Crystal system: orthorhombic
| a: | 8.3212 (±0.0004) Å |
| b: | 14.8573 (±0.0005) Å |
| c: | 8.5918 (±0.0011) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), CH3CH2NH3I (synthesized from CH3CH2NH2 (68.0%) and HI)
Product: Pale yellow, rectangular needles
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 CH3CH2NH3I (173 mg, 1 mmol) was added to the solution, which created a dense pale-yellow precipitate. Crystals formed immediately and grew inside the mother liquor for 2 hours at 120º C before being washed and collected.
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.
Crystal system: orthorhombic
| a: | 30.7151 (±0.0015) Å |
| b: | 8.7898 (±0.0004) Å |
| c: | 23.0047 (±0.0015) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), CH3CH2NH3I (synthesized from CH3CH2NH2 (68.0%) and HI)
Product: dark red 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 (1860 mg, 5 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 CH3CH2NH3I (865 mg, 5 mmol) was added to the solution, which created a pale-yellow precipitate within 5 minutes. Temperature was raised to 200º C, and precipitate changed to dark red.
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.