The crystal structure of solifenacin hydrogen succinate [C23H27N2O2(HC4H4O4)] has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Solifenacin hydrogen succinate crystallizes in space group P21 (#4) with a = 6.477 03(2), b = 7.830 95(2), c = 23.848 72(7) Å, β = 90.2373(3)°, V = 1209.63(1) Å3, and Z = 2. The hydrogen succinate anions form a chain linked by strong hydrogen bonds parallel to the a-axis. Discrete N–H···O hydrogen bonds lie on the sides of this chain, resulting in a layer parallel to the ab-plane rich in hydrogen bonds. Halfway between these layers the molecules meet in a herringbone packing of aromatic rings. The powder pattern has been submitted to ICDD for inclusion in future releases of the Powder Diffraction File™.

The quantification of stress in polycrystalline materials by diffraction-based methods relies on the proper choice of grain interaction model that links the observed strain to the elastic stress state in the aggregate. X-ray elastic constants (XEC) relate the strain as measured using X-rays to the state of stress in a quasi-isotropic ensemble of grains. However, the corresponding interaction models (e.g., Voigt and Reuss limits) often possess unlikely assumptions as to mechanical response of the individual grains. The Kröner limit, which employs a self-consistent scheme based on the Eshelby inclusion method, is based on a more physical representation of isotropic grain interaction. For polycrystalline aggregates composed of crystals with cubic symmetry, Kröner limit XEC are equal to those calculated from a linear combination of Reuss and Voigt XEC, where the weighting fraction, xKr, is solely a function of the single-crystal elastic constants and scales with the material's elastic anisotropy. This weighting fraction can also be experimentally determined using a linear, least-squares regression of diffraction data from multiple reflections. Data on metallic thin films reveals that this optimal experimental weighting fraction, x*, can vary significantly from xKr, as well as that of the Neerfeld limit (x = 0.5).

An X-ray diffractometer (XRD) was modified to a low-power total reflection X-ray fluorescence (TXRF) spectrometer. This was realized by reducing the XRD tube power (3 kW) down to 10 W by a Spellman power supply. The present spectrometer consisted of a waveguide slit, Si-PIN detector, a goniometer and two Z-axis stages that were set on a diffractometer guide rail. This unit was easy in assembly. The first measurements with this spectrometer were presented. The minimum detection limit for Cr was estimated to be a few nanograms or at the level of 1013 atoms cm−2.

We report on the analysis of virtual powder-diffraction patterns from serial femtosecond crystallography (SFX) data collected at an X-ray free-electron laser. Different approaches to binning and normalizing these patterns are discussed with respect to the microstructural characteristics which each highlights. Analysis of SFX data from a powder of Pr0.5Ca0.5MnO3 in this way finds evidence of other trace phases in its microstructure which was not detectable in a standard powder-diffraction measurement. Furthermore, a comparison between two virtual powder pattern integration strategies is shown to yield different diffraction peak broadening, indicating sensitivity to different types of microstrain. This paper is a first step in developing new data analysis methods for microstructure characterization from serial crystallography data.

The crystal structure of sitagliptin dihydrogen phosphate monohydrate (sometimes referred to as sitagliptin phosphate monohydrate) has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Sitagliptin dihydrogen phosphate monohydrate crystallizes in space group P212121 (#19) with a = 6.137 108(12), b = 9.304 018(14), c = 38.307 67(10) Å, V = 2187.359(8) Å3, and Z = 4. The sitagliptin cation folds so that the two planar portions are roughly parallel. The ammonium group of the sitagliptin cation, the phosphate anion, and the water molecule form a network of strong hydrogen bonds. The result is a two-dimensional network, parallel to the ab plane. Halfway between these hydrogen bond planes, there are planes of high fluorine density. The powder pattern is included in the Powder Diffraction File™ as entry 00-064-1500.

Electron backscatter diffraction (EBSD) is a micro-analytical technique typically attached to a scanning electron microscope (SEM). The vast majority of EBSD measurements is applied to planar and polished surfaces of polycrystalline bulk specimen. In this paper, we present examples of using EBSD and energy-dispersive X-ray spectroscopy (EDX) to analyze specimens that are not flat, not planar, or not bulk – but pillars, needles, and rods. The benefits of low vacuum SEM operation to reduced drift problems are displayed. It is further demonstrated that small and thin specimens enhance the attainable spatial resolution for orientation mapping (by EBSD or transmission Kikuchi diffraction) as well as for element mapping (by EDX).

Synthesis and structural characterization of a novel palladium Pd(II) complex with the amino acid L-citrulline (Cit, C6H13N3O3) are presented in this paper. Elemental analysis indicates a 1:2 metal/ligand molar composition for the complex, with the molecular formula PdC12H24N6O6. The compound was also characterized by infrared (IR) spectroscopic measurements and the crystal structure has been solved by powder X-ray diffraction data with simulated annealing strategy in real space. The Pd(II) complex crystallizes in the triclinic system with space group P-1 and cell parameters a = 4.6493(4) Å, b = 5.222(4) Å, c = 18.040(2) Å, α = 77.41(6)°, β = 94.72(7),° and γ = 101.45(7)°. The crystal structure confirms the presence of Pd(II) ions in a nearly square planar environment and the molecular formula with deprotonated citrulline as proposed by analytical and spectroscopic data.

The solid-state phase equilibria of the copper (Cu)–dysprosium (Dy)–titanium (Ti) ternary system at 973 K has been experimentally investigated. The existence of nine binary compounds, Cu4Ti, Cu3Ti2, Cu4Ti3, CuTi, CuTi2, CuTi3, CuDy, Cu2Dy, and Cu5Dy was confirmed. The controversial phase of CuTi3 was found in this work. The temperature range of Cu7Dy was determined to be from 1112 to 1183 K. The phase relations at 973 K are governed by ten ternary phase regions, 21 binary phase regions, and 12 single-phase regions. The solid solubility of Cu in Dy is undetectable. None of the other phase in this system reveals a remarkable homogeneity range at 973 K.

For the first time evidence is provided that a nanocrystalline and stacking-disordered, chemically stabilized β-cristobalite form of AlPO4 occurs in a sewage sludge ash (SSA). This proof is based on a combined X-ray powder diffraction and X-ray fluorescence investigation of an SSA produced at a large-scale fluidized bed incineration facility serving a catching area with a population of 2 million. The structural and chemical characterization was carried out on ‘as received’ SSA samples as well as on solid residues remaining after leaching this SSA in sodium hydroxide solution. Thus, it was ascertained that the observed nanocrystalline and stacking-disordered cristobalite-like component belongs to the aluminum phosphate component of this SSA, rather than to its silicon dioxide component. In addition, a direct proof is presented that the chemically stabilized β-cristobalite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850°C), typical for fluidized bed incinerators.

Crystal structure of BaxSr3–xMgSi2O8 has been determined by Raman spectroscopy and X-ray diffraction. The solid solution series have glaserite-type layered structures made of corner-sharing SiO4 tetrahedra and MgO6 octahedra. Ba2+ and Sr2+ ions are sandwiched in between the layers. Raman spectroscopy has found that structural symmetry changes at x = 0.5 and 2.5. Structural refinement by the Rietveld method has clarified that the symmetry changes occur among C2 (Z = 4), P${\bar 3}$m1 (Z = 1), and P${\bar 3}$ (Z = 3). They originate in SiO4 tilting caused by size mismatch between alkali–earth cations and their site spaces. For x ≤ 0.5, SiO4 tilting occur every other interlayer space, whereas for x ≥ 2.5, all the SiO4 tilt.

The ternary compound of AlCu4Y was synthesized by melting under argon atmosphere in the arc furnace. High-quality X-ray powder diffraction data of AlCu4Y have been collected using a Rigaku SmartLab X-ray powder diffractometer. The Rietveld refinement results of the X-ray diffraction pattern for the AlCu4Y compound showed that the AlCu4Y is the hexagonal structure, space-group P6/mmm (No. 191) with a = 5.0658(1) Å, c = 4.1569(1) Å, V = 92.38 Å3, Z = 1, and the density is 6.66 g cm−3, and the intensity ratio RIR is 1.96.

The crystal structure of lacosamide form I has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques (density functional theory). Lacosamide form I crystallizes in space group P21 (#4) with a = 10.677 73(5), b = 4.799 68(2), c = 13.639 16(9) Å, β = 91.6331(10)̊, V = 698.719(6) Å3, and Z = 2. Van der Waals interactions are important in the crystal structure. Two N–H···O hydrogen bonds form C1,1(4) chains along the b-axis. Several weaker C–H···O hydrogen bonds to the ketone oxygens also contribute to the packing energy. These C–H···O extend both along the b-axis and in the ac-plane, and help link the molecules in three dimensions. The powder pattern has been submitted to International Centre for Diffraction Data for inclusion in the Powder Diffraction File™.

The crystal structure of folic acid dihydrate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Folic acid dihydrate crystallizes in space group P212121 (#19) with a = 7.275 78(3), b = 8.632 17(4), c = 32.417 19(22) Å, V = 2035.985(18) Å3, and Z = 4. The structure is dominated by a three-dimensional network of hydrogen bonds. The dicarboxylic acid side chain occurs in a bent conformation, helping explain the ability of folate derivatives to coordinate metal cations. The powder pattern has been submitted to ICDD for inclusion in future releases of the Powder Diffraction File™.

An example of commercially available product, 2-(methylideneamino)acetonitrile (MAAN). This paper will address problems in discerning monomer–polymer ambiguity in organic compounds. Reliable three-step analysis of organic polymers will be proposed using the synergy of computational [density functional theory (DFT)] and experimental [infrared spectroscopy (IR); X-ray powder diffraction (XRPD)] techniques. First, possible conformations of monomeric and trimeric MAAN were calculated using stochastic search and DFT. Second, identification of the commercial sample was performed by comparing the measured IR spectrum with those calculated for monomer and trimer. Third, the examination of sample purity and structural analysis were carried out using XRPD data.

X-ray fluorescence (XRF) is a well-established method for quantitative elemental analysis. For accurate quantification, secondary excitation has to be taken into account. In this paper, the secondary excitation process was discussed for analysis by confocal micro-XRF. Experimental depth profiles were shown for a layered sample of Co and Cu. An additional peak was observed in the depth profile of Co, and it was explained by secondary excitation process. Additionally, a Mosaic model was proposed for quantification of confocal micro- XRF analysis.

X-ray powder diffraction data for 5-Chloro-N-(4-nitrophenyl)pentanamide, C11H13ClN2O3, are reported [a = 8.036(4) Å, b = 15.972(5) Å, c = 9.829(5) Å, α = 90°, β = 104.227(2)°, γ = 90°, V = 1222.98 Å3, Z = 4, ρx = 1.3941 g cm−3 and space group P21/c]. All measured lines were indexed and are consistent with the P21/c space group. No detectable impurities were observed.

Properties of a special double-crystal (DC) monochromator employing bent-perfect crystals of Si in (1, −1) and (n, −m) settings are presented. The first monochromator was the bent Si(111) crystal (4 mm thickness) and the second one was in the form of a sandwich consisting of two bent Si(111) and Si(220) slabs (2 and 1.3 mm thickness, respectively). It has been found that by a simple exchange of diffraction conditions on the second monochromator one can use either Si(111) + Si(111) bent crystals in (1, −1) setting providing good luminosity and worse diffractometer resolution or Si(111) + Si(220) bent crystals in quasi-dispersive (n, −m) setting providing very good diffractometer resolution and correspondingly weaker luminosity. It has been found that besides an excellent focusing and reflectivity properties of the dispersive double-bent-crystal setting the obtained monochromatic neutron current is sufficiently high for diffraction experiments even at the medium-power research reactor.

An interlaboratory study (ILS, round robin) was conducted to assess the accuracy and precision of the phase quantification of calcium phosphate (CaP) bioceramics by X-ray diffraction (XRD) and Rietveld refinement. For that purpose, a mixture of hydroxyapatite and β-tricalcium phosphate, two CaP phases commonly used in synthetic bone graft substitutes, was prepared and sent to 12 laboratories for XRD analysis. Results from 26 different instruments were received and evaluated statistically according to ASTM E691 – 13. The statistical analysis revealed that the reproducibility standard deviation of phase quantities was approximately two times greater than the repeatability standard deviation, which is obtained by repeating the analysis on a single instrument configuration multiple times. The 95% reproducibility limit for phase quantities was R = ±1.67 wt%. The study also demonstrated that several participants overinterpreted their data in an attempt to refine crystallite sizes of the minor phase.

The structure of La2LiTaO6 has been derived from the powder X-ray powder diffraction (XRD) data. La2LiTaO6 is monoclinic with unit-cell parameters a = 5.621(1) Å, b = 5.776(1) Å, c = 7.954(2) Å, β = 90.34(2)°, space group P21/n (14), and Z = 2. The structure of La2LiTaO6 is an ordered perovskite with alternating Li and Ta octahedra. A new set of powder XRD data (d-spacing and intensity listing) has been generated to replace entry 00-039-0897 within the Powder Diffraction File. The newly elucidated structural data for La2LiTaO6 shall facilitate quantitative analysis of this impurity phase which is often observed during synthesis of the fast-ion conductor phase Li5La3Ta2O12.

The authors present and discuss a method for simultaneous quantitative analysis of total loss on ignition (LOI) (CO2 + H2O) and CO2 content separate from the LOI, in an industrial environment of quicklime production. Total LOI is determined by the Compton scattered RhKα tube radiation which is used directly in the calibration equation. The resulting calibration curve for LOI, including matrix correction shows an accuracy of 0.15 mass%. The carbon content (CO2) is distinguished from total LOI by measuring CKα radiation, which is possible with the required accuracy by employing a new multilayer analyzer with greatly improved background characteristics. The method aims at high reliability and sample throughput and at becoming a less time-consuming alternative to the conventional method of LOI determination by weighing sequences before and after “ignition” at 1050 °C.