Crystal system: triclinic
| a: | 9.2424 (±0.0005) Å |
| b: | 12.6314 (±0.0007) Å |
| c: | 14.3871 (±0.0008) Å |
| α: | 67.071 (±0.004)° |
| β: | 85.695 (±0.004)° |
| γ: | 88.087 (±0.004)° |
Starting materials: HI, H3PO2, SnI2, solid C(NH2)3I
Product: black crystals
Description: Aq HI (7.58M, 6.8mL) and aq H3PO2 (9.14M, 1.7mL) mixture in a flask was degassed by nitrogen. SnI2 (2mmol) was then dissolved into the mixture and the flask was brought to boiling at 130°C using an oil bath under constant stirring. Solid C(NH2)3I (4mmol) was added to the solution and then evaporated by heating at 120°C. Solution was left to cool, where red rectangular crystals precipitated. After cleaned and washed with EtOH, compound converted to black oxidized species.
Method: Single crystal X-ray diffraction
Description: SC-XRD was performed with a STOE IPDS II or IPDS 2T diffractometer with Mo Kα radiation (λ = 0.71073 Å), operating at 50 kV and 40 mA. Integration/numerical absorption corrections were executed with X-AREA, X-RED, and X-SHAPE programs.