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Instruments / Technical Area	Publication Details	Published
I15-Extreme Conditions	Characterization of the high-pressure and high-temperature phase diagram and equation of state of chromium Simone Anzellini , Daniel Errandonea , Leonid Burakovsky , John E. Proctor , Robin Turnbull , Christine M. Beavers Scientific Reports 12 DOI: 10.1038/s41598-022-10523-2 Diamond Proposal Number(s): [26452, 28469] Open Access Show Abstract ▼ Abstract: The high-pressure and high-temperature phase diagram of chromium has been investigated both experimentally (in situ), using a laser-heated diamond-anvil cell technique coupled with synchrotron powder X-ray diffraction, and theoretically, using ab initio density-functional theory simulations. In the pressure–temperature range covered experimentally (up to 90 GPa and 4500 K, respectively) only the solid body-centred-cubic and liquid phases of chromium have been observed. Experiments and computer calculations give melting curves in agreement with each other that can both be described by the Simon–Glatzel equation 𝑇𝑚(𝑃)=2136𝐾(1+𝑃/25.9)0.41 T m ( P ) = 2136 K ( 1 + P / 25.9 ) 0.41 . In addition, a quasi-hydrostatic equation of state at ambient temperature has been experimentally characterized up to 131 GPa and compared with the present simulations. Both methods give very similar third-order Birch–Murnaghan equations of state with bulk moduli of 182–185 GPa and respective pressure derivatives of 4.74–5.15. According to the present calculations, the obtained melting curve and equation of state are valid up to at least 815 GPa, at which pressure the melting temperature is 9310 K. Finally, from the obtained results, it was possible to determine a thermal equation of state of chromium valid up to 65 GPa and 2100 K.	Apr 2022
Accelerator Physics	High-energy adventures at Diamond Light Source Thomas Connolley , Christine M. Beavers , Philip Chater Synchrotron Radiation News 33, 31 - 36 DOI: 10.1080/08940886.2020.1841494 Open Access Show Abstract ▼ Abstract: Diamond Light Source (DLS), the United Kingdom’s national synchrotron facility, is located on the campus of Rutherford Appleton Lab (RAL) in southern Oxfordshire. DLS is jointly funded by the Science and Technology Facilities Council (STFC) within UK Research and Innovation (UKRI) and the Wellcome Trust. Designed as a successor to the ground-breaking Daresbury SRS, Diamond is a third-generation, 3 GeV light source. Construction began in 2003, with beamlines constructed in three phases: Phase I beamlines commenced user operation in 2007 [1, 2], with a further 15 Phase II beamlines completed in 2012. Phase III, completed in 2019, brought the total beamlines to 32. An additional thirty-third beamline, K11 DIAD, was scheduled at press time to start operating in 2020.	Jan 2021
I19-Small Molecule Single Crystal Diffraction	Leading edge chemical crystallography service provision and its impact on crystallographic data science in the twenty-first century Simon J. Coles , David R. Allan , Christine M. Beavers , Simon J. Teat , Stephen J. W. Holgate , Clare A. Tovee DOI: 10.1007/430_2020_63 Show Abstract ▼ Abstract: National facilities provide state-of-the-art crystallographic instrumentation and processes and tend to act as an indicator for the direction of a community in the medium term. There has been a significant step up in terms of instrumentation and approach in the last 10 years which has driven data generation. This has had a significant impact on databases – in turn we observe a substantial change in the use of the Cambridge Structural Database (CSD) from relatively basic search/retrieve to gaining deep understanding about factors that govern the solid state. Databases are now able to drive new science in areas such as crystal engineering. Looking forward, we will see more automated pipelining of the data generation process, and this will require better integration with databases. Databases will provide more predictive power – and this will inform the science/crystallography that should be done.	Oct 2020
I15-Extreme Conditions	The HXD95: a modified Bassett-type hydrothermal diamond-anvil cell for in situ XRD experiments up to 5 GPa and 1300 K Marion Louvel , James W. E. Drewitt , Allan Ross , Richard Thwaites , Benedict J. Heinen , Dean S. Keeble , Christine M. Beavers , Michael J. Walter , Simone Anzellini Journal Of Synchrotron Radiation 27 DOI: 10.1107/S1600577519016801 Diamond Proposal Number(s): [19339] Open Access Show Abstract ▼ Abstract: A new diamond-anvil cell apparatus for in situ synchrotron X-ray diffraction measurements of liquids and glasses, at pressures from ambient to 5 GPa and temperatures from ambient to 1300 K, is reported. This portable setup enables in situ monitoring of the melting of complex compounds and the determination of the structure and properties of melts under moderately high pressure and high temperature conditions relevant to industrial processes and magmatic processes in the Earth's crust and shallow mantle. The device was constructed according to a modified Bassett-type hydrothermal diamond-anvil cell design with a large angular opening (θ = 95°). This paper reports the successful application of this device to record in situ synchrotron X-ray diffraction of liquid Ga and synthetic PbSiO3 glass to 1100 K and 3 GPa.	Mar 2020
	Corrosion of late- and post-transition metals into metal-organic chalcogenolates and implications for nanodevice architectures Matthew Yeung , Derek C. Popple , Elyse A. Schriber , Simon J. Teat , Christine M. Beavers , Aude Demessence , Tevye R. Kuykendall , J. Nathan Hohman Acs Applied Nano Materials DOI: 10.1021/acsanm.0c00057 Show Abstract ▼ Abstract: Metal chalcogenide compounds have attracted interest as materials for next generation semiconductors, catalysts, and device architectures. Hybrid compounds containing both a metal chalcogenide architecture and a supporting organic lattice combine the interesting structural and electronic properties of the material class with a configurable hybrid component that can lead to a wide range of tailorable materials. However, many of the methods available for preparing inorganic coordination polymers in this class require specialized solution-phase chemical preparations that are incompatible with solid-state fabrication techniques. Here we prepare metal-organic chalcogenolates (MOChas) of copper, indium, lead, and tin from benzeneselenol or benzenethiol directly from the organochalcogen and corresponding metal in a tube furnace at a relatively modest temperature. Scanning electron microscopy and X-ray diffraction confirmed conversion of the precursors to crystalline MOChas. X-ray photoelectron spectroscopy was used to investigate the chemical bonding for each of the materials and provides insight into the elemental composition of the synthesized compounds. This straightforward approach for preparing crystalline hybrid materials may be generalizable for the preparation of a wide variety of coordination compounds and complexes in form factors useful for subsequent development of device architectures.	Mar 2020
	High-pressure polymorphism in pyridine Nico Giordano , Christine M. Beavers , Branton J. Campbell , Václav Eigner , Eugene Gregoryanz , William G. Marshall , Miriam Peña-Álvarez , Simon J. Teat , Cara E. Vennari , Simon Parsons Iucrj 7, 58 - 70 DOI: 10.1107/S2052252519015616 Open Access Show Abstract ▼ Abstract: Single crystals of the high-pressure phases II and III of pyridine have been obtained by in situ crystallization at 1.09 and 1.69 GPa, revealing the crystal structure of phase III for the first time using X-ray diffraction. Phase II crystallizes in P212121 with Z′ = 1 and phase III in P41212 with Z′ = ½. Neutron powder diffraction experiments using pyridine-d5 establish approximate equations of state of both phases. The space group and unit-cell dimensions of phase III are similar to the structures of other simple compounds with C2v molecular symmetry, and the phase becomes stable at high pressure because it is topologically close-packed, resulting in a lower molar volume than the topologically body-centred cubic phase II. Phases II and III have been observed previously by Raman spectroscopy, but have been mis-identified or inconsistently named. Raman spectra collected on the same samples as used in the X-ray experiments establish the vibrational characteristics of both phases unambiguously. The pyridine molecules interact in both phases through CH⋯π and CH⋯N interactions. The nature of individual contacts is preserved through the phase transition between phases III and II, which occurs on decompression. A combination of rigid-body symmetry mode analysis and density functional theory calculations enables the soft vibrational lattice mode which governs the transformation to be identified.	Jan 2020
I15-Extreme Conditions	Thermal equation of state of ruthenium characterized by resistively heated diamond anvil cell Simone Anzellini , Daniel Errandonea , Claudio Cazorla , Simon Macleod , Virginia Monteseguro , Silvia Boccato , Enrico Bandiello , Daniel Diaz Anichtchenko , Catalin Popescu , Christine M. Beavers Scientific Reports 9 DOI: 10.1038/s41598-019-51037-8 Diamond Proposal Number(s): [23122] Open Access Show Abstract ▼ Abstract: The high-pressure and high-temperature structural and chemical stability of ruthenium has been investigated via synchrotron X-ray diffraction using a resistively heated diamond anvil cell. In the present experiment, ruthenium remains stable in the hcp phase up to 150 GPa and 960 K. The thermal equation of state has been determined based upon the data collected following four different isotherms. A quasi-hydrostatic equation of state at ambient temperature has also been characterized up to 150 GPa. The measured equation of state and structural parameters have been compared to the results of ab initio simulations performed with several exchange-correlation functionals. The agreement between theory and experiments is generally quite good. Phonon calculations were also carried out to show that hcp ruthenium is not only structurally but also dynamically stable up to extreme pressures. These calculations also allow the pressure dependence of the Raman-active E2g mode and the silent B1g mode of Ru to be determined.	Oct 2019
I24-Microfocus Macromolecular Crystallography	A rapidly-reversible absorptive and emissive vapochromic Pt(II) pincer-based chemical sensor M. J. Bryant , J. M. Skelton , L. E. Hatcher , C. Stubbs , E. Madrid , A. R. Pallipurath , L. H. Thomas , Ch. H. Woodall , J. Christensen , S. Fuertes , T. P. Robinson , C. M. Beavers , S. J. Teat , M. Warren , F. Pradaux-Caggiano , A. Walsh , F. Marken , D. R. Carbery , S. C. Parker , N. B. Mckeown , R. Malpass-Evans , M. Carta , P. R. Raithby Nature Communications 8 DOI: 10.1038/s41467-017-01941-2 Open Access Show Abstract ▼ Abstract: Selective, robust and cost-effective chemical sensors for detecting small volatile-organic compounds (VOCs) have widespread applications in industry, healthcare and environmental monitoring. Here we design a Pt(II) pincer-type material with selective absorptive and emissive responses to methanol and water. The yellow anhydrous form converts reversibly on a subsecond timescale to a red hydrate in the presence of parts-per-thousand levels of atmospheric water vapour. Exposure to methanol induces a similarly-rapid and reversible colour change to a blue methanol solvate. Stable smart coatings on glass demonstrate robust switching over 104 cycles, and flexible microporous polymer membranes incorporating microcrystals of the complex show identical vapochromic behaviour. The rapid vapochromic response can be rationalised from the crystal structure, and in combination with quantum-chemical modelling, we provide a complete microscopic picture of the switching mechanism. We discuss how this multiscale design approach can be used to obtain new compounds with tailored VOC selectivity and spectral responses.	Dec 2017
I19-Small Molecule Single Crystal Diffraction	Observation of a re-entrant phase transition in the molecular complex tris¬(μ2-3,5-diiso¬propyl-1,2,4-triazolato-κ2N1:N2)trigold(I) under high pressure Christopher H. Woodall , Jeppe Christensen , Jonathan M. Skelton , Lauren E. Hatcher , Andrew Parlett , Paul R. Raithby , Aron Walsh , Stephen C. Parker , Christine M. Beavers , Simon J. Teat , Mourad Intissar , Christian Reber , David R. Allan Iucrj 3, 367 - 376 DOI: 10.1107/S2052252516013129 Open Access Show Abstract ▼ Abstract: We report a molecular crystal that exhibits four successive phase transitions under hydrostatic pressure, driven by aurophilic interactions, with the ground-state structure re-emerging at high pressure. The effect of pressure on two polytypes of tris(μ2-3,5-diisopropyl-1,2,4-triazolato-κ2N1:N2)trigold(I) (denoted Form-I and Form-II) has been analysed using luminescence spectroscopy, single-crystal X-ray diffraction and first-principles computation. A unique phase behaviour was observed in Form-I, with a complex sequence of phase transitions between 1 and 3.5 GPa. The ambient C2/c mother cell transforms to a P21/n phase above 1 GPa, followed by a P21/a phase above 2 GPa and a large-volume C2/c supercell at 2.70 GPa, with the previously observed P21/n phase then reappearing at higher pressure. The observation of crystallographically identical low- and high-pressure P21/n phases makes this a rare example of a re-entrant phase transformation. The phase behaviour has been characterized using detailed crystallographic theory and modelling, and rationalized in terms of molecular structural distortions. The dramatic changes in conformation are correlated with shifts of the luminescence maxima, from a band maximum at 14040 cm−1 at 2.40 GPa, decreasing steeply to 13550 cm−1 at 3 GPa. A similar study of Form-II displays more conventional crystallographic behaviour, indicating that the complex behaviour observed in Form-I is likely to be a direct consequence of the differences in crystal packing between the two polytypes.	Sep 2016
	Thermal and photochemical control of nitro–nitrito linkage isomerism in single-crystals of [Ni(medpt)(NO2)(η2-ONO)] Lauren E. Hatcher , Edward J. Bigos , Mathew J. Bryant , Emily M. Maccready , Thomas P. Robinson , Lucy K. Saunders , Lynne H. Thomas , Christine M. Beavers , Simon J. Teat , Jeppe Christensen , Paul R. Raithby Crystengcomm 16 DOI: 10.1039/C4CE00675E Show Abstract ▼ Abstract: The known complex [Ni(medpt)(η1-NO2)(η2-ONO)] 1 (medpt = 3,3′-diamino-N-methyldipropylamine) crystallises in the monoclinic space group P21/m with 1.5 molecules in the asymmetric unit with two different η1-NO2 ligand environments in the crystal structure. At 298 K the molecule (A) sitting in a general crystallographic site displays a mixture of isomers, 78% of the η1-NO2 isomer and 22% of an endo-nitrito–(η1-ONO) form. The molecule (B) sitting on a crystallographic mirror plane adopts the η1-NO2 isomeric form exclusively. However, a variable temperature crystallographic study showed that the two isomers were in equilibrium and upon cooling to 150 K the η1-ONO isomer converted completely to the η1-NO2 isomer, so that both independent molecules in the asymmetric unit were 100% in the η1-NO2 form. A kinetic analysis of the equilibrium afforded values of ΔH = −9.6 (±0.4) kJ mol−1, ΔS = −21.5 (±1.8) J K−1 mol−1 and EA = −1.6 (±0.05) kJ mol−1. Photoirradiation of single crystals of 1 with 400 nm light, at 100 K, resulted in partial isomerisation of the η1-NO2 isomer to the metastable η1-ONO isomer, with 89% for molecule (A), and 32% for molecule (B). The crystallographic space group also reduced in symmetry to P21 with Z′ = 3. The metastable state existed up to a temperature of 150 K above which temperature it reverted to the ground state. An analysis of the crystal packing in the ground and metastable states suggests that hydrogen bonding is responsible for the difference in the conversion between molecules (A) and (B).	Jun 2014

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