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Zeitschrift für Kristallographie - Crystalline Materials

Editor-in-Chief: Pöttgen, Rainer

Ed. by Antipov, Evgeny / Boldyreva, Elena V. / Friese, Karen / Huppertz, Hubert / Jahn, Sandro / Tiekink, E. R. T.

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Volume 232, Issue 12


Synthesis, synchrotron diffraction study and twinning in Na2Ca4Mg2Si4O15 – a heteropolyhedral framework compound

Volker Kahlenberg
  • Corresponding author
  • Institut für Mineralogie und Petrographie, Universität Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
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/ Daniela Schmidmair
  • Institut für Mineralogie und Petrographie, Universität Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
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  • De Gruyter OnlineGoogle Scholar
/ Elias Hildebrandt
  • Institut für Mineralogie und Petrographie, Universität Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
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/ Patrick Ennemoser
  • Institut für Mineralogie und Petrographie, Universität Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
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/ Klaus Zöll
  • Institut für Mineralogie und Petrographie, Universität Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
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/ Hannes Krüger
  • Institut für Mineralogie und Petrographie, Universität Innsbruck, Innrain 52, A-6020 Innsbruck, Austria
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Published Online: 2017-06-29 | DOI: https://doi.org/10.1515/zkri-2017-2063


The formation of polycrystalline Na2Ca4Mg2Si4O15 from solid state reactions has been studied between 800 and 1050°C. Single crystals of the compound have been grown in a closed platinum capsule by slow cooling in the temperature range between 1300 and 1000°C. Basic crystallographic data are as follows: monoclinic symmetry, space group P12/c1, a=7.1717(3) Å, b=5.3512(2) Å, c=16.4789(7) Å, β=90.911(4)°, V=632.33(4) Å3, Z=2. A conspicuous feature of the crystals is an intensive lamellar non-merohedral twinning clearly observable already under a petrographic microscope. The diffraction pattern can be explained as a superposition of two reciprocal lattices with a two-fold axis parallel to [001] being the twin element. Using synchrotron radiation it was possible to solve the crystal structure of Na2Ca4Mg2Si4O15 from a twinned data set. Least-squares refinements resulted in a residual of R(|F|)=0.031 for 2899 observed reflections with I>2σ(I) and 127 parameters. The crystal structure contains both [Si2O7]-dimers and insular [SiO4]-moieties. Tetrahedra and [MgO6]-octahedra form a three-dimensional framework whose topological characteristics have been studied. The remaining calcium and sodium cations are distributed among four crystallographically independent positions located in voids of the network. On a microscopic scale the twinning observed in the diffraction experiments could be explained by the existence of a 21-screw axis parallel to [001] in (¼, 0, z) mapping both domains onto each other. A comparison with related compounds having an A+2B2+6Si4O15 stoichiometry is presented. More than 25 years after its first observation in refractories our investigation clarifies the crystal structure of a silicate that is of relevance for both Materials science and high pressure research.

This article offers supplementary material which is provided at the end of the article.

Keywords: crystal growth; heteropolyhedral framework; Na2Ca4Mg2Si4O15; solid-state reactions; synchrotron diffraction; twinning


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About the article

Received: 2017-04-07

Accepted: 2017-05-22

Published Online: 2017-06-29

Published in Print: 2017-11-27

Citation Information: Zeitschrift für Kristallographie - Crystalline Materials, Volume 232, Issue 12, Pages 815–825, ISSN (Online) 2196-7105, ISSN (Print) 2194-4946, DOI: https://doi.org/10.1515/zkri-2017-2063.

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