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.
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Original Russian Text © 2018 S. P. Khranenko, A. S. Sukhikh, D. P. Pishchur, P. S. Buneeva, V. Yu. Komarov, S. A. Gromilov.
Translated from Zhurnal Strukturnoi Khimii, Vol. 59, No. 8, pp. 1960–1966, November-December, 2018.
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Khranenko, S.P., Sukhikh, A.S., Pishchur, D.P. et al. [NiEn3]WO4. Crystal Structural Features Of The Phase Transition At 269 K. J Struct Chem 59, 1897–1902 (2018). https://doi.org/10.1134/S0022476618080188
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DOI: https://doi.org/10.1134/S0022476618080188