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Isolation of an Asymmetric Lanthanide Polyoxometalate, Na12H[(W5O18)Tb(H2W11O39)]·42H2O, Containing Two Distinct Isopolyanions

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Abstract

The structural characterization of a new, asymmetric polyoxoanion, Na12H[(W5O18)Tb(H2W11O39)]·42H2O, is reported herein. This new structure was isolated from a mixture of a number of compounds, including the symmetric Na9[Tb(W5O18)2] sandwich cluster, and the lanthanide-free cluster, Na10(H2W12O42). The major product of the reaction was Na9[Tb(W5O18)2], and the compound reported here is a minor product that is obtained reproducibly. The salts of these three clusters do not differ significantly in their crystal habit, size, and color. The crystal structure of Na12H[(W5O18)Tb(H2W11O39)]·42H2O was determined by single-crystal X-ray diffraction and shows that the cluster is composed of a lacunary Lindqvist (W5O18)6− building block and an unusual lacunary metatungstate (H2W11O39)10− polyanion connected through a central Ln3+ cation. The central Tb3+ cation has a square antiprismatic symmetry, the lacunary metatungstate has a square pyramidal symmetry, and the lacunary Lindqvist polyanion exhibits a cuboctahedral symmetry. This is the first example of a crystallographically characterized sandwich cluster possessing a lacunary metatungstate (H2W11O39)10− ligand.

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Notes

  1. Crystal data for Na12H[(W5O18)Tb(H2W11O39)]·42H2O: M = 5048.10, triclinic, a = 13.4052(7) Ǻ, b = 16.1979(9) Ǻ, c = 20.9109(11) Ǻ, α = 74.693(1)°, β = 88.069(1)°, γ = 88.369(1)°, V = 4376.0(4) Ǻ3, T = 140(2) K, space group P−1, Z = 2, μ(Mo Kα) = 21.922 mm−1, 49214 reflections measured, 19559 independent reflections (Rint = 0.0468). The final R1 value was 0.0367 for I > 2σ(I), 0.0480 for all data. The final wR(F2) value was 0.0818 for I > 2σ(I), 0.0861 for all data. The goodness-of-fit on F2 was 1.059.

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Acknowledgments

The authors gratefully acknowledge the support of this work by the U.S. Department of Energy through the LANL/LDRD Program. Los Alamos National Laboratory is operated by Los Alamos National Security, LLC, for the National Nuclear Security Administration of the U.S. Department of Energy under contract DE-AC52-06NA25396.

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Authors and Affiliations

  1. Chemical Diagnostics and Engineering, Los Alamos National Laboratory, PO BOX 1663, Mail Stop J964, Los Alamos, NM, 87545, USA

    Denisse Ortiz-Acosta

  2. Materials Chemistry, Los Alamos National Laboratory, PO Box 1663, Mail Stop J514, Los Alamos, NM, 87545, USA

    Russell K. Feller, Brian L. Scott & Rico E. Del Sesto

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  1. Denisse Ortiz-Acosta
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  2. Russell K. Feller
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  4. Rico E. Del Sesto
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Correspondence to Rico E. Del Sesto.

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Ortiz-Acosta, D., Feller, R.K., Scott, B.L. et al. Isolation of an Asymmetric Lanthanide Polyoxometalate, Na12H[(W5O18)Tb(H2W11O39)]·42H2O, Containing Two Distinct Isopolyanions. J Chem Crystallogr 42, 651–655 (2012). https://doi.org/10.1007/s10870-012-0311-z

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