Silver the new gold standard for high-pressure single crystal X-ray diffraction

Abstract

physicochemical properties through the application of pressure and temperature as a result of changes in crystal packing and distortion/ compression of coordination bonds. Measuring the structural changes of these complexes with relation to pressure and temperature allows for a greater insight into how these properties arise. Typically however it is difficult in current crystallographic studies to simultaneously alter the pressure and temperature of the experiment, due to the inherent difficulties associated with heating or cooling a diamond anvil cell, as well as difficulties in accurate and precise recording of the internal cell temperature. Successfully merging the fields of low-temperature and highpressure crystallography would however provide huge benefits to the study of structure-behaviour relationships. Low-temperature and highpressure studies could be performed simultaneously or consecutively using the same crystal and experimental setup, allowing for improved modelling of complicated multi-variable phase changes. Significant improvements in data quality would be observed for high pressure studies conducted at low temperatures due to reduced thermal and vibrational motion. Secondary radiation damage to crystals is also temperature dependant thus lower temperature acquisition will prolong the lifespan of crystals under high-pressure study [1]. The desire for this combined approach has thus necessitated the design of a novel diamond anvil cell which can be successfully implemented for highpressure low-temperature crystallographic studies.

Variation of M···H–C Interactions in Square-Planar Complexes of Nickel(II), Palladium(II), and Platinum(II) Probed by Luminescence Spectroscopy and X-ray Diffraction at Variable Pressure

“…Paraffin oil was used as a pressure medium. High-pressure single-crystal XRD data were collected at room temperature on a the XIPHOS II instrument at Newcastle University . This instrument was custom-built for high-pressure single-crystal XRD studies with an Incoatec Ag Iμs Kα (λ = 0.56086 Å) source.…”

“…High pressure X-ray single-crystal diffraction data were collected at room temperature on a the XIPHOS II instrument at Newcastle University. 56 This instrument was custom built for high pressure single crystal X-ray diffraction studies with an Incoatec Ag Iµs Kα (λ = 0.56086 Å) source. Data were collected, using 10 phi scans to maximise accessible coverage.…”

Expanding the Pyridine–Formic Acid Cocrystal Landscape under Extreme Conditions

“…The diamond anvil cell was directly attached to a goniometer head and mounted on the diffractometer. Data were collected using the XIPHOS II , diffractometer at Newcastle University, a four-circle Bruker diffractometer with a Ag–Kα IμS generator . The pressure inside the cell was measured after equilibration by the R 1 ruby fluorescence method .…”

High Pressure/Low Temperature Polymorphism in 2,6-Dimethylpyridine–Formic Acid Cocrystals

“…The sample was pressurized beyond the crystal growth pressure region in order to minimize melting during data collection. The DAC was mounted directly onto the goniometer of XIPHOS II, , a four circle Huber diffractometer with Ag–Kα IμS generator located at Newcastle University. High pressure data were handled using the Bruker APEX2 software suite, which incorporates SAINT and SADABS for integration, cell refinement, and scaling.…”