[NiEn3]MoO4: Features of the Phase Transition and Thermal Decomposition in the Presence of Lithium Hydride

A. S. Sukhikh, S. P. Khranenko, V. Yu Komarov, D. P. Pishchur, R. E. Nikolaev, P. S. Buneeva, P. E. Plyusnin’, S. A. Gromilov

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Abstract

The crystal structural characteristics of the [NiEn3]MoO4 complex salt (En is ethylenediamine) at 90 K are as follows: space group P3¯,a=15.9307(9)Å´,c=9.9238(6)Å´,V=2181.1(3)Å´3,Z=6,dx=1.822g/cm3, Ni-N is 2.1182(12)−2.1498(11)Å´, ∠Ni-N-N is 80.76(4)-82.27(4)°. According to the differential scanning calorimetry data in a range from 295 K to 310 K, there is a thermal anomaly with peaks at T1 = 299.6 K and T2 = 304.7 K. The crystal structural characteristics at 320 K are as follows: space group P3¯1c,a=9.2491(4)Å´,c=9.9713(4)Å´,V=738.72(7)Å´3,Z=2,dx=1.794g/cm3, Ni-N is 2.1302 (14) Å´, ∠N-Ni-N is 80.96(8)°. With increasing temperature from 90 K to 320 K a decrease in the average Mo-O distance from 1.769 Å´ to 1.725 Å´ is observed in the structure. The comparative analysis of the interionic N-H…O and C-H…O contacts is carried out. The ex situ powder X-ray diffraction study of the formation process of metal and carbide phases by the [NiEn3]MoO4 thermal decomposition in the presence of LiH in the He atmosphere is performed. At the temperature of 1323 K a Mo2C and MoNi4 phase mixture forms in the first minute. With increasing keeping time the Ni2Mo4Cx phase forms.

Original languageEnglish
Pages (from-to)780-788
Number of pages9
JournalJournal of Structural Chemistry
Volume60
Issue number5
DOIs
Publication statusPublished - 1 May 2019

Keywords

  • complex salt
  • crystal chemistry
  • differential scanning calorimetry
  • molybdate anion
  • thermal decomposition
  • tris(ethylenediamine)nickel
  • X-ray diffraction analysis
  • EXPANSION
  • GROWTH
  • CRYSTAL-STRUCTURES

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