A detailed analysis of multiple diffraction data collected by the stereoscopic multibeam imaging technique from a tetragonal lysozyme crystal is reported. Calculations based on the dynamical theory are employed to account for diffraction profiles obtained with Bragg-angle scan in stereoscopic imaging and the conventional azimuthal scan in Renninger arrangement. The formation of a multibeam intensity profile and the relationship and mutual influence between the two scans are investigated. A simple practical method of quantitative estimation of the reflection phases of structure-factor multiplets from the experimental data obtained with two inversion-symmetry-related diffractions is proposed. The procedures for data handling and for distinguishing "partial" diffraction images from "full" diffraction images are also developed considering multibeam diffraction geometry and experimental conditions. These procedures thus provide a practical way of reconstructing diffraction profiles for experimental phase determination for macromolecular crystals.
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http://dx.doi.org/10.1107/s0108767301015963 | DOI Listing |
Inorg Chem
January 2025
Department of Chemistry, Biochemistry and Pharmaceutical Sciences, University of Bern, 3012 Bern, Switzerland.
Binuclear silver(I) and copper(I) complexes, and , with bridging diphenylphosphine ligands were prepared. In , the silver(I) center is located inside a trigonal plane composed of three phosphorus donors from three separate and bridging dppm ligands. The fourth coordination site is filled with neighboring silver(I) ions.
View Article and Find Full Text PDFSci Rep
January 2025
Jadara University Research Center, Jadara University, PO Box 733, Irbid, Jordan.
In this study, the AlFeO@n-Pr@Et-SOH heterogeneous catalyst was successfully synthesized and utilized to produce biodiesel from oleic acid through an esterification process and to oxidize sulfides. To examine the physicochemical characteristics of the AlFeO@n-Pr@Et-SOH nanomaterial, a variety of advanced techniques were employed, including Fourier Transform infrared spectroscopy (FT-IR), Field emission scanning electron microscopy (FE-SEM), Energy dispersive X-ray spectroscopy (EDX), Vibrating sample magnetometer (VSM), Elemental Mapping, Transmission electron microscopy (TEM), Inductively coupled plasma (ICP), and X-ray diffraction (XRD). The AlFeO@n-Pr@Et-SOH materials demonstrated excellent performance in both the esterification of oleic acid and the oxidation of sulfides.
View Article and Find Full Text PDFInorg Chem
January 2025
College of Material, Chemistry and Chemical Engineering, Key Laboratory of Organosilicon Chemistry and Material Technology, Ministry of Education, Hangzhou Normal University, Hangzhou 311121, China.
The salt metathesis reaction involving a diamine-based antimony chloride precursor with sodium arsaethynolate in the presence of PMe leads to the formation of stibanyl-functionalized PMe-arsinidene (). Detailed analyses through single-crystal X-ray diffraction and density functional theory of confirm the presence of covalent Sb-As bonds and reveal its polarized nature with a multiple-bond character. In contrast to the formation of complex , substituting PMe with xylyl isocyanide or 1,3-diisopropyl-4,5-dimethyl-imidazolin-2-ylidene () produces an isocyanide-arsinidene adduct () and an -arsaketene complex (), respectively.
View Article and Find Full Text PDFJ Phys Chem Lett
January 2025
DST Unit of Nanoscience (DST UNS) and Thematic Unit of Excellence (TUE), Department of Chemistry, Indian Institute of Technology Madras, Chennai 600036, India.
Clathrate hydrates (CHs) are believed to exist in cold regions of space, such as comets and icy moons. While spectroscopic studies have explored their formation under similar laboratory conditions, direct structural characterization using diffraction techniques has remained elusive. We present the first electron diffraction study of tetrahydrofuran (THF) and 1,3-dioxolane (DIOX) CHs in the form of nanometer-thin ice films under an ultrahigh vacuum at cryogenic temperatures.
View Article and Find Full Text PDFPharm Res
January 2025
Synthetic Molecule Pharmaceutical Sciences, Genentech, Inc., 1 DNA Way, South San Francisco, CA, 94080, USA.
Purpose: The purpose of this study is to present a correlative microscopy-tomography approach in conjunction with machine learning-based image segmentation techniques, with the goal of enabling quantitative structural and compositional elucidation of real-world pharmaceutical tablets.
Methods: Specifically, the approach involves three sequential steps: 1) user-oriented tablet constituent identification and characterization using correlative mosaic field-of-view SEM and energy dispersive X-ray spectroscopy techniques, 2) phase contrast synchrotron X-ray micro-computed tomography (SyncCT) characterization of a large, representative volume of the tablet, and 3) constituent segmentation and quantification of the imaging data through user-guided, iterative supervised machine learning and deep learning.
Results: This approach was implemented on a real-world tablet containing 15% API and multiple common excipients.
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