A laser heating system for samples confined in diamond anvil cells paired with in situ X-ray diffraction measurements at the Extreme Conditions Beamline of PETRA III is presented. The system features two independent laser configurations (on-axis and off-axis of the X-ray path) allowing for a broad range of experiments using different designs of diamond anvil cells. The power of the continuous laser source can be modulated for use in various pulsed laser heating or flash heating applications. An example of such an application is illustrated here on the melting curve of iron at megabar pressures. The optical path of the spectroradiometry measurements is simulated with ray-tracing methods in order to assess the level of present aberrations in the system and the results are compared with other systems, that are using simpler lens optics. Based on the ray-tracing the choice of the first achromatic lens and other aspects for accurate temperature measurements are evaluated.

The crystal structure of L-threonine has been studied to a maximum pressure of 22.3 GPa using single-crystal X-ray and neutron powder diffraction. The data have been interpreted in the light of previous Raman spectroscopic data by Holanda et al. (J. Mol. Struct. (2015), 1092, 160–165) in which it is suggested that three phase transitions occur at ca. 2 GPa, between 8.2 and 9.2 GPa and between 14.0 and 15.5 GPa. In the first two of these transitions the crystal retains its P2₁2₁2₁ symmetry, in the third, although the unit cell dimensions are similar either side of the transition, the space group symmetry drops to P2₁. The ambient pressure form is labelled phase I, with the successive high-pressure forms designated I′, II and III, respectively. Phases I and I′ are very similar, the transition being manifested by a slight rotation of the carboxylate group. Phase II, which was found to form between 8.5 and 9.2 GPa, follows the gradual transformation of a long-range electrostatic contact becoming a hydrogen bond between 2.0 and 8.5 GPa, so that the transformation reflects a change in the way the structure accommodates compression rather than a gross change of structure. Phase III, which was found to form above 18.2 GPa in this work, is characterised by the bifurcation of a hydroxyl group in half of the molecules in the unit cell. Density functional theory (DFT) geometry optimisations were used to validate high-pressure structural models and PIXEL crystal lattice and intermolecular interaction energies are used to explain phase stabilities in terms of the intermolecular interactions.

The crystal structure of 4-iodobenzonitrile, which is monoclinic (space group I2/a) under ambient conditions, contains chains of molecules linked through C≡N···I halogen-bonds. The chains interact through CH···I, CH···N and π-stacking contacts. The crystal structure remains in the same phase up to 5.0 GPa, the b axis compressing by 3.3%, and the a and c axes by 12.3 and 10.9 %. Since the chains are exactly aligned with the crystallographic b axis these data characterise the compressibility of the I···N interaction relative to the inter-chain interactions, and indicate that the halogen bond is the most robust intermolecular interaction in the structure, shortening from 3.168(4) at ambient pressure to 2.840(1) Å at 5.0 GPa. The π∙∙∙π contacts are most sensitive to pressure, and in one case the perpendicular stacking distance shortens from 3.6420(8) to 3.139(4) Å. Packing energy calculations (PIXEL) indicate that the π∙∙∙π interactions have been distorted into a destabilising region of their potentials at 5.0 GPa. The structure undergoes a transition to a triclinic ( $P\overline{1}$ ) phase at 5.5 GPa. Over the course of the transition, the initially colourless and transparent crystal darkens on account of formation of microscopic cracks. The resistance drops by 10% and the optical transmittance drops by almost two orders of magnitude. The I···N bond increases in length to 2.928(10) Å and become less linear [<C−I∙∙∙N = 166.2(5)°]; the energy stabilises by 2.5 kJ mol⁻¹ and the mixed C-I/I..N stretching frequency observed by Raman spectroscopy increases from 249 to 252 cm⁻¹. The driving force of the transition is shown to be relief of strain built-up in the π∙∙∙π interactions rather than minimisation of the molar volume. The triclinic phase persists up to 8.1 GPa.

The phase behavior of rhodium (Rh) metal has been studied to 191 GPa and 2700 K using a combination of room-temperature isothermal compression and double-sided flash laser heating experiments. The isothermal compression data have been fitted with a second-order adapted polynomial of order L equation of state (EoS) with best-fitting parameters of $V_0=13.764\left(2\right){\AA }^3/\mathrm{atom}$, $K_0=258\left(3\right)\mathrm{GPa},$ and $K^{\prime }=5.36\left(9\right)$. Two-dimensional maps of the uniaxial stress component $t$ are presented for Rh at different pressures showing the spatial distribution of the local stress state of a relatively high-yield strength material encased in a Bi pressure medium. In addition, a simple, thermal pressure equation-of-state model, based on a single Einstein temperature, has been fitted to the high-pressure-temperature data up to 2700 K at 148 GPa and ambient-pressure thermal expansion data up to 1982 K. Also determined are the best-fitting parameters to reproduce the thermal EoS within the dioptas two-dimensional integration software. The optimized dioptas parameters are $V_0=13.764{\AA }^3/\mathrm{atom}$, $K_0=260.54\mathrm{GPa}$, $K^{\prime }=5.114$, ${\alpha }_T=2.99\times {10}^{-5}$ ${\mathrm{K}}^{-1}$, $\partial {\alpha }_T/\partial T=1.27\times {10}^{-9}$ ${\mathrm{K}}^{-2}$, $\partial K_0/\partial T=-6.43\times {10}^{-5}\mathrm{GPa}/\mathrm{K}$, and $\partial K^{\prime }/\partial T=-9.3\times {10}^{-10}{\mathrm{K}}^{-1}$.