[NiEn 3]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. Gromilov

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4 Citations (Scopus)

Abstract

The synthesis method for [NiEn3]WO4 complex salt is described. Data of single crystal X-ray diffraction at 115 K are: space group p3 ¯ , 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 p3 ¯ 1 c, 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.

Original languageEnglish
Pages (from-to)1897-1902
Number of pages6
JournalJournal of Structural Chemistry
Volume59
Issue number8
DOIs
Publication statusPublished - 1 Dec 2018

Keywords

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

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