Starting materials: Cs2CO3 (99+%, Strem Chemicals), HCl (Sigma-Aldrich, 37%), AgNO3 (99.9+%, Alfa Aesar), NaCl (ACS Reagent, GFS Chemicals), BiCl3 (≥98%, Aldrich)

Product: Polycrystalline Cs2AgBiCl6

Description: Cs2CO3 was reacted with HCl to prepare CsCl. The solution was evaporated, and the resulting solids were filtered and washed with ethanol. AgCl was precipitated by mixing aqueous solutions of AgNO3 and NaCl. Then, 8 mL of 12.1 M HCl and 2 mL of a 50% solution of H3PO2 were mixed and heated to 120 °C. To it, 1.89 mmol of AgCl and an equal amount of BiCl3 were added. When dissolved, 3.78 mmol of CsCl was added. The precipitate was collected [possibly after cooling down the solution to room temperature] on filter paper, washed with ethanol, and dried overnight.

Method: X-ray Powder Diffraction

Description: Powder XRD data were collected on a Bruker D8 powder diffractometer (40 kV, 50 mA, sealed Cu X-ray tube) equipped with an incident beam Ge 111 monochromator and Lynx Eye position-sensitive detector.