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Na 3 SbS 3 : Single Crystal X‐ray Diffraction, Raman Spectroscopy, and Impedance Measurements
Author(s) -
Pompe Constantin,
Pfitzner Arno
Publication year - 2013
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201200511
Subject(s) - raman spectroscopy , crystallography , single crystal , crystal structure , antimony , analytical chemistry (journal) , octahedron , chemistry , coordination number , x ray crystallography , materials science , diffraction , inorganic chemistry , ion , physics , organic chemistry , chromatography , optics
Na 3 SbS 3 was prepared by the reaction of anhydrous Na 2 S, antimony, and sulfur in a ratio of 3:2:3 at 870 K. The pale yellow compound is air and moisture sensitive. A microcrystalline sample was obtained after annealing Na 3 SbS 3 for two weeks at 720 K. The crystal structure of Na 3 SbS 3 was determined by single‐crystal X‐ray diffraction at 123 K. Na 3 SbS 3 crystallizes in the cubic space group P 2 1 3 (No. 198) with a = 8.6420(1) Å, V = 645.42(1) Å 3 and Z = 4. The structure refinement converged to R = 0.0099 ( wR = 0.0181) for 592 independent reflections and 23 parameters. Na 3 SbS 3 is isotypic with Na 3 AsS 3 . Sodium atoms are located on three different sites, which show a strongly distorted octahedral coordination sphere of sulfur. The coordination polyhedra of equivalent sodium sites share common vertices, whereas those of different sodium sites share common faces. Antimony and sulfur form trigonal SbS 3 pyramids, which coordinate sodium as a mono‐, bi‐, or tridentate ligand. Raman spectroscopic investigations result in stretching modes ν(Sb–S) at 334, 321, and 312 cm –1 , respectively. Thermoanalytical studies do not show any additional thermal effects up to the melting point of 875 K. Impedance spectroscopy on Na 3 SbS 3 in a range from 325 to 570 K shows a temperature dependent Na + conductivity, which is 1.9 × 10 –6 Ω –1 · cm –1 at 570 K.