The ternary compounds Tl2AgX3 (X = Cl, Br, I) were obtained as colorless single crystals by reaction of the binary halides AgX and TlX (X = Cl, Br, I) together with concentrated HX solutions under hydrothermal conditions. Silica glass ampoules were filled to 50 % with these solutions and heated for several days up to 250 °C. The reaction was carried out in steel autoclaves to prevent bursting. All the compounds are isostructural and crystallize trigonally with the already known Tl2AgI3 type (R3, Z = 9), but Tl2AgCl3 [a = 9.5075(6), c = 18.585(2) Å, R1 = 0.035, wR2 = 0.062] and Tl2AgBr3 [a = 9.8758(6), c = 19.1532(14) Å, R1 = 0.046, wR2 = 0.085] were characterized for the first time. The crystal structure consists of unique [Ag3X8]5– units, which are formed by a central [AgX6]5– octahedron with two face‐sharing [AgX4]4– tetrahedra in trans position. The Ag+···Ag+ distance is nearly independent from the anion size and amounts to 3.13–3.16 Å. The distance results just from repulsive interactions. Vibrational spectra were recorded for the complete series. DTA measurements confirm the peritectic formation of both compounds with X = Cl and Br.
Zaac-Journal of Inorganic and General Chemistry – Wiley
Published: Jan 15, 2018
Keywords: ; ; ; ;
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