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Instruments / Technical Area	Publication Details	Published	Actions
B21-High Throughput SAXS I24-Microfocus Macromolecular Crystallography	Systematic construction of progressively larger capsules from a fivefold linking pyrrole-based subcomponent Kai Wu , Tanya K. Ronson , Pingru Su , Zhi Chen , Leonard Goh , Andrew W. Heard , Xiaopeng Li , Fabian Klautzsch , Christoph A. Schalley , Mladen Vinković , Jonathan R. Nitschke Nature Synthesis 115 DOI: 10.1038/s44160-023-00276-9 Diamond Proposal Number(s): [31323, 31668] Show Abstract ▼ Abstract: Biological encapsulants, such as viral capsids and ferritin protein cages, use many identical subunits to tile the surface of a polyhedron. Inspired by these natural systems, synthetic chemists have prepared artificial nanocages with well-defined shapes and cavities. Rational control over the self-assembly of discrete, nanometre-scale, hollow coordination cages composed of simple components remains challenging as a result of the entropic costs associated with binding many subunits together, difficulties in the error-correction processes associated with assembly and increasing surface energy as their size grows. Here we demonstrate the construction of nanocages of increasing size derived from a single pentatopic pyrrole-based subcomponent. Reasoned shifts in the preferred coordination number of the metal ions used, along with the denticity and steric hindrance of the ligands, enabled the generation of progressively larger cages. These structural changes of the cages are reminiscent of the differences in the folding of proteins caused by minor variations in their amino acid sequences; understanding how they affect capsule structure and thus cavity size may help to elucidate the construction principles for larger and functional capsules, capable of binding and carrying large biomolecules as cargoes.	Apr 2023
I20-Scanning-X-ray spectroscopy (XAS/XES)	3D atomic-scale imaging of mixed Co-Fe spinel oxide nanoparticles during oxygen evolution reaction Weikai Xiang , Nating Yang , Xiaopeng Li , Julia Linnemann , Ulrich Hagemann , Olaf Ruediger , Markus Heidelmann , Tobias Falk , Matteo Aramini , Serena Debeer , Martin Muhler , Kristina Tschulik , Tong Li Nature Communications 13 DOI: 10.1038/s41467-021-27788-2 Diamond Proposal Number(s): [25636] Open Access Show Abstract ▼ Abstract: The three-dimensional (3D) distribution of individual atoms on the surface of catalyst nanoparticles plays a vital role in their activity and stability. Optimising the performance of electrocatalysts requires atomic-scale information, but it is difficult to obtain. Here, we use atom probe tomography to elucidate the 3D structure of 10 nm sized Co2FeO4 and CoFe2O4 nanoparticles during oxygen evolution reaction (OER). We reveal nanoscale spinodal decomposition in pristine Co2FeO4. The interfaces of Co-rich and Fe-rich nanodomains of Co2FeO4 become trapping sites for hydroxyl groups, contributing to a higher OER activity compared to that of CoFe2O4. However, the activity of Co2FeO4 drops considerably due to concurrent irreversible transformation towards CoIVO2 and pronounced Fe dissolution. In contrast, there is negligible elemental redistribution for CoFe2O4 after OER, except for surface structural transformation towards (FeIII, CoIII)2O3. Overall, our study provides a unique 3D compositional distribution of mixed Co-Fe spinel oxides, which gives atomic-scale insights into active sites and the deactivation of electrocatalysts during OER.	Jan 2022

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