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Instruments / Technical Area	Publication Details	Published	Actions
B18-Core EXAFS	Solvent-dependent nuclearity, geometry and catalytic activity of [(SPhos)Pd(Ph)Cl] 2 John B. Brazier , Mark A Newton , Elena M. Barreiro , Luis A. Adrio , Leticia Naya , King Kuok (mimi) Hii Dalton Trans. DOI: 10.1039/C7DT01019B Diamond Proposal Number(s): [7815] Show Abstract ▼ Abstract: The nuclearity and structures of the palladium complex [(SPhos)Pd(Ph]Cl]2 in the solid and solution states are revisited, using a combination of Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy, NMR spectroscopy, mass spectrometry, DFT calculations and trapping experiments. The complex was tested for its catalytic activity in the coupling reaction between chlorobenzene and n-hexylamine, where different deactivation behaviour were observed in toluene, 1,4-dioxane and DMF.	May 2017
B18-Core EXAFS	Effects of Cl on the reduction of supported PdO in ethanol/water solvent mixtures John B. Brazier , Mark A. Newton , Elena M. Barreiro , Stephen Parry , Luis A. Adrio , Christopher J. Mulligan , Klaus Hellgardt , King Kuok (mimi) Hii , Paul B. J. Thompson , Rachel Nichols , Bao N. Nguyen Catalysis, Structure & Reactivity 3, 54 - 62 DOI: 10.1080/2055074X.2016.1267296 Diamond Proposal Number(s): [9584] Open Access Show Abstract ▼ Abstract: The reduction of γ-Al2O3-supported PdO in flowing aqueous ethanol was investigated. Quick EXAFS (QEXAFS) performed at the Pd K-edge reveals that the presence of Cl can have a profound effect on the reduction process. At low loadings of Pd (1 wt-%), the size dependency of the process is inverted, compared to Cl-free samples. The extent of reduction was found to be dependent on loading/particles size. It is shown, using in situ QEXAFS at the Cl K- and Pd L3-edges, that residual Cl is not removed by the flowing solvent mixture, even at an elevated temperature of 350 K. The origins of these behaviours are discussed in terms of the differing effects that Cl may have when bonded to oxidic or reduced metal centres and the results were compared to earlier observations made on the effects of Cl on commercial polyurea encapsulated Pd ENCAT™ NP 30 catalysts.	Feb 2017

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