X-ray ptychography and ptychographic computed tomography have seen a rapid rise since the advent of fourth-generation synchrotrons with a high degree of coherent radiation. In addition to quantitative multiscale structural analysis, ptychography with spectral capabilities has been developed, allowing for spatial-localized multiscale structural and spectral information of samples. The SWING beamline of Synchrotron SOLEIL has recently developed a nanoprobe setup where the endstation's first spectral and resonant ptychographic measurements have been successfully conducted. A metallic nickel wire sample was measured using 2D spectral ptychography in XANES mode and resonant ptychographic tomography. From the 2D spectral ptychography measurements, the spectra of the components of the sample's complex-valued refractive index, δ and β, were extracted, integrated along the sample thickness. By performing resonance ptychographic tomography at two photon energies, 3D maps of the refractive index decrement, δ, were obtained at the Ni K-edge energy and another energy above the edge. These maps allowed the detection of impurities in the Ni wire. The significance of accounting for the atomic scattering factor is demonstrated in the calculation of electron density near a resonance through the use of the δ values. These results indicate that at the SWING beamline it is possible to conduct state-of-the-art spectral and resonant ptychography experiments using the nanoprobe setup.

Signal-to-noise ratio and spatial resolution are quantitatively analysed in the context of in-line (propagation based) X-ray phase-contrast imaging. It is known that free-space propagation of a coherent X-ray beam from the imaged object to the detector plane, followed by phase retrieval in accordance with Paganin's method, can increase the signal-to-noise in the resultant images without deteriorating the spatial resolution. This results in violation of the noise-resolution uncertainty principle and demonstrates `unreasonable' effectiveness of the method. On the other hand, when the process of free-space propagation is performed in software, using the detected intensity distribution in the object plane, it cannot reproduce the same effectiveness, due to the amplification of photon shot noise. Here, it is shown that the performance of Paganin's method is determined by just two dimensionless parameters: the Fresnel number and the ratio of the real decrement to the imaginary part of the refractive index of the imaged object. The relevant theoretical analysis is performed first, followed by computer simulations and then by a brief test using experimental images collected at a synchrotron beamline. More extensive experimental tests will be presented in the second part of this paper.

A multi-objective genetic algorithm (MOGA) is a powerful global optimization tool, but its results are considerably affected by the crossover parameter ηc. Finding an appropriate ηc demands too much computing time because MOGA needs be run several times in order to find a good ηc. In this paper, a self-adaptive crossover parameter is introduced in a strategy to adopt a new ηc for every generation while running MOGA. This new scheme has also been adopted for a multi-generation Gaussian process optimization (MGGPO) when producing trial solutions. Compared with the existing MGGPO and MOGA, the MGGPO and MOGA with the new strategy show better performance in nonlinear optimization for the design of low-emittance storage rings.

The BL17B beamline at the Shanghai Synchrotron Radiation Facility was first designed as a versatile high-throughput protein crystallography beamline and one of five beamlines affiliated to the National Facility for Protein Science in Shanghai. It was officially opened to users in July 2015. As a bending magnet beamline, BL17B has the advantages of high photon flux, brightness, energy resolution and continuous adjustable energy between 5 and 23 keV. The experimental station excels in crystal screening and structure determination, providing cost-effective routine experimental services to numerous users. Given the interdisciplinary and green energy research demands, BL17B beamline has undergone optimization, expanded its range of experimental methods and enhanced sample environments for a more user-friendly testing mode. These methods include single-crystal X-ray diffraction, powder crystal X-ray diffraction, wide-angle X-ray scattering, grazing-incidence wide-angle X-ray scattering (GIWAXS), and fully scattered atom pair distribution function analysis, covering structure detection from crystalline to amorphous states. This paper primarily presents the performance of the BL17B beamline and the application of the GIWAXS methodology at the beamline in the field of perovskite materials.

The Biomedical Imaging and Therapy facility of the Canadian Light Source comprises two beamlines, which together cover a wide X-ray energy range from 13 keV up to 140 keV. The beamlines were designed with a focus on synchrotron applications in preclinical imaging and veterinary science as well as microbeam radiation therapy. While these remain a major part of the activities of both beamlines, a number of recent upgrades have enhanced the versatility and performance of the beamlines, particularly for high-resolution microtomography experiments. As a result, the user community has been quickly expanding to include researchers in advanced materials, batteries, fuel cells, agriculture, and environmental studies. This article summarizes the beam properties, describes the endstations together with the detector pool, and presents several application cases of the various X-ray imaging techniques available to users.

The ID10 beamline of the SESAME (Synchrotron-light for Experimental Science and Applications in the Middle East) synchrotron light source in Jordan was inaugurated in June 2023 and is now open to scientific users. The beamline, which was designed and installed within the European Horizon 2020 project BEAmline for Tomography at SESAME (BEATS), provides full-field X-ray radiography and microtomography imaging with monochromatic or polychromatic X-rays up to photon energies of 100 keV. The photon source generated by a 2.9 T wavelength shifter with variable gap, and a double-multilayer monochromator system allow versatile application for experiments requiring either an X-ray beam with high intensity and flux, and/or a partially spatial coherent beam for phase-contrast applications. Sample manipulation and X-ray detection systems are designed to allow scanning samples with different size, weight and material, providing image voxel sizes from 13 µm down to 0.33 µm. A state-of-the-art computing infrastructure for data collection, three-dimensional (3D) image reconstruction and data analysis allows the visualization and exploration of results online within a few seconds from the completion of a scan. Insights from 3D X-ray imaging are key to the investigation of specimens from archaeology and cultural heritage, biology and health sciences, materials science and engineering, earth, environmental sciences and more. Microtomography scans and preliminary results obtained at the beamline demonstrate that the new beamline ID10-BEATS expands significantly the range of scientific applications that can be targeted at SESAME.

A broadband online X-ray spectrometer has been designed and commissioned at the SUD beamline of the Shanghai Soft X-ray Free-Electron Laser Facility, which can deliver both SASE and seeded FEL pulses to user experiments, spanning the photon energy range of 50–620 eV. The resolving powers of the spectrometer calibrated via online measurement at 92 eV and 249 eV are ∼20000 and ∼15000, respectively, and the absolute photon energy is characterized by an electron time-of-flight spectrometer. The high energy resolution provided by the spectrometer can differentiate the fine structure in the FEL spectrum, to determine its pulse length.

The split-and-delay unit (SDU) at FLASH2 will be upgraded to enable the simultaneous operation of two temporally, spatially and spectrally separated probe beams when the free-electron laser undulators are operated in a two-color scheme. By means of suitable thin filters and an optical grating beam path a wide range of combinations of photon energies in the spectral range from 150 eV to 780 eV can be chosen. In this paper, simulations of the spectral transmission and performance parameters of the filter technique are discussed, along with a monochromator with dispersion compensation presently under construction.

Full-field transmission X-ray microscopy has been recently implemented at the hard X-ray ROCK–SOLEIL quick-EXAFS beamline, adding micrometre spatial resolution to the second time resolution characterizing the beamline. Benefiting from a beam size versatility due to the beamline focusing optics, full-field hyperspectral XANES imaging has been successfully used at the Fe K-edge for monitoring the pressure-induced spin transition of a 150 µm × 150 µm Fe(o-phen)2(NCS)2 single crystal and the charge of millimetre-sized LiFePO4 battery electrodes. Hyperspectral imaging over 2000 eV has been reported for the simultaneous monitoring of Fe and Cu speciation changes during activation of a FeCu bimetallic catalyst along a millimetre-sized catalyst bed. Strategies of data acquisition and post-data analysis using Jupyter notebooks and multivariate data analysis are presented, and the gain obtained using full-field hyperspectral quick-EXAFS imaging for studies of functional materials under process conditions in comparison with macroscopic information obtained by non-spatially resolved quick-EXAFS techniques is discussed.

Beamline BL08U1A is a soft X-ray spectromicroscopy beamline at Shanghai Synchrotron Radiation Facility (SSRF) that exhibits the capabilities of high spatial resolution (30 nm) and high energy resolving power (over 104). As a first-generation beamline of SSRF, owing to its continuous operation over the last ten years, an urgent upgrade of the equipment including the monochromator was deemed necessary. The upgrade work included the overall construction of the monochromator and replacement of the mirrors upstream and downstream of the monochromator. Based on its original skeleton, two elliptically cylinder mirrors were designed to focus the beam horizontally, which can increase the flux density by about three times on the exit slits. Meanwhile, the application of variable-line-space gratings in the monochromator demonstrates the dual functions of dispersing and focusing on the exit slits which can decrease abberations dramatically. After the upgrade of the main components of the beamline, the energy range is 180–2000 eV, the energy resolving power reaches 16333 @ 244 eV and 12730 @ 401 eV, and the photon flux measured in the experimental station is over 2.45 × 109 photons s−1 (E/ΔE = 6440 @ 244 eV).

A state-of-the-art multilayer deposition system with a 4200 mm-long linear substrate translator housed within an ultra-high vacuum chamber has been developed. This instrument is engineered to produce single and multilayer coatings, accommodating mirrors up to 2000 mm in length through the utilization of eight rectangular cathodes. To ensure the quality and reliability of the coatings, the system incorporates various diagnostic tools for in situ thickness uniformity and stress measurement. Furthermore, the system features an annealing process capable of heating up to 700°C within the load-lock chamber. The entire operation, including pump down, deposition and venting processes, is automated through user-friendly software. In addition, all essential log data, power of sputtering source, working pressure and motion positions are automatically stored for comprehensive data analysis. Preliminary commissioning results demonstrate excellent lateral film thickness uniformity, achieving 0.26% along the translation direction over 1500 mm in dynamic mode. The multilayer deposition system is poised for use in fabricating periodic, lateral-graded and depth-graded multilayers, specifically catering to the beamlines for diverse scientific applications at Diamond Light Source.

The development of hard X-ray nanoprobe techniques has given rise to a number of experimental methods, like nano-XAS, nano-XRD, nano-XRF, ptychography and tomography. Each method has its own unique data processing algorithms. With the increase in data acquisition rate, the large amount of generated data is now a big challenge to these algorithms. In this work, an intuitive, user-friendly software system is introduced to integrate and manage these algorithms; by taking advantage of the loosely coupled, component-based design approach of the system, the data processing speed of the imaging algorithm is enhanced through optimization of the parallelism efficiency. This study provides meaningful solutions to tackle complexity challenges faced in synchrotron data processing.

A second crystalline modification of the title compound, C12H19N3S [common name: cis-jasmone thio­semicarbazone] was crystallized from tetra­hydro­furane at room temperature. There is one crystallographic independent mol­ecule in the asymmetric unit, showing disorder in the cis-jasmone chain [site-occupancy ratio = 0.590 (14):0.410 (14)]. The thio­semicarbazone entity is approximately planar, with the maximum deviation from the mean plane through the N/N/C/S/N atoms being 0.0463 (14) Å [r.m.s.d. = 0.0324 Å], while for the five-membered ring of the jasmone fragment, the maximum deviation from the mean plane through the carbon atoms amounts to 0.0465 (15) Å [r.m.s.d. = 0.0338 Å]. The mol­ecule is not planar due to the dihedral angle between these two fragments, which is 8.93 (1)°, and due to the sp3-hybridized carbon atoms in the jasmone fragment chain. In the crystal, the mol­ecules are connected by N—H⋯S and C—H⋯S inter­actions, with graph-set motifs R22(8) and R21(7), building mono-periodic hydrogen-bonded ribbons along [010]. A Hirshfeld surface analysis indicates that the major contributions for the crystal cohesion are H⋯H (67.8%), H⋯S/S⋯H (15.0%), H⋯C/C⋯H (8.5%) and H⋯N/N⋯H (5.6%) [only non-disordered atoms and those with the highest s.o.f. were considered]. This work reports the second crystalline modification of the cis-jasmone thio­semicarbazone structure, the first one being published recently [Orsoni et al. (2020). Int. J. Mol. Sci. 21, 8681–8697] with the crystals obtained in ethanol at 273 K.

In the title complex, [ZnCl2(C14H12N2O2)], the ZnII atom is located on a twofold rotation axis and is fourfold coordinated by two chlorido ligands and a bidentate 4,7-meth­oxy-1,10-phenanthroline ligand in a distorted tetra­hedral environment. Weak π–π stacking inter­actions between adjacent 4,7-dimeth­oxy-1,10-phenanthroline rings [centroid-to-centroid distances = 3.5969 (11) and 3.7738 (11) Å] contribute to the alignment of the complexes in layers parallel to (overline{2}01).

The title pyrene-fused spiro­pyran derivative, C30H25NO, crystallizes with two mol­ecules in the asymmetric unit with dihedral angles between their fused-ring sub units of 76.20 (8) and 89.38 (9)°. In the crystal, weak C—H⋯π inter­actions link the mol­ecules into a three-dimensional network.

The structure of the title compound, [C14H18N2)2Ag2](NO3)2, contains subtle differences in ligand, metal, and counter-anion coordination. One quinoxaline ligand uses one of its quinoxaline N atoms to bond to one silver cation. That silver cation is bound to a second quinoxaline which, in turn, is bound to a second silver atom; thereby using both of its quinoxaline N atoms. A nitrate group bonds with one of its O atoms to the first silver and uses the same oxygen to bond to a silver atom (related by symmetry to the second), thereby forming an extended network. The second nitrate group on the other silver bonds via two nitrate O atoms; one silver cation therefore has a coordination number of three whereas the second has a coordination number of four. One of the quinoxaline ligands has a disordered ethyl group.

In the title compound, [Ni(C13H13N4S)2]·0.33CH3OH·0.67H2O, the NiII atom is coordinated by two tridentate quinoline-2-carboxaldehyde 4-ethyl­thio­semi­car­ba­zonate ligands in a distorted octa­hedral shape. At 100 K, the crystal symmetry is monoclinic (space group P21/n). A mixture of water and methanol crystallizes with the title complex, and one of the ethyl groups in the coordinating ligands is disordered over two positions, with an occupancy ratio of 58:42. There is inter­molecular hydrogen bonding between the solvent mol­ecules and the amine and thiol­ate groups in the ligands. No other significant inter­actions are present in the crystal packing.

In the title compound, C26H18BrN, the central benzene ring makes dihedral angles with its adjacent anthracene ring system and pendant benzene ring of 87.49 (13) and 62.01 (17)°, respectively. The N—H moiety is sterically blocked from forming a hydrogen bond, but weak C—H⋯π inter­actions occur in the extended structure.

The title compound, [Fe(C84H52N12O4)Cl], crystallizes in space group C2/c. The central FeIII cation (site symmetry 2) is coordinated in a fivefold manner, with four pyrrole N atoms of the porphyrin core in the basal sites and one Cl atom (site symmetry 2) in the apical position, which completes a slightly distorted square-pyramidal environment. The porphyrin macrocycle shows a characteristic ruffled-shape distortion and the iron atom is displaced out of the porphyrin plane by 0.42 Å with the average Fe—N distance being 2.054 (4) Å; the Fe—Cl bond length is 2.2042 (7) Å. Inter­molecular C—H⋯N and C—H⋯O hydrogen bonds occur in the crystal structure.

The reaction of nickel(II) chloride with 3-meth­oxy­aniline yielded di­chlorido­tetra­kis­(3-meth­oxy­aniline)nickel(II), [NiCl2(C7H9NO)4], as yellow crystals. The NiII ion is pseudo-octa­hedral with the chloride ions trans to each other. The four 3-meth­oxy­aniline ligands differ primarily due to different conformations about the Ni—N bond, which also affect the hydrogen bonding. Inter­molecular N—H⋯ Cl hydrogen bonds and short Cl⋯Cl contacts between mol­ecules link them into chains parallel to the b axis.

The title coordination polymer, [Co(N3)2(C9H8N2)]n, was synthesized solvothermally. The CoII atom exhibits a distorted octa­hedral [CoN6] coordination geometry with a bidentate 8-amino­quinoline ligand and four azide ligands. Bridging azide ligands result in chains extending along [100]. N—H⋯N hydrogen bonds join the chains to give an extended structure with sheets parallel to (002).

The title compound, [Ir(C15H10N)2(C19H12N4)]PF6·CH3OH, crystallizes in the C2/c space group with one monocationic iridium complex, one hexa­fluorido­phosphate anion, and one methanol solvent mol­ecule of crystallization in the asymmetric unit, all in general positions. The anion and solvent are linked to the iridium complex cation via hydrogen bonding. All bond lengths and angles fall into expected ranges compared to similar compounds.

The title compound, [Ru(C12H14NO2)2(C12H8N2)]PF6 crystallizes in the tetra­gonal Sohnke space group P41212. The two bidentate chiral salicyloxazoline ligands and the phenanthroline co-ligand coordinate to the central RuIII atom through N,O and N,N atom pairs to form bite angles of 89.76 (15) and 79.0 (2)°, respectively. The octa­hedral coordination of the bidentate ligands leads to a propeller-like shape, which induces metal-centered chirality onto the complex, with a right-handed (Δ) absolute configuration [the Flack parameter value is −0.003 (14)]. Both the complex cation and the disordered PF6− counter-anion are located on twofold rotation axes. Apart from Coulombic forces, the crystal cohesion is ensured by non-classical C—H⋯O and C—H⋯F inter­actions.

The receptor ability of diethyl N,N'-(1,3-phenyl­ene)dicarbamate (1) to form host–guest com­plexes with theophylline (TEO) and caffeine (CAF) by mechanochemistry was evaluated. The formation of the 1–TEO com­plex (C12H16N2O4·C7H8N4O2) was preferred and involves the conformational change of one of the ethyl carbamate groups of 1 from the endo conformation to the exo conformation to allow the formation of inter­molecular inter­actions. The formation of an N—H⋯O=C hydrogen bond between 1 and TEO triggers the conformational change of 1. CAF mol­ecules are unable to form an N—H⋯O=C hydrogen bond with 1, making the conformational change and, therefore, the formation of the com­plex impossible. Conformational change and selective binding were monitored by IR spectroscopy, solid-state 13C nuclear magnetic resonance and single-crystal X-ray diffraction. The 1–TEO com­plex was characterized by IR spectroscopy, solid-state 13C nuclear magnetic resonance, powder X-ray diffraction and single-crystal X-ray diffraction.

The crystal structures of two coordination com­pounds, (acetato-κO)(2,2'-bi­py­ri­dine-κ2N,N')(1,10-phenanthroline-κ2N,N')copper(II) acetate hexa­hydrate, [Cu(C2H3O2)(C10H8N2)(C12H8N2)](C2H3O2)·6H2O or [Cu(bipy)(phen)Ac]Ac·6H2O, and (acetato-κO)bis­(2,2'-bi­py­ri­dine-κ2N,N')copper(II) acetate–acetic acid–water (1/1/3), [Cu(C2H3O2)(C10H8N2)2](C2H3O2)·C2H4O2·3H2O or [Cu(bipy)2Ac]Ac·HAc·3H2O, are reported and com­pared with the previously published structure of [Cu(phen)2Ac]Ac·7H2O (phen is 1,10-phenanthroline, bipy for 2,2'-bi­py­ri­dine, ac is acetate and Hac is acetic acid). The geometry around the metal centre is penta­coordinated, but highly distorted in all three cases. The coordination number and the geometric distortion are both discussed in detail, and all com­plexes belong to the space group Poverline{1}. The analysis of the geometric parameters and the Hirshfeld surface properties dnorm and curvedness provide information about the metal–ligand inter­actions in these com­plexes and allow com­parison with similar systems.

This article describes the High-Pressure Freezing Laboratory for Macromolecular Crystallography (HPMX) at the ESRF, and highlights new and complementary research opportunities that can be explored using this facility. The laboratory is dedicated to investigating interactions between macromolecules and gases in crystallo, and finds applications in many fields of research, including fundamental biology, biochemistry, and environmental and medical science. At present, the HPMX laboratory offers the use of different high-pressure cells adapted for helium, argon, krypton, xenon, nitrogen, oxygen, carbon dioxide and methane. Important scientific applications of high pressure to macromolecules at the HPMX include noble-gas derivatization of crystals to detect and map the internal architecture of proteins (pockets, tunnels and channels) that allows the storage and diffusion of ligands or substrates/products, the investigation of the catalytic mechanisms of gas-employing enzymes (using oxygen, carbon dioxide or methane as substrates) to possibly decipher intermediates, and studies of the conformational fluctuations or structure modifications that are necessary for proteins to function. Additionally, cryo-cooling protein crystals under high pressure (helium or argon at 2000 bar) enables the addition of cryo-protectant to be avoided and noble gases can be employed to produce derivatives for structure resolution. The high-pressure systems are designed to process crystals along a well defined pathway in the phase diagram (pressure–temperature) of the gas to cryo-cool the samples according to the three-step `soak-and-freeze method'. Firstly, crystals are soaked in a pressurized pure gas atmosphere (at 294 K) to introduce the gas and facilitate its inter­actions within the macromolecules. Samples are then flash-cooled (at 100 K) while still under pressure to cryo-trap macromolecule–gas complexation states or pressure-induced protein modifications. Finally, the samples are recovered after depressurization at cryo-temperatures. The final section of this publication presents a selection of different typical high-pressure experiments carried out at the HPMX, showing that this technique has already answered a wide range of scientific questions. It is shown that the use of different gases and pressure conditions can be used to probe various effects, such as mapping the functional internal architectures of enzymes (tunnels in the haloalkane dehalogenase DhaA) and allosteric sites on membrane-protein surfaces, the interaction of non-inert gases with proteins (oxygen in the hydrogenase ReMBH) and pressure-induced structural changes of proteins (tetramer dissociation in urate oxidase). The technique is versatile and the provision of pressure cells and their application at the HPMX is gradually being extended to address new scientific questions.

Electron cryo-microscopy image-processing workflows are typically composed of elements that may, broadly speaking, be categorized as high-throughput workloads which transition to high-performance workloads as preprocessed data are aggregated. The high-throughput elements are of particular importance in the context of live processing, where an optimal response is highly coupled to the temporal profile of the data collection. In other words, each movie should be processed as quickly as possible at the earliest opportunity. The high level of disconnected parallelization in the high-throughput problem directly allows a completely scalable solution across a distributed computer system, with the only technical obstacle being an efficient and reliable implementation. The cloud computing frameworks primarily developed for the deployment of high-availability web applications provide an environment with a number of appealing features for such high-throughput processing tasks. Here, an implementation of an early-stage processing pipeline for electron cryotomography experiments using a service-based architecture deployed on a Kubernetes cluster is discussed in order to demonstrate the benefits of this approach and how it may be extended to scenarios of considerably increased complexity.

Data acquisition and processing for cryo-electron tomography can be a significant bottleneck for users. To simplify and streamline the cryo-ET workflow, Tomo Live, an on-the-fly solution that automates the alignment and reconstruction of tilt-series data, enabling real-time data-quality assessment, has been developed. Through the integration of Tomo Live into the data-acquisition workflow for cryo-ET, motion correction is performed directly after each of the acquired tilt angles. Immediately after the tilt-series acquisition has completed, an unattended tilt-series alignment and reconstruction into a 3D volume is performed. The results are displayed in real time in a dedicated remote web platform that runs on the microscope hardware. Through this web platform, users can review the acquired data (aligned stack and 3D volume) and several quality metrics that are obtained during the alignment and reconstruction process. These quality metrics can be used for fast feedback for subsequent acquisitions to save time. Parameters such as Alignment Accuracy, Deleted Tilts and Tilt Axis Correction Angle are visualized as graphs and can be used as filters to export only the best tomograms (raw data, reconstruction and intermediate data) for further processing. Here, the Tomo Live algorithms and workflow are described and representative results on several biological samples are presented. The Tomo Live workflow is accessible to both expert and non-expert users, making it a valuable tool for the continued advancement of structural biology, cell biology and histology.

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 TEM Imaging and Analysis (TIA) scripting and TEM scripting to access the STEM functionalities of the microscope, and DigitalMicrograph scripting to control the camera for snapshot data acquisition. Data analysis adapts the existing workflow using the software CrystFEL, 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, ab initio 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 ab initio structure determination of ZSM-25.

The application of grazing-incidence total X-ray scattering (GITXS) for pair distribution function (PDF) analysis using >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.

Investigation of the analyte soaking conditions on the crystalline sponge {[(ZnI2)3(tpt)2·x(solvent)]n} method using a statistical design of experiments model has provided fundamental insights into the influence of experimental variables. This approach focuses on a single analyte tested via 60 experiments (20 unique conditions) to identify the main effects for success and overall guest structure quality. This is employed as a basis for the development of a novel molecular structure grading system that enables the quantification of guest exchange quality.

Crystallographic texture is a key organization feature of many technical and biological materials. In these materials, especially hierarchically structured ones, the preferential alignment of the nano constituents heavily influences the macroscopic behavior of the material. To study local crystallographic texture with both high spatial and angular resolution, we developed Texture Tomography (TexTOM). This approach allows the user to model the diffraction data of polycrystalline materials using the full reciprocal space of the crystal ensemble and describe the texture in each voxel via an orientation distribution function, hence it provides 3D reconstructions of the local texture by measuring the probabilities of all crystal orientations. The TexTOM approach addresses limitations associated with existing models: it correlates the intensities from several Bragg reflections, thus reducing ambiguities resulting from symmetry. Further, it yields quantitative probability distributions of local real space crystal orientations without further assumptions about the sample structure. Finally, its efficient mathematical formulation enables reconstructions faster than the time scale of the experiment. This manuscript presents the mathematical model, the inversion strategy and its current experimental implementation. We show characterizations of simulated data as well as experimental data obtained from a synthetic, inorganic model sample: the silica–witherite biomorph. TexTOM provides a versatile framework to reconstruct 3D quantitative texture information for polycrystalline samples; it opens the door for unprecedented insights into the nanostructural makeup of natural and technical materials.

A few real case examples are presented on how to report magnetic structures, with precise step-by-step explanations, following the guidelines of the IUCr Commission on Magnetic Structures [Perez-Mato et al. (2024). Acta Cryst. B80, 219–234]. Four examples have been chosen, illustrating different types of single-k magnetic orders, from the basic case to more complex ones, including odd-harmonics, and one multi-k order. In addition to acquainting researchers with the process of communicating commensurate magnetic structures, these examples also aim to clarify important concepts, which are used throughout the guidelines, such as the transformation to a standard setting of a magnetic space group.

The compounds bis­(morpholine-κN)gold(I) chloride, [Au(C4H9NO)2]Cl, 1, and bis­(morpholine-κN)gold(I) bromide, [Au(C4H9NO)2]Br, 2, crystallize isotypically in space group C2/c with Z = 4. The gold atoms, which are axially positioned at the morpholine rings, lie on inversion centres (so that the N—Au—N coordination is exactly linear) and the halide anions on twofold axes. The residues are connected by a classical hydrogen bond N—H⋯halide and by a short gold⋯halide contact to form a layer structure parallel to the bc plane. The morpholine oxygen atom is not involved in classical hydrogen bonding.

In the title benzyl­ideneaniline Schiff base, C18H22N2O, the aromatic rings are inclined to each other by 46.01 (6)°, while the Car—N= C—Car torsion angle is 176.9 (1)°. In the crystal, the only identifiable directional inter­action is a weak C—H⋯π hydrogen bond, which generates inversion dimers that stack along the a-axis direction.

The in­do­line portion of the title mol­ecule, C16H13NO2, is planar. In the crystal, a layer structure is generated by C—H⋯O hydrogen bonds and C—H⋯π(ring), π-stacking and C=O⋯π(ring) inter­actions. The Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (43.0%), H⋯C/C⋯H (25.0%) and H⋯O/O⋯H (22.8%) inter­actions. Hydrogen bonding and van der Waals inter­actions are the dominant inter­actions in the crystal packing. The volume of the crystal voids and the percentage of free space were calculated to be 120.52 Å3 and 9.64%, respectively, showing that there is no large cavity in the crystal packing. Evaluation of the electrostatic, dispersion and total energy frameworks indicate that the stabilization is dominated by the dispersion energy contributions in the title compound. Moreover, the DFT-optimized structure at the B3LYP/6-311G(d,p) level is compared with the experimentally determined mol­ecular structure in the solid state.

The title compound, [CdBr2(C6H14N2O)], was synthesized upon complexation of 4-(2-aminoethyl)morpholine and cadmium(II) bromide tetra­hydrate at 303 K. It crystallizes as a centrosymmetric dimer, with one cadmium atom, two bromine atoms and one N,N'-bidentate 4-(2-aminoethyl)morpholine ligand in the asymmetric unit. The metal atom is six-coordinated and has a distorted octa­hedral geometry. In the crystal, O⋯Cd inter­actions link the dimers into a polymeric double chain and inter­molecular C—H⋯O hydrogen bonds form R22(6) ring motifs. Further C—H⋯Br and N—H⋯Br hydrogen bonds link the components into a three-dimensional network. As the N—H⋯Br hydrogen bonds are shorter than the C—H⋯Br inter­actions, they have a larger effect on the packing. A Hirshfeld surface analysis reveals that the largest contributions to the packing are from H⋯H (46.1%) and Br⋯H/H⋯Br (38.9%) inter­actions with smaller contributions from the O⋯H/H⋯O (4.7%), Br⋯Cd/Cd⋯Br (4.4%), O⋯Cd/Cd⋯O (3.5%), Br⋯Br (1.1%), Cd⋯H/H⋯Cd (0.9%), Br⋯O/O⋯Br (0.3%) and O⋯N/N⋯O (0.1%) contacts.

The title mol­ecule, [Fe2(C5H5)2(C23H17ClN2)]·C3H7NO, is twisted end to end and the central N/C/N unit is disordered. In the crystal, several C—H⋯π(ring) inter­actions lead to the formation of layers, which are connected by further C—H⋯π(ring) inter­actions. A Hirshfeld surface analysis of the crystal structure indicates that the most important contributions for the crystal packing are from H⋯H (60.2%) and H⋯C/C⋯H (27.0%) inter­actions. Hydrogen bonding, C—H⋯π(ring) inter­actions and van der Waals inter­actions dominate the crystal packing.

The crystal structures and Hirshfeld surface analyses of three similar compounds are reported. Methyl 4-[4-(di­fluoro­meth­oxy)phen­yl]-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexa­hydro­quinoline-3-carboxyl­ate, (C21H23F2NO4), (I), crystallizes in the monoclinic space group C2/c with Z = 8, while isopropyl 4-[4-(di­fluoro­meth­oxy)phen­yl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexa­hydro­quinoline-3-carb­oxyl­ate, (C23H27F2NO4), (II) and tert-butyl 4-[4-(di­fluoro­meth­oxy)phen­yl]-2,6,6-trimethyl-5-oxo-1,4,5,6,7,8-hexa­hydro­quinoline-3-carboxyl­ate, (C24H29F2NO4), (III) crystallize in the ortho­rhom­bic space group Pbca with Z = 8. In the crystal structure of (I), mol­ecules are linked by N—H⋯O and C—H⋯O inter­actions, forming a tri-periodic network, while mol­ecules of (II) and (III) are linked by N—H⋯O, C—H⋯F and C—H⋯π inter­actions, forming layers parallel to (002). The cohesion of the mol­ecular packing is ensured by van der Waals forces between these layers. In (I), the atoms of the 4-di­fluoro­meth­oxy­phenyl group are disordered over two sets of sites in a 0.647 (3): 0.353 (3) ratio. In (III), the atoms of the dimethyl group attached to the cyclo­hexane ring, and the two carbon atoms of the cyclo­hexane ring are disordered over two sets of sites in a 0.646 (3):0.354 (3) ratio.

The crystal structure of the title compound {systematic name: (4S,4aS,5aR,12aR)-4,7-bis­(di­methyl­amino)-9-[(2,2-di­methyl­propyl­amino)­meth­yl]-1,10,11,12a-tetra­hydroxy-3,12-dioxo-4a,5,5a,6-tetra­hydro-4H-tetra­cene-2-carb­oxamide dihydrate, C29H40N4O7·2H2O} has been solved and refined using synchrotron X-ray powder diffraction data: it crystallizes in space group R3 with a = 24.34430 (7), c = 14.55212 (4) Å, V = 7468.81 (2) Å3 and Z = 9. Most of the hydrogen bonds are intra­molecular, but two classical N—H⋯O inter­molecular hydrogen bonds (along with probable weak C—H⋯O and C—H⋯N hydrogen bonds) link the mol­ecules into a three-dimensional framework. The framework contains voids, which contain disordered water mol­ecules. Keto–enol tautomerism is apparently important in this mol­ecule, and the exact mol­ecular structure is ambiguous.

In the title compound, C17H12N2O, the quinoxaline moiety shows deviations of 0.0288 (7) to −0.0370 (7) Å from the mean plane (r.m.s. deviation of fitted atoms = 0.0223 Å). In the crystal, corrugated layers two mol­ecules thick are formed by C—H⋯N hydrogen bonds and π-stacking inter­actions.

The title coordination polymer with the 4-methyl-N-(pyridin-2-yl­methyl­idene)aniline Schiff base ligand (L, C13H12N2), [Cd2Cl4(C13H12N2)]n (1), exhibits a columnar structure extending parallel to [100]. The columns are aligned in parallel and are decorated with chelating L ligands on both sides. They are elongated into a supra­molecular sheet extending parallel to (01overline{1}) through π–π stacking inter­actions involving L ligands of neighbouring columns. Adjacent sheets are packed into the tri-periodic supra­molecular network through weak C—H⋯Cl hydrogen-bonding inter­actions that involve the phenyl CH groups and chlorido ligands. The thermal stability and photoluminescent properties of (1) have also been examined.

The reaction of lithium hexa­methyl­disilyl­amide, [Li{N(Si(CH3)3)2}] (LiHMDS), with 4,4-dimethyl-2-phenyl-2-oxazoline (Phox, C11H13NO) in hexane produced colourless crystals of bis­(4,4-dimethyl-2-phenyl-2-oxazoline-κN)(hexa­methyl­disilyl­amido-κN)lithium, [Li(C6H18NSi2)(C11H13NO)2] or [Li{N(Si(CH3)3)2}(Phox)2] in high yield (89%). Despite the 1:1 proportion of the starting materials in the reaction mixture, the product formed with a 1:2 amide:oxazoline ratio. In the unit cell of the C2/c space group, the neutral mol­ecules lie on twofold rotation axes coinciding with the Li—N(amide) bonds. The lithium(I) centre adopts a trigonal–planar coordination geometry with three nitro­gen donor atoms, one from the HMDS anion and two from the oxazolines. All ligands are monodentate. In the phenyl­oxazoline units, the dihedral angle defined by the five-membered heterocyclic rings is 35.81 (5)°, while the phenyl substituents are approximately face-to-face, separated by 3.908 (5) Å. In the amide, the methyl groups assume a nearly eclipsed arrangement to minimize steric repulsion with the analogous substituents on the oxazoline rings. The non-covalent inter­actions in the solid-state structure of [Li{N(Si(CH3)3)2}(Phox)2] were assessed by Hirshfeld surface analysis and fingerprint plots. This new compound is attractive for catalysis due to its unique structural features.

Three organoplatinum(II) complexes bearing natural aryl­olefin and quinoline derivatives, namely, [4-meth­oxy-5-(2-meth­oxy-2-oxoeth­oxy)-2-(prop-2-en-1-yl)phen­yl](quinolin-8-olato)platinum(II), [Pt(C13H15O4)(C9H6NO)], (I), [4-meth­oxy-5-(2-oxo-2-propoxyeth­oxy)-2-(prop-2-en-1-yl)phen­yl](quinoline-2-carboxy­l­ato)platinum(II), [Pt(C15H19O4)(C10H6NO2)], (II), and chlorido­[4-meth­oxy-5-(2-oxo-2-propoxyeth­oxy)-2-(prop-2-en-1-yl)phen­yl](quinoline)­plat­inum(II), [Pt(C15H19O4)Cl(C9H7N)], (III), were synthesized and structurally characterized by IR and 1H NMR spectroscopy, and by single-crystal X-ray diffraction. The results showed that the cyclo­platinated aryl­olefin coordinates with PtII via the carbon atom of the phenyl ring and the C=Colefinic group. The deprotonated 8-hy­droxy­quinoline (C9H6NO) and quinoline-2-carb­oxy­lic acid (C10H6NO2) coordinate with the PtII atom via the N and O atoms in complexes (I) and (II) while the quinoline (C9H7N) coordinates via the N atom in (III). Moreover, the coordinating N atom in complexes (I)–(III) is in the cis position compared to the C=Colefinic group. The crystal packing is characterized by C—H⋯π, C—H⋯O [for (II) and (III)], C—H⋯Cl [for (III) and π–π [for (I)] inter­actions.

The structural characterization is reported of the supra­molecular complex between the tetra­quinoxaline-based cavitand 2,8,14,20-tetra­hexyl-6,10:12,16:18,22:24,4-O,O'-tetra­kis­(quinoxaline-2,3-di­yl)calix[4]resorcinarene (QxCav) with benzo­nitrile. The complex, of general formula C84H80N8O8·2C7H5N, crystallizes in the space group Poverline{1} with two independent mol­ecules in the asymmetric unit, displaying very similar geometrical parameters. For each complex, one of the benzo­nitrile mol­ecules is engulfed inside the cavity, while the other is located among the alkyl legs at the lower rim. The host and the guests mainly inter­act through weak C—H⋯π, C—H⋯N and dispersion inter­actions. These inter­actions help to consolidate the formation of supra­molecular chains running along the crystallographic b-axis direction.

A new quinoline derivative, namely, 6-(di­ethyl­amino)-4-phenyl-2-(pyridin-2-yl)quinoline, C24H23N3 (QP), and its MnII complex aqua-1κO-di-μ-chlorido-1:2κ4Cl:Cl-di­chlorido-1κCl,2κCl-bis­[6-(di­ethyl­amino)-4-phenyl-2-(pyridin-2-yl)quinoline]-1κ2N1,N2;2κ2N1,N2-dimanganese(II), [Mn2Cl4(C24H23N3)2(H2O)] (MnQP), were synthesized. Their compositions have been determined with ESI-MS, IR, and 1H NMR spectroscopy. The crystal-structure determination of MnQP revealed a dinuclear complex with a central four-membered Mn2Cl2 ring. Both MnII atoms bind to an additional Cl atom and to two N atoms of the QP ligand. One MnII atom expands its coordination sphere with an extra water mol­ecule, resulting in a distorted octa­hedral shape. The second MnII atom shows a distorted trigonal–bipyramidal shape. The UV–vis absorption and emission spectra of the examined compounds were studied. Furthermore, when investigating the aggregation-induced emission (AIE) properties, it was found that the fluorescent color changes from blue to green and eventually becomes yellow as the fraction of water in the THF/water mixture increases from 0% to 99%. In particular, these color and intensity changes are most pronounced at a water fraction of 60%. The crystal structure contains disordered solvent mol­ecules, which could not be modeled. The SQUEEZE procedure [Spek (2015). Acta Cryst. C71, 9–18] was used to obtain information on the type and qu­antity of solvent mol­ecules, which resulted in 44 electrons in a void volume of 274 Å3, corresponding to approximately 1.7 mol­ecules of ethanol in the unit cell. These ethanol mol­ecules are not considered in the given chemical formula and other crystal data.

The asymmetric unit of the title compound is composed of two independent ion pairs of 4-(di­methyl­amino)­pyridin-1-ium 8-hy­droxy­quinoline-5-sulfonate (HDMAP+·HqSA−, C7H11N2+·C9H6NO4S−) and neutral N,N-di­methyl­pyridin-4-amine mol­ecules (DMAP, C7H10N2), co-crystallized as a 1:1:1 HDMAP+:HqSA−:DMAP adduct in the monoclinic system, space group Pc. The compound has a layered structure, including cation layers of HDMAP+ with DMAP and anion layers of HqSA− in the crystal. In the cation layer, there are inter­molecular N—H⋯N hydrogen bonds between the protonated HDMAP+ mol­ecule and the neutral DMAP mol­ecule. In the anion layer, each HqSA− is surrounded by other six HqSA−, where the planar network structure is formed by inter­molecular O—H⋯O and C—H⋯O hydrogen bonds. The cation and anion layers are linked by inter­molecular C—H⋯O hydrogen bonds and C—H⋯π inter­actions.

The cyclic peptide cyclo(Val-Leu-Leu-d-Phe-Pro)2 (peptide 1) was specifically designed for structural chemistry investigations, drawing inspiration from Gramicidin S (GS). Previous studies have shown that Pro residues within 1 adopt a down-puckering conformation of the pyrrolidine ring. By incorporating fluoride-Pro with 4-trans/cis-isomers into 1, an up-puckering conformation was successfully induced. In the current investigation, introducing hy­droxy­prolines with 4-trans/cis-isomer configurations (tHyp/cHyp) into 1 gave cyclo(Val-Leu-Leu-d-Phe-tHyp)2 methanol disolvate monohydrate, C62H94N10O12·2CH4O·H2O (4), and cyclo(Val-Leu-Leu-d-Phe-cHyp)2 monohydrate, C62H94N10O12·H2O (5), respectively. However, the puckering of 4 and 5 remained in the down conformation, regardless of the geometric position of the hydroxyl group. Although the backbone structure of 4 with trans-substitution was asymmetric, the asymmetric backbone of 5 with cis-substitution was unexpected. It is speculated that the anti­cipated influence of stress from the geometric positioning, which was expected to affect the puckering, may have been mitigated by inter­actions between the hydroxyl groups of hy­droxy­proline, the solvent mol­ecules, and peptides.

In the structure of the title salt, {[Ba(μ3-C3H2N3O2)2(μ-H2O)(H2O)]·H2O}n, the barium ion and all three oxygen atoms of the water mol­ecules reside on a mirror plane. The hydrogen atoms of the bridging water and the solvate water mol­ecules are arranged across a mirror plane whereas all atoms of the monodentate aqua ligand are situated on this mirror plane. The distorted ninefold coord­ination of the Ba ions is completed with four nitroso-, two carbonyl- and three aqua-O atoms at the distances of 2.763 (3)–2.961 (4) Å and it is best described as tricapped trigonal prism. The three-dimensional framework structure is formed by face-sharing of the trigonal prisms, via μ-nitroso- and μ-aqua-O atoms, and also by the bridging coordination of the anions via carbonyl-O atoms occupying two out of the three cap positions. The solvate water mol­ecules populate the crystal channels and facilitate a set of four directional hydrogen bonds. The principal Ba–carbamoyl­cyano­nitro­somethanido linkage reveals a rare example of the inherently polar binodal six- and three-coordinated bipartite topology (three-letter notation sit). It suggests that small resonance-stabilized cyano­nitroso anions can be utilized as bridging ligands for the supra­molecular synthesis of MOF solids. Such an outcome may be anti­cipated for a broader range of hard Lewis acidic alkaline earth metal ions, which perfectly match the coordination preferences of highly nucleophilic nitroso-O atoms. Thermal analysis reveals two-stage dehydration of the title compound (383 and 473 K) followed by decomposition with release of CO2, HCN and H2O at 558 K.

This work describes the X-ray structure of orange–red crystals of 2-meth­oxy-5-nitro­aniline, C7H8N2O3. The compound displays concentration-dependent UV-Vis spectra, which is attributed to dipole-induced aggregation, and light absorption arising from an inter­molecular charge-transfer process that decreases in energy as the degree of aggregation increases. The crystals display π-stacking where the dipole moments align anti­parallel. Stacked mol­ecules inter­act with the next stack via hydrogen bonds, which is a state of maximum aggregation. Light absorption by charge transfer can be compared to colored inorganic semiconductors such as orange–red CdS, with a band gap of 2.0–2.5 eV.