Crystal system: monoclinic
| a: | 9.3044 (±0.0004) Å |
| b: | 21.1918 (±0.001) Å |
| c: | 18.5797 (±0.0007) Å |
| α: | 90° |
| β: | 119.962 (±0.003)° |
| γ: | 90° |
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), C(NH2)3I (synthesized from (C(NH2)3)2CO3 (99%) and HI)
Product: Dark red (after exposure to air for 30 min, product became black oxidized species).
Description: Two-necked flask was charged with aqueous HI (6.8 mL, 7.58 M) and aqueous H3PO2 (1.7 mL, 9.14 M). Nitrogen was passed through the liquid to degass the solution. SnI2 (372 mg, 1 mmol) was dissolved in solution, and flask was heated to boiling (~130 ºC) via an oil bath. A bright yellow solution formed under magnetic stirring. Solid C(NH2)3I (187 mg, 1 mmol) was added to the solution, and the solution was then heated at 120º C for 2 hours, then cooled to room temperature.which created a dense pale-yellow precipitate. Solution was stirred for 5 more minutes and then cooled to room temperature.
Method: Dark red (after exposure to air for 30 min, product became black oxidized species).
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.
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: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), C(NH2)3I (synthesized from (C(NH2)3)2CO3 (99%) and HI)
Product: red, rectangular crystals
Description: Two-necked flask was charged with aqueous HI (6.8 mL, 7.58 M) and aqueous H3PO2 (1.7 mL, 9.14 M). Nitrogen was passed through the liquid to degass the solution. SnI2 (744 mg, 2 mmol) was dissolved in solution, and flask was heated to boiling (~130 ºC) via an oil bath. A bright yellow solution formed under magnetic stirring. Solid C(NH2)3I (750 mg, 4 mmol) was added to the solution, and the solution was heated to 120º C. The solution then cooled to room temperature, and crystals grew in the mother liquor for 24 hours.
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.