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Na3SbS3 was prepared by the reaction of anhydrous Na2S, 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 Na3SbS3 for two weeks at 720 K. The crystal structure of Na3SbS3 was determined by single‐crystal X‐ray diffraction at 123 K. Na3SbS3 crystallizes in the cubic space group P213 (No....
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