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Zeitschrift für Naturforschung B

A Journal of Chemical Sciences

12 Issues per year


IMPACT FACTOR 2017: 0.757

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1865-7117
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Volume 45, Issue 1

Issues

Ammonium Hexavanadate, (NH4)2V6O16: Preparation, Crystal Structure, Infrared Spectra and High-Pressure Reactions

Klaus-Jürgen Range
  • Institute of Inorganic Chemistry, University of Regensburg, Universitätsstraße 31, D-8400 Regensburg, FRG
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Christiane Eglmeier
  • Institute of Inorganic Chemistry, University of Regensburg, Universitätsstraße 31, D-8400 Regensburg, FRG
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Danita de Waal / Anton M. Heyns
Published Online: 2014-06-02 | DOI: https://doi.org/10.1515/znb-1990-0108

Abstract

Following a re-examination of several published methods for the preparation of ammonium

hexavanadate, single crystals of (NH4)2V6O16 have been grown by a reaction of V2O5 with

NH4Cl in hot aqueous solution. They are monoclinic, space group P 21/m , with a = 7.858(2),

b = 8.412(2), c = 4.995(1) Å , β = 96.43(2)°, and Z = 1. The structure was refined to R = 0.060,

wR = 0.039 for 745 unique reflections. It comprises layers built of V2O8 double square pyramids

( V - O = 1.595- 1.988 Å) and distorted VO6 octahedra ( V - O = 1.589-2.287 Å). The infrared

bands of the NH4+- and ND4+- groups in (NH4)2V6O16 and its deuterated analogue can be

assigned with a fair amount of certainty at 90 K under the space group P 21/m (C2h2). The N - D

stretching modes of isotopically diluted NH3D+-groups in (NH4)2V6O16 are in agreement with

the predicted splitting into Cs, Cs and C1(2) components. The frequencies and shapes of these

modes seem to suggest that bifurcated hydrogen bonds are formed, closely resembling the corresponding

bonds in NH4VO3. The NH4+ ions are dynamic in character in (NH4)2V6O16 and

remain so down to temperatures of 90 K. At high temperatures in a closed high-pressure system

a redox reaction between vanadium (V ) and ammonia takes place which yields VO2 as

main product. Intermediates have been found, but up to now their com position is still unknown.

Keywords: Ammonium Hexavanadate; Preparation; Crystal Structure; Infrared Spectra; High-Pressure Reactions

About the article

Received: 1989-09-11

Published Online: 2014-06-02

Published in Print: 1990-01-01


Citation Information: Zeitschrift für Naturforschung B, Volume 45, Issue 1, Pages 31–38, ISSN (Online) 1865-7117, ISSN (Print) 0932-0776, DOI: https://doi.org/10.1515/znb-1990-0108.

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© 1946 – 2014: Verlag der Zeitschrift für Naturforschung. This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License. BY-NC-ND 3.0

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