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.

Surface roughness is a critical factor affecting the performance of dental implants. One approach to influence this is through sandblasted, large grit, acid-etched (SLA) modification on pure titanium implant surfaces. In this study, SLA was performed on grade IV pure titanium. Sandblasting was conducted at distances of 2, 4, and 6 cm. Subsequently, the samples were etched with a mixed acid solution of HCl, H2SO4, and H2O for 0, 30, and 60 min. Surface roughness and X-ray diffraction (XRD) characterizations were conducted on the samples. The results revealed that surface roughness increased but was not too significant as the sandblasting distance decreased. Longer etching durations for sandblasted with acid-etched samples led to reduced surface roughness (Sa and Sz). It was found that a 60 min-etched sample resulted in optimal Sa, Sz, and Ssk values, i.e., 1.19 μm, 13.76 μm, and −0.60, respectively. The XRD texture was significantly influenced by sandblasting, with compressive residual stress increasing as the sandblasting distance decreased. Normal stress causes hill formations at shorter sandblasting distances. For etched samples, the residual stress decreased with longer etching durations. Normal stress-decreasing trend aligns with the initial reduction in hill and valley within the samples and subsequent hill enhancement at extended etching duration.

Six different types of Majiang bronze drums from Hechi City, Guangxi, China were collected from the Guangxi Museum to characterize the original scheme of polychromy and materials used for the drums. The composition of all the samples were determined by using scanning electron microscopy with energy-dispersive X-ray spectroscopy. All the bronze drums contain mainly Cu, Sn, Pb, and As. Qualitative analysis of the structure by X-ray powder diffraction indicates that each of the six bronze drums contains four or five phases, namely (Cu, As), Pb, Cu3Sn, and Cu10Sn3 or Cu, Pb, As0.2Cu1.8, Cu3Sn, and Cu10Sn3. The Rietveld structural refinement is performed first time for the quantitative analysis of ancient bronze drums and inorganic cultural relics. This paper reports the result.

Equations are given which allow an analyst to obtain a correct absolute quantitative phase analysis via the internal standard method when a reference material with a known crystallinity of less than 100% is used. Comparisons are made with previous equations, and a numerical example is given.

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®)

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 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.

In this work, the synthesis, characterization, and X-ray powder diffraction data for dichloridodioxido-[(4,7-dimethyl)-1,10-phenanthroline]molybdenum(VI) are reported. The crystal structure of this compound was solved from powder diffraction data using the simulated annealing method with a subsequent refinement using the Rietveld method. The dioxo-molybdenum (VI) complex C14H12Cl2MoN2O2 crystallizes in a monoclinic system with space group C2/c (N° 15) with refined unit-cell parameters a = 12.9495 (5) Å, b = 9.7752 (4) Å,c = 12.0069 (6) Å, β = 101.702 (3) °, unit-cell volume V = 1488.27 (11) Å3, and values of Z′ = 0.5 and Z = 4. The molecules are organized into chains diagonally along the a and c axis. Parallel polyhedra are observed along these axes formed by the interactions of Mo, Cl, O, and N atoms present in the coordination sphere. The crystalline packing of this dioxo-molybdenum (VI) complex is dominated by five intermolecular hydrogen bonds, two intramolecular hydrogen bonds, and the four interactions between the centroids (CgI⋯CgJ) of the aromatic rings. An analysis of the Hirshfeld surface revealed that the greatest contributions of the attractive forces are given by H⋯Cl/Cl⋯H, H⋯C/C⋯H, H⋯O/O⋯H, and H⋯H interactions.

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.

The crystal structure of palbociclib (C24H29N7O2) used as a medication for the treatment of breast cancer has been solved and refined using synchrotron radiation after density functional theory optimization. Palbociclib crystallizes in the monoclinic system (space group P21/c, #14) at room temperature with crystal parameters: a = 11.3133(2), b = 5.62626(9), c = 35.9299(9) Å, β = 101.5071(12), V = 2241.03(8) Å3, and Z = 4. The crystal structure contains infinite N–H⋯N bonded layers. 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 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®).