Crystal system: trigonal
| a: | 16.04 (±0.0004) Å |
| b: | 16.04 (±0.0004) Å |
| c: | 72.226 (±0.003) Å |
| α: | 90° |
| β: | 90° |
| γ: | 120° |
Starting materials: SnI2 (synthesized from Sn and I2), (CH3)3N (45% aqueous), HI (99.95% aqueous), and H3PO2 (50% aqueous)
Product: pale yellow needles
Description: (CH3)3NI was prepared by reacting equimolar amounts of (CH3)3N and HI. The entire reaction was performed under N2 atmosphere. SnI2 (372 mg, 1 mmol) was dissolved in aqueous HI (6.8 mL, 7.58 M) and aqueous H3PO2 (1.7 mL, 9.14 M) by heating at 130 °C and stirring. To it, (CH3)3NHI (187 mg, 1 mmol) was added. After 5 minutes, the heating and stirring were stopped, and the solution was allowed to cool down to room temperature.
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: trigonal
| Band gap (optical, diffuse reflectance), eV |
|---|
Starting materials: SnI2 (synthesized from Sn and I2), (CH3)3N (45% aqueous), HI (99.95% aqueous), and H3PO2 (50% aqueous)
Product: pale yellow needles
Description: (CH3)3NI was prepared by reacting equimolar amounts of (CH3)3N and HI. The entire reaction was performed under N2 atmosphere. SnI2 (372 mg, 1 mmol) was dissolved in aqueous HI (6.8 mL, 7.58 M) and aqueous H3PO2 (1.7 mL, 9.14 M) by heating at 130 °C and stirring. To it, (CH3)3NHI (187 mg, 1 mmol) was added. After 5 minutes, the heating and stirring were stopped and the solution was allowed to cool down to room temperature.
Method: UV-vis absorbance (diffuse reflectance)
Description: Diffuse-reflectance measurements were performed and collected at room temperature. A Shimadzu UV-3600 PC double-beam and double monochromator spectrophotometer (operating between 200 to 2500 nm) was used.BaSO4 was used as a nonabsorbing reflectance reference. Generated reflectance v. wavelength data was used to estimate the band gap. The Kubelka-Munk equation α/S = (1-R)^{2}/(2R) was used.
Starting materials: SnI2 (synthesized from Sn and I2), (CH3)3N (45% aqueous), HI (99.95% aqueous), and H3PO2 (50% aqueous)
Product: pale yellow needles
Description: (CH3)3NI was prepared by reacting equimolar amounts of (CH3)3N and HI. The entire reaction was performed under N2 atmosphere. SnI2 (372 mg, 1 mmol) was dissolved in aqueous HI (6.8 mL, 7.58 M) and aqueous H3PO2 (1.7 mL, 9.14 M) by heating at 130 °C and stirring. To it, (CH3)3NHI (187 mg, 1 mmol) was added. After 5 minutes, the heating and stirring were stopped and the solution was allowed to cool down to room temperature.
Method: UV-vis absorbance (diffuse reflectance)
Description: Diffuse-reflectance measurements were performed and collected at room temperature. A Shimadzu UV-3600 PC double-beam and double monochromator spectrophotometer (operating between 200 to 2500 nm) was used.BaSO4 was used as a nonabsorbing reflectance reference.