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Crystal structures of Co3(SeO3)3·H2O and Ni3(SeO3)3·H2O, two new isotypic compounds

Die Kristallstrukturen von Co3(SeO3)3·H2O und Ni3(SeO3)3·H2O, zwei neue isotype Verbindungen

  • Anorganische Und Physikalische Chemie
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Summary

The crystal structures of the new, hydrothermally synthesized, isotypic compounds Co3(SeO3)3·H2O and Ni3(SeO3)3·H2O were determined by direct and Fourier methods and refined toR w=0.023, 0.032 using single crystal X-ray data up to sinϑ/λ=0.81 Å−1 [space group P\(\bar 1\),a=8.102 (2), 7.986 (3) Å;b=8.219 (2), 8.133 (3) Å;c=8.572 (2), 8.422 (3) Å, α=69.15 (1), 69.50 (1)°; β=62.88 (1), 62.50 (1)°; γ=67.23 (1), 67.64 (1)°;Z=2]. The structures are built up from [Me 5(SeO3)6·2H2O]2− sheets containing three crystallographically different types of octahedrally coordinatedMe 2+ and trigonal pyramidal coordinated Se4+ atoms, respectively. These sheets are linked only by a fourth type ofMe 2+[6] atom. All coordination polyhedra deviate significantly from their ideal shapes, bond lengths within the extremly distortedMe(4)O6 polyhedra range from 1.983 (2) Å to 2.403 (2) Å in Co3(SeO3)3·H2O and from 1.987 (4) Å to 2.301 (3) Å in the Ni compound, O-Se-O bond angles were found between 92.8 (2)° and 104.9 (1)°. Hydrogen bond lengths are 2.802 (3)Å and 2.600 (4)Å in the Co compound, and 2.762 (6) Å and 2.561 (6) Å in Ni3(SeO3)3·H2O. The latter is one of the shortest known hydrogen bonds donated by a water molecule.

Zusammenfassung

Die Kristallstrukturen der neuen, hydrothermal synthetisierten, isotypen Verbindungen Co3(SeO3)3·H2O und Ni3(SeO3)3·H2O wurden mit direkten und Fourier-Methoden bestimmt und unter Verwendung von Einkristallröntgendaten bis sinϑ/λ=0.81 Å−1 aufR w-Werte von 0.023, 0.032 verfeinert [Raumgruppe P\(\bar 1\),a=8.102 (2), 7.986 (3) Å;b=8.219 (2), 8.133 (3) Å;c=8.572 (2), 8.422 (3) Å, α=69.15 (1), 69.50 (1)°; β=62.88 (1), 62.50 (1)°; γ=67.23 (1), 67.64 (1)°;Z=2]. Die Strukturen werden von [Me 5(SeO3)6·2H2O]2− Schichten aufgebaut, die je drei kristallographisch unterschiedliche Arten von oktaedrisch koordiniertenMe 2+ und trigonal pyramidal koordinierten Se4+ Atomen enthalten. Diese Schichten sind nur durch eine vierte Art vonMe 2+[6] Atomen verknüpft. Alle Koordinationspolyeder weichen deutlich von ihren Idealformen ab, Bindungslängen in den extrem verzerrtenMe(4)O6 Polyedern variieren zwischen 1.983 (2) Å und 2.403 (2) Å in Co3(SeO3)3·H2O und zwischen 1.987 (4) Å und 2.301 (3) Å in der Ni-Verbindung, O-Se-O-Bindungswinkel liegen zwischen 92.8 (2)° und 104.9 (1)°. Wasserstoffbrückenlängen sind 2.802 (3) Å und 2.600 (4) Å in der Co-Verbindung, und 2.762 (6) Å und 2.561 (6) Å in Ni3(SeO3)3·H2O. Letztere ist eine der kürzesten bekannten Wasserstoffbrücken eines Wassermoleküls.

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  1. Institut für Mineralogie und Kristallographie, Universität Wien, A-1010, Wien, Austria

    Manfred Wildner

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Wildner, M. Crystal structures of Co3(SeO3)3·H2O and Ni3(SeO3)3·H2O, two new isotypic compounds. Monatsh Chem 122, 585–594 (1991). https://doi.org/10.1007/BF00811457

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