A deconvolutional method for preprocessing powder diffraction data has been improved. The cumulants of instrumental aberration functions of Bragg-Brentano (Parrish) diffractometer calculated up to the fourth order are presented. The treatments of axial-divergence aberration and the effective spectroscopic profile of the source X-ray have been simplified from those used in previous methods. The current

The crystal structure of trimethylarsine oxide dihydrate, (CH3)3AsO⋅2H2O, (TMAO dihydrate) has been solved using parallel tempering with the FOX software package and refined using synchrotron powder diffraction data obtained from beamline 08B1-1 at the Canadian Light Source. Rietveld refinement, performed with the software package GSASII, yielded orthorhombic lattice parameters of a = 13.3937(4) Å

The crystal structure of ceftriaxone sodium hemiheptahydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Ceftriaxone sodium hemiheptahydrate crystallizes in the space group C2 (#5) with a = 30.56 492(16), b = 4.75 264(2), c = 18.54 978(16) Å, β = 90.3545(6), V = 2694.562(21) Å3, and Z = 4. Both Na exhibit trigonal bipyramidal

Single-crystal and powder X-ray diffraction data, collected at room temperature, unit-cell parameters and space group for eluxadoline nitrate monohydrate, C32H35N5O5⋅2HNO3⋅H2O, are reported [a = 11.066(5) Å, b = 13.452(6) Å, c = 24.373(9) Å, unit-cell volume V = 3628.15 Å3, Z = 4, ρcal = 1.344 g⋅cm−3, and space group P212121]. All the diffraction peaks in the experimental pattern have been indexed

Li4Ti5O12 (LTO) and its doped analogues Li4Ti4.95M0.05O12 (M = Al3+, Co3+, Ni2+, and Mg2+) were synthesized and characterized using in situ PXRD to monitor the phase transitions during the sol–gel synthesis of the spinel material. These results are complimented by thermogravimetric analysis, which illustrates the decomposition of the materials synthesized, where the final LTO products are seen to form

X-ray powder diffraction data for estra-4,9-diene-3,17-dione, C18H22O2, are reported [a = 9.236(7) Å, b = 10.294(4) Å, c = 15.471(1) Å, unit cell volume V = 1471.11 Å3, Z = 4, and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurities were observed. The single-crystallographic data of the compound are also reported [a = 9.2392(7)

Precious ornaments from the Museum Royal Tombs of Sipán were analyzed by X-ray computed microtomography (microCT). The ornaments analyzed were golden earrings produced by the Moche culture that flourished along the north coast of present-day Peru between approximately 100 and 600 AD. Sipán, also known as Huava Rajada, is a mochica archaeological complex in the north of Peru. In particular, the spectacular

A provisional setup for X-ray microprobe experiments at 35 keV is described. It is based on compound refractive lenses (CRLs) for nanofocusing and a Vortex silicon drift detector with 2 mm sensor thickness for increased sensitivity at high energies. The Microprobe experiment (PETRA III) generally uses Kirkpatrick-Baez mirrors for submicrometer focusing in the energy range of 5–21 keV. However, various

Ba3−xSrxTb3−xCexO9 (x = 1 and 1.5) ceramics (BSTC) with a relative density of 93% and a grain size distribution of 0.2–3 µm were prepared by the mixed-oxides reaction route. The crystalline structures, microstructures, valence states, and electrical properties of two ceramics were analyzed using X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS)

The application of powder X-ray diffraction (PXRD) for the detection and quantification of low levels of a solid-state chemical impurity, BrettPhos oxide, in an active pharmaceutical ingredient is discussed. It is demonstrated that with appropriate methodology and experimentation, the impurity levels of as low as 0.07% w/w could be detected reliably and limit of quantification of 0.10% w/w could be

Single crystals of Sm0.55Sr0.45Mn0.4Fe0.6O3 were grown by an optical floating zone technique in an oxygen atmosphere. The powder X-ray diffraction pattern for the grown crystal revealed single-crystalline nature. The lattice parameters and atomic structure were refined and indexed using a General Structure Analysis System (GSAS) to an orthorhombic structure with lattice parameters a = 5.4415 (32) Å

The National Institute of Standards and Technology (NIST) certifies a suite of Standard Reference Materials (SRMs) to be used to evaluate specific aspects of the instrument performance of both X-ray and neutron powder diffractometers. This report describes SRM 640f, the seventh generation of this powder diffraction SRM, which is designed to be used primarily for calibrating powder diffractometers with

A commercial Empyrean X-ray diffractometer was adapted for combined grazing incidence X-ray fluorescence analysis (GIXRF) measurements with X-ray reflectivity (XRR) measurements. An energy-dispersive silicon drift detector was mounted and integrated in the angle-dependent data acquisition of the Empyrean. Different monochromator/X-ray optics units have been compared with the values obtained by the

A total pattern analysis suite of programs has been developed and incorporated into the ICDD® PDF-4 database. While the suite of programs is intended for the analysis of any diffraction pattern, particular attention was focused on the analysis of common amorphous, non-crystalline, or partially crystalline materials found in minerals, polymers, and pharmaceuticals. The suite of programs directly interfaces

Residual strain in electrodeposited Li films may affect safety and performance in Li metal battery anodes, so it is important to understand how to detect residual strain in electrodeposited Li and the conditions under which it arises. To explore this Li films, electrodeposited onto Cu metal substrates, were prepared under an applied pressure of either 10 or 1000 kPa and subsequently tested for the

One challenge impeding the analysis of terabyte scale X-ray scattering data from the Linac Coherent Light Source (LCLS) is determining the number of clusters required for the execution of traditional clustering algorithms. Here, we demonstrate that the previous work using bi-cross validation to determine the number of singular vectors directly maps to the spectral clustering problem of estimating both

Tooth enamel, the outermost layer of human teeth, is a complex, hierarchically structured biocomposite. The details of this structure are important in multiple human health contexts, from understanding the progression of dental caries (tooth decay) to understanding the process of amelogenesis and related developmental defects. Enamel is composed primarily of long, nanoscale crystallites of hydroxyapatite

X-ray powder diffraction data for new metal-organic compounds: tetrakis(3-ethylanilinium) octamolybdate Mo8O26(C8H12N)4 [a = 10.682(4), b = 16.589(5), c = 7.307(2) Å, α = 92.79(2)°, β = 97.99(3)°, γ = 103.89(3)°, V = 1240.27 Å3, Z = 1, space group P−1]; tetrakis(3-ethylanilinium) octamolybdate tetrahydrate Mo8O26(C8H12N)4·(H2O)4 [a = 18.801(7), b = 17.943(6), c = 7.334(3) Å, β = 98.50(5)°, V = 2446

X-ray reference powder patterns and structures have been determined for a series of cobalt- and tungsten-containing cubic alkaline-earth perovskites, (BaxSr1–x)2CoWO6 (x = 0.1, 0.2, 0.3, 0.5, 0.7, and 0.9). The structure of the end members of the series, Sr2CoWO6 and Ba2CoWO6, were tetragonal and cubic, respectively, agreeing with the literature data. From Rietveld refinements, it was found that when

This paper describes a new flow-through capillary sample holder that allows the in situ study of re-solvation processes. The holder can be aligned to the goniometer's center using two perpendicular micrometric tables that move in y and z directions. The re-solvation of two ibrutinib solvates of anisole and fluorobenzene was tested using the holder to show the practical application of this technique

The crystal structure of oseltamivir phosphate has been refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Oseltamivir phosphate crystallizes in space group P21212 (#18) with a = 24.0079(3), b = 24.6716(2), c = 7.45254(5) Å, V = 4414.24(5) Å3 at 295 K, and Z = 8. Prominent in the crystal structure are hydrogen bonds between the phosphate groups

Silicon nanowires (SiNWs) were fabricated in a metal-assisted chemical etching method with two steps including dipping silicon wafers in AgNO3/HF solutions and then in H2O2/HF solutions. Grazing incidence X-ray diffraction measurements with a set of incidence angles were carried out on the resulting samples to detect characteristics of silver nanoparticles in the etched silicon. Compared with the uniform

An alternative neutron diffractometer performance, which documents the feasibility of using a high-resolution three-axis neutron diffractometer for elastic and plastic deformation studies of bulk metallic polycrystalline samples, is presented. Contrary to the conventional double-axis setting, the suggested alternative consists of an unconventional three-axis set-up employing a bent perfect crystal

The giant gypsum crystals of Naica cave have fascinated scientists since their discovery in 2000. Human activity has changed the microclimate inside the cave, making scientists wonder about the potential environmental impact on the crystals. Over the last 9 years, we have studied approximately 70 samples. This paper reports on the detailed chemical–structural characterization of the impurities present

The I13 transmission X-ray microscope at Diamond Light Source (DLS) has been designed to cover a broad range of energies and field of views. The beamline operates on an undulator source, and a multilayer monochromator can be used to work at a larger bandwidth to enable faster acquisitions. The experimental design includes large working distances for the optics to allow installing in situ sample environments

Although the concept, first demonstration, and potential applications of X-ray transmission mirrors (XTMs) were initially described over 30 years ago, only a few implementations exist in the literature. This is attributed to the unsolved challenge of a thick frame supporting a thin, reflecting membrane which does not itself block the transmitted beam. Here, we introduce a novel approach to solve this

The speciation of vanadium in the electrolyte of vanadium redox flow batteries (VRFBs) is important to determine the state of charge of the battery. To obtain a better understanding of the transport of the different vanadium species through the separator polymer electrolyte membranes, it is necessary to be able to determine concentration and species of the vanadium ions inside the nanoscopic water

Single crystals of Sm0.55Sr0.45Mn0.4Fe0.6O3 were grown by an optical floating zone technique in an oxygen atmosphere. The powder X-ray diffraction pattern for the grown crystal revealed single-crystalline nature. The lattice parameters and atomic structure were refined and indexed using a General Structure Analysis System (GSAS) to an orthorhombic structure with lattice parameters a = 5.4415 (32) Å

Commercial fluorometholone, CAS #426-13-1, crystallizes in the monoclinic space group P21 (#4) with a = 6.40648(2), b = 13.43260(5), c = 11.00060(8) Å, β = 92.8203(5)°, V = 945.517(5) Å3, and Z = 2. A reduced cell search in the Cambridge Structural Database yielded one previous structure determination, using single-crystal data at 292 K. In this work, the sample was ordered from the United States Pharmacopeial

As a producer of certified reference materials (CRMs), NIST faces high demand for Standard Reference Materials (SRMs). The demand is exacerbated by widespread misuse of CRMs. When should one use CRMs? When should one not use CRMs? Must labs always use NIST SRMs? How can labs demonstrate analytical capabilities for their accreditation scopes? Why so many questions? Standards developers, laboratory accreditors

Particulate matter (PM) specimens from a traffic site were sampled on Teflon filters using a low volume sampler. The sampling campaign ran over a one-year period with sampling frequency of twice a week for both PM2.5 and PM10. X-ray diffraction (XRD) methods, which are not commonly used in PM analysis, have been utilized successfully to identify crystalline phases present, including secondary pollutants

The crystal and molecular structure of fenspiride, a bronchodilator and anti-inflammatory drug, are reported. Fenspiride crystallizes in the monoclinic system, with two crystallographically independent molecules in the general position of the space group P21/n (No. 14) and Z = 8. Rietveld refined unit cell parameters are a = 11.52013(8) Å, b = 5.614091(31) Å, c = 44.1567(4) Å, α = 90°, β = 93.0885(6)°

The crystal structure of atazanavir has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Atazanavir crystallizes in space group P21 (#4) with a = 15.33545(7), b = 5.90396(3), c = 21.56949(13) Å, β = 96.2923(4)°, V = 1941.134(11) Å3, and Z = 2. Despite being labeled as “atazanavir sulfate”, the commercial reagent sample consisted

The crystal structure of atorvastatin calcium trihydrate (ACT) has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. ACT crystallizes in space group P1 (#1) with a = 5.44731(4), b = 9.88858(16), c = 29.5925(10) Å, α = 95.859(3), β = 94.211(1), γ = 105.2790(1)°, V = 1521.277(10) Å3, and Z = 1. The most prominent feature

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This mini review summarizes recent advances in experimental thermodynamics of metal–organic frameworks (MOFs). Taking advantage of the development in mechanochemistry, near-room temperature solution calorimetry, and low-temperature heat capacity measurements, the energetic landscape, entropy trends, and Gibbs free energy evolutions of MOFs with true polymorphism [Zn(MeIm)2, Zn(EtIm)2, and Zn(CF3Im)2]

Porphyrinic compounds are of increasing interest to the materials science community, yet little attention has been paid to crystallographically controlled voids and channels in these materials. We have conducted an initial survey of the voids and channels in a random subset of 1000 porphyrinic compounds with known crystal structures. From calculations using a rolling-probe subroutine, we have found

Additional crystallographic data are given for the recently reported mineral middlebackite, which has been described for discoveries at Iron Knob in South Australia and Passo di San Lugano near Trento, Italy. The material examined in the present study was from a third finding of the mineral, viz. from a quartz outcrop at Mooloo Downs Station in Western Australia within which it was co-located with

3-[1-[4-(2-Methylpropyl)phenyl]ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C21H21FN4S) has been synthesized as a member of a series of triazolothiadiazoles having NSAIDs moieties with cytotoxic activity. The crystal structure of this new compound has been solved and refined using conventional laboratory X-ray powder diffraction data and optimized using density functional techniques

Structure and optical properties have been successfully determined for a series of niobium- and tantalum-containing layered alkaline-earth silicate compounds, Ba3(Nb6−xTax)Si4O26 (x = 0.6, 1.8, 3.0, 4.2, 5.4). The structure of this solid solution was found to be hexagonal P-62m (No. 189), with Z = 1. With x increases from 0.6 to 5.4, the lattice parameter a increases from 8.98804(8) to 9.00565(9) Å

Crystal structure and electronic structure of YMnO3 were investigated by X-ray diffraction and transmission electron microscopy related techniques. According to the density of states (DOS), the individual interband transitions to energy loss peaks in the low energy loss spectrum were assigned. The hybridization of O 2p with Mn 3d and Y 4d analyzed by the partial DOS was critical to the ferroelectric

We report the dielectric properties of ACu3Ti4O12 (A = Eu2/3, Tb2/3, and Na1/2Eu1/2) (ACTO) in the frequency range of 40 Hz–2.5 MHz and in the temperature range of 293–473 K. The experimental results show that substituting for Ca improves the loss tangent of CaCu3Ti4O12 (CCTO). Although the dielectric constants largely decrease, they remain at a high level of 103. To identify the observed dielectric

The ICDD's Powder Diffraction File™ (PDF®) is a database of inorganic and organic diffraction data used for phase identification and materials characterization by powder diffraction. The PDF has been available for over 75 years and finds application in X-ray, synchrotron, electron, and neutron diffraction analyses. With entries based on powder and single crystal data, the PDF is the only crystallographic

The crystal structure of metolazone has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Metolazone crystallizes in space group P-1 (#2) with a = 8.1976(5), b = 14.4615(69), c = 16.0993(86) Å, α = 115.009(18), β = 90.096(7), γ = 106.264(4)°, V = 1644.52(9) Å3, and Z = 4. The broad (02-1) peak at 3.42° 2θ indicates stacking faults

The crystal structure of prednicarbate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Prednicarbate crystallizes in space group P212121 (#19) with a = 7.69990(3), b = 10.75725(3), c = 31.36008(11) Å, V = 2597.55(1) Å3, and Z = 4. In the crystal structure the long axis of the steroid ring system lies roughly parallel to

The crystal structure of cloxacillin sodium monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Cloxacillin sodium monohydrate crystallizes in space group P212121 (#19) with a = 7.989 36(12), b = 10.918 09(10), c = 25.559 3(6) Å, V = 2229.50(5) Å3, and Z = 4. The crystal structure is characterized by corner-sharing

The crystal structure of cefprozil monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Cefprozil monohydrate crystallizes in space group P21 (#4) with a = 11.26513(6), b = 11.34004(5), c = 14.72649(11) Å, β = 90.1250(4)°, V = 1881.262(15) Å3, and Z = 4. Although a reasonable fit was obtained using an orthorhombic

The crystal structure of atropine sulfate monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Atropine sulfate monohydrate crystallizes in space group P21/n (#14) with a = 19.2948(5), b = 6.9749(2), c = 26.9036(5) Å, β = 94.215(2)°, V = 3610.86(9) Å3, and Z = 4. Each of the two independent protonated nitrogen atoms

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