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Formation of Silicon-Containing Polyoxoniobates from Hexaniobate Under High Temperature Conditions

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Abstract

Hydrothermal reaction of K7H[Nb6O19]·13H2O with Na2SiO3·9H2O (220 °C, 24 h) produces a lacunary siliconiobate [Si4Nb16O56]16−, which was isolated as mixed salt NaK8H6[Na@Si4Nb16O56]·26H2O (1). Changing the silicon source to Ph2Si(OH)2 under the same conditions slightly improves the yield of [Si4Nb16O56]16−, which was isolated as K14H[K@Si4Nb16O56]·26H2O (2). Extending the reaction time leads to rearrangement of [Si4Nb16O56]16− into Keggin-type silicododecaniobate [SiNb12O40]16−, which was isolated and characterized as K8H2(Nb2O2)[SiNb12O40]·20H2O (3). The complexes were characterized by X-ray single crystal analysis, elemental analysis, thermogravimetry, 29Si NMR.

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Acknowledgements

This study was supported by Russian Science Foundation (Grant No. 14-13-00645). The authors thank Dr. Irina V. Kalinina for experimental help.

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Authors and Affiliations

  1. Nikolaev Institute of Inorganic Chemistry SB RAS, 3, Akad. Lavrentiev Ave, Novosibirsk, Russia, 630090

    P. A. Abramov, A. T. Davletgildeeva & M. N. Sokolov

  2. Novosibirsk State University, 2 Pirogova Ave, Novosibirsk, Russia, 630090

    P. A. Abramov, A. T. Davletgildeeva & M. N. Sokolov

Authors
  1. P. A. Abramov
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  2. A. T. Davletgildeeva
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  3. M. N. Sokolov
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Correspondence to P. A. Abramov.

Electronic Supplementary Material

Below is the link to the electronic supplementary material.

10876_2016_1121_MOESM1_ESM.docx

Supplementary material 1 (DOCX 3253 kb) Supporting information available 29Si NMR and FTIR. Crystallographic data in CIF format have been deposited at Cambridge Crystallographic Data Center on quoting the depository number CSD 431691 (1), 431692 (2), 431693 (3). Copies of this information may be obtained free of charge from http://www.ccdc.cam.ac.uk

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Abramov, P.A., Davletgildeeva, A.T. & Sokolov, M.N. Formation of Silicon-Containing Polyoxoniobates from Hexaniobate Under High Temperature Conditions. J Clust Sci 28, 735–744 (2017). https://doi.org/10.1007/s10876-016-1121-9

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  • DOI: https://doi.org/10.1007/s10876-016-1121-9

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