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Journal of Structural Chemistry

, Volume 59, Issue 8, pp 1897–1902 | Cite as

[NiEn3]WO4. Crystal Structural Features Of The Phase Transition At 269 K

  • S. P. Khranenko
  • A. S. Sukhikh
  • D. P. Pishchur
  • P. S. Buneeva
  • V. Yu. Komarov
  • S. A. GromilovEmail author
Article
  • 3 Downloads

Abstract

The synthesis method for [NiEn3]WO4 complex salt is described. Data of single crystal X-ray diffraction at 115 K are: space group \(p\bar 3\), a = 15.9633(5) Å, c = 9.9446(4) Å, V = 2194.6(1) Å3, Z = 6, dx = 2.210 g/cm3, Ni–N is 2.120(2)-2.149(2) Å, ∠N–Ni–N is 80.69(7)-82.28(7)°. From the differential scanning calorimetry data it is found that a phase transition occurs at 269 K. The crystal structural characteristics at 298 K are as follows: space group \(p\bar 31c\), a = 9.2641(3) Å, c = 9.9817(3) Å, V = 741.89(4) Å3, Z = 2, dx = 2.179 g/cm3, Ni–N is 2.128(2) Å, ∠N–Ni–N is 81.05(12)°. The phase transition is shown to correspond to the disordering of tungstate anions over three positions. The comparative analysis of N–H…O and C–H…O interionic contacts is performed.

Keywords

bimetallic complex salt tris(ethylenediamine)nickel tungstate anion differential scanning calorimetry single crystal X-ray diffraction analysis crystal chemistry 

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Copyright information

© Pleiades Publishing, Ltd. 2018

Authors and Affiliations

  • S. P. Khranenko
    • 1
  • A. S. Sukhikh
    • 1
    • 2
  • D. P. Pishchur
    • 1
    • 2
  • P. S. Buneeva
    • 1
    • 2
  • V. Yu. Komarov
    • 1
    • 2
  • S. A. Gromilov
    • 1
    • 2
    Email author
  1. 1.Nikolaev Institute of Inorganic Chemistry, Siberian BranchRussian Academy of SciencesNovosibirskRussia
  2. 2.Novosibirsk State UniversityNovosibirskRussia

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