An X-ray Diffractometer for Extreme Conditions Research

Lead Research Organisation: University of Edinburgh
Department Name: Sch of Chemistry

Abstract

We are interested in the effect of pressure on molecular solids. In organic materials pressure modifies and rearranges intermolecular contacts such as hydrogen bonds and van der Waals contacts leading to rich polymorphic diversity. Pressure is thus a very effective tool for exploring the structural flexibility, the so-called 'energy landscapes', of organic solids, a very important factor in the development of pharmaceuticals, which also provides valuable data for computational work such as first-principals prediction of crystal structures.

Changes in primary molecular bond distances tend not to be observed in organic systems at least up to 10 GPa (100 000 atm). By contrast, work on metal coordination compounds has revealed that, unlike organic systems, intramolecular metal-ligand bonding can be affected by pressure. This makes pressure a perfect tool for exploring the relationship between structure and properties in functional coordination materials such as molecular magnets: a material can be studied in different states of distortion, providing the most direct way to study correlations between structure and properties.

The same methodology can be used to study metals, minerals and other extended materials, to show, for example, how rocks change their structures in planetary interiors, how materials can be modified for advanced technological applications and how materials change structure under the influence of shock waves during detonations, and how transport can be made more efficient by controlling the response of additives to the extreme conditions of modern engines.

Pressure can be applied to a sample using a diamond anvil cell, in which a sample is held between the faces of two diamonds. When load is applied to the diamonds, pressure many thousands of times atmospheric pressure can be generated at the sample. The sample can then be studied using single-crystal X-ray diffraction, which is the most precise and convenient way to obtain structural information on the atomic scale, to reveal how the material responds to pressure.

In this project we seek funding for a diffractometer that will enable these studies to be carried out at The Centre for Science at Extreme Conditions, an institute dedicated to extreme conditions research at The University of Edinburgh. The new instrument will be equipped with state-of-the-art detector and X-ray sources, to enable data to be collected very quickly but with high precision. We will design and build new pressure cells which will enable data to be obtained simultaneously at high pressure and variable temperature. The new facility will enable much more complex supramolecular materials to be studied than has hitherto been possible.

The combination of these facilities will provide a unique instrument which enables variation of two fundamentally important thermodynamic variables of temperature and pressure to provide deep insight into the factors which govern phase stability in solid materials.

Planned Impact

The principal impacts of this grant will be:

1. Provision of personnel trained to the highest level in advanced experimental techniques, data analysis, the interpretation of disparate data and the communication of the results. These skills are highly transferable and are strengthened by our close links with external partners, including central facilities, research institutes and in the commercial sector. The academic community benefits from the research itself for the reasons summarised in the Academic Beneficiaries section, but also because staff move on to post-doctoral or lectureship positions, where the training can be applied and diversified. Research and development activities in the commercial sector also benefits from highly-trained scientists who often move into strategic management roles as they progress in their careers. The transferability of the skills acquired means that society benefits because scientifically-trained staff who move into careers such as teaching, the environmental sector, engineering and sectors (e.g. finance) which rely on analysis, modelling and interpretation of numerical data. We ensure suitable training in the use of the instrument in a series of training workshops over the course of the grant

2. Provision of unique instrumentation to the UK's research infrastructure. This benefits Academia by providing facilities to develop new research areas, but also a diverse range of industries where a fundamental understanding of the behaviour of solids at extreme conditions is relevant to the development of improved modelling of lubricants, biofuels, energetic materials, phase change materials for energy storage and pharmaceuticals. In addition to training in the use of the instrument described above, we have requested funds for two high-pressure cells which can be provided to new users, ensuring maximum usage and diversification of the science supported.

3. Provision of new research results, to be published in the scientific literature, presented at conferences and included in data-bases. Although interest in application of extreme conditions is growing rapidly, work on complex molecular materials is still a relatively young field with enormous scope for new and disruptive research. This research provides usual data which probes the extremes of inter- and intra-molecular interactions, leading to improved models of the molecular solid state.

4. Provision of opportunities for outreach and public engagement. These include regular hands-on workshops and talks at the annual Edinburgh International Science Festival; attendance at two Royal Society Summer Exhibitions; regular participation in the "I'm a Scientist - Get me out of here!" scheme; and attendance at the annual Midlothian Science Festival as well as visits to schools and community groups. There are also several opportunities throughout the year to show off equipment in CSEC to public audiences through open days and coordinated visits. The centenary of the King's Buildings Campus will be an ideal opportunity for public engagement, and events will include exhibitions and tours. Crystal structures possess eye-catching visual impact, and engage interest in the context of the extreme conditions e.g. of planetary interiors and engineering, and we will continue to exploit links with The Edinburgh College of Art. Training for staff in Public Engagement and Outreach is provided by UoE.

Publications

10 25 50

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Borys AM (2021) The Phospha-Bora-Wittig Reaction. in Journal of the American Chemical Society

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Broadhurst ET (2022) A first-order phase transition in Blatter's radical at high pressure. in Acta crystallographica Section B, Structural science, crystal engineering and materials

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Falconer RL (2021) Reversible Dissociation of a Dialumene*. in Angewandte Chemie (International ed. in English)

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Falconer RL (2021) Reversible Reductive Elimination in Aluminum(II) Dihydrides. in Angewandte Chemie (International ed. in English)

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Lemus M (2021) Mg 2+ and Mn 2+ coordinate Cap-0-RNA to position substrates for efficient 2'- O- methyl transfer by SARS-CoV-2 nsp16 in Acta Crystallographica Section A Foundations and Advances

 
Description This grant covers purchase of a new diffractometer specialised for extreme conditions research. The instrument was installed an accepted in September 2019 and has thus far been used for research in polymorphism, materials science, pharmaceuticals and energy storage. We are, however, at a rather early stage of the grant. Data from the instrument has yielded only one publication to date, a comparative study demonstrating significant difference in compressibility in polymorphs of the amino acid L-histidine which revealed that H-bonded networks in molecular crystals have a compressibility similar to a metal such as titanium. The high compressibility of molecular crystals is a consequence of the void space they contain.
Exploitation Route This a key piece of equipment in the Centre for Extreme Conditions. The majority (~90%) of the time has been used by a range of groups in CSEC but our unique facilities and expertise have attracted users from outside Edinburgh (thus far, Imperial College London and Strathclyde University).
Sectors Chemicals

 
Description An X-ray Diffractometer for Extreme Conditions Research
Amount £561,796 (GBP)
Funding ID EP/R042845/1 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 07/2018 
End 07/2022
 
Description High Energy Single-Crystal Microdiffraction on I15 Applied to Noble-Gas Compounds
Amount £45,129 (GBP)
Funding ID 2581384 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 07/2021 
End 02/2025
 
Description Molecular Minerals Discovery
Amount £359,206 (FKP)
Funding ID RPG-2021-176 
Organisation The Leverhulme Trust 
Sector Charity/Non Profit
Country United Kingdom
Start 08/2021 
End 08/2024
 
Description Polymorph stabilities of pharmaceuticals used in the treatment of COVID-19
Amount £67,974 (GBP)
Funding ID 2589477 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 11/2021 
End 04/2025
 
Description The role of entropy in crystal structures
Amount £33,863 (GBP)
Funding ID 2424291 
Organisation Engineering and Physical Sciences Research Council (EPSRC) 
Sector Public
Country United Kingdom
Start 07/2020 
End 02/2024
 
Description Cairns Group (Imperial) 
Organisation Imperial College London
Country United Kingdom 
Sector Academic/University 
PI Contribution Access to state of the art in-house diffraction equipment for high-pressure crystallography together with training in data collection and analysis.
Collaborator Contribution Conceived the project and prepared suitable materials for measurement. They also came to Edinburgh for in person training and data collection. This group were our first outside users (Feb 2020).
Impact Fellowship proposals including support and training from the new facility.
Start Year 2020
 
Description Oswald Group (Strathclyde University) 
Organisation University of Strathclyde
Department Strathclyde Institute of Pharmacy & Biomedical Sciences
Country United Kingdom 
Sector Academic/University 
PI Contribution Access to state of the art in-house diffraction equipment for high-pressure crystallography together with training in data collection and analysis.
Collaborator Contribution Conceived the project and prepared suitable materials for measurement. They also came to Edinburgh for in person training and data collection. This group were our second outside users (Aug 2020).
Impact Research proposals including support and training from the new facility.
Start Year 2020