Crystal system: monoclinic
| a: | 17.795 (±0.001) Å |
| b: | 8.5195 (±0.0007) Å |
| c: | 23.1666 (±0.0015) Å |
| α: | 90° |
| β: | 98.719 (±0.005)° |
| γ: | 90° |
Starting materials: PbI2, HI (47%), HSC2H4NH2·HCl
Product: Orange crystals
Description: PbI2 (0.252 mmol; 0.116 g) was dissolved in 4 mL HI solution. Then HSC2H4NH2·HCl (0.880 mmol; 0.1 g) was added and immediately formed a yellow solid. The solution was then heated 90 degrees Celsius, causing the solution to become clear after a few minutes. The solution was then cooled to room temperature at the rate of 2 degrees per hour, causing yellow and orange crystals to precipitate. The orange crystals were the perovskite compound and the yellow crystals were (NH3(CH2)2S-S(CH2)2NH3)2PbI5·I.
Method: Single-crystal X-ray diffraction
Description: A Bruker SMART 1K CCD area detector diffractometer using Mo Kalpha radiation was used to measure SCXRD at 173 K. Omega-scans of width 0.3 degrees were used. The SAINT+ version 6.02 program was used for data reduction and the XPREP program was used for absorption corrections. SHELXS-97 was used to directly solve the structure. SHELXL-97 was used for refinement of the structure.