electron lasers (XFELs) is a promising technique for observing nanoscale biological samples under near-physiological conditions. However, as the sample’s orientation in each diffraction pattern is unknown, advanced algorithms are required to reconstruct the 3D diffraction intensity volume and subsequently the sample’s density model. While most approaches perform 3D reconstruction via determining the orientation of each diffraction pattern, a correlation-based approach utilizes the averaged spatial correlations of diffraction intensities over all patterns, making it well suited for processing experimental data with a poor signal-to-noise ratio of individual patterns. Here, a method is proposed to determine the 3D structure of a sample by analyzing the double, triple and quadruple spatial correlations in diffraction patterns. This <em>ab initio</em> method can reconstruct the basic shape of an irregular unsymmetric 3D sample without requiring any prior knowledge of the sample. The impact of background and noise on correlations is investigated and corrected to ensure the success of reconstruction under simulated experimental conditions. Additionally, the feasibility of using the correlation-based approach to process incomplete partial diffraction patterns is demonstrated. The proposed method is a variable addition to existing algorithms for 3D reconstruction and will further promote the development and adoption of XFEL single-particle imaging techniques.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 92-108"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833384/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138804103","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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":"Refining short-range order parameters from the three-dimensional diffuse scattering in single-crystal electron diffraction data","authors":"Romy Poppe ,&nbsp;Nikolaj Roth ,&nbsp;Reinhard B. Neder ,&nbsp;Lukas Palatinus ,&nbsp;Bo Brummerstedt Iversen ,&nbsp;Joke Hadermann ,&nbsp;L. Meshi (Editor)","doi":"10.1107/S2052252523010254","DOIUrl":"10.1107/S2052252523010254","url":null,"abstract":"<div><p>This study compares, for the first time, short-range order parameters refined from the diffuse scattering in single-crystal X-ray and single-crystal electron diffraction data.</p></div><div><p>Our study compares short-range order parameters refined from the diffuse scattering in single-crystal X-ray and single-crystal electron diffraction data. Nb_0.84CoSb was chosen as a reference material. The correlations between neighbouring vacancies and the displacements of Sb and Co atoms were refined from the diffuse scattering using a Monte Carlo refinement in <em>DISCUS</em>. The difference between the Sb and Co displacements refined from the diffuse scattering and the Sb and Co displacements refined from the Bragg reflections in single-crystal X-ray diffraction data is 0.012 (7) Å for the refinement on diffuse scattering in single-crystal X-ray diffraction data and 0.03 (2) Å for the refinement on the diffuse scattering in single-crystal electron diffraction data. As electron diffraction requires much smaller crystals than X-ray diffraction, this opens up the possibility of refining short-range order parameters in many technologically relevant materials for which no crystals large enough for single-crystal X-ray diffraction are available.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 82-91"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833392/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138804102","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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 new approach for serial electron diffraction data collection","authors":"Brent L. Nannenga","doi":"10.1107/S2052252523010953","DOIUrl":"10.1107/S2052252523010953","url":null,"abstract":"<div><p>This commentary describes a novel method for serial electron diffraction data collection in electron crystallography, utilizing a scanning transmission electron microscope to rapidly obtain patterns with low radiation dose. This approach, demonstrated with zeolite samples, has the potential to provide highly automated and rapid structures from nanocrystalline materials.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 7-8"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833380/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138829824","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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":"Orientational analysis of atomic pair correlations in nanocrystalline indium oxide thin films","authors":"Justin M. Hoffman ,&nbsp;Niklas B. Thompson ,&nbsp;Olaf Borkiewicz ,&nbsp;Xiang He ,&nbsp;Samuel Amsterdam ,&nbsp;Zhu-lin Xie ,&nbsp;Aaron Taggart ,&nbsp;Karen L. Mulfort ,&nbsp;Alex B. F. Martinson ,&nbsp;Lin X. Chen ,&nbsp;Uta Ruett ,&nbsp;David M. Tiede ,&nbsp;I. Robinson (Editor)","doi":"10.1107/S2052252523010357","DOIUrl":"10.1107/S2052252523010357","url":null,"abstract":"<div><p>Grazing-incidence total X-ray scattering allows for orientational pair distribution function analysis of indium oxide thin films with only a single measurement. Elucidation of information such as effects of film anisotropy on bond lengths in specific orientations relative to the substrate and determination of orientation in X-ray amorphous films is demonstrated.</p></div><div><p>The application of grazing-incidence total X-ray scattering (GITXS) for pair distribution function (PDF) analysis using &gt;50 keV X-rays from synchrotron light sources has created new opportunities for structural characterization of supported thin films with high resolution. Compared with grazing-incidence wide-angle X-ray scattering, which is only useful for highly ordered materials, GITXS/PDFs expand such analysis to largely disordered or nanostructured materials by examining the atomic pair correlations dependent on the direction relative to the surface of the supporting substrate. A characterization of nanocrystalline In₂O₃-derived thin films is presented here with in-plane-isotropic and out-of-plane-anisotropic orientational ordering of the atomic structure, each synthesized using different techniques. The atomic orientations of such films are known to vary based on the synthetic conditions. Here, an azimuthal orientational analysis of these films using GITXS with a single incident angle is shown to resolve the markedly different orientations of the atomic structures with respect to the planar support and the different degrees of long-range order, and hence, the terminal surface chemistries. It is anticipated that orientational analysis of GITXS/PDF data will offer opportunities to extend structural analyses of thin films by providing a means to qualitatively determine the major atomic orientation within nanocrystalline and, eventually, non-crystalline films.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 120-128"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833382/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138829826","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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":"STEM SerialED: achieving high-resolution data for ab initio structure determination of beam-sensitive nanocrystalline materials","authors":"Pascal Hogan-Lamarre ,&nbsp;Yi Luo ,&nbsp;Robert Bücker ,&nbsp;R. J. Dwayne Miller ,&nbsp;Xiaodong Zou ,&nbsp;M. Gemmi (Editor)","doi":"10.1107/S2052252523009661","DOIUrl":"10.1107/S2052252523009661","url":null,"abstract":"<div><p>An implementation of scanning transmission electron microscopy serial electron diffraction (SerialED) through scripting is proposed. SerialED and continuous-rotation electron diffraction refinement results for the structure of zeolite Y are compared, and the structure of beam-sensitive ZSM-25 is solved by direct methods from electron diffraction data for the first time.</p></div><div><p>Serial electron diffraction (SerialED), which applies a snapshot data acquisition strategy for each crystal, was introduced to tackle the problem of radiation damage in the structure determination of beam-sensitive materials by three-dimensional electron diffraction (3DED). The snapshot data acquisition in SerialED can be realized using both transmission and scanning transmission electron microscopes (TEM/STEM). However, the current SerialED workflow based on STEM setups requires special external devices and software, which limits broader adoption. Here, we present a simplified experimental implementation of STEM-based SerialED on Thermo Fisher Scientific STEMs using common proprietary software interfaced through Python scripts to automate data collection. Specifically, we utilize <em>TEM Imaging and Analysis</em> (<em>TIA</em>) scripting and TEM scripting to access the STEM functionalities of the microscope, and <em>DigitalMicrograph</em> scripting to control the camera for snapshot data acquisition. Data analysis adapts the existing workflow using the software <em>CrystFEL</em>, which was developed for serial X-ray crystallography. Our workflow for STEM SerialED can be used on any Gatan or Thermo Fisher Scientific camera. We apply this workflow to collect high-resolution STEM SerialED data from two aluminosilicate zeolites, zeolite Y and ZSM-25. We demonstrate, for the first time, <em>ab initio</em> structure determination through direct methods using STEM SerialED data. Zeolite Y is relatively stable under the electron beam, and STEM SerialED data extend to 0.60 Å. We show that the structural model obtained using STEM SerialED data merged from 358 crystals is nearly identical to that using continuous rotation electron diffraction data from one crystal. This demonstrates that accurate structures can be obtained from STEM SerialED. Zeolite ZSM-25 is very beam-sensitive and has a complex structure. We show that STEM SerialED greatly improves the data resolution of ZSM-25, compared with serial rotation electron diffraction (SerialRED), from 1.50 to 0.90 Å. This allows, for the first time, the use of standard phasing methods, such as direct methods, for the <em>ab initio</em> structure determination of ZSM-25.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 62-72"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833385/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138460054","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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":"Orientational ordering and assembly of silica–nickel Janus particles in a magnetic field","authors":"Gouranga Manna ,&nbsp;Thomas Zinn ,&nbsp;Lewis Sharpnack ,&nbsp;Theyencheri Narayanan ,&nbsp;V. T. Forsyth (Editor)","doi":"10.1107/S205225252301000X","DOIUrl":"10.1107/S205225252301000X","url":null,"abstract":"<div><p>The alignment and self-assembly behavior of silica–nickel Janus particles in an external magnetic field were probed by ultra small-angle X-ray scattering. A theoretical framework is provided for the quantitative interpretation of the observed anisotropic scattering features.</p></div><div><p>The orientation ordering and assembly behavior of silica–nickel Janus particles in a static external magnetic field were probed by ultra small-angle X-ray scattering (USAXS). Even in a weak applied field, the net magnetic moments of the individual particles aligned in the direction of the field, as indicated by the anisotropy in the recorded USAXS patterns. X-ray photon correlation spectroscopy (XPCS) measurements on these suspensions revealed that the corresponding particle dynamics are primarily Brownian diffusion [Zinn, Sharpnack &amp; Narayanan (2023<span>#</span>). <em>Soft Matter</em>, <strong>19</strong>, 2311–2318]. At higher fields, the magnetic forces led to chain-like configurations of particles, as indicated by an additional feature in the USAXS pattern. A theoretical framework is provided for the quantitative interpretation of the observed anisotropic scattering diagrams and the corresponding degree of orientation. No anisotropy was detected when the magnetic field was applied along the beam direction, which is also replicated by the model. The method presented here could be useful for the interpretation of oriented scattering patterns from a wide variety of particulate systems. The combination of USAXS and XPCS is a powerful approach for investigating asymmetric colloidal particles in external fields.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"11 1","pages":"Pages 109-119"},"PeriodicalIF":3.9,"publicationDate":"2024-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10833383/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138804101","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"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":"3D-printed sheet jet for stable megahertz liquid sample delivery at X-ray free-electron lasers","authors":"Patrick E. Konold ,&nbsp;Tong You ,&nbsp;Johan Bielecki ,&nbsp;Joana Valerio ,&nbsp;Marco Kloos ,&nbsp;Daniel Westphal ,&nbsp;Alfredo Bellisario ,&nbsp;Tej Varma Yenupuri ,&nbsp;August Wollter ,&nbsp;Jayanath C. P. Koliyadu ,&nbsp;Faisal H.M. Koua ,&nbsp;Romain Letrun ,&nbsp;Adam Round ,&nbsp;Tokushi Sato ,&nbsp;Petra Mészáros ,&nbsp;Leonardo Monrroy ,&nbsp;Jennifer Mutisya ,&nbsp;Szabolcs Bódizs ,&nbsp;Taru Larkiala ,&nbsp;Amke Nimmrich ,&nbsp;T. Ishikawa (Editor)","doi":"10.1107/S2052252523007972","DOIUrl":"10.1107/S2052252523007972","url":null,"abstract":"<div><p>In this study, liquid sheet jet sample injection was demonstrated at the EuXFEL SPB/SFX beamline. A 3D-printed gas-accelerated nozzle design was used to produce sheet jet thicknesses below 100 nm resulting in a significantly more stable scattering signal compared with a conventional cylindrical liquid jet. The radiation-induced explosion was found to not perturb data collection for repetition rates approaching megahertz. These results demonstrate the great potential of sheet jets for high-repetition-rate liquid sample injection and their adoption for both scattering and spectroscopy experiments.</p></div><div><p>X-ray free-electron lasers (XFELs) can probe chemical and biological reactions as they unfold with unprecedented spatial and temporal resolution. A principal challenge in this pursuit involves the delivery of samples to the X-ray interaction point in such a way that produces data of the highest possible quality and with maximal efficiency. This is hampered by intrinsic constraints posed by the light source and operation within a beamline environment. For liquid samples, the solution typically involves some form of high-speed liquid jet, capable of keeping up with the rate of X-ray pulses. However, conventional jets are not ideal because of radiation-induced explosions of the jet, as well as their cylindrical geometry combined with the X-ray pointing instability of many beamlines which causes the interaction volume to differ for every pulse. This complicates data analysis and contributes to measurement errors. An alternative geometry is a liquid sheet jet which, with its constant thickness over large areas, eliminates the problems related to X-ray pointing. Since liquid sheets can be made very thin, the radiation-induced explosion is reduced, boosting their stability. These are especially attractive for experiments which benefit from small interaction volumes such as fluctuation X-ray scattering and several types of spectroscopy. Although their use has increased for soft X-ray applications in recent years, there has not yet been wide-scale adoption at XFELs. Here, gas-accelerated liquid sheet jet sample injection is demonstrated at the European XFEL SPB/SFX nano focus beamline. Its performance relative to a conventional liquid jet is evaluated and superior performance across several key factors has been found. This includes a thickness profile ranging from hundreds of nanometres to 60 nm, a fourfold increase in background stability and favorable radiation-induced explosion dynamics at high repetition rates up to 1.13 MHz. Its minute thickness also suggests that ultrafast single-particle solution scattering is a possibility.</p></div>","PeriodicalId":14775,"journal":{"name":"IUCrJ","volume":"10 6","pages":"Pages 662-670"},"PeriodicalIF":3.9,"publicationDate":"2023-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10619454/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"10291882","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}