The authors present here the superior result of synchrotron X-ray diffraction indexing of the 8 × 8 × 8 fluorite supercell, murataite, M8 (formula Ca66.37Mn29.33Ti186.76Zr83.35Al46.30Fe74.09O817, a = 39.277(3) Å, Z = 4). The authors present evidence that Fd$\bar 3$m (227) is the most likely space group.

Baileychlore is Zn-end member trioctahedral chlorite, named by Audrey C. Rule and Frank Radke in 1988 for the honor of Professor Sturges W. Bailey of the University of Wisconsin – Madison, USA. Baileychlore occurs as dark green chlorite on calcite veins from garnet-vesuvianite skarn clasts at Red Dome ore deposit, Chillagoe, Queensland, Australia. The baileychlore has been studied by using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray energy-dispersive analytical electron microscopy analyses to determine crystal structure and interstratified layers. Baileychlore with stacking disorder displays streaking reflections of 0k0 (≠6n) hhl (h ≠ 3n). Unit-cell parameters for baileychlore (type I polytype) with a space group of C$ \bar 1$ are: a = 5.351(3), b = 9.266(5), c = 14.418(8) Å, α = 89.741(3)°, β = 96.741(4)°, and γ = 90.122(2)°. The strong lines of the measured XRD pattern [d(Å)(I)(hkl)] are: 14.331(7.151)(90.5)(002); 4.574(23.2)(1$ \bar 1$0, 11$ \bar 1$); 3.572(38.5)(004); 2.653(31.4)($ \bar 1$31, 200, 13$ \bar 1$); 2.406(49.4)(202, $ \bar 1$33, 13$ \bar 3$); 1.543(27.6)($ \bar 3$31, 060, 33$ \bar 1$), respectively. Reitveld refinement provides a composition (Zn2.49Al0.09Fe2+ 0.09□0.33)0.61− for the octahedral sheet and (Si3.53Al0.47)0.47− for the tetrahedral sheets within the 2:1 layer with (Al1.08Fe1.08Mg0.84)1.08+ for the interlayer sheet. The refinement results indicate that baileychlore is an intergrowth of type I and II polytypes. High-resolution TEM images show stacking disorder of baileychlore with small amount of isolated smectite layers.

The electrochemical behaviour of a number of Pb-based anode alloys, under simulated electrowinning conditions, in a 1.6 M H2SO4 electrolyte at 45 °C was studied. Namely, the evolution of PbO2 and PbSO4 surface layers was investigated by quantitative in situ synchrotron X-ray diffraction (S-XRD) and subsequent Rietveld-based quantitative phase analysis (QPA). In the context of seeking new anode alloys, this research shows that the industry standard Pb-0.08Ca-1.52Sn (wt%) anode, when exposed to a galvanostatic current and intermittent power interruptions, exhibited poor electrochemical performance relative to select custom Pb-based binary alloys; Pb–0.73Mg, Pb–5.05Ag, Pb–0.07Rh, and Pb–1.4Zn (wt%). The in situ S-XRD measurements and subsequent QPA indicated that this was linked to a lower proportion of β-PbO2, relative to PbSO4, on the Pb-0.08Ca-1.52Sn alloy at all stages of the electrochemical cycling. The best performing alloy, in terms of minimisation of overpotential during normal electrowinning operation and minimising the deleterious effects of repeated power interruptions – both of which are significant factors in energy consumption – was determined to be Pb–0.07Rh.

The 3-[1-(6-methoxy-2-naphtyl)ethyl]-6-(2,4-dichlorophenyl)-7H-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazine, C23H18Cl2N4OS compound was synthesized, as a member of the family of novel potential anticancer agents. The structure of the title compound was characterized by IR, 1H-NMR, mass spectroscopy, and elemental analysis, previously. In this study, the crystal structure of this compound has been determined from synchrotron X-ray powder diffraction data. The crystal structure was solved by simulated annealing and the final structure was achieved by Rietveld refinement method using soft restrains on all interatomic bond lengths and angles. This compound crystallizes in space group P21, Z = 2, with the unit-cell parameters a = 15.55645(11) Å, b = 8.61693(6) Å, c = 8.56702(6) Å, β = 104.3270(4)°, and V = 1112.68(1) Å3. In the crystal structure, strong C−H⋯π and weak intermolecular hydrogen-bonding interactions link the molecules into a three-dimensional network. The molecules are in a head-to-head arrangement in the unit cell.

X-ray powder diffraction data, unit-cell parameters, and space group for alogliptin benzoate, C18H21N5O2·C7H6O2, are reported [a = 28.8260(8) Å, b = 9.9654(4) Å, c = 8.1477(8) Å, α = 90, β = 90, γ = 90°, unit-cell volume V = 2340.57 Å3, Z = 4, ρcal = 1.3097 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.

A full-pattern fitting procedure based on the Rietveld method was applied to electron diffraction ring patterns of a two-phase system, exhibiting the co-presence of zinc sulfide (sphalerite) and zinc oxide (Wurtzite). Bright and dark field (DF) images reveal the presence of micrometric aggregates, composed of quasi-spherical nanosized crystallites. These conventional transmission electron microscopy imaging methods provide a general morphological characterization of the specimens although, in the present case, they are not suitable for a detailed characterization of the microstructural features of the analyzed samples. Owing to the overlap and broadening of the diffraction rings of the two phases, DF images cannot provide a satisfactory picture of the individual crystallites of each single phase. To overcome this limit, the mentioned Rietveld approach was applied to model the electron diffraction data. The crystalline domain size and relevant shapes for both phases were successfully evaluated using the proposed methodological approach. The excellent results obtained in the microstructural characterization of the nanostructured multiphase samples demonstrate the capability of this technique, that may represents a fully quantitative method for the routine characterization of crystalline nanomaterials.

X-ray fluorescence (XRF) has been employed as one of several orthogonal means of screening materials to prevent counterfeit and adulterated products from entering the product stream. We document the use of principal component analysis (PCA) of XRF data on compositionally similar and dissimilar stainless steels for the purpose of testing the feasibility of employing XRF spectra to parse and bin these alloys as the same or significantly different alloy materials. The results indicate that XRF spectra can separate and assign alloys via PCA, but that important corrections for detector drift and scaling must be performed in order to achieve valid results.

A series of phase transformations of a novel fluoroaluminosilicate glass forming a range of fluorapatite glass-ceramics on sintering are reported. The sintering process induces formation of fluorapatite, mullite, and anorthite phases within the amorphous silicate matrices of the glass-ceramics. The fluoroaluminosilicate glass, SiO2–Al2O3–P2O5–CaO–CaF2, is prepared from waste materials, such as rice husk ash, pacific oyster shells, and disposable aluminium cans. The thermally induced crystallographic and microstructure evolution of the fluoroaluminosilicate glass towards the fluorapatite glass-ceramics, with applications in dental and bone restoration, are investigated by powder X-ray diffraction and small-angle neutron-scattering techniques.

The VF3-type compound GaF3 has been studied by high-pressure angle-dispersive X-ray diffraction in the pressure range from 0.0001 to 10 GPa. The compression mechanism was found to be highly anisotropic. The c-axis shows little pressure dependence (≈0.4%), but exhibits negative linear compressibility up to ≈3 GPa where it achieves its maximum length. In contrast, the length of the a-axis is reduced by ≈8.8% at the highest measured pressure and an anomalous reduction in the linear compressibility is observed at 4 GPa. The zero pressure bulk modulus B0 was determined to B0 = 28(1) GPa. The compression mechanism of GaF3 is discussed in terms of deformation of an 8/3/c2 sphere-packing model. The volume reduction of GaF3 is mainly achieved through coupled rotations of the GaF6 octahedra within the entire measured pressure range, which reduces the volume of the cubooctahedral voids. In addition, the volume of the GaF6 octahedra also decreases for p ≲ 4.0 GPa, but remains constant above this pressure. The volume reduction of the GaF6 octahedra is accompanied by an increasing octahedral strain. Isosurfaces of the procrystal electron density are used for visualization of the cubooctahedral voids at different pressures.

Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) (1) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) (2), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space group $P\bar 1$, Z = 2, with the unit-cell parameters a = 6.37433(9), b = 11.3641(2), c = 14.09115(19) Å, α = 80.1740(8)°, β = 85.1164(8)°, γ = 80.9831(10)°, V = 991.55(3) Å3 of compound (1) and a = 6.53736(6), b = 11.55725(15), c = 14.01373(13) Å, α = 80.3323(7)°, β = 84.8939(6)°, γ = 79.3954(8)°, V = 1024.08(2) Å3 of compound (2). Structural analyses reveal that the title compounds are isostructural.

A new methodology for very high-speed, energy-dispersive detection of X-ray fluorescence is being developed. The underlying reasoning behind it, as well as early results from the evaluation of the first prototype, is presented.

The alkaline content of mixed transition metal phosphates Li(1−y)·zNay·zM0.5Fe0.5PO4 (M = Mn, Co; 0 ≤ y < 1; 0.5 ≤ z ≤ 1) was determined by powder X-ray diffraction data by means of Rietveld analysis and multi-fraction models. The compounds LiM0.5Fe0.5PO4 were synthesized via solid-state reactions. Chemical extraction of Li with bromine in acetonitrile yielded well-crystalline Li0.5M0.5Fe0.5PO4. Subsequent reduction with Na2S in acetonitrile gave a product with a triphylite-type phase of the average composition Li0.5Na0.5M0.5Fe0.5PO4 showing a broad distribution of Li-to-Na-ratios. For Rietveld refinements a set of 11 fractions Li1−yNayM0.5Fe0.5PO4 was used to represent the triphylite-type phase and its composition fluctuation. To obtain samples with compositions close to NazM0.5Fe0.5PO4 (z = 0.5 or z = 1) up to two additional cycles of chemical oxidation and reduction were required. Because of a complex distribution of Li and Na within the triphylite-type phase a model of 121 fractions of Li(1−y)·zNay·zM0.5Fe0.5PO4 was developed to enable proper Rietveld refinements. The scaling factors of the 121 fractions were constrained by a bimodal bivariate normality. The evaluation of the pattern revealed a type of passivation, preventing the compound from complete oxidation or reduction of Fe for higher cycle numbers. Hence, no completely Li-free samples could be obtained.

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 decrease in quality of Australian iron ore, coupled with the demand for more efficient energy use, means that closer monitoring and optimisation of process conditions for iron ore sinter production is required. Here, the suitability of using partial least-squares regression analysis of powder X-ray diffraction data, collected for iron ore sinter samples, for the prediction of iron ore sinter strength has been further assessed. In addition, a preliminary assessment of the effect of 2θ range on the quality of prediction has been made. For the purposes of process control, the level of correlation between predicted strength and actual sinter strength would inform an operator whether or not the process was operating within the acceptable limits, or whether there was a potential problem requiring further investigation or rapid intervention. Reducing the 2θ range was found to reduce the level of correlation between predicted and actual strength, to a point where the particular analysis may no longer be suitable for process control.

X-ray diffraction data revealed that the initial SiO2/Ag nanocomposite, manufactured in a chemical synthesis process, is mainly composed of silica in amorphous phase (95.5 wt.%), crystalline Ag with a cubic structure (Fm-3m) and cristobalite (SiO2) with a tetragonal structure (P41212) in the amount of 4.2 and 0.3 wt.%, respectively. High-temperature diffraction data revealed high stability of the SiO2/Ag composite up to 1000 °C. High-temperature X-ray diffraction measurements revealed phase cristallization temperatures of silica at 1060 °C for cristobalite and 1080 °C for tridymite as well as temperature of silver evaporation starting from the composite (ca. 1000 °C). Infrared spectroscopy data confirmed the presence of amorphous matrix with embedded silver ions and crystalline compounds in the form of cristobalite and tridymite without silver after thermal treatment.

The crystal structure of Na(NH4)Mo3O10·H2O has been solved by parallel tempering using the FOX software package with synchrotron powder diffraction data obtained from beamline 08B1-1 at the Canadian Light Source. Rietveld refinement, performed with the software package GSAS, yielded orthorhombic lattice parameters of a = 13.549 82(10), b = 7.618 50(6), and c = 9.302 74(7) Å (Z = 4, space group Pnma). The structure is composed of molybdate chains running parallel to the b-axis. The Rietveld refinement results were compared with density functional theory calculations performed with CRYSTAL14, and show excellent agreement with the calculated structure.