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Instruments / Technical Area	Publication Details	Published
I11-High Resolution Powder Diffraction	Evidence of paracrystalline cation order in the ruddlesden–popper phase LaSr3NiRuO8 through neutron total scattering techniques Margaret Lea Robinson , Ernestine Whitaker , Lun Jin , Michael A. Hayward , Geneva Laurita Inorganic Chemistry DOI: 10.1021/acs.inorgchem.9b03382 Diamond Proposal Number(s): [13284] Show Abstract ▼ Abstract: Cation ordering in perovskite-derived phases can lead to a wealth of tunable physical properties. Ordering is typically driven by a large difference between the cation size and charge, but many Ruddlesden–Popper phases An+1BnO3n+1 appear to lack such B-site ordering, even when these differences are present. One such example is the “double” Ruddlesden–Popper n = 1 composition LaSr3NiRuO8. In this material, a lack of B-site ordering is observed through traditional crystallographic techniques, but antiferromagnetic ordering in the magnetism data suggests that B-site cation ordering is indeed present. Neutron total scattering, particularly analysis of the neutron pair distribution function, reveals that the structure is locally B-site-ordered below 6 Å but becomes slightly disordered in the midrange structure around 12 Å. This provides evidence for paracrystalline order in this material: cation ordering within a single perovskite sheet that lacks perfect registry within the three-dimensional stack of sheets. This work highlights the importance of employing a structural technique that can probe both the local and midrange order in addition to the crystallographic structure and provides a structural origin to the observed magnetic properties of LaSr3NiRuO8. Further, it is proposed that paracrystalline order is likely to be common among these layered-type oxides.	Feb 2020
I11-High Resolution Powder Diffraction	Hole and electron doping of the 4d transition‐metal oxyhydride LaSr3NiRuO4H4 Lun Jin , Michael A. Hayward Angewandte Chemie International Edition 59, 2076 - 2079 DOI: 10.1002/anie.201913951 Diamond Proposal Number(s): [13284] Show Abstract ▼ Abstract: Hole or electron doping of phases prepared by topochemical reactions (e.g. anion deintercalation or anion‐exchange) is extremely challenging as these low‐temperature conversion reactions are typically very sensitive to the electron counts of precursor phases. Herein we report the successful hole and electron doping of the transition‐metal oxyhydride LaSr3NiRuO4H4 by first preparing precursors in the range LaxSr4−xNiRuO8 0.5	Jan 2020
I11-High Resolution Powder Diffraction	Exsolution of SrO during the topochemical conversion of LaSr3CoRuO8 to the oxyhydride LaSr3CoRuO4H4 Lun Jin , Maria Batuk , Franziska K. K. Kirschner , Franz Lang , Stephen J. Blundell , Joke Hadermann , Michael A. Hayward Inorganic Chemistry DOI: 10.1021/acs.inorgchem.9b02552 Diamond Proposal Number(s): [13284] Show Abstract ▼ Abstract: Reaction of the n = 1 Ruddlesden–Popper oxide LaSr3CoRuO8 with CaH2 yields the oxyhydride phase LaSr3CoRuO4H4 via a topochemical anion exchange. Close inspection of the X-ray and neutron powder diffraction data in combination with HAADF-STEM images reveals that the nanoparticles of SrO are exsolved from the system during the reaction, with the change in cation stoichiometry accommodated by the inclusion of n > 1 (Co/Ru)nOn+1H2n “perovskite” layers into the Ruddlesden–Popper stacking sequence. This novel pseudotopochemical process offers a new route for the formation of n > 1 Ruddlesden–Popper structured materials. Magnetization data are consistent with a LaSr3Co+Ru2+O4H4 (Co+, d8, S = 1; Ru2+, d6, S = 0) oxidation/spin state combination. Neutron diffraction and μ+SR data show no evidence for long-range magnetic order down to 2 K, suggesting the diamagnetic Ru2+ centers impede the Co–Co magnetic-exchange interactions.	Oct 2019
I11-High Resolution Powder Diffraction	LaSr3NiRuO4H4: a 4d transition-metal oxide-hydride containing metal hydride sheets Lun Jin , Michael Lane , Dihao Zeng , Franziska K. K. Kirschner , Franz Lang , Pascal Manuel , Stephen J. Blundell , John E. Mcgrady , Michael Hayward Angewandte Chemie International Edition DOI: 10.1002/anie.201800989 Diamond Proposal Number(s): [13284] Show Abstract ▼ Abstract: We report the synthesis of the first 4d transition metal oxide‐hydride, LaSr3NiRuO4H4, prepared via topochemical anion exchange. Neutron diffraction data show that the hydride ions occupy the equatorial anion sites in the host lattice and as a result the Ru and Ni cations are located in a plane containing only hydride ligands ‐ a unique structural feature with obvious parallels to the CuO2 sheets present in the superconducting cuprates. DFT calculations confirm the presence of S = ½ Ni1+ and S = 0, Ru2+ centres, but neutron diffraction and μSR data show no evidence for long‐range magnetic order between the Ni centres down to 1.8 K. The observed weak inter‐cation magnetic coupling can be attributed to poor overlap between Ni 3d_(z^2 ) and H 1s in the super‐exchange pathways.	Mar 2018

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