graphic Analysis of crystallographic phase retrieval using iterative projection algorithms By journals.iucr.org Published On :: 2024-10-23 For protein crystals in which more than two thirds of the volume is occupied by solvent, the featureless nature of the solvent region often generates a constraint that is powerful enough to allow direct phasing of X-ray diffraction data. Practical implementation relies on the use of iterative projection algorithms with good global convergence properties to solve the difficult nonconvex phase-retrieval problem. In this paper, some aspects of phase retrieval using iterative projection algorithms are systematically explored, where the diffraction data and density-value distributions in the protein and solvent regions provide the sole constraints. The analysis is based on the addition of random error to the phases of previously determined protein crystal structures, followed by evaluation of the ability to recover the correct phase set as the distance from the solution increases. The properties of the difference-map (DM), relaxed–reflect–reflect (RRR) and relaxed averaged alternating reflectors (RAAR) algorithms are compared. All of these algorithms prove to be effective for crystallographic phase retrieval, and the useful ranges of the adjustable parameter which controls their behavior are established. When these algorithms converge to the solution, the algorithm trajectory becomes stationary; however, the density function continues to fluctuate significantly around its mean position. It is shown that averaging over the algorithm trajectory in the stationary region, following convergence, improves the density estimate, with this procedure outperforming previous approaches for phase or density refinement. Full Article text
graphic The interoperability of crystallographic data and databases By journals.iucr.org Published On :: 2024-01-01 Interoperability of crystallographic data with other disciplines is essential for the smooth and rapid progress of structure-based science in the computer age. Within crystallography and closely related subject areas, there is already a high level of conformance to the generally accepted FAIR principles (that data be findable, accessible, interoperable and reusable) through the adoption of common information exchange protocols by databases, publishers, instrument vendors, experimental facilities and software authors. Driven by the success within these domains, the IUCr has worked closely with CODATA (the Committee on Data of the International Science Council) to help develop the latter's commitment to cross-domain integration of discipline-specific data. The IUCr has, in particular, emphasized the need for standards relating to data quality and completeness as an adjunct to the FAIR data landscape. This can ensure definitive reusable data, which in turn can aid interoperability across domains. A microsymposium at the IUCr 2023 Congress provided an up-to-date survey of data interoperability within and outside of crystallography, expounded using a broad range of examples. Full Article text
graphic From X-ray crystallographic structure to intrinsic thermodynamics of protein–ligand binding using carbonic anhydrase isozymes as a model system By journals.iucr.org Published On :: 2024-06-10 Carbonic anhydrase (CA) was among the first proteins whose X-ray crystal structure was solved to atomic resolution. CA proteins have essentially the same fold and similar active centers that differ in only several amino acids. Primary sulfonamides are well defined, strong and specific binders of CA. However, minor variations in chemical structure can significantly alter their binding properties. Over 1000 sulfonamides have been designed, synthesized and evaluated to understand the correlations between the structure and thermodynamics of their binding to the human CA isozyme family. Compound binding was determined by several binding assays: fluorescence-based thermal shift assay, stopped-flow enzyme activity inhibition assay, isothermal titration calorimetry and competition assay for enzyme expressed on cancer cell surfaces. All assays have advantages and limitations but are necessary for deeper characterization of these protein–ligand interactions. Here, the concept and importance of intrinsic binding thermodynamics is emphasized and the role of structure–thermodynamics correlations for the novel inhibitors of CA IX is discussed – an isozyme that is overexpressed in solid hypoxic tumors, and thus these inhibitors may serve as anticancer drugs. The abundant structural and thermodynamic data are assembled into the Protein–Ligand Binding Database to understand general protein–ligand recognition principles that could be used in drug discovery. Full Article text
graphic Crystallographic phase identifier of a convolutional self-attention neural network (CPICANN) on powder diffraction patterns By journals.iucr.org Published On :: 2024-06-27 Spectroscopic data, particularly diffraction data, are essential for materials characterization due to their comprehensive crystallographic information. The current crystallographic phase identification, however, is very time consuming. To address this challenge, we have developed a real-time crystallographic phase identifier based on a convolutional self-attention neural network (CPICANN). Trained on 692 190 simulated powder X-ray diffraction (XRD) patterns from 23 073 distinct inorganic crystallographic information files, CPICANN demonstrates superior phase-identification power. Single-phase identification on simulated XRD patterns yields 98.5 and 87.5% accuracies with and without elemental information, respectively, outperforming JADE software (68.2 and 38.7%, respectively). Bi-phase identification on simulated XRD patterns achieves 84.2 and 51.5% accuracies, respectively. In experimental settings, CPICANN achieves an 80% identification accuracy, surpassing JADE software (61%). Integration of CPICANN into XRD refinement software will significantly advance the cutting-edge technology in XRD materials characterization. Full Article text
graphic Determining magnetic structures in GSAS-II using the Bilbao Crystallographic Server tool k-SUBGROUPSMAG By journals.iucr.org Published On :: 2024-09-20 The embedded call to a special version of the web-based Bilbao Crystallographic Server tool k-SUBGROUPSMAG from within GSAS-II to form a list of all possible commensurate magnetic subgroups of a parent magnetic grey group is described. It facilitates the selection and refinement of the best commensurate magnetic structure model by having all the analysis tools including Rietveld refinement in one place as part of GSAS-II. It also provides the chosen magnetic space group as one of the 1421 possible standard Belov–Neronova–Smirnova forms or equivalent non-standard versions. Full Article text
graphic Acta Crystallographica Section F By journals.iucr.org Published On :: Full Article Still image
graphic Synthesis and crystallographic characterization of 6-hydroxy-1,2-dihydropyridin-2-one By journals.iucr.org Published On :: 2023-11-14 The title compound, C5H5NO2, is a hydroxylated pyridine ring that has been studied for its involvement in microbial degradation of nicotinic acid. Here we describe its synthesis as a formic acid salt, rather than the standard hydrochloride salt that is commercially available, and its spectroscopic and crystallographic characterization. Full Article text
graphic When a dream comes true: birth of the African Crystallographic Association (AfCA) By journals.iucr.org Published On :: 2024-01-05 This paper summarizes brief perspectives on the historic process of establishing an African Crystallographic Association (AfCA) and includes representative references. It covers activities within four arbitrarily selected, approximate time slots, i.e., 1890s–1999, 2000–2013, 2014–2019 and 2020–2023. A genuine attempt is made to include appropriate role players, organizations and accompanying events within these periods. It concludes with the official admission of AfCA as the fifth Regional Associate of the IUCr at the 26th Congress and General Assembly of the IUCr in Melbourne, Australia in 2023. Full Article text
graphic FLEXR GUI: a graphical user interface for multi-conformer modeling of proteins By journals.iucr.org Published On :: 2024-03-27 Proteins are well known `shapeshifters' which change conformation to function. In crystallography, multiple conformational states are often present within the crystal and the resulting electron-density map. Yet, explicitly incorporating alternative states into models to disentangle multi-conformer ensembles is challenging. We previously reported the tool FLEXR, which, within a few minutes, automatically separates conformational signal from noise and builds the corresponding, often missing, structural features into a multi-conformer model. To make the method widely accessible for routine multi-conformer building as part of the computational toolkit for macromolecular crystallography, we present a graphical user interface (GUI) for FLEXR, designed as a plugin for Coot 1. The GUI implementation seamlessly connects FLEXR models with the existing suite of validation and modeling tools available in Coot. We envision that FLEXR will aid crystallographers by increasing access to a multi-conformer modeling method that will ultimately lead to a better representation of protein conformational heterogeneity in the Protein Data Bank. In turn, deeper insights into the protein conformational landscape may inform biology or provide new opportunities for ligand design. The code is open source and freely available on GitHub at https://github.com/TheFischerLab/FLEXR-GUI. Full Article text
graphic Ray-tracing analytical absorption correction for X-ray crystallography based on tomographic reconstructions By journals.iucr.org Published On :: 2024-04-15 Processing of single-crystal X-ray diffraction data from area detectors can be separated into two steps. First, raw intensities are obtained by integration of the diffraction images, and then data correction and reduction are performed to determine structure-factor amplitudes and their uncertainties. The second step considers the diffraction geometry, sample illumination, decay, absorption and other effects. While absorption is only a minor effect in standard macromolecular crystallography (MX), it can become the largest source of uncertainty for experiments performed at long wavelengths. Current software packages for MX typically employ empirical models to correct for the effects of absorption, with the corrections determined through the procedure of minimizing the differences in intensities between symmetry-equivalent reflections; these models are well suited to capturing smoothly varying experimental effects. However, for very long wavelengths, empirical methods become an unreliable approach to model strong absorption effects with high fidelity. This problem is particularly acute when data multiplicity is low. This paper presents an analytical absorption correction strategy (implemented in new software AnACor) based on a volumetric model of the sample derived from X-ray tomography. Individual path lengths through the different sample materials for all reflections are determined by a ray-tracing method. Several approaches for absorption corrections (spherical harmonics correction, analytical absorption correction and a combination of the two) are compared for two samples, the membrane protein OmpK36 GD, measured at a wavelength of λ = 3.54 Å, and chlorite dismutase, measured at λ = 4.13 Å. Data set statistics, the peak heights in the anomalous difference Fourier maps and the success of experimental phasing are used to compare the results from the different absorption correction approaches. The strategies using the new analytical absorption correction are shown to be superior to the standard spherical harmonics corrections. While the improvements are modest in the 3.54 Å data, the analytical absorption correction outperforms spherical harmonics in the longer-wavelength data (λ = 4.13 Å), which is also reflected in the reduced amount of data being required for successful experimental phasing. Full Article text
graphic Ptychographic phase retrieval via a deep-learning-assisted iterative algorithm By journals.iucr.org Published On :: 2024-08-19 Ptychography is a powerful computational imaging technique with microscopic imaging capability and adaptability to various specimens. To obtain an imaging result, it requires a phase-retrieval algorithm whose performance directly determines the imaging quality. Recently, deep neural network (DNN)-based phase retrieval has been proposed to improve the imaging quality from the ordinary model-based iterative algorithms. However, the DNN-based methods have some limitations because of the sensitivity to changes in experimental conditions and the difficulty of collecting enough measured specimen images for training the DNN. To overcome these limitations, a ptychographic phase-retrieval algorithm that combines model-based and DNN-based approaches is proposed. This method exploits a DNN-based denoiser to assist an iterative algorithm like ePIE in finding better reconstruction images. This combination of DNN and iterative algorithms allows the measurement model to be explicitly incorporated into the DNN-based approach, improving its robustness to changes in experimental conditions. Furthermore, to circumvent the difficulty of collecting the training data, it is proposed that the DNN-based denoiser be trained without using actual measured specimen images but using a formula-driven supervised approach that systemically generates synthetic images. In experiments using simulation based on a hard X-ray ptychographic measurement system, the imaging capability of the proposed method was evaluated by comparing it with ePIE and rPIE. These results demonstrated that the proposed method was able to reconstruct higher-spatial-resolution images with half the number of iterations required by ePIE and rPIE, even for data with low illumination intensity. Also, the proposed method was shown to be robust to its hyperparameters. In addition, the proposed method was applied to ptychographic datasets of a Simens star chart and ink toner particles measured at SPring-8 BL24XU, which confirmed that it can successfully reconstruct images from measurement scans with a lower overlap ratio of the illumination regions than is required by ePIE and rPIE. Full Article text
graphic Energy-dispersive Laue diffraction analysis of the influence of statherin and histatin on the crystallographic texture during human dental enamel demineralization By journals.iucr.org Published On :: 2024-09-25 Energy-dispersive Laue diffraction (EDLD) is a powerful method to obtain position-resolved texture information in inhomogeneous biological samples without the need for sample rotation. This study employs EDLD texture scanning to investigate the impact of two salivary peptides, statherin (STN) and histatin-1 (HTN) 21 N-terminal peptides (STN21 and HTN21), on the crystallographic structure of dental enamel. These proteins are known to play crucial roles in dental caries progression. Three healthy incisors were randomly assigned to three groups: artificially demineralized, demineralized after HTN21 peptide pre-treatment and demineralized after STN21 peptide pre-treatment. To understand the micro-scale structure of the enamel, each specimen was scanned from the enamel surface to a depth of 250 µm using microbeam EDLD. Via the use of a white beam and a pixelated detector, where each pixel functions as a spectrometer, pole figures were obtained in a single exposure at each measurement point. The results revealed distinct orientations of hydroxyapatite crystallites and notable texture variation in the peptide-treated demineralized samples compared with the demineralized control. Specifically, the peptide-treated demineralized samples exhibited up to three orientation populations, in contrast to the demineralized control which displayed only a single orientation population. The texture index of the demineralized control (2.00 ± 0.21) was found to be lower than that of either the STN21 (2.32 ± 0.20) or the HTN21 (2.90 ± 0.46) treated samples. Hence, texture scanning with EDLD gives new insights into dental enamel crystallite orientation and links the present understanding of enamel demineralization to the underlying crystalline texture. For the first time, the feasibility of EDLD texture measurements for quantitative texture evaluation in demineralized dental enamel samples is demonstrated. Full Article text
graphic Free tools for crystallographic symmetry handling and visualization By journals.iucr.org Published On :: 2024-09-20 Online courses and innovative teaching methods have triggered a trend in education, where the integration of multimedia, online resources and interactive tools is reshaping the view of both virtual and traditional classrooms. The use of interactive tools extends beyond the boundaries of the physical classroom, offering students the flexibility to access materials at their own speed and convenience and enhancing their learning experience. In the field of crystallography, there are a wide variety of free online resources such as web pages, interactive applets, databases and programs that can be implemented in fundamental crystallography courses for different academic levels and curricula. This paper discusses a variety of resources that can be helpful for crystallographic symmetry handling and visualization, discussing four specific resources in detail: the Bilbao Crystallographic Server, the Cambridge Structural Database, VESTA and Jmol. The utility of these resources is explained and shown by several illustrative examples. Full Article text
graphic Towards dynamically configured databases for CIFs: the new modulated structures open database at the Bilbao Crystallographic Server By journals.iucr.org Published On :: 2024-09-17 This article presents a web-based framework to build a database without in-depth programming knowledge given a set of CIF dictionaries and a collection of CIFs. The framework consists of two main elements: the public site that displays the information contained in the CIFs in an ordered manner, and the restricted administrative site which defines how that information is stored, processed and, eventually, displayed. Thus, the web application allows users to easily explore, filter and access the data, download the original CIFs, and visualize the structures via JSmol. The modulated structures open database B-IncStrDB, the official International Union of Crystallography repository for this type of material and available through the Bilbao Crystallographic Server, has been re-implemented following the proposed framework. Full Article text
graphic SUBGROUPS: a computer tool at the Bilbao Crystallographic Server for the study of pseudo-symmetric or distorted structures By journals.iucr.org Published On :: 2024-10-01 SUBGROUPS is a free online program at the Bilbao Crystallographic Server (https://www.cryst.ehu.es/). It permits the exploration of all possible symmetries resulting from the distortion of a higher-symmetry parent structure, provided that the relation between the lattices of the distorted and parent structures is known. The program calculates all the subgroups of the parent space group which comply with this relation. The required minimal input is the space-group information of the parent structure and the relation of the unit cell of the distorted or pseudo-symmetric structure with that of the parent structure. Alternatively, the wavevector(s) observed in the diffraction data characterizing the distortion can be introduced. Additional conditions can be added, including filters related to space-group representations. The program provides very detailed information on all the subgroups, including group–subgroup hierarchy graphs. If a Crystallographic Information Framework (CIF) file of the parent high-symmetry structure is uploaded, the program generates CIF files of the parent structure described under each of the chosen lower symmetries. These CIF files may then be used as starting points for the refinement of the distorted structure under these possible symmetries. They can also be used for density functional theory calculations or for any other type of analysis. The power and efficiency of the program are illustrated with a few examples. Full Article text
graphic USGS Releases New Topographic Maps for Puerto Rico and the U.S. Virgin Islands - Updated Maps for Essential Needs By www.usgs.gov Published On :: Thu, 31 Oct 2024 16:53:06 EDT The USGS is pleased to announce the release of new US Topo maps for Puerto Rico and the U.S. Virgin Islands. These updated topographic maps offer valuable, current geographic information for residents, visitors, and professionals, providing essential resources for communities in these areas. Full Article
graphic Eleven Questions for the Next Decade of Geographical Sciences Identified By Published On :: Thu, 25 Mar 2010 05:00:00 GMT Eleven questions that should shape the next decade of geographical sciences research were identified today in a new report by the National Research Council. Full Article
graphic Marketing Magic: How contractors can get the most out of their fleet graphics and branding By www.pmmag.com Published On :: Thu, 08 Jul 2021 00:00:00 -0400 According to a white paper authored by venture capital firm ARD Ventures, each fleet vehicle, on average, receives between 30,000 -70,000 impressions daily. Full Article
graphic Gnarly Head x Grateful Dead wines feature holographic labels By www.bevindustry.com Published On :: Fri, 13 Sep 2024 10:00:00 -0400 Gnarly Head wines and the Grateful Dead announced three new limited-release wine offerings packaged in eye-catching bottles that rock two of the band’s most beloved icons in shimmering holographic labels, the company says. Full Article
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