Crystal system: cubic
| a: | 11.2499 (±0.0004) Å |
| b: | 11.2499 (±0.0004) Å |
| c: | 11.2499 (±0.0004) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: Solid CsBr, BiBr, 9-M HBr, Solid AgBr
Product: red-orange crystals
Description: First, solid CsBr (0.426 g, 2.00 mmol) and BiBr (0.449 g, 1.00 mmol) were dissolved in 10 mL of 9-M HBr. Afterward, solid AgBr (0.188 g, 1.00 mmol) was added to the mixture. The vial was then capped, heated to 110º C for 2 hours, and cooled to room temperature by controlling the cooling rate to 2ºC/hr or 1ºC/hr. The obtained crystals were filtered on a glass frit and dried under low pressure overnight.
Method: X-ray diffraction
Description: A crystal was coated in Paratone-N oil, placed on a Kapton loop, and transferred to a Bruker D8 Venture diffractometer with a Photon 100 CMOS detector. Data was collected using ωv and ψ scans with 18-keV synchrotron radiation (λ = 0.68880 Å)
Crystal system: cubic
| a: | 11.27123 (±0.00011) Å |
| b: | 11.27123 (±0.00011) Å |
| c: | 11.27123 (±0.00011) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: Cs2CO3 (99+%, Strem Chemicals), HBr (Fluka, ≥48%), AgNO3 (99.9+%, Alfa Aesar), KBr (99+%, Alfa Aesar), Bi2O3 (≥99.0%, J.T. Baker)
Product: Polycrystalline Cs2AgBiCl6
Description: Cs2CO3 was reacted with HBr to prepare CsBr. The solution was evaporated, and the resulting solids were filtered and washed with ethanol. AgBr was precipitated by mixing aqueous solutions of AgNO3 and KBr. BiBr3 was prepared by reacting Bi2O3 with HBr. The mixture was heated until fully dissolved, evaporated to dryness, and then filtered and washed with ethanol. Then, 8 mL of 8.84 M HBr and 2 mL of a 50% solution of H3PO2 were mixed and heated to 120 °C. To it, 1.41 mmol of AgBr and an equal amount of BiBr3 were added. When dissolved, 2.82 mmol of CsBr 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.