The crystal structure of flumethasone has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Flumethasone crystallizes in space group P21 (#4) with a = 6.46741(5), b = 24.91607(20), c = 12.23875(11) Å, β = 90.9512(6)°, V = 1971.91(4) Å3, and Z = 4 at 298 K. The crystal structure consists of O–H⋯O hydrogen-bonded double layers of flumethasone molecules parallel to the ac-plane. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

Sample transparency aberration in Bragg–Brentano geometry affected by interference with opaque and translucent sample holders has been formulated. The formulation for an opaque sample holder should be classified to 5 cases, depending on the apparent diffraction angle, beam width, specimen width, and specimen thickness. The cumulants of the aberration function for a translucent sample holder with an arbitrary linear attenuation coefficient can numerically be evaluated by a Gauss–Legendre quadrature. The use of a function defined by the convolution of truncated exponential and rectangular functions has been tested as the model for the aberration function. A double deconvolutional treatment (DCT) designed to cancel the effects of the first and third order cumulants of the aberration function has been applied to the XRD data of Si standard powder, NIST SRM640d. The diffraction peak profile in the data treated by the DCT method certainly shows improved symmetry. The main features of the symmetrized peak profile in the DCT data have been simulated by instrumental and specimen parameters. It is suggested that the current analytical method could be utilized for texture analysis, if the manufacturer of an XRD instrument should supply a more accurate information about the instrument.

The crystal structure of diroximel fumarate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Diroximel fumarate crystallizes in space group P-1 (#2) with a = 6.12496(15), b = 8.16516(18), c = 12.7375(6) Å, α = 85.8174(21), β = 81.1434(12), γ = 71.1303(3)°, V = 595.414(23) Å3, and Z = 2 at 298 K. The crystal structure consists of interleaved double layers of hook-shaped molecules parallel to the ab-plane. The side chains form the inner portion of the layers, and the rings comprise the outer surfaces. There are no classical hydrogen bonds in the structure, but 9 C▬H⋯O hydrogen bonds contribute to the crystal energy. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of etrasimod has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Etrasimod crystallizes in space group P1 (#1) with a = 10.6131(5), b = 10.7003(5), c = 11.1219(8) Å, α = 72.756(2), β = 76.947(2), γ = 77.340(1)°, V = 1159.28(6) Å3, and Z = 2 at 298 K. The crystal structure contains O▬H⋯O hydrogen-bonded etrasimod dimers, which lie in layers approximately parallel to the (2,0,−1) plane. The amino group of each molecule forms an intramolecular N▬H⋯O hydrogen bond to the carbonyl group of the adjacent carboxylic acid group. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The room-temperature X-ray powder diffraction data for bosentan monohydrate, an API used in the treatment of pulmonary arterial hypertension, is presented. Bosentan monohydrate is monoclinic, P21/c (No. 14), with unit cell parameters a = 12.4520(7) Å, b = 15.110(1) Å, c = 15.0849(9) Å, β = 95.119(5)°, V = 2827.0(3) Å3, Z = 4. All the diffraction maxima recorded were indexed and are consistent with the P21/c space group. The crystal structure of this material corresponds to the phase associated with Cambridge Structural Database entry NEQHEY, which was determined at 123 K. The successful Rietveld refinement, carried out with TOPAS-Academic, showed the single-phase nature of the material and the good quality of the data. A comprehensive analysis of intra- and intermolecular interactions corroborates that the structure is dominated by extensive hydrogen bonding, accompanied by C▬H⋯π and π⋯π interactions. Hirshfeld surface analysis and fingerprint plots indicate that the most important interactions are H⋯H and O⋯H/H⋯O in bosentan and the water molecule and C⋯H/H⋯C interactions in bosentan.

The magnetostrictive response of a Terfenol-D pellet was measured via a laboratory-based X-ray diffractometer. X-ray diffraction patterns were collected from the pellet sample with and without the presence of an applied magnetic field (~30 mT) generated by placing a large magnet under the pellet. A standard reference material, Silicon 640c, was employed as an internal standard. Magnetostriction values of 323 and 227 ppm Δl/l were determined for the (104) and (110) indexed peaks, respectively, assuming a rhombohedral structure for Terfenol-D. A threshold noise level value of ~20 to 30 ppm Δl/l was suggested based on before/after measurements in the absence of the applied field. No clear evidence of domain wall rotation was detected via changes in relative intensities of diffraction peaks in the presence of the applied magnetic field.

Molnupiravir Form I crystallizes in space group C2 (#5) with a = 6.48110(17), b = 8.71848(19), c = 27.0607(19) Å, β = 91.920(4)°, V = 1528.22(12) Å3, and Z = 4 at 295 K. The crystal structure consists of supramolecular double layers of molecules parallel to the ab-plane. The layer centers consist of hydrogen-bonded rings forming a 2D network and the outer surfaces of isopropyl groups, with van der Waals interactions between the layers. Each O atom acts as an acceptor in at least one hydrogen bond. A strong O–H⋯O hydrogen bond forms between the hydroxyl group of the oxolane ring and the carbonyl group of the oxopyrimidine ring. The other oxolane hydroxyl group forms bifurcated intra- and intermolecular hydrogen bonds. The hydroxylamino group forms an intramolecular O–H⋯N hydrogen bond with an N atom of the oxopyrimidine ring. The amino group forms an intermolecular N–H⋯N hydrogen bond to the same N atom of the ring. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

We present a simple analytical formalism based on the Lorentz-Scherrer equation and Bernoulli statistics for estimating the fraction of crystallites (and the associated uncertainty parameters) contributing to all finite Bragg peaks of a typical powder pattern obtained from a static polycrystalline sample. We test and validate this formalism using numerical simulations, and show that they can be applied to experiments using monochromatic or polychromatic (pink-beam) radiation. Our results show that enhancing the sampling efficiency of a given powder diffraction experiment for such samples requires optimizing the sum of the multiplicities of reflections included in the pattern along with the wavelength used in acquiring the pattern. Utilizing these equations in planning powder diffraction experiments for sampling efficiency is also discussed.

The crystal structure of cariprazine dihydrochloride has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Cariprazine dihydrochloride crystallizes in space group P21/n (#14) with a = 27.26430(14), b = 7.29241(1), c = 12.80879(4) Å, β = 99.5963(2)°, V = 2511.038(8) Å3, and Z = 4 at 295 K. The crystal structure consists of layers of cations parallel to the bc-plane. The cations stack along the b-axis. Each H atom on the two protonated N atoms participates in a discrete N–H⋯Cl hydrogen bond. One Cl anion acts as an acceptor in two of these bonds, while the other Cl is an acceptor in only one bond. The result is to link the cations and anions into columns parallel to the b-axis. The powder pattern has been submitted to the ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of benserazide hydrochloride Form I has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Benserazide hydrochloride Form I crystallizes in space group P21/n (#14) with a = 19.22983(15), b = 14.45066(10), c = 4.57982(2) Å, β = 93.6935(3), V = 1270.014(15) Å3, and Z = 4 at 295 K. The crystal structure contains pairs of hydrogen-bonded benserazide cations, which are hydrogen bonded to chloride anions, resulting in chains along the c-axis. In addition, O–H⋯Cl, N–H⋯O, O–H⋯N, and O–H⋯O hydrogen bonds link the cations and anions into a three-dimensional framework. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

A proposed crystal structure of lifitegrast Form A has been derived using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Lifitegrast sesquihydrate Form A crystallizes in space group P21 (#4) with a = 18.2526(4), b = 5.15219(6), c = 30.1962(6) Å, β = 90.8670(19), V = 2839.35(7) Å3, and Z = 4 at 295 K. The crystal structure consists of discrete lifitegrast molecules linked by hydrogen bonds among carboxylic acid groups, carbonyl groups, and water molecules into a three-dimensional framework. The water molecules occur in clusters. Each water molecule acts as a donor in two O–H⋯O hydrogen bonds, and as an acceptor. One water molecule acts as an acceptor in a water–water O–H⋯O hydrogen bond, and all three water molecules are acceptors in C–H⋯O hydrogen bonds. Each carboxylic acid group acts as a donor in a strong discrete O–H⋯O hydrogen bond; one to a water molecule and the other to a carbonyl group. The amino groups both form N–H⋯O hydrogen bonds to carbonyl groups. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

The crystal structure of decoquinate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Decoquinate crystallizes in space group P21/n (#14) with a = 46.8261(5), b = 12.94937(12), c = 7.65745(10) Å, β = 91.972(1), V = 4640.48(7) Å3, and Z = 8 at 295 K. The crystal structure consists of alternating layers of hydrocarbon chains and ring systems along the a-axis. Hydrogen bonds link the ring systems along the b-axis. The rings stack along the c-axis. The two independent decoquinate molecules have very different conformations, one of which is typical and the other has an unusual orientation of the decyl chain with respect to the hydroxyquinoline ring system, facilitating chain packing. The powder pattern has been submitted to the ICDD for inclusion in the Powder Diffraction File™ (PDF®).

Ba2Bi0.572TeO6±δ and SrLa2NiFeNbO9 ceramics were prepared in polycrystalline form by conventional solid-state reaction techniques in air. The crystal structures of the title compounds were determined at room temperature from X-ray powder diffraction (XRPD) data using the Rietveld method. The Ba2Bi0.572TeO6±δ structure crystallizes in a triclinic space group I–1 with unit-cell parameters a = 6.0272(2) Å, b = 6.0367(1) Å, c = 8.5273(3) Å, α = 90.007(7)°, β = 90.061(2)°, and γ = 90.015(4)°. The tilt system of the BiO6 and TeO6 octahedra corresponds to the notation a–b–c–. The crystal structure of the SrLa2NiFeNbO9 compound adopts an orthorhombic Pbnm space group with lattice parameters a = 5.6038(5) Å, b = 5.5988(4) Å, and c = 7.9124(6) Å. The BO6 octahedra (B = Ni/Fe/Nb) sharing the corners in 3D. Along the c-axis, the octahedra are connected by O(1) atoms of (x,y,1/4) positions; while in the ab-plane, they are linked by O(2) atoms of (x,y,z) positions. The bond angle of B–O1–B is 168.7° and that of B–O2–B is 156.3°. The octahedral lattice corresponds to the tilt pattern a–a–c+; it indicates that the octahedra tilt out-of-phase along the a,b-axes and in phase along the c-axis.

The crystal structure of gepirone has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Gepirone crystallizes in space group P21/a (#14) with a = 16.81794(14), b = 11.71959(5), c = 10.10195(4) Å, β = 95.7012(5)°, V = 1981.239(14) Å3, and Z = 4 at 298 K. The crystal structure consists of discrete gepirone molecules. There are no classical hydrogen bonds in the crystal structure, but several intra- and intermolecular C–H⋯N and C–H⋯O hydrogen bonds contribute to the lattice energy. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

The previously unindexed laboratory X-ray powder diffraction data of mosapride dihydrogen citrate dihydrate, an API used to stimulate gastrointestinal motility, has been recorded at room temperature. Using these data, the crystal structure of this API has been refined in space group P21/c (No. 14) with a = 18.707(4) Å, b = 9.6187(1) Å, c = 18.2176(4) Å, β = 114.164(1)°, V = 2990.74(8) Å3, and Z = 4. The structure of this material corresponds to the phase associated with CSD Refcode LUWPOL determined at 93 K. The Rietveld refinement, carried out with TOPAS-Academic, proved the single nature of the sample and the quality of the data recorded.

The crystal structure of perfluorononanoic acid (PFNA) was solved via parallel tempering using synchrotron powder diffraction data obtained from the Brockhouse X-ray Diffraction and Scattering (BXDS) Wiggler Lower Energy (WLE) beamline at the Canadian Light Source. PFNA crystallizes in monoclinic space group P21/c (#14) with lattice parameters a = 26.172(1) Å, b = 5.6345(2) Å, c = 10.9501(4) Å, and β = 98.752(2)°. The crystal structure is composed of dimers, with pairs of PFNA molecules connected by hydrogen bonds via the carboxylic acid functional groups. The Rietveld-refined structure was compared to a density functional theory-optimized structure, and the root-mean-square Cartesian difference was larger than normally observed for correct powder structures. The powder data likely exhibited evidence of disorder which was not successfully modeled.

Physical vapor deposited (PVD) molybdenum disulfide (nominal composition MoS2) is employed as a thin film solid lubricant for extreme environments where liquid lubricants are not viable. The tribological properties of MoS2 are highly dependent on morphological attributes such as film thickness, orientation, crystallinity, film density, and stoichiometry. These structural characteristics are controlled by tuning the PVD process parameters, yet undesirable alterations in the structure often occur due to process variations between deposition runs. Nondestructive film diagnostics can enable improved yield and serve as a means of tuning a deposition process, thus enabling quality control and materials exploration. Grazing incidence X-ray diffraction (GIXRD) for MoS2 film characterization provides valuable information about film density and grain orientation (texture). However, the determination of film stoichiometry can only be indirectly inferred via GIXRD. The combination of density and microstructure via GIXRD with chemical composition via grazing incidence X-ray fluorescence (GIXRF) enables the isolation and decoupling of film density, composition, and microstructure and their ultimate impact on film layer thickness, thereby improving coating thickness predictions via X-ray fluorescence. We have augmented an existing GIXRD instrument with an additional X-ray detector for the simultaneous measurement of energy-dispersive X-ray fluorescence spectra during the GIXRD analysis. This combined GIXRD/GIXRF analysis has proven synergetic for correlating chemical composition to the structural aspects of MoS2 films provided by GIXRD. We present the usefulness of the combined diagnostic technique via exemplar MoS2 film samples and provide a discussion regarding data extraction techniques of grazing angle series measurements.

Crystal structures, microtopography, morphologies, elemental compositions, and ionic conductivity have been investigated for Li5-xLa3(Nb,Ta)O12-y using X-ray diffraction (XRD), field-emission analytical scanning and transmission electron microscopies (S/TEM), and electrochemical impedance spectroscopy. Using Rietveld refinements with powder XRD patterns, we determined that the number of Li atoms in the formula is less than 5 and that Li5-xLa3(NbTa)O12-y crystallizes in the cubic garnet structure with a space group Ia-3d. Sintering at varying temperatures (750–1000 °C) for 5 h in an ambient atmosphere produced distinct outcomes. Rietveld refinements disclosed that the sample sintered at 1000 °C (Li3.43(2)La3Nb1.07(2)Ta0.93(2)O12-y, a = 12.8361(7) Å, V = 2114.96(3) Å3) exhibited the highest ionic conductivity, while the 850 °C sample had the lowest conductivity, characterized by lower Li concentration and impurity phases (Li(Nb,Ta)3O88, Li2CO3). Analyses, including XRD and electron microscopy, confirmed the 1000 °C sample as a relatively phase pure with enhanced Li content (Li/La = 1.2), larger grains (15 μm), and uniform crystallinity. The 1000 °C sample introduced additional partially filled Li3 (96h) sites, promoting Li migration, and enhancing ionic conductivity. The resulting XRD pattern at 1000 °C has been submitted to the Powder Diffraction File as a reference.

The crystal structure of ribociclib hydrogen succinate (commonly referred to as ribociclib succinate) has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Ribociclib hydrogen succinate crystallizes in space group P-1 (#2) with a = 6.52215(4), b = 12.67120(16), c = 18.16978(33) Å, α = 74.0855(8), β = 82.0814(4), γ = 88.6943(1)°, V = 1430.112(6) Å3, and Z = 2 at 295 K. The crystal structure consists of alternating layers of cations and anions parallel to the ab-plane. The protonated N in each ribociclib cation acts as a donor in two strong N–H⋯O hydrogen bonds to two different succinate anions. Strong O–H⋯O hydrogen bonds link the hydrogen succinate anions into chains parallel to the a-axis. N–H⋯N hydrogen bonds link the cations into dimers, with a graph set R2,2(8). The result is a three-dimensional hydrogen bond network. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®)

The crystal structure of acalabrutinib dihydrate Form III has been refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Acalabrutinib dihydrate Form III crystallizes in space group P21 (#4) with a = 8.38117(5), b = 21.16085(14), c = 14.12494(16) Å, β = 94.5343(6)°, V = 2497.256(20) Å3, and Z = 4 (Z′ = 2) at 295 K. The crystal structure consists of herringbone layers parallel to the ac-plane. Hydrogen bonds between the acalabrutinib and water molecules generate a three-dimensional framework. Each water molecule acts as a donor in two hydrogen bonds and as an acceptor in at least one hydrogen bond. Amino groups and pyridine N atoms link the acalabrutinib molecules into dimers. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).