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Crystal Structures of Two New Holmium Polysulfides in the Series of Rare-Earth Polychalcogenides

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Abstract

The crystal structures of two polysulfide phases HoS1.885(5) (I) and HoS1.863(8) (II) were determined; the integer stoichiometric ratio was found to be Ho8S15. The data were collected on an Enraf-Nonius CAD-4 automatic diffractometer using the standard procedure (MoKα, graphite monochromator, an absorption correction applied based on ϕ-scan data). Crystal I: space group P4/nmm, a = 3.820(1), c = 7.840(3) Å, V = 114.40(6) Å3, Z = 2 for the composition HoS1.885(5), d calc = 6.542 g/cm3, R = 0.0520 for 184 unique reflections with Ihkl > 2 σI; crystal II: space group P21/m, a = 10.961(2), b = 11.465(2), c = 10.984(2) Å, β = 91.27(3)°, V = 1380.0(4) Å3, Z = 24 for the composition HoS1.863(8), d calc = 6.486 g/cm3, R = 0.0596 for 5354 unique reflections with Ihkl > 2 σI. In both compounds, the Ho atoms are surrounded by 9 (8+1 for three atoms in II) S atoms forming monocapped square antiprisms. The Ho–S distances vary from 2.717 to 3.067 Å irrespective of the type of ion [S2– or (S2)2–]; the maximal distance to the atoms completing the coordination is 3.684 Å. The compounds have PbFCl type structures composed of ...(S2)2–...Ho3+...S2–...S2–...Ho3+...(S2)2–... layer packets differently oriented in space relative to the unit cell axes. The S2–...S2– and S2–...(S2)2– interlayer distances are mostly shorter than the sum of the ionic radii and vary within the limits of 3.331-3.558 and 3.029-3.784 Å for the first and second types, respectively. For I, the calculated site occupancies and densities are given depending on the composition Ho-S2-x (x = 0.25-0); for II, the most probable formulas of rational compositions in the same range of x are presented.

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Authors and Affiliations

  1. Siberian Branch, Russian Academy of Sciences, Institute of Inorganic Chemistry, Novosibirsk

    N. V. Podberezskaya, N. V. Pervukhina, S. V. Belaya, I. G. Vasilieva & S. V. Borisov

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  1. N. V. Podberezskaya
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  2. N. V. Pervukhina
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  3. S. V. Belaya
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  4. I. G. Vasilieva
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  5. S. V. Borisov
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Podberezskaya, N.V., Pervukhina, N.V., Belaya, S.V. et al. Crystal Structures of Two New Holmium Polysulfides in the Series of Rare-Earth Polychalcogenides. Journal of Structural Chemistry 42, 617–627 (2001). https://doi.org/10.1023/A:1013198027339

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