Startseite Naturwissenschaften Laboratory synthesis and characterization of Knasibfite K3Na4[SiF6]3[BF4] and the homologous Ge compound K3Na4[GeF6]3[BF4]
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Laboratory synthesis and characterization of Knasibfite K3Na4[SiF6]3[BF4] and the homologous Ge compound K3Na4[GeF6]3[BF4]

  • Jascha Bandemehr , Josefin Klippstein , Sergei I. Ivlev , Malte Sachs und Florian Kraus EMAIL logo
Veröffentlicht/Copyright: 29. Februar 2020
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Zeitschrift für Kristallographie - Crystalline Materials
Aus der Zeitschrift Zeitschrift für Kristallographie - Crystalline Materials Band 235 Heft 8-9

Abstract

Herein we present the synthesis, crystal structure, and the infrared and Raman spectra of K3Na4[SiF6]3[BF4]. The compound also occurs in nature as the mineral Knasibfite. We obtained it from the reaction of stoichiometric amounts of SiO2, Na[BF4], K2CO3, and Na2CO3 in hydrofluoric acid at room temperature. Hydrofluorothermal synthesis at 200 °C lead to a product of higher purity. Knasibfite is colorless and crystallizes in space group Im 2m with a = 5.546(2), b = 9.261(2), c = 17.184(4) Å, V = 882.5(4) Å3, Z = 2, at T = 400(2) K. At 342 K a phase transition to a monoclinic structure was observed (I 2, a = 5.5003(6), b = 9.0890(9), c = 17.0048(2) Å, β = 90.041(9)°, V = 852.2(2) Å3, Z = 2, T = 100(2) K). By replacing SiO2 with GeO2 as a starting material K3Na4[GeF6]3[BF4] was obtained. This compound also crystallizes in form of two polymorphs, both of which are isotypic to the respective ones of K3Na4[SiF6]3[BF4].

Keywords: crystal structure; hexafluoridogermanate; hexafluoridosilicate; Knasibfite; tetrafluoridoborate

Dedicated to: Prof. Dr. Ulrich Müller on the Occasion of his 80th Birthday.

Corresponding author: Prof. Dr. Florian Kraus, Fachbereich Chemie, Philipps-Universität Marburg, Hans-Meerwein-Str. 4, 35032 Marburg, Germany

Acknowledgements

We want to thank the DFG for funding, the X-ray facilities of Philipps University of Marburg (PUM), for their services, H. L. Deubner (PUM) for measuring Raman spectra and the department of Dr. Linne (PUM) for elemental analysis.

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Supplementary Material

The online version of this article offers supplementary material (https://doi.org/10.1515/zkri-2019-0068).

Received: 2019-12-09
Accepted: 2020-02-11
Published Online: 2020-02-29
Published in Print: 2020-09-25

©2020 Walter de Gruyter GmbH, Berlin/Boston

Artikel in diesem Heft

  1. Frontmatter
  2. In this issue
  3. Original papers
  4. Ulrich Müller zum 80. Geburtstag gewidmet
  5. Laboratory synthesis and characterization of Knasibfite K3Na4[SiF6]3[BF4] and the homologous Ge compound K3Na4[GeF6]3[BF4]
  6. The crystal structures of α-Rb7Sb3Br16, α- and β-Tl7Bi3Br16 and their relationship to close packings of spheres
  7. Beryllium triflates: synthesis and structure of BeL2(OTf)2 (L=H2O, THF, nBu2O)
  8. Synthesis and crystal structures of two layered Cu(I) and Ag(I) iodidometalates
  9. New mixed-valent alkali chain sulfido ferrates A1+x[FeS2] (A = K, Rb, Cs; x = 0.333–0.787)
  10. Structure solution of incommensurately modulated La6MnSb15
  11. Polymorphs of VO(PO3)2: synthesis and crystal structure refinement revisited
  12. On tungstates of divalent cations (III) – Pb5O2[WO6]
  13. Hydrogen order in hydrides of Laves phases
  14. High-pressure synthesis of SmGe3
  15. The complete series of sodium rare-earth metal(III) chloride oxotellurates(IV) Na2RE3Cl3[TeO3]4 (RE = Y, La–Nd, Sm–Lu)
  16. Structural diversity of salts of terpyridine derivatives with europium(III) located in both, cation and anion, in comparison to molecular complexes
  17. Elucidating structure–property relationships in imidazolium-based halide ionic liquids: crystal structures and thermal behavior
  18. Syntheses and crystal structures of the manganese hydroxide halides Mn5(OH)6Cl4, Mn5(OH)7I3, and Mn7(OH)10I4
  19. Site-preferential copper substitution for silicon leads to Cu-chains in the new ternary silicide Ir4−xCuSi2
  20. Syntheses and crystal structures of solvate complexes of alkaline earth and lanthanoid metal iodides with N,N-dimethylformamide
https://doi.org/10.1515/zkri-2019-0068
Schlagwörter für diesen Artikel
crystal structure; hexafluoridogermanate; hexafluoridosilicate; Knasibfite; tetrafluoridoborate

Artikel in diesem Heft

  1. Frontmatter
  2. In this issue
  3. Original papers
  4. Ulrich Müller zum 80. Geburtstag gewidmet
  5. Laboratory synthesis and characterization of Knasibfite K3Na4[SiF6]3[BF4] and the homologous Ge compound K3Na4[GeF6]3[BF4]
  6. The crystal structures of α-Rb7Sb3Br16, α- and β-Tl7Bi3Br16 and their relationship to close packings of spheres
  7. Beryllium triflates: synthesis and structure of BeL2(OTf)2 (L=H2O, THF, nBu2O)
  8. Synthesis and crystal structures of two layered Cu(I) and Ag(I) iodidometalates
  9. New mixed-valent alkali chain sulfido ferrates A1+x[FeS2] (A = K, Rb, Cs; x = 0.333–0.787)
  10. Structure solution of incommensurately modulated La6MnSb15
  11. Polymorphs of VO(PO3)2: synthesis and crystal structure refinement revisited
  12. On tungstates of divalent cations (III) – Pb5O2[WO6]
  13. Hydrogen order in hydrides of Laves phases
  14. High-pressure synthesis of SmGe3
  15. The complete series of sodium rare-earth metal(III) chloride oxotellurates(IV) Na2RE3Cl3[TeO3]4 (RE = Y, La–Nd, Sm–Lu)
  16. Structural diversity of salts of terpyridine derivatives with europium(III) located in both, cation and anion, in comparison to molecular complexes
  17. Elucidating structure–property relationships in imidazolium-based halide ionic liquids: crystal structures and thermal behavior
  18. Syntheses and crystal structures of the manganese hydroxide halides Mn5(OH)6Cl4, Mn5(OH)7I3, and Mn7(OH)10I4
  19. Site-preferential copper substitution for silicon leads to Cu-chains in the new ternary silicide Ir4−xCuSi2
  20. Syntheses and crystal structures of solvate complexes of alkaline earth and lanthanoid metal iodides with N,N-dimethylformamide
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