XIPHOS has been developed to expand home laboratory facilities closer to those found at central facilities, offering extremes of sample environment and flux densities far greater than standard laboratory sources. The system has a minimum operating temperature of 1.9 K, and has a direct‐drive molybdenum rotating‐anode generator coupled with the latest multilayer optics. XIPHOS has been specifically designed to accommodate various sample environments and is now operational. Furthermore, it has been calibrated with structural phase transitions from 14 to 148 K. Results are also presented from a full low‐temperature data collection of m‐nitroaniline to demonstrate the quality of results attainable from XIPHOS.

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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.

X-ray diffraction experiments at very low temperatures require samples to be isolated from atmospheric conditions and held under vacuum. These conditions are usually maintained via the use of beryllium chambers, which also scatter X-rays, causing unwanted contamination of the sample's diffraction pattern. The removal of this contamination requires novel data-collection and processing procedures to be employed. Herein a new approach is described, which utilizes the differences in origin of scattering vectors from the sample and the beryllium to eliminate non-sample scattering. The program Masquerade has been written to remove contaminated regions of the diffraction data from the processing programs. Coupled with experiments at different detector distances, it allows for the acquisition of decontaminated data. Studies of several single crystals have shown that this approach increases data quality, highlighted by the improvement in internal agreement factor with the test case of cytidine presented herein. research papers J. Appl. Cryst. (2012). 45, 292-298 J. A. Coome et al. Masquerade 293 Figure 1Calculating the distance between the crystal and the shroud wall, n. The crystal position is at point A, the shroud wall is at point B, and the PIP of the Be reflection is at point C. S 1 is the vector from the crystal position to the PIP, with components S 1 ðxÞ, S 1 ðyÞ and S 1 ðzÞ. 2 Be is the angle between the direct beam and the vector from the PIP to the shroud wall.

Ultra-low temperature structure determination of a Mn 12 single-molecule magnet and the interplay between lattice solvent and structural disorder3{