The subsolidus phase relations in the ternary system La2O3–Bi2O3–CuO at 900 °C were investigated by X-ray powder diffraction. A new binary compound, Bi2La4O9, was found, as well as a binary and a ternary solid solution series, Bi1−xLaxO1.5 (0.16≤x≤0.33) and La2−xBixCuO4 (0≤x≤0.11), respectively.

The X-ray powder diffraction data for δ-Na2Si2O5 are reported. The sample was prepared from water glass solution applied to pressed powder tablets of finely ground quartz using a heating program with a maximal temperature of 700 °C. The crystallographic data for δ-disilicate obtained from a Rietveld analysis are: space group P21/n, a=8.3818(4) Å, b=12.0726(5) Å, c=4.8455(2) Å, β=90.303(5)°, V=490.31 Å3, Z=4, and Dcalc.=2.468 g/cm3.

A series of double-perovskite oxides, Sr2RNbO6 (R = Sm, Gd, Dy, Ho, Y, Tm, and Lu) were prepared and their crystal structure and powder diffraction reference patterns were determined using the Rietveld analysis technique. The crystal structure of each of the Sr2RNbO6 phase is reported in this paper. The R = Gd, Ho, and Lu samples were studied using synchrotron radiation, while R = Sm, Dy, Y, and Tm samples were studied using laboratory X-ray diffraction. Members of Sr2RNbO6 are monoclinic with a space group of P21/n and are isostructural with each other. Following the trend of “lanthanide contraction”, from R = Sm to Lu, the lattice parameters “a” of these compounds decreases from 5.84672(10) to 5.78100(3) Å, b from 5.93192(13) to 5.80977(3) Å, c from 8.3142(2) to 8.18957(5) Å, and V decreases from 288.355(11) to 275.057(2) Å3. In this double-perovskite series, the R3+ and Nb5+ ions are structurally ordered. The average Nb–O bond length is nearly constant, while the average R–O bond length decreases with the decreasing ionic radius of R3+. Powder diffraction patterns for these compounds have been submitted to the Powder Diffraction File (PDF).

The crystal structure of the partially ordered vacancy compound Cu2In14/3□4/3Se8, belonging to the system I3-III7-□2-VI12, was analyzed using X-ray powder diffraction data. Several structural models were derived from the structure of the selenium-rich phase β-Cu0.39In1.2Se2 by permuting the cations in the available Wyckoff positions. The refinement of the best model by the Rietveld method in the tetragonal space group P$\overline 4 $ 2c (No 112), with unit-cell parameters a = 5.7487(3) Å, c = 11.5106(6) Å, V = 380.40(3) Å3, led to Rp = 9.0%, Rwp = 9.9%, Rexp = 7.2%, S = 1.4 for 134 independent reflections. This model has the following Wyckoff site atomic distribution: Cu in 2e (0,0,0); In in 2b (½,0,¼), 2d (0,½,¼), and 2f (½,½,0);□ in 2f (½,½,0); Se in 8n (x,y,z).

Polycrystalline Sm0.55Sr0.45MnO3 was prepared by solid-state reaction at 1300 °C. Single phase of the compound was analysed by a powder X-ray diffraction technique. The powder pattern of Sm1−xSrxMnO3 was indexed and refined using a General Structure Analysis System (GSAS) to an orthorhombic structure with space group Pnma, a = 5.4323(7), b = 7.6585(4), and c = 5.4343(7) Å.

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 body of the membranes. The speciation of V in the electrolyte of VRFBs has been performed by others at the synchrotron by X-ray absorption near-edge structure analysis (XANES). However, the concentrations are quite high and not necessarily justify the use of a large-scale facility. Here, we show that vanadium species in the electrolyte and inside the ionomeric membranes can be determined by laboratory XANES. We were able to determine V species in the 1.6 M electrolyte with a measurement time of 2.3 h and V species having a concentration of 9.8 g kg−1 inside the membranes (178 µm thick) with a measurement time of 5 h. Our results show that laboratory XANES is an appropriate tool to study these kind of samples.

In the conventional X-ray reflectivity (XRR) analysis, the reflectivity is calculated based on the Parratt formalism, incorporating the effect of the interface roughness according to Nevot and Croce. However, the results of calculations of the XRR have shown strange outcomes, where interference effects increase at a rough surface because of a lack of consideration of diffuse scattering within the Parratt formalism. Therefore, we have developed a new improved formalism in which the effects of the surface and interface roughness are included correctly. In this study, for deriving a more accurate formalism of XRR, we tried to compare the measurements of surface roughness of the same sample by atomic force microscopy (AFM) and XRR. It is found that the AFM result could not be completely reproduced even with the improved XRR formalism. By careful study of the AFM results, we determined the need for an additional effective roughness term within the XRR simulation that depends on the angle of incidence of the beam.

Stability of Na-titanate-based nanotubes at high temperature and pressure is investigated using X-ray diffraction and energy-dispersive X-ray diffraction (EDXRD). Our results show that the nanotubes can be stable at ~400 °C. Higher temperature annealing of nanotubes result in opening and flattening of the nanotubes, and subsequent structural transformation to Na2Ti6O13-based structure via an intermediate phase with Na0.23TiO2-like structure. In situ EDXRD using diamond anvil cell indicates that the nanotubes collapse at about 15 GPa, and are finally transformed into an amorphous phase at about 30 GPa. The nanotubes kept in an amorphous state were further compressed to 50 GPa according to our in situ EDXRD observation. Titanate nanotubes are mechanically stronger than carbon nanotubes under static compression.

Mirabegron, (C21H24N4O2S), is a β3-adrenoceptor agonist approved in Japan, the USA, Canada and Europe, for the treatment of overactive bladder symptoms. There are no entries for this important active pharmaceutical ingredient in the Cambridge Structural Database or the Powder Diffraction File-4/Organics database. In this contribution, the powder diffraction pattern of Mirabegron, an unreported phase, are presented with a study by spectroscopy methods (Fourier-transform infrared spectroscopy [FT-IR] and RAMAN) and thermal analysis (thermogravimetric analysis [TGA]-differential scanning calorimetry [DSC]).

The Nd1.7Ba0.3Ni0.9Cr0.1O4+δ polycrystalline sample was synthesized by the sol–gel process and a subsequent annealing at 1523 K in 1 atm of flowing argon. X-ray diffraction (XRD) analysis and electrical transport properties have been investigated as well. The oxygen non-stoichiometry was determined by iodometric titration. The sample shows adoption of the K2NiF4-type structure based on a tolerance factor calculation. Rietveld refinement of the crystal structure from X-ray powder diffraction data confirmed that Nd1.7Ba0.3Ni0.9Cr0.1O4+δ adopts the tetragonal structure (space group I4/mmm, Z = 2). The room temperature unit-cell parameters are determined to be a = 3.82515(2) and c = 12.47528(6) Å. The reliability factors are: RB = 0.043, Rwp = 0.012 and χ2 = 3.00. The Nd1.7Ba0.3Ni0.9Cr0.1O4+δ compound exhibits a semi-conductive behaviour. The electrical transport mechanism has been investigated and it agrees with the adiabatic small polaron hopping model in the temperature range 313 K ≤ T ≤ 708 K.

The evaluation of the performance of a geological barrier, consisting essentially of a clay matrix, in the context of industrial and household waste confinement must go with the study of its hydration behavior respectively under extreme atmospheric conditions and variable mechanical soil constraints. Na-montmorillonite (Swy-2) is used, as starting materials, in order to establish the link between applied externals strain (variable relative humidity rate %RH and axial mechanical constraint) and the hydration material response. All constraints are realized at the laboratory scale. This work is achieved using oedometric testing and quantitative X-ray diffraction (XRD) analysis, based on the modeling approach, which consists in the comparison of experimental 00l reflections with the calculated ones deduced from structural models. This approach allows us to quantify the interlamellar space configuration and all structural changes along the c* axis. Obtained results show a decrease for the void ratio e value along the compaction/reswelling process. The “insitu” XRD analysis realized at 5%RH demonstrates hydration shift, from dehydrated water layer (i.e. 0W) to monohydrated water layer (i.e. 1W), attributed to the applied mechanical constraint. At 90%RH, the sample hydration state remains at tri-hydrated water layer (3W) with a clear interstratified trends.

All known occurrences of nickelphosphide (Ni,Fe)3P—a mineral encountered mainly in meteoritic irons—represent relatively small grains, which prevents acquiring powder data of a reasonable quality. Synthetic analogues of this mineral, corresponding chemically to that found in the meteorite Vicenice, have been synthesized. Powder data collected using a standard laboratory diffractometer in the Bragg–Brentano geometry are presented. The space group of nickelphosphide is identical to that of schreibersite (Fe,Ni,Co)3P and synthetic Ni3P—I4. The unit-cell dimensions refined from the powder data are a=9.0168(1) Å, c=4.4501(1) Å, and V=361.80(1) Å3, with Z=8.

The synthesis, thermal behavior, crystallographic and X-ray powder diffraction data, and infrared spectral data for Ca8ZnSi4O16Cl2 have been determined. This compound is cubic with isolated silicate tetrahedra.

Structures of [Cd(C2H8N2)Cl2]n(1) and [Cd(C2H8N2)Br2]n(2) were solved from powder diffraction data. Compound (1) crystallizes in the space group Pbam (No. 55), a = 9.9021(7) Å, b = 7.8186(6) Å, c = 4.0705(3) Å, V = 315.13(3) Å3, Z = 2. (2) is isostructural: space group Pbam (No. 55), a = 10.405(2) Å, b = 7.8634(8) Å, c = 4.2079(5) Å, V = 344.28(6) Å3, Z = 2. The investigated compounds are examples of two-dimensional hybrid coordination polymers, in which neighboring metal centers are bridged via both organic and inorganic moieties: ethylenediamine molecules and halide anions. Both crystal structures were solved ab initio from powder data using direct methods.

The structure of a series of lanthanide iron cobalt perovskite oxides, R(Fe0.5Co0.5)O3 (R = Pr, Nd, Sm, Eu, and Gd), have been investigated. The space group of these compounds was confirmed to be orthorhombic Pnma (No. 62), Z = 4. From Pr to Gd, the lattice parameter a varies from 5.466 35(13) Å to 5.507 10(13) Å, b from 7.7018(2) to 7.561 75(13) Å, c from 5.443 38(10) to 5.292 00(8) Å, and unit-cell volume V from 229.170(9) Å3 to 220.376(9) Å3, respectively. While the trend of V follows the trend of the lanthanide contraction, the lattice parameter “a” increases as the ionic radius r(R3+) decreases. X-ray diffraction (XRD) and transmission electron microscopy confirm that Fe and Co are disordered over the octahedral sites. The structure distortion of these compounds is evidenced in the tilt angles θ, ϕ, and ω, which represent rotations of an octahedron about the pseudocubic perovskite [110]p, [001]p, and [111]p axes. All three tilt angles increase across the lanthanide series (for R = Pr to R = Gd: θ increases from 12.3° to 15.2°, ϕ from 7.5° to 15.8°, and ω from 14.4° to 21.7°), indicating a greater octahedral distortion as r(R3+) decreases. The bond valence sum for the sixfold (Fe/Co) site and the eightfold R site of R(Fe0.5Co0.5)O3 reveal no significant bond strain. Density Functional Theory calculations for Pr(Fe0.5Co0.5)O3 support the disorder of Fe and Co and suggest that this compound to be a narrow band gap semiconductor. XRD patterns of the R(Fe0.5Co0.5)O3 samples were submitted to the Powder Diffraction File.

The structure of [Pd(NH3)4]Cr2O7 has been determined ab initio from conventional X-Ray powder diffraction data by the Patterson method. The cell is monoclinic (space group P21/c, Z = 4), with a = 7.771(3) Å, b=11.578(1) Å, c=11.852(4) Å, and β= 105.50(4)°. Refinements of 57 parameters by the Rietveld method, using 852 reflections lead to RB = 0.032, RP = 0.075, and Rwp = 0.092. The structure is built up from PdN4 square planes linked to Cr2O7 groups by hydrogen bonds. Hydrogen atoms could not be located.

The crystal structure of the mullite in a commercial material was refined by the Rietveld method using laboratory X-ray powder diffraction data. In this one refinement, most of the common challenges—including variable stoichiometry (partially occupied sites), multiple impurity phases, amorphous material, constraints, restraints, correlation, anisotropic profiles, microabsorption, and contamination during grinding—are encountered and the thought processes during the refinement are described step-by-step. Interpretation of the refinements includes bulk chemical analysis, chemical composition of the mullite, assessment of the geometry, bond valence sums, the displacement coefficients, crystallite size and microstrain, comparison to similar structures to assess chemical reasonableness, and the nature of the amorphous phase.

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 data with DASH, refined by the Rietveld method with TOPAS-Academic, and optimized using DFT-D calculations. The new form of 1-benzothiophene-2-carboxylic acid crystallizes in space group C2/c (No. 15) with a = 14.635(4), b = 5.8543(9), c = 19.347(3) Å, β = 103.95(1)°, V = 1608.8(6) Å3, and Z = 8. The structure is a complex 3D arrangement which can be described in terms of hydrogen-bonded dimers of BTCA molecules, joined by the acid–acid homosynthon, which interact through C–H⋯O hydrogen bonds to produce tapes further connected through head-to-tail π⋯π and edge-to-face C–H⋯π interactions. A comparison with a previously reported triclinic polymorph and with the related 1-benzofuran-2-carboxylic acid (BFCA) is also presented.

A model for the long awaited crystal structure of metastable NaAlF4 is established from the powder diffraction pattern of a partly disproportionated sample. Orthorhombic, Cmcm, a=3.6121(3), b=14.952(1), c=5.2692(4) Å, Z=4, V=284.58(4) Å3. Sodium atoms are in NaF6 trigonal prisms interconnected by edges in compact layers. AlF6 octahedra are both cis- and trans-corner connected forming a layer structure similar to that observed in the NaNbO2F2 (P21/c) and BaZnF4 (Cmc21) structure types. NaAlF4 is ideally simple and symmetrical, isostructural with BiReO4 (Cmcm), representing the aristotype of the NaMIIIF4 and BaMIIF4 series.

New powder X-ray data for cancrinite [ideally Na8Si6Al6O24 (CO3)2·2 H2O] are reported along with in-situ real-time thermal processes recorded using energy dispersive X-ray diffractometry (EDXD). A completely anhydrous phase is obtained after heating the sample up to 600 °C and quickly cooling it to room temperature, as shown by means of both Rietveld analysis and IR spectroscopy. The anhydrous phase does not show any tendency to re-acquire molecular water. During the heating process, at around 450 °C, a peak splitting is observed, possibly due to a reversible phase transition.