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Instruments / Technical Area	Publication Details	Published	Actions
I19-Small Molecule Single Crystal Diffraction	Peptide sequence mediated self-assembly of molybdenum blue nanowheel superstructures Shan She , Weimin Xuan , Nicola L. Bell , Robert Pow , Eduard Garrido Ribo , Zoe Sinclair , De-Liang Long , Leroy Cronin Chemical Science 3 DOI: 10.1039/D0SC06098D Open Access Show Abstract ▼ Abstract: The precise control over the formation of complex nanostructures, e.g. polyoxometalates (POMs), at the sub-nanoscale is challenging but critical if non-covalent architectures are to be designed. Combining biologically-evolved systems with inorganic nanostructures could lead to sequence-mediated assembly. Herein, we exploit oligopeptides as multidentate structure-directing ligands via metal-coordination and hydrogen bonded interactions to modulate the self-assembly of POM superstructures. Six oligopeptides (GH, AH, SH, G2H, G4H and G5H) are incorporated into the cavities of Molybdenum Blue (MB) POM nanowheels. It is found that the helicity of the nanowheel can be readily switched (Δ to Λ) by simply altering the N-terminal amino acid on the peptide chain rather than their overall stereochemistry. We also reveal a delicate balance between the Mo-coordination and the hydrogen bonds found within the internal cavity of the inorganic nanowheels which results in the sequence mediated formation of two unprecedented asymmetrical nanowheel frameworks: {Mo122Ce5} and {Mo126Ce4}.	Dec 2020
I19-Small Molecule Single Crystal Diffraction	Synthesis, assembly and sizing of neutral, lanthanide substituted molybdenum blue wheels {Mo90+2nLn10-n} Eduard Garrido Ribo , Nicola L. Bell , Weimin Xuan , Jiancheng Luo , De-Liang Long , Tianbo Liu , Leroy Cronin Journal Of The American Chemical Society DOI: 10.1021/jacs.0c07146 Diamond Proposal Number(s): [22214] Show Abstract ▼ Abstract: Polyoxometalate Molybdenum blue (MBs) complexes typically exist as discrete multianionic clusters and are composed of repeating Mo building units. MB Wheels, such as {Mo176} and {Mo154} are made from pentagon-centered {Mo8} building blocks joined by equal number of {Mo1} units as loin, and {Mo2} dimer units as skirt along the ring edge and the ring sizes of the Mo-blue wheels are modulated by the {Mo2} units. Herein we report a new class of contracted lanthanide-doped MB structures that have replaced all the {Mo2} units with lanthanide ions on the ring edge with the general formula {Mo90+2nLn10-n} (n = 0, 1). We show three examples of this new decameric {Mo90Ln10} (Ln = La, Ce and Pr) framework synthesized by hydrothermal methods, and demonstrate that later Ln ions result in {Mo92Nd9}, conserving one {Mo2} linker unit in its structure, as a consequence of the lanthanide contraction. Remarkably the decameric {Mo90Ln10} compounds are the first examples of charge-neutral molybdenum wheels as confirmed by BVS and redox titrations. We detail our full synthetic optimization for the isolation of these clusters and complete characterization by X-ray, TGA, UV-vis and ICP studies. Finally we show that this fine-tuned self assembly process can be utilised to selectively enrich Ln-Mo Blue wheels for effective separation of lanthanide ions.	Sep 2020

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