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The crystal structure of bis(1,4-dithioniumdicyclo-[2,2,2]-octane) μ-oxo-bis[tetracyanooxorhenate(V)]tetrahydrate
Authors:Stephen S Basson  Johann G Leipoldt  Andreas Roodt  Walter Purcell
Institution:(1) Department of Chemistry, University of the Orange Free State, Bloemfontein, Republic of South Africa
Abstract:Summary The structure of S(CH2CH2)3S]2Re2O3(CN)8]·4H2O has been determined from three-dimensional x-ray diffraction data. The blue crystals are monoclinic, space group P21/c, with cell dimensionsa=9.431(2),b=10.879(2),c=16.217(3)Å, beta=110.84(2)°,Z=2 andD m=2.11 gcm–3. Anisotropic refinement by least-squares methods of 2483 observed reflections converged toR=0.050.The centrosymmetric binuclear anion has a linear O=Re–O–Re=O grouping with an eclipsed configuration for the cyano ligands. Bond distances: Re–O (terminal)=1.69(1), Re–O (bridging)=1.921(1) and Re–Cav=2.12(2)Å. Each Re atom is displaced by 0.11(2)Å towards the terminal oxygen atom giving a slight square-pyramidal distortion of the octahedral environment. The ring-constrained cation has C–Sav=1.82(2)Å with averaged bond angles C–S–C=101(1) and S–C–C=113(1)°.
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