X-ray powder diffraction data for 3,3-dichloro-1-(4-nitrophenyl)-2-piperidinone, C11H10Cl2N2O3, are reported [a = 11.088(4) Å, b = 11.594(5) Å, c = 12.689(3) Å, α = 118.456(1)°, β = 100.320(3)°, γ = 107.763(3)°, V = 1259.27 Å3, Z = 4 and space group P-1 ]. All measured lines were indexed and are consistent with the P-1 space group. No detectable impurities were observed.

X-ray powder diffraction data, unit-cell parameters, and space group for beta-methyl vinyl phosphate (MAP), C29H27N2O10P, are reported [a = 17.293(4) Å, b = 6.142(6) Å, c = 14.464(8) Å, α = γ = 90°, β = 112.048(0)°, unit-cell volume V = 1424.19 Å3, Z = 2, and space group P21]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurity was observed.

Structural measurements have been performed on the La0.7Sr0.3Mn3+0.85Nb5+0.15O3 compound with oxidation state of manganese close to +3. The composition undergoes a structural transition from rhombohedral to orthorhombic symmetry below room temperature. The calculated structural parameters show that the orthorhombic phase is not long-range orbitally ordered and that the structural transition is associated with a steric effect. The compound is ferromagnetic with a Curie point of around 150 K and a magnetic moment of 3.1 μB/Mn. It is suggested that ferromagnetism is originated from superexchange interactions via oxygen. Covalence enhances the positive part of the superexchange interactions whereas structural disorder leads to suppression of ferromagnetism.

Single crystals of Ca0.9Nd0.1Ti0.9Al0.1O3 (CNTAO) were grown using optical floating zone technique and the grown crystals were characterized by Laue diffraction and powder X-ray diffraction techniques for crystal quality and its composition, respectively. The powder pattern of CNTAO was indexed and refined using GSAS program to an orthorhombic structure with space group Pbnm (#62), a = 5.3832(1), b = 5.4343(1), c = 7.6389(2) Å, V = 223.4677 Å3′, and Z = 4.

X-ray powder diffraction data, unit cell parameters, and space group for 1-methylhydantoin, C4H6N2O2, are reported [a = 5.6070(9) Å, b = 12.170(1) Å, c = 8.097(1) Å, β = 105.41(1), Z = 4, unit cell volume V = 532.66(9) Å3, with M20 = 50.2 and F30 = 62.2 (0.0082, 59)]. All measured lines were indexed and are consistent with the monoclinic P21/c space group.

New phosphates Ca9–xPbxEu(PO4)7 were obtained by solid state reaction techniques at 1213–1253 K in air atmosphere and were found to be isotypic with whitlockite-type β-Ca3(PO4)2. The unit cell parameters were determinate using Le Bail decomposition. Rietveld method structural refining showed that Eu3+ ions are located statistically with calcium in M1, M2, and M3 sites, whereas Pb2+-ions are preferentially located in the M3. Examination of optical second harmonic generation evidences nonlinear optical activity and confirms polar space group R3c.

X-ray powder diffraction data, unit cell parameters, and space group for a new organometallic compound, lanthanum trilactate trihydrate, LaC9H21O12, are reported [a = 9.986(1) Å, b = 9.158(1) Å, c = 11.200(1) Å, α = 115.08(1), β = 117.41(1), γ = 88.61(1), unit cell volume V = 804.70 Å3, Z = 2 and space group P1]. All measured lines were indexed. No detectable impurity was observed.

The method of degree of inversion calculation presented in the present paper was based on the determination of several temperature-dependent parameters such as: oxygen positional parameter, lattice parameter, cation site occupancies, and a cation–anion distance in tetrahedral and octahedral sites. The theoretical basis of the method as well as the required derivation of formulae and the conditions of its application has been described.

The values of the measured temperature-dependent parameters were used to calculate the degree of inversion vs. temperature in the spinel structure. Initial temperatures of the order–disorder transformation were determined. The described method of investigating the order–disorder phase transformation based on three examples of spinel solid solutions: Mg(Al0.5Fe0.5)2O4, (Mg0.75Ni0.25)Al2O4, and (Mg0.75Co0.25)Al2O4 has been presented. Investigations by means of the high-temperature X-ray diffraction method at temperatures ranging from 25 to 1100 °C were carried out. It has been shown that using the present method, it is possible to determine the distribution of each cation in tetrahedral and octahedral sites at each temperature. In consequence, the unidirectional order–disorder phase transformation as well the bidirectional transformation in the spinel structure can be investigated. The advantages and disadvantages of the method have been discussed and its uncertainties presented.

X-ray powder diffraction data, unit-cell parameters, and space group for calcium(II)–naproxen complex, C28H26CaO6·2H2O, are reported [a = 36.918(2) Å, b = 5.655(6) Å, c = 12.505(6) Å, β = 91.263(2)°, cell volume V = 2610.47 Å3, Z = 4, and space group C2]. All measured lines were indexed and are consistent with the C2 space group. No detectable impurities were observed.

Hydrothermally altered rocks hosting precious metal deposits frequently contain stacking disordered layer silicates. X-ray diffraction analysis using the Rietveld method can be used to determine mineral abundances in these rocks if suitable disorder models are applied. It is shown here that disorder models of kaolinite and pyrophyllite can be described by a recursive calculation of structure factors. This permits the physically sound refinement of real structure parameters of these disordered minerals and the determination of mineral abundances. Even mixtures containing two disordered Si–Al layer silicates can be quantified reliably. The developed disorder models can now be implemented in routine phase analysis, allowing the quantification of large numbers of samples to identify mineralogical gradients surrounding ore deposits.

The size of dopant-rich nanodomains was assessed in four samples of Ce1−μYμO2−μ/2 through systematic pair distribution function (PDF) refinements. Experimental G(r) curves were fitted by different structural models with the aim of finding a description which balanced precise structure parameterization and reasonable number of parameters. The most reliable model was a single Y2O3-like phase, which best accommodated to the close relationship between the fluorite (CeO2-like) and C-type (Y2O3-like) structures. In this model, a refined cation coordinate, x(M2), measured the relative occurrence in the G(r) of the chemical environment of Y and Ce at any value of r. The r-value at which x(M2) vanished, i.e. at which the refined C-type cell becomes a redundant, low-symmetry description of a fluorite cell, was assumed as the size of a C-type domain. Subtle features in G(r) could be attributed to the fluorite or C-type phase up to ~500 Å thanks to the narrow instrumental resolution function of the ID31 beamline (now ID22) at the ESRF, which allows us to get high resolution PDF data.

Hydrochlorothiazide (HCTZ) is a diuretic used for the treatment of blood pressure (hypertension). HCTZ has two anhydrous polymorphs denoted as Forms I and II. Aiming at solid-state characterization, X-ray powder diffraction (XRPD) is known to be a powerful technique which has been successfully applied in investigating polymorphism in medicines. In this work, three tablets of HCTZ (a reference and two generic) were analyzed. The data were collected using Rigaku RINT2000 diffractometer copper rotate anode. The Rietveld method (RM) was applied for the characterization of HCTZ polymorphic form. For the crystalline excipients where the crystal structure is known, their phases were identified by the RM either. The results showed that all the tablets exhibit Form I of HCTZ, while the excipient lactose monohydrate is found to exhibit the crystalline form. One of the generics is also found to exhibit the excipient sodium lauryl sulfate (SLS) in the crystalline form. Therefore, the RM and XRPD are an efficient methodology for characterization of the crystalline Form I of the active principle of HCTZ and crystalline excipients lactose monohydrate and SLS in solid formulations. It is also interesting to observe excipients not described in the package insert of the medicament.