The crystal structure of nilotinib has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Nilotinib crystallizes in space group P1 (#1) with a = 4.518 14(3), b = 10.638 01(5), c = 13.703 77(8) Å, α = 68.8607(4), β = 82.1486(5), γ = 84.1978(5)°, V = 607.62(1) Å3, and Z = 1. The most prominent feature of the structure is two strong hydrogen bonds. These form chains with a graph set C1,1(13); the chains run along [111]. Several weak C–H···O hydrogen bonds also contribute to the packing. The powder pattern has been submitted to ICDD for inclusion in future releases of the Powder Diffraction File™.

A new method is introduced for the evaluation of experimental stress–strain dependence in thermally cycled thin films. The method is demonstrated on the analysis of an Al thin film on a Si(100) substrate characterized using in situ high-temperature X-ray diffraction 25–450 °C. Diffraction data are used to evaluate in-plane elastic strain in the film as a function of thermal strain originating from the mismatch of thermal expansion coefficients (TECs) between the film and the substrate. The magnitude of the thermal strain is calculated from experimental TECs of the film and the substrate at every measurement temperature. By relating in-plane stresses to thermal strains, an experimental stress–strain dependence for the Al thin film is obtained. The proposed method allows one to identify elastic behavior and to quantify plastic strain in the film. Finally, advantages of the method are discussed in particular its independence from using TECs reported in the literature.

The engineering of strained semiconductor materials represents an important aspect of the enhancement in CMOS device performance required for current and future generations of microelectronic technology. An understanding of the mechanical response of the Si channel regions and their environment is key to the prediction and design of device operation. Because of the complexity of the composite geometries associated with microelectronic circuitry, in situ characterization at a submicron resolution is necessary to verify the predicted strain distributions. Of the measurement techniques commonly used for strain characterization, synchrotron-based X-ray microbeam diffraction represents the best nondestructive method to provide spatially resolved information. The mapping of strain distributions in silicon-on-insulator (SOI) features induced by overlying silicon nitride structures and embedded heteroepitaxial features adjacent to SOI device channels are presented. The interaction regions of the SOI strain were observed to extend large distances from the SOI/stressor interfaces leading to significant overlap in the strain distributions at technically relevant dimensions. Experimental data were also compared to several mechanical models to assess their validity in predicting these strain distributions.

Afghanite is a feldspathoid of the cancrinite-group: It is hexagonal, space group P63mc. The afghanite sample was found in the M. Somma-Vesuvio volcanic complex (Italy) and was previously described as davyne: Calculated cell parameters are a = 12.7997(4) Å, c = 21.4062(11) Å; the volume is 3037.2(2) Å3. The strongest lines are: 3.694(100), 3.647(56), 4.826(30), 2.678(25), 2.134(18), 3.999(12), 2.750(12), and 2.771(10). The new data provide quantitative measurement of intensities, an increased number of indexed peaks, and a different empirical formula with respect to the PDF 20-1086.

Silver halide based photographic imaging elements have been utilized as detectors for X-rays for over 100 years. These elements comprised of gelatin dispersed silver halide coated on one or both sides of a support, have been utilized in diffraction experiments since the discovery of X-ray diffraction by Laue and co-workers. X-ray film has high spatial resolution and can be adapted to flat or curved two-dimensional detection geometries. This paper describes the use of X-ray film as a two-dimensional detector for X-ray diffraction analysis, and discusses X-ray film composition, exposure, and processing, along with considerations for analyzing X-ray diffraction data collected using X-ray film.

X-ray powder diffraction data collected in transmission and high-throughput geometries were used to analyze form I of atorvastatin. The X-ray wavelength of the synchrotron radiation used in this study was determined to be λ=1.3771 Å. Form I of atorvastatin was found to be triclinic with space group P1 and unit cell parameters a=5.4568(2) Å, b=9.8887(4) Å, c=30.3091(9) Å, α=76.801(3)°, β=99.177(5)°, γ=105.318(5)°, V=1527.1(1) Å3, Z=1, and M=1209.41 g mol−1 Alternatively, another unit cell dimension can be used to describe the same P1 crystal with a=5.4564(2) Å, b=9.8883(4) Å, c=29.6555(8) Å, α=95.745(3)°, β=94.297(5)°, γ=105.327(5)°, and V=1526.8(1) Å3.

We present a detailed description of the SESAME Materials Science (MS) beamline for X-ray diffraction (XRD) applications, presently under construction in Allan, Jordan. The beamline is based on components previously installed at the Swiss Light Source, but modifications in the beamline design have been introduced to match the characteristics of the SESAME storage ring. The SESAME MS beamline will accommodate XRD experiments in the energy range between 5 and 25 keV. The beamline ray tracing analysis at 10 keV estimates the flux at the sample to be of the order of 1013 (photons s−1), the energy resolution is about 2 eV and the effective beam size at the sample of 300 × 2800 µm2. Investigations of microstruture will be possible as the instrumental broadening, resulted from simulating the diffraction pattern for a standard material, is of the order of 0.01° at 15 keV. A wide range of applications will be possible at the beamline, such as powder diffraction studies, single crystals and in situ XRD. The commisioning of the beamline is expected to be in the second half of 2017.

Synchrotron powder diffraction data have been obtained and indexed for ferrous gluconate, a common supplement used for the treatment and prevention of iron-deficiency anemia. Ferrous gluconate (Fe(C6H11O7)2 · x H2O, Z = 4) crystallizes in a monoclinic cell (space group I2, #5) with lattice parameters a = 19.953 16(9) Å, b = 5.513 92(3) Å, c = 18.470 58(9) Å, and β = 111.3826(3)°. The pattern shows no evidence of impurity reflections.

A polycrystalline sample of Ca4ZrGe3O12 was synthesized using the nitrate–citrate method and heated at 850–1100 °C. Structural refinement based on X-ray powder diffraction data showed that the crystal structure is of the garnet type with a cubic unit-cell parameter [a = 12.71299(3) Å] and the space group Ia$\bar 3$d. The structural formula is presented as Ca3[CaZr]octa[Ge]tetraO12.

This paper presents an example of comparing geochemical and mineralogical data by means of the statistical analysis of the X-ray diffraction patterns and the chemical compositions of bulk samples. The proposed methodology was tested on samples of metasomatic rocks from two geologically different objects. Its application allows us to mathematically identify all the main, secondary and some accessory minerals, to qualitatively estimate the contents of these minerals, as well as to assess their effect on the distribution of all petrogenic and investigated trace elements in a short period of time at the earliest stages of the research. We found that the interpretation of the results is significantly influenced by the number of samples studied and the quality of diffractograms.

A method is presented to examine consecutive in-situ X-ray diffraction (XRD) diffractograms using exploratory factor analysis. Systematic changes in the diffractograms are described numerically by score values that could be used to correlate diffraction data with other non-stationary sample properties. Phase and structure evolution in a reacting material can be studied by in-situ XRD. The consecutively collected data can be considered a time series of datasets. Time series are non-stationary data. Such non-stationary data are often hard to examine fully by conventional evaluation methods including applications of the Rietveld method. Here a method is presented to avoid shortcomings of conventional evaluation methods. The new method helps to identify and describe significant systematic changes in in-situ XRD datasets by numerical values. These systematic changes can represent structural changes as well as changes in phase composition. The method can be used to describe the development of the complex processes of compositional and structural changes. The method is demonstrated using the example of a hydrating Portland cement mortar. This hydration process involves at least 11 phases including non-crystalline phases. In the presented example factor analysis of in-situ XRD data results in three variables (factors) describing the observed changes numerically.

A quantitative phase analysis often requires advanced numerical studies to determine the appropriate intensity values. In this paper the method of fitting analytical functions to the experimental profile is applied to X-ray powder diffraction patterns obtained with FeK radiation. In the present work, the authors examine some problems connected with numerical studies, especially the function describing the experimental profile. The usefulness of the α2 elimination procedure and the angular dependence FWHM are also examined.

The Rietveld method can be combined with the addition method to determine the absolute quantities of the phases treated by Rietveld refinement plus the quantity of phase(s) not treated by it (amorphous or unobserved). If q is the added proportion of a defined phase already present in the sample, and a1 and a2 its relative proportions as determined by Rietveld refinement prior and after the addition, the proportion of the amorphous (untreated) phase(s) in the original sample is calculated as xo=[a2−(1−q)a1−q]/(1−q)(a2−a1). The absolute quantities of the phases treated by Rietveld refinement are then determined by a correction for the content of the amorphous phase(s), or they can be calculated directly from specific equations. The advantage of the method is that no new variables are introduced in the refinement when the added standard already is a part of the original mixture.

The nanostructural features of the gas-phase displacement reaction 2Mg(g)+SiO2→2MgO(s)+{Si}, where SiO2 is in the form of diatom shells were studied via X-ray diffraction and Fourier methods. Diatomaceous powder heated to 700 °C in a sealed graphite cell in the presence of Mg vapor formed MgO via a displacement reaction. Warren-Averbach analysis performed on samples reacted for different times showed an initial sharp MgO grain size distribution which broadened with time. New MgO crystallization was shown to occur until about 60 min, whereafter only MgO grain growth occurred. Median MgO crystallite size increased from 7.5 to 24.9 nm during this period, whereas microstrain decreased dramatically past 60 min annealing time.

We have used conventional X-ray powder diffraction to study one of the largest volume inorganic mixed oxide unit-supercell structures done so far. This necessitated some small-angle X-ray scattering-like observations at low angles from <2° 2θ to concord with electron diffraction, which had indicated an 8 × 8 × 8 huge volume supercell of a fluorite-type basic sub-cell. Emphasis is on the detection of, possibly very weak, fingerprint, low-angle/long lines/peaks which will indicate the (often unsuspected) presence of complex polytypic arrangements of simple very strong basic sub-cells and so facilitate future synthetic studies.

Internal elastic strain (i.e., residual stress) and the diffracted X-ray intensity variation over several orientations of crystallites with respect to the specimen surface were investigated as a means of differentiating two qualities of polycrystalline nickel plating. A unique instrument based upon a position-sensitive scintillation X-ray detector was used to apply all of the techniques commonly applied to X-ray stress analysis in this investigation. It was concluded that residual stress measurements did not provide a clear distinction between the two specimens, but comparison of the relative intensities diffracted from crystallographic planes at certain orientations with the surface did provide a distinction.

θ-KAlF4 is a new nanosized potassium tetrafluoroaluminate metastable polymorph (13×18×55 nm3). The crystal structure is solved ab initio from X-ray powder diffraction data in direct space [orthorhombic unit cell with a=8.3242(3) Å, b=7.2502(3) Å, c=11.8875(4) Å, V=717.44(5) Å3, Z=8, and space group Pnma]. This new structure type, unique in the whole AIMIIIF4 family, is related to the fluorite structure and consists of AlF6 octahedra linked via a common edge forming a bioctahedral motif which is trans-connected through the corner-shared fluorine, resulting in the formation of infinite ladderlike double file of octahedra ([Al2F8]2−)n running along the b axis.

The kalipyrochlore (K,Sr,Na,Ca,H2O)2−m(Nb,Ti)2−xO6−wY1−n, with (0<m<0.8, x∼0.2, w = 0 and 0.2<n<1) from Lueshe, Zaire is a defect pyrochlore species whose A-site weakly depleted. The measured powder diffraction is presented with a calculated figure of merit F(30) = 74.7(0.010,39). The structure has been refined by single-crystal from X-ray diffraction data collected on a Huber four-circle diffractometer and by Rietveld analysis from X-ray powder diffraction data. The slightly weathered crystal (studied by single crystal) has a cubic pyrochlore-type structure with the same atomic positions and a unit-cell parameter a = 10.603(5) Å, space group (S.G.): Fd3m. The highly weathered crystal (studied by Rietveld) has the same cubic pyrochlore-type structure except for the oxygen position. The oxygen moved from the 48f position with x, y, z equal to 0.284, 0, 0 to x = 0.308(5), y = 0.024(6) and z = –0.028(9). The cell parameter is a = 10.569(6)±0.0007 Å. These modifications of positions induce a distortion of the A-site into an hexagonal bipyramid and an elongation of the B-site along the c axis of the octahedron.

CaTi1−xSnxO3 (x = 0.0–1.0) solid solutions were prepared by solid-state reaction at 1450 °C. Rietveld refinement of their powder X-ray diffraction patterns revealed that all the solid solutions crystallized in orthorhombic cells with the perovskite-type structure, the space group Pbnm. The refined unit-cell parameters linearly increased with nominal tin contents x.

Neutron diffraction studies were carried out to ascertain the structural details of the composition Ce0.5Nd0.5O1.750. The structure was unequivocally found to be that of C-type cubic. The refinement on an F-type cubic lattice was found to be unacceptable because of high R values. Selected bond distances are also being reported. In addition, the neutron diffraction studies on a typical defective F-type composition Ce0.75Nd0.25O1.875 were also carried out.