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X-ray powder diffraction data for nicotine 3,5-dihydroxybenzoate dihydrate, C10H15N2⋅C7H5O4⋅2H2O Power Diffr. (IF 0.919) Pub Date : 2021-01-25 Ji Yang; Zhi Hua Liu; Rui Zhi Zhu; Neng Jun Xiang; Shi Yun Tang; Pei He; Zi Li Suo; Hui Li
Nicotine 3,5-dihydroxybenzoate dihydrate is a nicotine salt and can be used as compositions in tobacco products. X-ray powder diffraction data, unit-cell parameters, and space group for nicotine 3,5-dihydroxybenzoate, C10H15N2⋅C7H5O4⋅2H2O, are reported [a = 8.424(1) Å, b = 13.179(8) Å, c = 8.591(1) Å, α = 90°, β = 102.073(8)°, γ = 90°, unit-cell volume V = 932.765(3) Å3, Z = 2, ρcal = 1.256 g⋅cm−3
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Crystal structure of loteprednol etabonate Form II, C24H31ClO7 Power Diffr. (IF 0.919) Pub Date : 2021-01-19 James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
The crystal structure of loteprednol etabonate Form II has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Loteprednol etabonate Form II crystallizes in the space group P21 (#4) with a = 11.96312(6), b = 14.91862(5), c = 6.75715(3) Å, β = 94.1584(3)°, V = 1202.796(6) Å3, and Z = 2. The crystal structure is characterized by
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Powder X-ray diffraction of escitalopram oxalate oxalic acid hydrate, (C20H21FN2O)2(C2O4)(H2C2O4)(H2O)0.16 Power Diffr. (IF 0.919) Pub Date : 2021-01-19 James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
Commercial escitalopram oxalate crystallizes as a hydrated adduct with oxalic acid, in the space group P21 with a = 8.029897(21), b = 25.09397(6), c = 11.138930(31) Å, β = 106.7759(2)°, V = 2148.992(7) Å3, and Z = 4. The agreement of the Rietveld and previous single-crystal structures is excellent; the root-mean-square Cartesian displacements of the non-H atoms of the two independent cations are 0
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X-ray powder diffraction data of LaNi0.5Ti0.45Co0.05O3, LaNi0.45Co0.05Ti0.5O3, and LaNi0.5Ti0.5O3 perovskites Power Diffr. (IF 0.919) Pub Date : 2021-01-18 Mariana M. V. M. Souza; Alex Maza; Pablo V. Tuza
In the present work, LaNi0.5Ti0.45Co0.05O3, LaNi0.45Co0.05Ti0.5O3, and LaNi0.5Ti0.5O3 perovskites were synthesized by the modified Pechini method. These materials were characterized using X-ray fluorescence, scanning electron microscopy, and powder X-ray diffraction coupled to the Rietveld method. The crystal structure of these materials is orthorhombic, with space group Pbnm (No 62). The unit-cell
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Crystal structure from laboratory X-ray powder diffraction data, DFT-D calculations, Hirshfeld surface analysis, and energy frameworks of a new polymorph of 1-benzothiophene-2-carboxylic acid Power Diffr. (IF 0.919) Pub Date : 2021-01-14 Analio J. Dugarte-Dugarte; Jacco van de Streek; Graciela Díaz de Delgado; Alicja Rafalska-Lasocha; José Miguel Delgado
Several benzothiophene-based compounds, including 1-benzothiophene-2-carboxylic acid, exhibit a wide variety of pharmacological activities. They have been extensively used to treat various types of diseases with high therapeutic effectiveness. In this contribution, the crystal structure of a new polymorph of 1-benzothiophene-2-carboxylic acid (BTCA) was determined from laboratory X-ray powder diffraction
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Powder diffraction data and preliminary spectroscopic and thermal characterization of pinaverium bromide, a drug used for functional gastrointestinal disorders Power Diffr. (IF 0.919) Pub Date : 2021-01-14 José H. Quintana Mendoza; Andrea P. Aparicio; J. A. Henao
Pinaverium bromide (C26H41Br2NO4) is an active pharmaceutical ingredient (API) usually prescribed for the relief of spasm and functional gastrointestinal disorders. This work reports its powder diffraction data, Raman and FT-IR spectroscopy and thermal characterization. Indexing of the powder diffraction pattern showed this material crystallizes in a monoclinic unit cell with a = 16.00(4) Å, b = 8
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X-ray powder diffraction data for norethisterone enanthate, C27H38O3 Power Diffr. (IF 0.919) Pub Date : 2021-01-12 Jingwen Fan; Zhicheng Zha; Qing Wang; Shoujun Zheng
X-ray powder diffraction data, unit-cell parameters, and space group for norethisterone enanthate, C27H38O3, are reported [a = 6.191(4) Å, b = 12.711(3) Å, c = 31.396(2) Å, α = 90°, β = 90°, γ = 90°, unit-cell volume V = 2471.16 Å3, Z = 4, ρcal = 1.104 g cm−3, and space group P212121]. All measured lines were indexed and are consistent with the P212121 space group. No detectable impurities were observed
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In situ XRPD study of the ambient-pressure synthesis of nonstoichiometric Ag3O from Ag–Ag2O thin films: Phase abundance, unit-cell parameters, and c/a as a function of temperature and time Power Diffr. (IF 0.919) Pub Date : 2020-10-28 Paul J. Schields; Nicholas Dunwoody; David Field; Zachary Wilson
Ag3O was synthesized by jet-milling magnetron-sputtered Ag–Ag2O thin films. Heating the jet-milled powders in air and N2 from 40 to 148 °C at ambient pressure produced Ag3O-rich powders. The phase composition and unit-cell parameters of the jet-milled powders were measured as a function of temperature with in situ X-ray powder diffraction experiments from −186 to 293 °C. Ag3O was also produced by ball
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Validation of XRD phase quantification using semi-synthetic data Power Diffr. (IF 0.919) Pub Date : 2020-10-13 Nicola Döbelin
Validating phase quantification procedures of powder X-ray diffraction (XRD) data for an implementation in an ISO/IEC 17025 accredited environment has been challenging due to a general lack of suitable certified reference materials. The preparation of highly pure and crystalline reference materials and mixtures thereof may exceed the costs for a profitable and justifiable implementation. This study
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Synthesis and optical properties of single-crystalline SnS1−xSex nanobelts Power Diffr. (IF 0.919) Pub Date : 2020-11-04 Shengru Wang; Xiaofang Lai; Bingsheng Du; Junhao Ma; Peihua Wang; Jikang Jian
In this work, SnS1−xSex ternary nanobelts were synthesized by a facile hydrothermal method without the assistance of surfactants. The structure, morphology, microstructure, compositions, chemical valences, phonon modes, and optical band gaps of the SnS1−xSex nanobelts were characterized in detail. The results indicate that the SnS1−xSex nanobelts have uniform one-dimensional morphology and are single
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Crystal structure of hyoscyamine sulfate monohydrate, (C17H24NO3)2(SO4)(H2O) Power Diffr. (IF 0.919) Pub Date : 2020-11-03 James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
The crystal structure of hyoscyamine sulfate monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Hyoscyamine sulfate monohydrate crystallizes in space group P21 (#4) with a = 6.60196(2), b = 12.95496(3), c = 20.93090(8) Å, β = 94.8839(2)°, V = 1783.680(5) Å3, and Z = 2. Despite the traditional description as a dihydrate
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Crystal structure of cephalexin monohydrate, C16H17N3O4S(H2O) Power Diffr. (IF 0.919) Pub Date : 2020-11-03 James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
The crystal structure of cephalexin monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Cephalexin monohydrate crystallizes in space group C2 (#5) with a = 27.32290(17), b = 11.92850(4), c = 16.75355(8) Å, β = 108.8661(4)°, V = 5166.99(3) Å3, and Z = 12. Although the general arrangement of molecules is similar to
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Powder X-ray diffraction of azelastine hydrochloride, C22H25ClN3O·Cl Power Diffr. (IF 0.919) Pub Date : 2020-11-18 James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
Commercial azelastine hydrochloride crystallizes in the monoclinic space group P21/n (#14) with a = 13.7844(5), b = 16.39920(14), c = 9.41231(22) Å, β = 97.5340(20)°, V = 2109.32(4) Å3, and Z = 4. The lattice parameters differ by −0.02, +0.04, and +0.04% from those in the previous determination (reflecting differences in the temperature and the sample source), and are more precise, from the use of
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Application of deconvolutional treatment to powder diffraction data collected with a Bragg-Brentano diffractometer with a contaminated Cu target and a Ni filter Power Diffr. (IF 0.919) Pub Date : 2020-07-15 Takashi Ida
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
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Crystal structure and X-ray absorption spectroscopy of trimethylarsine oxide dihydrate, (CH3)3AsO⋅2H2O Power Diffr. (IF 0.919) Pub Date : 2020-07-13 Joel W. Reid; James A. Kaduk; Peter E. R. Blanchard
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
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Crystal structure of ceftriaxone sodium hemiheptahydrate, C18H16N8O7S3Na2(H2O)3.5 Power Diffr. (IF 0.919) Pub Date : 2020-08-25 Diana Gonzalez; Joseph T. Golab; Jan Y. Eilert; Rong Wang; James A. Kaduk
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
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X-ray powder diffraction data for eluxadoline nitrate monohydrate, C32H35N5O5⋅2HNO3⋅H2O Power Diffr. (IF 0.919) Pub Date : 2020-09-17 Xin Wei; Zi Li Suo; Man Zhang; Pei Xiao Tang; Hui Li
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
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An investigation into the temperature phase transitions of synthesized lithium titanate materials doped with Al, Co, Ni and Mg by in situ powder X-ray diffraction Power Diffr. (IF 0.919) Pub Date : 2020-08-25 X. van Niekerk; E. E. Ferg; C. Gelant; D. G. Billing
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
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X-ray powder diffraction data for estra-4,9-diene-3,17-dione, C18H22O2 Power Diffr. (IF 0.919) Pub Date : 2020-08-25 Zhicheng Zha; Ting Tang; Xiaoyan Bian; Qing Wang
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)
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X-ray computed microtomography for the structural analysis of jewelry from the Museum “Royal Tombs of Sipán” Power Diffr. (IF 0.919) Pub Date : 2020-08-24 Soraia Rodrigues de Azeredo; Roberto Cesareo; Angel Guillermo Bustamante Dominguez; Ricardo Tadeu Lopes
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
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CRL optics and silicon drift detector for P06 Microprobe experiments at 35 keV Power Diffr. (IF 0.919) Pub Date : 2020-08-05 Gerald Falkenberg; Frank Seiboth; Frieder Koch; Ken Vidar Falch; Andreas Schropp; Dennis Brückner; Jan Garrevoet
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
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Characterization and Rietveld refinements of new dense ceramics Ba3−xSrxTb3−xCexO9 (x = 1 and 1.5) perovskites – ADDENDUM Power Diffr. (IF 0.919) Pub Date : 2020-07-27 Yali Su; Dayong Lu; Shan Wang
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)
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Rietveld refinement of Sm0.55Sr0.45Mn0.4Fe0.6O3 – ADDENDUM Power Diffr. (IF 0.919) Pub Date : 2020-07-27 G. Murugesan; R. Nithya; S. Kalainathan
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
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Quantification of solid-state impurity with powder X-ray diffraction using laboratory source Power Diffr. (IF 0.919) Pub Date : 2020-07-27 Meenakshi Sundaram; Saravanan Natarajan; Amol G. Dikundwar; Hemant Bhutani
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
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Certification of SRM 640f line position and line shape standard for powder diffraction Power Diffr. (IF 0.919) Pub Date : 2020-07-02 David R. Black; Marcus H. Mendenhall; Albert Henins; James Filliben; James P. Cline
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
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Refitting an X-ray diffraction system for combined GIXRF and XRR measurements Power Diffr. (IF 0.919) Pub Date : 2020-07-01 Dieter Ingerle; Werner Artner; Klaudia Hradil; Christina Streli
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
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Total pattern analyses for non-crystalline materials Power Diffr. (IF 0.919) Pub Date : 2020-05-27 T. G. Fawcett; S. Gates-Rector; A. M. Gindhart; M. Rost; S. N. Kabekkodu; J. R. Blanton; T. N. Blanton
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
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Use of a Be-dome holder for texture and strain characterization of Li metal thin films via sin2(ψ) methodology Power Diffr. (IF 0.919) Pub Date : 2020-06-04 Mark A. Rodriguez; Katharine L. Harrison; Subrahmanyam Goriparti; James J. M. Griego; Brad L. Boyce; Brian R. Perdue
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
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Bi-cross validation of spectral clustering hyperparameters Power Diffr. (IF 0.919) Pub Date : 2020-04-24 Sioan Zohar; Chun Hong Yoon
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
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A method for mapping submicron-scale crystallographic order/disorder applied to human tooth enamel Power Diffr. (IF 0.919) Pub Date : 2020-05-08 R. Free; K. DeRocher; R. Xu; D. Joester; S. R. Stock
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
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X-ray powder diffraction data for three new 3-ethylanilinium molybdates Power Diffr. (IF 0.919) Pub Date : 2020-04-29 Alicja Rafalska-Łasocha; Michał Duda; Wiesław Łasocha
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
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Crystal chemistry, X-ray diffraction reference patterns, and bandgap studies for (BaxSr1–x)2CoWO6 (x = 0.1, 0.2, 0.3, 0.5, 0.7, and 0.9) Power Diffr. (IF 0.919) Pub Date : 2020-06-23 W. Wong-Ng; G. Y. Liu; D. D. Shi; Y. Q. Yang; R. Derbeshi; D. Windover; J. A. Kaduk
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
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Testing the flow-through capillary for the study of re-solvation processes in pharmaceutical compounds Power Diffr. (IF 0.919) Pub Date : 2020-06-23 Jan Rohlíček; Vít Zvoníček; Eliška Skořepová; Miroslav Šoóš
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
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Powder X-ray diffraction of oseltamivir phosphate (Tamiflu®), C16H31N2O8P Power Diffr. (IF 0.919) Pub Date : 2020-06-03 Ryan L. Hodge; James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
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
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Grazing incidence X-ray diffraction measurement of silver nanoparticles in metal-assisted etching of silicon Power Diffr. (IF 0.919) Pub Date : 2020-06-01 Yunhui Tang; Bo Wang; Rui Xue; Hui Yan
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
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An alternative neutron diffractometer performance for strain/stress measurements Power Diffr. (IF 0.919) Pub Date : 2020-05-28 Pavol Mikula; Jan Saroun; Vasyl Ryukhtin; James Stammers
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
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Are the Naica giant crystals deteriorating because of human action? Power Diffr. (IF 0.919) Pub Date : 2020-05-11 M. E. Montero-Cabrera; I. J. A. Carreño-Márquez; I. Castillo-Sandoval; B. Pérez-Cázares; L. E. Fuentes-Cobas; H. E. Esparza-Ponce; E. Menéndez-Méndez; M. E. Fuentes-Montero; H. Castillo-Michel; D. Eichert; R. Loredo-Portales; J. Canche-Tello; M. Y. Luna-Porres; G. González-Sánchez; D. Burciaga-Valencia; C. Caraveo-Castro; G. Gómez-Méndez; L. Muñoz-Castellanos; I. Reyes-Cortes
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
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The Diamond I13 full-field transmission X-ray microscope: a Zernike phase-contrast setup for material sciences Power Diffr. (IF 0.919) Pub Date : 2020-04-29 Malte Storm; Florian Döring; Shashidhara Marathe; Christian David; Christoph Rau
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
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Efficient high-pass filtering with practical, high-yield X-ray transmission mirror optics Power Diffr. (IF 0.919) Pub Date : 2020-04-29 David N. Agyeman-Budu; Joel D. Brock; Arthur R. Woll
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
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Laboratory XANES to study vanadium species in vanadium redox flow batteries Power Diffr. (IF 0.919) Pub Date : 2020-04-29 Christian Lutz; Ursula Elisabeth Adriane Fittschen
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
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Rietveld refinement of Sm0.55Sr0.45Mn0.4Fe0.6O3 Power Diffr. (IF 0.919) Pub Date : 2020-03-27 G. Murugesan; R. Nithya; S. Kalainathan
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
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Powder X-ray diffraction of fluorometholone, C22H29FO4 Power Diffr. (IF 0.919) Pub Date : 2020-03-27 Diana Gonzalez; Joseph T. Golab; James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
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
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How to use and how not to use certified reference materials in industrial chemical metrology laboratories Power Diffr. (IF 0.919) Pub Date : 2020-04-15 John R. Sieber
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
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X-ray diffraction as a major tool for the analysis of PM2.5 and PM10 aerosols Power Diffr. (IF 0.919) Pub Date : 2020-04-15 Nasser M. Hamdan; Hussain Alawadhi
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
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Crystal and molecular structure of fenspiride, C15H20N2O2 Power Diffr. (IF 0.919) Pub Date : 2020-04-14 Silvina Pagola
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)°
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Crystal structure of atazanavir, C38H52N6O7 Power Diffr. (IF 0.919) Pub Date : 2020-04-06 James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
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
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Crystal structure of atorvastatin calcium trihydrate Form I (Lipitor®), (C33H34FN2O5)2Ca(H2O)3 Power Diffr. (IF 0.919) Pub Date : 2020-04-06 Ryan L. Hodge; James A. Kaduk; Amy M. Gindhart; Thomas N. Blanton
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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New PDJ news and reminders Power Diffr. (IF 0.919) Pub Date : 2020-03-27 Camden Hubbard; Nicole Ernst Boris
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Special section – Crystallography and properties of metal–organic framework (MOF) compounds Power Diffr. (IF 0.919) Pub Date : 2020-03-27 Craig M. Brown; Winnie Wong-Ng
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Calendar of Short Courses and Workshops Power Diffr. (IF 0.919) Pub Date : 2020-03-27 Gang Wang
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68th Annual Denver X-ray Conference Report Power Diffr. (IF 0.919) Pub Date : 2020-03-27 Denise Zulli
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Denver X-ray conference comments and reflections on current issue of Powder Diffraction Journal (PDJ) — CORRIGENDUM Power Diffr. (IF 0.919) Pub Date : 2019-04-23 Camden Hubbard
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Special section: Crystallography and properties of metal–organic framework compounds Power Diffr. (IF 0.919) Pub Date : 2019-11-29 Winnie Wong-Ng
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Powder Diffraction Journal is now Open Access – Hybrid Power Diffr. (IF 0.919) Pub Date : 2019-11-29 Nicole Ernst Boris
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Recent advances in experimental thermodynamics of metal–organic frameworks Power Diffr. (IF 0.919) Pub Date : 2019-09-20 Hui Sun; Di Wu
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]
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Topology of voids and channels in selected porphyrinic compounds Power Diffr. (IF 0.919) Pub Date : 2019-09-30 Lawrence P. Cook; Greg A. Brewer; Daniel Siderius; Winnie Wong-Ng
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
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X-ray diffraction study of middlebackite [CuII2C2O4(OH)2, di-copper oxalate dihydroxide], using a mineral specimen from Mooloo Downs Station, Western Australia and chemically synthesized material Power Diffr. (IF 0.919) Pub Date : 2019-09-12 B. H. O'Connor; R. M. Clarke; J. A. Kimpton; D. G. Allen
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
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