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Instruments / Technical Area	Publication Details	Published
B16-Test Beamline	Spatially resolved mapping of phase transitions in liquid-crystalline materials by X-ray birefringence imaging Yating Zhou , Rhian Patterson , Benjamin A. Palmer , Gregory Edwards-Gau , Benson M. Kariuki , N. S. Saleesh Kumar , Duncan W. Bruce , Igor P. Dolbnya , Stephen P. Collins , Andrew Malandain , Kenneth D. M. Harris Chemical Science 33 DOI: 10.1039/C8SC05285A Diamond Proposal Number(s): [11893, 13819] Open Access Show Abstract ▼ Abstract: The X-ray Birefringence Imaging (XBI) technique, first reported in 2014, is a sensitive method for spatially resolved mapping of the local orientational properties of anisotropic materials. We report the first application of the XBI technique to characterize molecular orientational ordering in a liquid crystalline material, demonstrating significant potential for exploiting XBI measurements to advance structural understanding of liquid crystal phases.	Jan 2019
B18-Core EXAFS	Alumina-grafted SBA-15 as a high performance support for Pd-catalysed cinnamyl alcohol selective oxidation Christopher M. A. Parlett , Lee J. Durndell , Andreia Machado , Giannantonio Cibin , Duncan W. Bruce , Nicole S. Hondow , Karen Wilson , Adam F. Lee Catalysis Today DOI: 10.1016/j.cattod.2013.11.056 Diamond Proposal Number(s): [7668] Show Abstract ▼ Abstract: Ultrathin alumina monolayers grafted onto an ordered mesoporous SBA-15 silica framework afford a composite catalyst support with unique structural properties and surface chemistry. Palladium nanoparticles deposited onto Al-SBA-15 via wet impregnation exhibit the high dispersion and surface oxidation characteristic of pure aluminas, in conjunction with the high active site densities characteristic of thermally stable, high-area mesoporous silicas. This combination confers significant rate enhancements in the aerobic selective oxidation (selox) of cinnamyl alcohol over Pd/Al-SBA-15 compared to mesoporous alumina or silica supports. Operando, liquid-phase XAS highlights the interplay between dissolved oxygen and the oxidation state of palladium nanoparticles dispersed over Al-SBA-15 towards on-stream reduction: ambient pressures of flowing oxygen are sufficient to hinder palladium oxide reduction to metal, enabling a high selox activity to be maintained, whereas rapid PdO reduction and concomitant catalyst deactivation occurs under static oxygen. Selectivity to the desired cinnamaldehyde product mirrors these trends in activity, with flowing oxygen minimising CO cleavage of the cinnamyl alcohol reactant to trans-β-methylstyrene, and of cinnamaldehyde decarbonylation to styrene.	Jan 2014
I19-Small Molecule Single Crystal Diffraction	Homo- and hetero-bimetallic complexes of TTHA Navpreet K. Sethi , Adrian C. Whitwood , Duncan W. Bruce Polyhedron 33 (1), 378 - 387 DOI: 10.1016/j.poly.2011.11.052 Diamond Proposal Number(s): [8521] Show Abstract ▼ Abstract: The preparation is described of bimetallic complexes of the multidentate ligand, H6TTHA – triethylenetetraamine-N,N′,N″,N‴-hexaacetic acid. Attempts to use a stepwise approach systematically to prepare heterobimetallic complexes were unsuccessful and led in most cases to homobimetallic complexes or to heterobimetallic complexes whose stoichiometry did not reflect the stoichiometry of the preparation. Nonetheless, on one occasion a monodisperse heterobimetallic complex of rhodium and zinc was isolated, which represents the first properly characterised heterobimetallic complex of TTHA.	Feb 2012

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