Crystal system: orthorhombic
| a: | 9.0068 (±0.0004) Å |
| b: | 12.4329 (±0.0008) Å |
| c: | 22.4324 (±0.001) 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%)),(CH3)2CHNH3I (synthesized from (CH3)2C(H)NH2 (99.5%) and HI)
Product: 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 (CH3)2CHNH3I (561 mg, 3 mmol) was added to the solution, and the solution was heated to 120º C. Stirring stopped, and the solution cool dot room temperature. Crystals precipitated 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.
Crystal system: tetragonal
| a: | 8.9525 (±0.0003) Å |
| b: | 8.9525 (±0.0003) Å |
| c: | 36.5514 (±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%)),(CH3)2CHNH3I (synthesized from (CH3)2C(H)NH2 (99.5%) and HI)
Product: 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 (1116 mg, 3 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 (CH3)2CHNH3I (1683 mg, 9 mmol) was added to the solution, and a pale-yellow precipitate formed within 5 minutes. The temperature was raised to 200º C, and the precipitate turned red. The solution was cooled and precipitate changed back to yellow.
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.