We discuss the use of regression diagnostics combined with nonlinear least-squares to refine cell parameters from powder diffraction data, presenting a method which minimizes residuals in the experimentally-determined quantity (usually 2θhkl or energy, Ehkl). Regression diagnostics, particularly deletion diagnostics, are invaluable in detection of outliers and influential data which could be deleterious to the regressed results. The usual practice of simple inspection of calculated residuals alone often fails to detect the seriously deleterious outliers in a dataset, because bare residuals provide no information on the leverage (sensitivity) of the datum concerned. The regression diagnostics which predict the change expected in each cell constant upon deletion of each observation (hkl reflection) are particularly valuable in assessing the sensitivity of the calculated results to individual reflections. A new computer program, implementing nonlinear regression methods and providing the diagnostic output, is described.

Lattice parameters of synthetic titanite powder, CaTiOSiO4, have been determined between room temperature and 1023 K. Only the e11 and e13 components contribute significantly to the strain tensor associated with the antiferroelectric-paraelectric phase transition at Tc = 487 K. A finite strain component e13 is observed in the paraelectric phase for 487 K < T < 825 K. The disappearance of this shear strain marks the isosymmetric transition near 825 K. The temperature evolution of the volume strain and of e11 is proportional to the squared order parameter observed in single-crystal diffraction experiments. The magnitude of the volume strain is sufficiently large to relate the observed near tricritical behaviour of the antiferroelectric-paraelectric phase transition to strain coupling.

Nanocrystalline anatase powders synthesised by various chemical processes as super/subcritical fluid extraction, sol-gel technique and hydrolysis of titanium alkoxides in hydrogen peroxide were studied by X-ray diffraction (XRD) whole profile modelling method (WPPM) in order to reveal correlations between structural and micro-structural parameters as well as sample treatment conditions. Anisotropy of the diffraction line broadening due to truncated bipyramidal shape of anatase crystals was discussed. The hkl-anisotropy can be very strong but also almost negligible in dependence on relative ratio of the crystallite dimensions. The latter was the case for the studied samples. The size of synthesised anatase nanoparticles was within the range 3–25 nm. The theoretical total surface area of crystallites calculated from XRD was in a good correlation with the surface area measured by the nitrogen physisorption up to the temperature 400–450 °C, when the particles started to agglomerate. At atomic scale a unit cell volume contraction with decreasing crystallite size and a significant deficiency in the Ti-site occupancy was observed. Both effects were attributed to the presence of Ti-vacancies and a linear coefficient between the relative cell volume contraction and the fraction of Ti-vacancies was estimated to (–0.017 ± 0.003).

X-ray powder diffraction data for buckminsterfullerene, C60 are reported. The crystal structure is a face-centered cubic unit cell with a = 14.165 (1) Å. The reference intensity ratio (I/Icor) is 2.20.

The lattice parameters of α-alumina have been determined for temperatures in the range 20<T<1050 °C, using the lattice parameter of tungsten as a thermometer and a simple furnace in the diffractometer on the Australian beamline at the Photon Factory, Tsukuba, Japan. It is shown that the accuracy of this technique for measurement of cell parameters at temperatures up to ∼1200 °C is limited at present by uncertainty in the cell parameters of the reference material (i.e., tungsten) at high temperatures. Some problems with the equipment are discussed.