Abstract
The title compound, tetraethylammonium tetrathiorhenate, [(C2H5)4N][ReS4], has, at room temperature, a disordered structure in the space group P63mc (Z= 2, α-phase). A phase transition to the monoclinic space group P21 (Z= 2, γ-phase) at 285 K leads to a pseudo-merohedral twin. The high deviation from the hexagonal metric causes split reflections. However, the different orientations could not be separated, but were integrated using a large integration box. Rapid cooling to 110-170 K produces a metastable β-phase (P63, Z= 18) in addition to the γ-phase. All crystals of the β-phase are contaminated with the γ-phase. Additionally, the crystals of the β-phase are merohedrally twinned. In contrast to the α-phase, the β- and γ-phases do not show disorder.
Highlights
Salts with the ReS4À anion were synthesized for the first time in 1970 (Muller et al, 1970)
Was to verify that the unit cell of Et4NReS4 would be larger at room temperature. Another goal of this work was to investigate whether a phase transition to an ordered structure could be observed at lower temperatures
The crystal structure of the -phase at 297 K was refined in the space group P63mc (Table 1) starting from the structure of Et4NFeCl4 at 290 K (Lutz et al, 2014)
Summary
Salts with the ReS4À anion were synthesized for the first time in 1970 (Muller et al, 1970). 0.052, 0.138, 1.09 2814 87 89 2.01, À4.80 Twinning involves mirror, so Flack parameter cannot be determined – Computer programs: CrysAlis PRO (Oxford Diffraction, 2016), SHELXS97 (Sheldrick, 2008), SHELXL2018 (Sheldrick, 2015) and DIAMOND (Brandenburg, 2001). Was to verify that the unit cell of Et4NReS4 would be larger at room temperature. Another goal of this work was to investigate whether a phase transition to an ordered structure could be observed at lower temperatures
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