001022220 001__ 1022220 001022220 005__ 20240311125735.0 001022220 0247_ $$2doi$$a10.3390/cryst13121670 001022220 0247_ $$2datacite_doi$$a10.34734/FZJ-2024-01341 001022220 0247_ $$2WOS$$aWOS:001132741600001 001022220 037__ $$aFZJ-2024-01341 001022220 082__ $$a540 001022220 1001_ $$00009-0004-3983-427X$$aHareesh, Chavana$$b0 001022220 245__ $$aSynthesis and Structural Characterization of Layered Ni$^{+1/+2}$ Oxides Obtained by Topotactic Oxygen Release on Nd$_{2−x}$Sr$_{x}$NiO$_{4−δ}$ Single Crystals 001022220 260__ $$aBasel$$bMDPI$$c2023 001022220 3367_ $$2DRIVER$$aarticle 001022220 3367_ $$2DataCite$$aOutput Types/Journal article 001022220 3367_ $$0PUB:(DE-HGF)16$$2PUB:(DE-HGF)$$aJournal Article$$bjournal$$mjournal$$s1708328164_14975 001022220 3367_ $$2BibTeX$$aARTICLE 001022220 3367_ $$2ORCID$$aJOURNAL_ARTICLE 001022220 3367_ $$00$$2EndNote$$aJournal Article 001022220 520__ $$aLayered nickelate oxides containing Ni$^{1+}$/Ni$^{2+}$ are isoelectronic to Cu$^{2+}$/Cu$^{3+}$ compounds and of present interest with respect to recent findings of superconductivity in a series of different compositions. It is thereby questionable why superconductivity is still rare to find in nickelates, compared to the much larger amount of superconducting cuprates. Anisotropic $d_{z^2}$ vs. $d_{x^2−y^2}$ orbital occupation as well as interface-induced superconductivity are two of the main advanced arguments. We are here interested in investigating the feasibility of synthesizing layered nickelate-type oxides, where the Ni$^{1+}$/Ni$^{2+}$ ratio can be tuned by oxygen and/or cation doping. Our strategy is to synthesize Sr-doped $n$ = 1 Ruddlesden–Popper type Nd$_{2−x}$Sr$_x$NiO$_{4+δ}$ single crystals, which are then reduced by H$_2$ gas, forming Nd$_{2−x}$Sr$_x$NiO$_{4−δ}$ via a topotactic oxygen release at moderate temperatures. We report here on structural studies carried out on single crystals by laboratory and synchrotron diffraction using pixel detectors. We evidence the general possibility to obtain reduced single crystals despite their increased orthorhombicity. 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