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Research at St Andrews

Russell Edward Morris

Person

Russell Edward Morris, FRS FRSE FRSC FLSW

Research overview

Framework solids have long been known to be important chemicals in both industry and academia and Morris has a long track record of creativity in developing new areas of science that have not only impacted fundamental porous materials science but have also changed approaches across a wide swathe of chemistry outside his own direct field.  Morris has also been active in spinning out companies, with two startups developing the industrial applications of his science.

Morris's specific contributions have been to overturn conventional thinking in several areas. His development of ionothermal chemistry has led to a whole new endeavour that has impacted on many aspects of chemistry outside his own specific field. He is a pioneer in the area of porous materials chemistry for biological/medical applications, initiating a field of BioMOFs and is responsible for exposing many physicians and biologists to the concepts involved. Morris’s recent work on the ADOR principle offers to significantly change the way synthetic chemists view what is possible – his preparation of ‘unfeasible’ materials solves a long standing problem and offers insight into how to avoid the limitations of solvent-based synthetic approaches in materials chemistry.

Morris’s contributions can be split into three main areas; synthesis, application and characterisation.

A. Materials Synthesis

Morris has made world-leading contributions in materials synthesis by

  • developing the ADOR mechanism, which provides routes to compounds previously labelled ‘unfeasible’ synthetic targets and provides unprecedented continuous control over porosity.1-4
  • introducing and developing ionothermal synthesis techniques  - these are now well established in the world of materials chemistry6,8,13,15-17
  • developing new concepts in MOF chemistry, such as ‘hemilabile’ and ‘switchable’ MOFs7,9,10,131.     The ADOR principle – Solving the zeolite conundrum

For the last 60 or so years hydrothermal techniques have been used to prepare zeolites and other related materials, leading to a total of just over 200 known zeolite topologies. However, simple calculations reveal that there are at least 300,000 (and possibly millions) of potential topologies. This is the zeolite conundrum – why can we make so few topologies? Recent work by Morris1-4 has shown that the paucity of zeolite frameworks is caused by the mechanism of hydrothermal synthesis, and by developing new synthesis mechanisms (the ADOR principle1-4) Morris has shown that materials that were hitherto described as ‘unfeasible’ synthetic targets can now be prepared – effectively solving the long-standing zeolite conundrum.1 This work is published in a series of papers in Nature Chemistry.1,2,4

The ADOR principle (Assembly-Disassembly-Organisation-Reassembly)1-4 is a top-down approach to the synthesis of zeolites and other porous materials with predictable structures. The work has overturned the conventional thinking of how control over porous materials can be achieved. Morris has shown that the ADOR methodology, where a preformed material is selectively disassembled before being reassembled in a new way, can lead to continuous control over porosity that covers the whole range of useful zeolite pore sizes.3,4 Morris has developed this into a general method for zeolites1 and has demonstrated that similar approaches lead to unusual properties in metal-organic frameworks and other materials.2 The most important aspect of the work is that the new pathway allows the preparation of previously impossible to prepare solids,1,2 accessing areas of synthesis space that were kinetically and energetically impossible to reach using hydrothermal synthesis.1 Morris’s recent work on the ADOR process has led to a nomination for the  Donald Breck award, which is awarded triennially (next in 2016) for the most important work done worldwide in porous materials science.

2.       Ionothermal Materials Chemistry, Chiral Induction and Quantum spin Liquids

The ionothermal method for the preparation and processing of solids, developed by Morris, is widely viewed as a ground-breaking and world-leading advance in the field. The primary concept, first published in Nature,17 is the use of ionic liquids as both solvent and structure directing agent in the formation of unusual materials with unique structure and function. Originally designed for the synthesis of porous solids,15,16,17 the technique has been extended to almost all types of inorganic, organic and hybrid materials,6,8,13 and is now a widely used technique in materials chemistry. The ionothermal method exhibits many unique features, such as the use of ambient pressure solvothermal conditions, the controlled delivery of structure directing agents, anion control(and the exquisite control over water as a mineraliser it allows) and effective chiral induction etc, which have enabled the synthesis of many new materials that cannot be accessed using other routes. An outstanding extension of this work is the use of ionothermal synthesis to produce a whole new class of quantum spin liquid, which are of great interest to the condensed matter physics community for their potential in quantum computing.6

The work at St Andrews on ionothermal chemistry has stimulated a whole new field that is followed by many research groups around the world – since 2006 there have been thousands of papers that can be traced back to the original Nature paper. Morris is the acknowledged worldwide leader in the field (with eight of the top ten cited ionothermal papers – Source ISI Web of Knowledge).

3.       New concepts in Metal-Organic Framework (MOF) Chemistry

With his work on ionothermal synthesis and medical applications (see section B) Morris is already regarded as a leader in the metal-organic framework (MOF) community (Inaugural President of the International Zeolite Association MOF commission, Chairman of the International MOF meeting in 2012, plenary lecturer at the first international MOF meeting, 2008 etc). However, he has also developed several new concepts in MOF chemistry. One example is ‘hemilabile’ MOFs,5,9,10 where unique properties (such as ultraselective adsorption10) can be engineered into a material by controlling the relative bonding in different parts of the structure. In addition he has also developed the very first example of a MOF where adsorption can be switched on demand between two channels with different surface chemistries.7 As always the new concepts are underpinned by exquisite chemical and structural studies (see section C below), deciphering features such as the synthesis mechanisms5,9 of the in situ ligand functionalisation that is vital for switchable adsorption.7 A new concept that is about to be published is adsorption crossover, based on using a change in adsorption mechanism (chemi- to physisorption) to control gas storage.

B. Materials Application

Morris has been a pioneer in developing materials chemistry for medical applications. His world-leading achievements include

  • Developing porous materials for the delivery of biologically active gases such as nitric oxide. Morris was the first to develop this chemistry and the field now includes several leading scientists in Europe, the USA and Asia.
  • Taking the technologies he has developed towards commercialisation. There are two companies that are dedicated to developing Morris’s work and who are in the advanced stages of commercialisation.
  • Earning international recognition for this work through several different awards, including the Royal Society Brian Mercer Award and the GEMI award from Germany.

4.       Translational Medicinal Chemistry -  Porous materials in medicine

Morris is well-known as the originator of the use of porous materials to store and deliver medically active gases. It is quite a paradox that many gases of medical interest are extremely toxic in larger amounts (e.g. nitric oxide, hydrogen sulfide, carbon monoxide), and so safe storage and delivery in only beneficial amounts becomes a major challenge. Morris’s research developed zeolites13 and metal-organic frameworks11,12 that show exceptional properties for this process, delivering controllable amounts of gas at biologically suitable rates.  The research is truly translational – beginning in the chemistry laboratory and developing through in vitro biological testing, to in vivo testing first in animal models and then to humans (and in fact well into the commercialisation phase – see below). The research is also truly multidisciplinary - encompassing chemistry, biology, medicine and materials science. He is now a popular invited speaker at international conferences where such interdisciplinarity is highlighted.

His research is full of notable firsts in this area – the first demonstration of a biological action of metal-organic frameworks (anti-thrombosis activity in human blood) and the first clinical experiments on human skin to name but two. This primarily commercially targeted applications research is also underpinned by leading science in the synthesis and characterisation. The high level characterisation of the gas-framework interactions has been vital to a real understanding of the ongoing processes in the applications, and the development of polymer-MOF hybrid materials that demonstrate outstanding gas storage and delivery, while maintaining their mechanical properties, brings real applications of MOFs much nearer. His developing work on delivering multiple therapeutic agents at different rates offers a step change in the controllability of delivery technologies. Morris is acknowledged as one of the first two group leaders in the world to develop biological applications of MOFs – an area that is increasingly important. He is an author on two of the most highly cited papers in the area.

5.     Industrial and Commercial Chemistry

A significant recent focus of Morris’s research has been the translation of his leading academic research into industrial and commercial impact. His medical gas delivery technology has led to the largest commercial licence at St Andrews and a subsequent spin out company (Zeomedix LLP) who are taking the technology to the market place through clinical trials. Morris’s technology in the MOF area is being developed by MOFgen Ltd, a University of St Andrew spin out company. In addition Morris has spent significant time developing chemicals industry applications of porous solids in his role as a Royal Society Industry Fellow with Sasol Technology UK. Morris’s commercially focussed activity has led to several awards from the Royal Society (e.g. Brian Mercer Award for Innovation), the Royal Society of Edinburgh, GEMI (Germany) and the Royal Society of Chemistry Applied Inorganic Chemistry award.

C. Materials Characterisation

Morris has always been at the forefront of applying characterisation techniques, with his research being published in the highest quality journals (eg Science and Nature family journals).

6.       Characterisation: Powder and Microcrystal X-ray diffraction, NMR and PDF

A continuing theme throughout Morris’s career has been the development and application of cutting edge characterisation, especially in the area of X-ray diffraction. Early work concentrated on powder X-ray and neutron diffraction,19,20 but since the mid-nineties Morris has been a major developer of X-ray diffraction on micron-sized crystals at synchrotron sources around the world.9,15,17 His work allowed not only the structure solution of novel and exciting materials but also enabled mechanistic studies of interesting physical properties of zeolites, such as negative thermal expansion. The simultaneous use of multiple techniques to solve complex problems that are not tractable using one technique alone is a recurring aspect of Morris’s research. Diffraction studies combined with solid-state NMR18 and X-ray PDF5 allowed the solution of structural problems and the solution of zeolite and MOF architectures. Almost all the papers listed below involve high-level characterisation of these types.

 

  1. Mazur, M., Wheatley, P.S., Navarro, M., Roth, W. J., Polozij, M., Mayoral, A., Chlubná-Eliášová, P., Nachtigall, P., Čejka, J., Morris R.E., The Synthesis of ‘Unfeasible’ Zeolites Nature Chemistry 2016, DOI: 10.1038/NCHEM.2374
  2. Morris R.E & ČejkaJ. Exploiting chemically selective weakness in solids as a route to new porous materials Nature Chemistry 2015, 7, 381-388
  3. Wheatley, P.S., Chlubná-Eliášová, P., Greer, H., Zhou, W., Seymour, V. R., Dawson, D. M., Ashbrook, S. E., Pinar, A. B., McCusker, L. B., Opanasenko, M., Čejka, J., Morris, R. E. Zeolites with continuously tuneable porosity Angew. Chemie 2014, 53, 13210-13214
    1. Roth, W. J.; Nachtigall, P.; Morris, R. E.; Wheatley, P. S.; Seymour, V. R.; Ashbrook, S. E.; Chlubna, P.; Grajciar, L.; Polozij, M.; Zukal, A.; Shvets, O.; Cejka, J., A family of zeolites with controlled pore size prepared using a top-down method. Nature Chemistry 2013, 5, 628-633
  4. Allan, P. K.; Chapman, K. W.; Chupas, P. J.; Hriljac, J. A.; Renouf, C. L.; Lucas, T. C. A.; Morris, R. E.: Pair distribution function-derived mechanism of a single-crystal to disordered to single-crystal transformation in a hemilabile metal-organic framework. Chemical Science 2012, 3, 2559-2564
  5. Aidoudi F.H., Aldous, D.W., Goff, R.J.; Slawin A.M.Z.; Attfield, J.P., Morris, R.E., Lightfoot, P. An ionothermally prepared S = 1/2 vanadium oxyfluoride kagome lattice Nature Chemistry2011, 3, 801-806
  6. Mohideen. M. I. H.; Xiao, B.; Wheatley, P. S.; McKinlay, A. C.; Li, Y.; Slawin, A. M. Z.; Aldous, D. W.; Cessford, N. F.; Duren, T.; Zhao, X. B.; Gill, R.; Thomas, K. M.; Griffin, J. M.; Ashbrook, S. E.; Morris, R. E., Protecting group and switchable pore-discriminating adsorption properties of a hydrophilic-hydrophobic metal-organic framework. Nature Chemistry2011, 3, 304-310.
  7. Morris, R. E.; Bu, X. H., Induction of chiral porous solids containing only achiral building blocks. Nature Chemistry2010, 2, 353-361.
  8. Allan, P. K.; Xiao, B.; Teat, S. J.; Knight, J. W.; Morris, R. E., In Situ Single-Crystal Diffraction Studies of the Structural Transition of Metal-Organic Framework Copper 5-Sulfoisophthalate, Cu-SIP-3. Journal of the American Chemical Society 2010, 132 (10), 3605-3611.
  9. Xiao, B.; Byrne, P. J.; Wheatley, P. S.; Wragg, D. S.; Zhao, X. B.; Fletcher, A. J.; Thomas, K. M.; Peters, L.; Evans, J. S. O.; Warren, J. E.; Zhou, W. Z.; Morris, R. E., Chemically blockable transformation and ultraselective low-pressure gas adsorption in a non-porous metal organic framework. Nature Chemistry 2009, 1 (4), 289-294.
  10. McKinlay, A. C.; Xiao, B.; Wragg, D. S.; Wheatley, P. S.; Megson, I. L.; Morris, R. E., Exceptional behavior over the whole adsorption-storage-delivery cycle for NO in porous metal organic frameworks. Journal of the American Chemical Society 2008, 130 (31), 10440-10444.
  11. Xiao, B.; Wheatley, P. S.; Zhao, X. B.; Fletcher, A. J.; Fox, S.; Rossi, A. G.; Megson, I. L.; Bordiga, S.; Regli, L.; Thomas, K. M.; Morris, R. E., High-capacity hydrogen and nitric oxide adsorption and storage in a metal-organic framework. Journal of the American Chemical Society2007, 129 (5), 1203-1209.
  12. Lin, Z. J.; Slawin, A. M. Z.; Morris, R. E., Chiral induction in the ionothermal synthesis of a 3-D coordination polymer. Journal of the American Chemical Society2007, 129 (16), 4880-4881.
  13. Wheatley, P. S.; Butler, A. R.; Crane, M. S.; Fox, S.; Xiao, B.; Rossi, A. G.; Megson, I. L.; Morris, R. E., NO-releasing zeolites and their antithrombotic properties. Journal of the American Chemical Society2006, 128 (2), 502-509.
  14. Parnham, E. R.; Morris, R. E., The ionothermal synthesis of cobalt aluminophosphate zeolite frameworks. Journal of the American Chemical Society2006, 128 (7), 2204-2205.
  15. Parnham, E. R.; Drylie, E. A.; Wheatley, P. S.; Slawin, A. M. Z.; Morris, R. E., Ionothermal materials synthesis using unstable deep-eutectic solvents as template-delivery agents. Angewandte Chemie-International Edition2006, 45 (30), 4962-4966.
  16. Cooper, E. R.; Andrews, C. D.; Wheatley, P. S.; Webb, P. B.; Wormald, P.; Morris, R. E., Ionic liquids and eutectic mixtures as solvent and template in synthesis of zeolite analogues. Nature2004, 430 (7003), 1012-1016.
  17. Fyfe, C. A.; Brouwer, D. H.; Lewis, A. R.; Villaescusa, L. A.; Morris, R. E., Combined solid state NMR and X-ray diffraction investigation of the local structure of the five-coordinate silicon in fluoride-containing as-synthesized STF zeolite. Journal of the American Chemical Society2002, 124 (26), 7770-7778.
  18. Smith, L.; Cheetham, A. K.; Morris, R. E.; Marchese, L.; Thomas, J. M.; Wright, P. A.; Chen, J., On the nature of water bound to a solid acid catalyst. Science1996, 271 (5250), 799-802.
  19. Morris, R. E.; Harrison, W. T. A.; Nicol, J. M.; Wilkinson, A. P.; Cheetham, A. K., Determination of complex structures by combined neutron and synchrotron x-ray-powder diffraction. Nature1992, 359 (6395), 519-522.

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