The crystal structure and powder patterns were prepared for the distorted perovskite series R(Co3/4Ti1/4)O3 (R = La, Pr, Nd, Sm, Eu, Gd, Dy, Ho). The R(Co3/4Ti1/4)O3 members are isostructural with each other and are crystallized in the orthorhombic crystal system with space group Pnma, Z = 4. From R = La to Ho, the lattice parameters a range from 5.4614(3) to 5.5368(2) Å, b range from 7.7442(4) to 7.4859(2) Å, and c range from 5.5046(3) to 5.2170(2) Å. The unit-cell volumes, V which range from 232.81(2) to 216.237(11) Å3 follow the trend of “lanthanide contraction”. The structure distortion of these compounds is evidenced in the tilt angles θ, ϕ, and ω, which represent rotations of an octahedron about the pseudo-cubic perovskite [110]p, [001]p and [111]p axes. All three tilt angles increase across the lanthanide series (for R = La to R = Ho: θ increases from 8.34° to 17.00°, ϕ from 6.24° to 8.53°, and ω from 10.41° to 18.96°), indicating a greater octahedral distortion as the ionic radius of R3+ [r(R3+)] decreases. The bond valence sum values for the (Co/Ti) site and the R site of R(Co3/4Ti1/4)O3 reveal no significant bond strain in these compounds. X-ray diffraction patterns of the R(Co3/4Ti1/4)O3 samples were submitted to the Powder Diffraction File.

An organic polar hydrate was obtained through cocrystallization of 2,4-diaminotoluene (2,4-DAT) and L(+)-tartaric acid (TA) from ethanol. Dehydration behavior of the obtained hydrate was investigated using variable temperature powder X-ray diffraction (PXRD) and thermal analysis. Proton transfer from L(+)-TA to 2,4-DAT in both hydrate and dehydrated form was revealed via Fourier transform infrared spectroscopy. The crystal structures of both forms were determined using PXRD techniques. The similarities and differences between two crystal structures were analyzed and the role of water in the hydrate crystal structure was demonstrated.

The crystal structure of the purpureo salt, [Co(NH3)5Cl]Cl2, first reported in 1963 and later revised in 1968 (in both cases from single-crystal diffraction) in the space group Pnma (No. 62), has been recently re-examined from synchrotron X-ray powder diffraction using direct methods and the software EXPO2013. The comparison of the Rietveld analysis results using the two published models and the atomic coordinates obtained from powders leads to an improved crystal structure description in the lower symmetry space group Pn21a (No. 33). As a result, the overall atom connectivity and crystal packing remain similar; however, the symmetry and internal geometry of the coordination complex are changed. The distortions from an idealized geometry in Pnma (No. 62) are likely because of energetically favorable hydrogen-bonding motifs in the crystal. The three models are compared, and their validity and limitations are discussed.

Elemental, chemical, and structural analysis of polycrystalline materials at the micron scale is frequently carried out using microfocused synchrotron X-ray beams, sometimes on multiple instruments. The Maia pixelated energy-dispersive X-ray area detector enables the simultaneous collection of X-ray fluorescence (XRF) and diffraction because of the relatively large solid angle and number of pixels when compared with other systems. The large solid angle also permits extraction of surface topography because of changes in self-absorption. This work demonstrates the capability of the Maia detector for simultaneous measurement of XRF and diffraction for mapping the short- and long-range order across the grain structure in a Ni polycrystalline foil.

Linezolid (LZD) is one of the first commercially available synthetic oxazolidinone antibiotics and is widely used for the treatment of multidrug-resistant Gram-positive bacterial infection. LZD was found to have five polymorphic forms. The most stable and commercialized polymorphs are known as forms II and IV. Trace content of form II in LZD form IV will cause to transition LZD form IV to II rapidly. Powder X-ray diffraction (PXRD) methods were evaluated for the determination of the polymorphic content of the drug substance and drug product. The estimated limit of detection values of the single peak method for LZD polymorph form II in drug substance and tablet formulation were 0.4 and 0.6%, respectively, while the limit of detection value of Rietveld Refinement (full-profile fitting) evaluated LZD polymorph form II in drug substance was 0.2%. The results clearly show that levels <1 wt.% (in active pharmaceutical ingredients) and 2 wt.% (in tablets) LZD form II in form IV can be detected and quantified by PXRD. Validation of the analytical method proved that the method is repeatable, sensitive, and accurate.

The Pd2HgSe3 phase was synthetized from individual elements by the silica glass tube technique and its crystal structure has been refined by the Rietveld method. The Pd2HgSe3 phase crystalizes in P$\bar 3$m1 space group with the unit-cell parameters a = 7.3096(2) Å, c = 5.2829(1) Å, V = 244.45(1) Å3, Dc = 8.84 g/cm3, and Z = 2. In its layered crystal structure, the [PdSe6] octahedra share opposing Se–Se edges with adjacent [PdSe4] squares forming layers parallel with the (001) plane. The layers show AA type stacking along the c-axis. Hg atoms occupy the anti-cubooctahedral voids between two consecutive layers. Pd2HgSe3 is isostructural with Pt2HgSe3 and Pt4Tl2X6 (X = S, Se, or Te) phases. The structure can be viewed as a 2a.2a.c superstructure of PtSe2.

Three spinel materials were prepared and characterized by in situ powder X-ray diffraction (PXRD) techniques to track their phase changes that occurred in the typical batch synthesis process from a sol–gel mixture to the final crystalline spinel oxide. The materials were also characterized by thermal gravimetric analysis, whereby the materials decomposition mechanisms that were observed as the precursor, was gradually heated to the final oxide. The results showed that all the materials achieved their total weight loss at about 400 °C. The in situ PXRD analysis showed the progression of the phase transitions where certain of the materials changed from a crystalline precursor to an amorphous intermediate phase and finally to the spinel cathode oxide (Li1.03Mg0.2Mn1.77O4). For other materials, the precursor would start as an amorphous phase and upon heating, convert into an impure intermediate phase (Mn2O3) before forming the final spinel oxide (Li1.03Mn1.97O4). On the other hand, the LiAl0.4Mn1.6O4 would start with an amorphous precursor, with no intermediate phases and immediately formed the final spinel oxide phase. The in situ PXRD study also showed the increases in the materials respective lattice parameters of the crystalline unit cells upon heating and the significant increases in their crystallite sizes when heated above 600 °C.

Characterization of semi and noncrystalline materials, monitoring structural phase transitions in situ, and obtaining structural information together with spatial distribution of the investigated material are only a few applications that hugely benefitted from the combination of high-energy X-rays and modern algorithms for data processing. This work examines the possibility of advancing these applications by shortening the data acquisition and improving the data quality by using the new high-energy PILATUS3 CdTe detector.

Lithol reds belong to the group of azo pigments, which were popular artists’ colouring materials in the first half of the twentieth century. These pigments were also used in many branches of industry. Here, we report X-ray powder diffraction data, unit-cell parameters, and space groups for three compounds from this group: sodium (E)-2-((2-hydroxynaphthalen-1-yl)diazenyl)naphthalene-1-sulphonate monohydrate (Na lithol red), monoclinic, space group C2/c, with cell parameters a = 33.343(7), b = 6.667(2), c = 16.397(4) Å, β = 90.83°, V = 3644.51 Å3, Z = 8; barium (E)-2-[(2-hydroxynaphthalen-1-yl)diazenyl]naphthalene-1-sulphonate trihydrate (Ba lithol red), monoclinic, space group P21/m, with cell parameters a = 17.758(9), b = 6.209(4), c = 16.857(8) Å, β = 92.07°, V = 1857.39 Å3, Z = 2; and ammonium (E)-2-[(2-hydroxynaphthalen-1-yl)diazenyl]naphthalene-1-sulphonate monohydrate (NH4 lithol red), monoclinic, space group P2/c, with cell parameters a = 17.721(5), b = 6.428(3), c = 16.911(5) Å, β = 100.31(3)°, V = 1895.31 Å3, and Z = 4. In the first and third cases we synthesised the pigments in their monohydrate form, performed X-ray powder diffraction measurements, and indexed all of the obtained diffraction maxima. In the case of the barium compound, despite many efforts in the course of the synthesis procedure, the powder diffraction patterns of the obtained samples were not of the best quality. Nevertheless, we indexed the best one and found a reliable space group and cell parameters.

In this work, we developed an X-ray powder diffractometer system equipped with six solid-state detectors and used it to perform ab initio structure determination from the powder diffraction pattern data obtained for a caffeine–oxalic acid co-crystal. The crystal structure obtained from the powder diffraction data was consistent with the previously solved single-crystal structure (Trask reference), although slightly larger (by about 2%). The co-crystallization of pharmaceutically active molecules can modulate their physical properties such as solubility, stability, and bioavailability. For the investigation of pharmaceutical complexes, the ability to visualize molecular interactions such as hydrogen bonding would be very helpful toward understanding their physical properties. Given the rate at which the high-throughput screening of pharmaceutical complexes has grown, an analogous high-volume, high-resolution X-ray powder diffraction technique with high-throughput data collection ability would be useful. We also solved the crystal structures of an inorganic complex and metal organic framework, zinc acetate dihydrate and CPL-1, in order to demonstrate the performance of our new diffractometer system.

In this study, the application of (an)isotropic size determination using a recently proposed model for the double-Voigt approach is demonstrated and validated against line profile simulations using the Whole Powder Pattern Modelling approach. The fitting of simulated line profiles demonstrates that the attained crystallite sizes and morphologies are in very reasonable agreement with the simulated values and thus demonstrate that even in routine application scenarios credible size and morphology information can be obtained using the double-Voigt approximation. The aim of this contribution is to provide a comprehensive introduction to the problem, address the practical application of the developed model, and discuss the accuracy of the double-Voigt approach and derived size parameters. Mathematical formulations for the visualization of modeled morphologies, supporting the application of the recently developed macros, are additionally provided.

The syntheses and crystal structures and magnetic properties of novel RIn3−xTx (R = Gd，Pr；T = Fe，Co，Mn；x = 0–0.3) intermetallic compounds in rare earth-In-3d transition metal ternary system have been systematically investigated. It reveals that RIn3−xTx crystallizes in cubic AuCu3 type structure with a space group of Pm$\bar 3$m and Z = 1. The 1a and 3c crystal positions are occupied by R and In atoms, respectively. The 3d transition metals substitute partly for In and prefer to occupy the 3c site. The lattice parameters and unit cell volumes decrease with increasing the content of 3d transition metal in RIn3−xTx intermetallic compounds. The magnetic properties of RIn3−xTx are sensitive to T content. With increasing T content, GdIn3−xTx alloys show the paramagnetic, mixture of ferromagnetic and paramagnetic and ferromagnetic behavior. T doping into RIn3 induces the presence of ferromagnetic phase in GdIn3−xTx, which is totally different from those of the pure binary RIn3.

X-ray powder diffraction data, unit-cell parameters, and space group for S-2-(methylamino)-2-phenylcyclohexan-1-one hydrochloride, C13H18ClNO, are reported [a = 6.578 (1) Å, b = 13.250 (2) Å, c = 15.096 (2) Å, β = 91.619 (3)°, unit-cell volume V = 1315(1) Å3, Z = 4, and space group P21]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurities were observed.

In pursuit of design and characterisation of Cu adsorbing in thin films, we present data from a large variety of Cu-K edge X-ray Absorption Near Edge Spectroscopy (XANES) spectra obtained from organic and inorganic standards. Additionally, we have explored the impact of beam damage inducing redox alterations. Polymer nanoparticles were tested against films to produce higher concentration samples while maintaining high surface area to bulk effects. Spectra from nanoparticles were highly comparable to thin films of ~8 nm thickness, implying comparable contributions by surface effects on copper association. Finally, we observed no impact on Cu XANES spectra from vitrification with dimethyl sulfoxide to produce amorphous frozen, hydrated samples. The spectra should act as a valuable resource in assisting the design of experiments and identification of copper associations.

The crystal structure of hydrocortisone acetate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Hydrocortisone acetate crystallizes in space group P21 (#4) with a = 8.85173(3) Å, b = 13.53859(3) Å, c = 8.86980(4) Å, β = 101.5438(3)°, V = 1041.455(6) Å3, and Z = 2. Both hydroxyl groups form hydrogen bonds to the ketone oxygen atom on the steroid ring system, resulting in a three-dimensional hydrogen bond network. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™.

A polycrystalline sample of a new triple molybdate AgMg3Ga(MoO4)5 was obtained by solid-state reaction techniques. Structural refinement based on X-ray powder diffraction data showed that the crystal structure is isotypic with NaMg3In(MoO4)5 (sp. gr. P$\bar 1$). In the structure pairs of edge-shared (Mg, Ga)O6,  octahedra are connected by common vertices to form a three-dimensional framework. Large framework cavities involve Ag+ cations. The title compound was found to melt at 1079 K.

A robust analysis script was developed in MATLAB for cross-correlative quantification of internalised gold nanoparticle (AuNP) uptake in a large number of individual cells with the corresponding number of DNA double-strand breaks (DSBs) in the same cells. The correlation of inorganic NP content with a biological marker at the single-cell level will aid in the elucidation of mechanisms of NP radiosensitisation. PC-3 cells were co-cultured with AuNPs and irradiated using an iridium-192 source. AuNP uptake was measured using synchrotron X-ray fluorescence (XRF) and DSBs imaged via confocal microscopy. MATLAB 2016a was used to develop a script to cross-correlate the two imaging modalities and quantify both DSBs and internalised AuNP content in the same cell. Various user-defined options written into the script give a high degree of versatility, which can account for a large number of variables in experimental parameters and data acquisition. The analysis procedure is flexible and robust, which gives consistent consideration to the wide spectrum of potential input image/data sets. Quantitative correlative microscopy was achieved with a custom MATLAB script used to correlate γH2AX foci (a marker of DNA DSBs) from confocal microscopy with AuNP content acquired using synchrotron XRF at the single-cell level. The script can be extended to a broad range of multi-modality imaging spectroscopies.

The silver (Ag) powder was synthesized in a mechanochemical (MC) process by inducing a solid-state displacement reaction between silver chloride (AgCl) and copper (Cu). This process was carried out in argon atmosphere conditions using a planetary ball mill. The reaction caused the mixture of AgCl and Cu to change the composition of the mixture to Ag and copper chloride (CuCl). CuCl was separated from MC product by leaching with ammonium hydroxide. Thus, Ag powder was obtained as the final product. Stearic acid (C18H36O2) was used as the additive to improve dispersion of Ag powder during the MC process. The ground powders, formed in the presence and absence of additive, were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The XRD determined that the reaction between AgCl and Cu was completed in 18 h milling. SEM and particle size analysis examinations revealed that the size of the particles in the synthesized metallic Ag powder was in the range of 30–300 nm.

Crystal structure determination on the basis of powder diffraction data frequently involves the question how the given diffraction data with some appreciably hkl-dependent line broadening should be interpreted. In many cases, such line broadening may either: (i) reasonably well be reconciled with a certain high-symmetry structure model or (ii) with a variant of the former with lower symmetry crystal family, which frequently will give a somewhat better fit in Rietveld refinement. In this work, it is shown mathematically that symmetry reduction induced reflection spitting masked by other line broadening contributions, thus leading to some reflection splitting-induced line broadening, shows a similar hkl dependence as typically adopted for anisotropic microstrain broadening with respect to the high-symmetry structure. This implies that Rietveld refinement on the basis of the low-symmetry model (including typically isotropic line broadening) and on the basis of the high-symmetry model with anisotropic microstrain broadening can both lead to similar qualities of the fit. Hence, the refinement results for both possibilities should be carefully considered in combination with possibly available additional information (e.g. results of first-principles calculations) to arrive at adequate conclusions concerning the true symmetry of the material under investigation.