Crystal structures of (Li0.925Eu3+0.025)TaO3, (Li0.968Eu3+0.032)(Ta0.81Ti0.19)O2.937, (Li0.967Sm3+0.033)(Ta0.89Ti0.11)O2.978, and (Li0.950Sm3+0.033Mg0.017)(Ta0.89Ti0.11)O2.987 were investigated by X-ray powder diffraction. The initial structural parameters, taken from those of the isomorphous compound (Li0.977Eu3+0.023)(Ta0.89Ti0.11)O2.968 (space group R3c and Z = 6), were refined by the Rietveld method. A pattern-fitting method based on the maximum-entropy method was subsequently used to determine the three-dimensional electron-density distributions (EDDs) that are free from the structural bias. We confirmed that the EDDs are in accord with the resulting structural models, each of which was composed of the [(Ta, Ti)O6] octahedron and [(Li, Eu, Sm, Mg)O12] polyhedron. We compared these polyhedra and found that the prominent difference among these compounds was the centroid-to-(Li, Eu, Sm, Mg) distance (eccentricity) of [(Li, Eu, Sm, Mg)O12]. The high correlation was demonstrated between the magnitude of eccentricity and photoluminescence intensity under near ultraviolet excitation.

The crystal structure of salmeterol xinafoate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Salmeterol xinafoate crystallizes in space group P−1 (#2) with a = 9.173 89(13), b = 9.483 79(14), c = 21.3666(4) Å, α = 82.2646(13), β = 85.2531(12), γ = 62.1565(11)°, V = 1628.37(5) Å3, and Z = 2. Key to the structure solution was linking the two fragments by a Li atom along the expected N–H···O hydrogen bond. The salmeterol cation and xinafoate anion are linked by N–H···O and O–H···O hydrogen bonds, interactions which cause the salmeterol to adjust its conformation. The hydrogen bonds result in complex chains along the b-axis. The powder pattern is included in the Powder Diffraction File™ as entry 00-065-1430.

A method is presented to examine consecutive in-situ X-ray diffraction (XRD) diffractograms using exploratory factor analysis. Systematic changes in the diffractograms are described numerically by score values that could be used to correlate diffraction data with other non-stationary sample properties. Phase and structure evolution in a reacting material can be studied by in-situ XRD. The consecutively collected data can be considered a time series of datasets. Time series are non-stationary data. Such non-stationary data are often hard to examine fully by conventional evaluation methods including applications of the Rietveld method. Here a method is presented to avoid shortcomings of conventional evaluation methods. The new method helps to identify and describe significant systematic changes in in-situ XRD datasets by numerical values. These systematic changes can represent structural changes as well as changes in phase composition. The method can be used to describe the development of the complex processes of compositional and structural changes. The method is demonstrated using the example of a hydrating Portland cement mortar. This hydration process involves at least 11 phases including non-crystalline phases. In the presented example factor analysis of in-situ XRD data results in three variables (factors) describing the observed changes numerically.

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.

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 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.

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.

X-ray powder diffraction data for 1-(4-Nitrophenyl)-2-piperidinone, C11H12N2O3, are reported [a = 9.514(3) Å, b = 12.308(6) Å, c = 9.175(1) Å, α = 90°, β = 91.811(2)°, γ = 90°, V = 1073.94 Å3, Z = 4, ρcal = 1.362 g cm−3 and space group P21/n]. All measured lines were indexed and are consistent with the P21/n space group. No detectable impurities were observed.

X-ray powder diffraction data for 1-(4-aminophenyl)-5,6-dihydro-3-(4-morpholinyl)-2(1H)-pyridinone, C15H19N3O2, are reported [a = 14.877(4) Å, b = 5.893(6) Å, c = 18.984(3) Å, α = 90°, β = 122.298(3)°, γ = 90°, unit-cell volume V = 1406.86 Å3, Z = 4, and space group P21/c]. All measured lines were indexed and are consistent with the P21/c space group. No detectable impurities were observed.

X-ray powder diffraction data for 3-(4-Morpholinyl)-1-(4-nitrophenyl)-5,6-dihydro-2(1H)-pyridinone, C15H17N3O4, are reported [a = 7.112(1) Å, b = 33.360(2) Å, c = 6.265(1) Å, α = 90°, β = 94.037(1)°, γ = 90°, V = 1483.08 Å3, Z = 4, ρcal = 1.358 g cm−3 and space group P21]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurities were observed.

The room-temperature crystal structure of levothyroxine sodium pentahydrate has been refined using synchrotron powder diffraction data. The compound crystallizes in space group P1 (#1) with a = 8.2489(4), b = 9.4868(5), c = 15.8298(6) Å, α = 84.1387(4), β = 83.1560(3), γ = 85.0482(3) deg, V = 1220.071(9) Å3, and Z = 2. Hydrogen atoms (missing from the previously-reported structure) were included.

X-ray powder diffraction data, unit-cell parameters, and space group for letrozole, C17H11N5, are reported [a = 7.034(0) Å, b = 16.177(5) Å, c = 13.411(3) Å, α = γ = 90°, β = 105.71(9)°, unit-cell volume V = 1469.0(3) Å3, Z = 4, and space-group P21/c]. All measured lines were indexed and are consistent with the P21/c space group. No detectable impurity was observed.

Experimental X-ray powder diffraction data, unit-cell parameters, and space group for niclosamide, C13H8N2O4Cl2, are reported [a = 13.571(1) Å, b = 7.181(8) Å, c = 13.742(3) Å, β = 97.984(7)°, unit-cell volume V = 1326.40 Å3, Z = 4, and space group P21/c]. All measured lines were indexed and are consistent with the P21/c space group. No detectable impurity was observed.