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Instruments / Technical Area	Publication Details	Published
B18-Core EXAFS	Proton chelating ligands drive improved chemical separations for rhodium Hirokazu Narita , Rebecca M. Nicolson , Ryuhei Motokawa , Fumiyuki Ito , Kazuko Morisaku , Midori Goto , Mikiya Tanaka , William T. Heller , Hideaki Shiwaku , Tsuyoshi Yaita , Ross J. Gordon , Jason B. Love , Peter A. Tasker , Emma R. Schoﬁeld , Mark R. Antonio , Carole A. Morrison Inorganic Chemistry DOI: 10.1021/acs.inorgchem.9b01136 Diamond Proposal Number(s): [15757] Show Abstract ▼ Abstract: Current methods for the extraction of rhodium carry the highest carbon footprint and worst pollution metrics of all of the elements used in modern technological applications. Improving upon existing methods is made difficult by the limited understanding of the molecular-level chemistry occurring in extraction processes, particularly in the hydrometallurgical separation step. While many of the precious metals can be separated by solvent extraction, there currently exist no commercial extractants for Rh. This is due to its complicated mixed speciation upon leaching into hydrochloric acid, which gives rise to difficulties in designing effective reagents for solvent extraction. Herein we show that the diamidoamine reagent N-n-hexylbis(N-methyl-N-n-octylethylamide)amine transports Rh(III) from aqueous HCl into an organic phase as the monoaquated dianion [RhCl5(H2O)]2– through the formation of an outer-sphere assembly; this assembly has been characterized by experimentation (slope analysis, FT-IR and NMR spectroscopy, EXAFS, SANS, and ESI-MS) and computational modeling. The paper demonstrates the importance of applying a broad range of techniques to obtain a convincing mode of action for the complex processes involved in anion recognition in the solution phase. A consistent and comprehensive understanding of how the ligand operates to achieve Rh(III) selectivity over the competitor anion Cl– has emerged. This knowledge will guide the design of extractants and thus offers promise for improving the sustainability of metal extraction from both traditional mining sources and the recycling of secondary source materials.	Jun 2019
B18-Core EXAFS	Earth-abundant mixed-metal catalysts for hydrocarbon oxygenation James R. Pankhurst , Massimiliano Curcio , Stephen Sproules , Guy C. Lloyd-Jones , Jason B. Love Inorganic Chemistry DOI: 10.1021/acs.inorgchem.8b00420 Diamond Proposal Number(s): [15756] Show Abstract ▼ Abstract: A Cu2 Pacman complex acts as a cooperative catalyst for the oxygenation of benzylic C−H bonds by organic peroxides when activated by ferric chloride (FeCl3). Analytical and solution spectroscopies suggest that an interaction between the dinuclear Cu unit and the chloride of FeCl3 occurs, and a full kinetic modeling of the reaction reveals a network of oxidation pathways, via the formation of metal-associated radical intermediates.	Apr 2018
B18-Core EXAFS	A simple primary amide for the selective recovery of gold from secondary resources Euan D. Doidge , Innis Carson , Peter A. Tasker , Ross J. Ellis , Carole A. Morrison , Jason B. Love Angewandte Chemie International Edition 55, 12436 - 12439 DOI: 10.1002/anie.201606113 Diamond Proposal Number(s): [14310] Show Abstract ▼ Abstract: Waste electrical and electronic equipment (WEEE) such as mobile phones contains a plethora of metals of which gold is by far the most valuable. Herein a simple primary amide is described that achieves the selective separation of gold from a mixture of metals typically found in mobile phones by extraction into toluene from an aqueous HCl solution; unlike current processes, reverse phase transfer is achieved simply using water. Phase transfer occurs by dynamic assembly of protonated and neutral amides with [AuCl4]− ions through hydrogen bonding in the organic phase, as shown by EXAFS, mass spectrometry measurements, and computational calculations, and supported by distribution coefficient analysis. The fundamental chemical understanding gained herein should be integral to the development of metal-recovery processes, in particular through the use of dynamic assembly processes to build complexity from simplicity.	Sep 2016
I19-Small Molecule Single Crystal Diffraction	Inter- versus intramolecular structural manipulation of a dichromium(II) pacman complex through pressure variation Charlotte J. Stevens , Alessandro Prescimone , Floriana Tuna , Eric J. L. Mcinnes , Simon Parsons , Carole A. Morrison , Polly L. Arnold , Jason B. Love Inorganic Chemistry 55, 214 - 220 DOI: 10.1021/acs.inorgchem.5b02151 Diamond Proposal Number(s): [9205] Show Abstract ▼ Abstract: The effect of pressure on the intranuclear M···M separation and intermolecular secondary interactions in the dinuclear chromium Pacman complex [Cr2(L)](C6H6) was evaluated because this compound contains both a short Cr···Cr separation and an exogenously bound molecule of benzene in the solid state. The electronic structure of [Cr2(L)] was determined by electron paramagnetic resonance spectroscopy, SQUID magnetometry, and density functional theory calculations and shows a diamagnetic ground state through antiferromagnetic exchange, with no evidence for a Cr−Cr bond. Analysis of the solid-state structures of [Cr2(L)](C6H6) at pressures varying from ambient to 3.0 GPa shows little deformation in the Cr···Cr separation, i.e., no Cr−Cr bond formation, but instead a significantly increased interaction between the exogenous arene and the chromium iminopyrrolide environment. It is therefore apparent from this analysis that [Cr2(L)] would be best exploited as a rigid chemical synthon, with pressure regulation being used to mediate the approach and secondary interactions of possible substrates.	Jan 2016

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