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Instruments / Technical Area	Publication Details	Published
I15-1-X-ray Pair Distribution Function (XPDF)	Pair distribution function analysis of the reassembly step of the assembly-disassembly-organisation-reassembly (ADOR) process Samantha Russell , Fanny N. Costa , Maria Diaz-Lopez , Russell E. Morris Dalton Transactions 5 DOI: 10.1039/D2DT03389E Diamond Proposal Number(s): [26990] Open Access Show Abstract ▼ Abstract: An in situ pair distribution function study assessing the reassembly of three IM-12 (UTL) intermediate materials to the corresponding fully connected materials. A greater level of atomic change is observed at higher temperatures for the reassembly of the fully disconnected intermediate, IPC-1P, compared to the two partially connected intermediates of IPC-2P and IPC-6P.	Nov 2022
I19-Small Molecule Single Crystal Diffraction	Controlled synthesis of large single crystals of metal‐organic framework CPO‐27‐Ni prepared by a modulation approach: in situ single crystal X‐ray diffraction studies Simon Maximilian Vornholt , Caroline Elliott , Cameron Rice , Samantha Russell , Peter J. Kerr , Daniel N. Rainer , Michal Mazur , Mark R. Warren , Paul S. Wheatley , Russell E. Morris Chemistry – A European Journal DOI: 10.1002/chem.202100528 Diamond Proposal Number(s): [24028] Open Access Show Abstract ▼ Abstract: The size of single crystals of the metal-organic framework CPO-27-Ni was incrementally increased through a series of modulated syntheses. A novel linker modulated synthesis using 2,5-dihydroxyterephthalic acid and the isomeric ligand 4,6-dihydroxyisophthalic acid yielded large single crystals of CPO-27-Ni (~70 µm). All materials proved high crystallinity and phase pure through powder X-ray diffraction, electron microscopy methods, thermogravimetric, and compositional analysis. For the first time single crystal structure analyses were carried out on CPO-27-Ni. High BET surface areas and nitric oxide (NO) release efficiencies were recorded for all materials. Large single crystals of CPO-27-Ni showed a prolonged NO release and proved suitable for in situ single crystal diffraction experiments to follow the NO adsorption. An efficient activation protocol was developed, leading to a dehydrated structure after just 4 h, which subsequently was NO-loaded, giving a first NO loaded single crystal structural model of CPO-27-Ni.	Mar 2021
I11-High Resolution Powder Diffraction	Zeolite catalysts for nitric oxide production Samantha Russell DOI: 10.17630/10023-17918 Show Abstract ▼ Abstract: This thesis considers the nitric oxide production from a range of zeolite catalysts with either acid or copper active sites. The aim of the research was to find potential candidates for stent coatings that could help to prevent stent thrombosis. Acid site mordenite, ferrierite, SSZ-13 and ZSM-5 are studied in chapter 4 for the catalytic conversion of sodium nitrite to nitric oxide. All zeolites successfully produced nitric oxide, with ranging levels of conversion from 14 – 24 %. Recycled samples revealed the consumption of the acid site, rendering the acid site zeolites non-catalytic. Copper site zeolites were considered in chapters 5 and 6, with copper mordenite, ferrierite, SSZ-13, ZSM-5 and UZM-4 being studied. All zeolites successfully converted sodium nitrite to nitric oxide, with SSZ-13, ZSM-5 and UZM-4 producing around 100 % conversion. The use of cysteine as a sacrificial reductant to activate the copper sites allowed catalytic nitric oxide production. The promising catalytic tests led to further studies of the materials, including copper leaching and toxicology. Chapter 6 looked further into the catalytic copper zeolites with nitric oxide flow studies and polymer incorporation. Flow studies showed sustained levels of nitric oxide production. Incorporation of the zeolite powders into the polymer of intrinsic microporosity, EATB(Me), showed good nitric oxide production from the initial studies. Recycled samples, however, showed a drop in production. Lastly, chapter 7 explored the use of the ADOR (Assembly-Disassembly-Organisation- Reassembly) process to generate a series of zeolites for catalysis. Aluminium was incorporated into zeolites IPC-2, 4 and 6 through the organisation step to create aluminated zeolites. The aforementioned zeolites, as well as Al-UTL, were assessed for nitric oxide production with acid active sites. The results showed an interesting relation between ring size and nitric oxide production, with the largest rings of Al-UTL having the highest production and the smallest rings of Al-IPC-4 having the lowest.	Jun 2019

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