Crystal system: monoclinic
| a: | 11.3748 (±0.0002) Å |
| b: | 8.729 (±0.0001) Å |
| c: | 29.2867 (±0.0004) Å |
| α: | 90° |
| β: | 95.004 (±0.001)° |
| γ: | 90° |
Starting materials: PbI2, HI (47%), HSC2H4NH2·HCl
Product: Yellow 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 yellow crystals were used for the experiment.
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.