A new non-stoichiometric calcium ruthenate [Ca4−xRuO6−x with x = 1.17(1)] was synthesized by the flux growth method and characterized by the X-ray powder diffraction. The crystal structure is isostructural to the K4CdCl6 type with space group R$\bar 3$c. Unit-cell parameters are a = 9.2881(1), c = 11.1634(2) Å, V = 834.03(3) Å3, and Z = 6.

Recipes are given to assist in setting up rigid bodies for common molecules and coordination polyhedra, to define satellite groups, to perform rotations around arbitrary axes through the origin of the rigid body, and to refine intramolecular degrees of freedom under consideration of the special needs of powder diffraction. To the greatest possible extent, the notation follows that of the well known Rietveld refinement program GSAS (Larson and Von Dreele, 1994).

A modified method for polynomial smoothing and the calculation of derivatives of equally spaced step scan powder diffraction data is presented. The algorithm takes the angular dependence of the full width at half maximum (FWHM) of diffraction peaks into account, is very effective, and easy to code.

The characteristics of the (101) peak of α-quartz and the (104) peak of the NIST SRM 1976 alumina flat plate standard have been measured in dependence of time for 60 h with Cu-Kα1 radiation in Bragg-Brentano geometry with a Philips X’Pert diffractometer equipped with a primary Ge(111) monochromator. It was found that the reproducibility of the peak position and the peak shape falls well in the ±3σ range, whereas the peak intensity strongly depends on the power history of the X-ray generator and the temperature of the diffraction system. The effects on Rietveld refinements are discussed and recommendations are given for optimized data collection.

In the course of an investigation of cracks in certain magnesia floors containing the mineral chlorartinite [Mg2(CO3)(H2O)(OH)]Cl·H2O, the dehydration process of chlorartinite was carried out in high vacuum. The crystal structure of dehydrated chlorartinite [Mg2(CO3)(H2O)(OH)]Cl was refined from laboratory X-ray powder diffraction data using the Rietveld method [R3c, a=22.6791(5) Å, c=7.22336(14) Å, V=3217.52(11) Å3, Z=18, Rp=4.13%, Rwp=5.82%]. Dehydrated chlorartinite exhibits the same type of 3D honeycomb zeolite-like crystal structure with large channels as the hydrated form. Compared to the hydrated form, the channels of dehydrated chlorartinite are empty because of the removal of all non-coordinating water molecules with the cell volume shrinking by 4.0%, leading to a more distorted environment of the magnesium atoms.

The solid-state phase transformation from α- to β-copper phthalocyanine, using isothermal data obtained at T=250 °C and nonisothermal data obtained in the temperature range of 30 °C≤T≤330 °C with a constant heating rate of 1.67 °/min, was investigated by sequential and parametric full quantitative Rietveld analyses. Results obtained in this study show that the parametric Rietveld refinement technique is most suitable and applicable for kinetic studies of isothermal powder diffraction data. On the other hand, the sequential Rietveld refinement technique can give reliable results for the kinetic analysis of nonisothermal data. The main advantages of the parametric Rietveld refinement over the sequential Rietveld refinement are increased robustness against outliers, low weight fractions, and noisy data and an increase in computational speed.