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.
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.
See all entries for this property (2 total)
Crystal system: orthorhombic
| Band gap (optical, diffuse reflectance), eV |
|---|
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 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 degas 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. The crystals started appearing in the solution and the solution was held at 120 °C for 2 h. Following this, the solution was cooled and the crystals were separated.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
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 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 degas 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. The crystals started appearing in the solution and the solution was held at 120 °C for 2 h. Following this, the solution was cooled and the crystals were separated.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
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.
See all entries for this property (2 total)
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: 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 the 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 dense pale-yellow precipitate. The hot plate temperature was raised to 200 ºC, leading to the formation of the dark red metastable phase.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
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.
Crystal system: hexagonal
| Band gap (optical, diffuse reflectance), eV |
|---|
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: Orange hexagonal 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 C(NH2)3I (187 mg, 1 mmol) was added to the solution. The solution was evaporated to half its volume by boiling at 120 ºC and was held at the same temperature for 2 h.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
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: Orange hexagonal 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 C(NH2)3I (187 mg, 1 mmol) was added to the solution. The solution was evaporated to half its volume by boiling at 120 ºC and was held at the same temperature for 2 h.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
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.
See all entries for this property (2 total)
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.
See all entries for this property (2 total)
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: UV-vis absorption (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.
See all entries for this property (2 total)
Crystal system: orthorhombic
| a: | 9.1771 (±0.0002) Å |
| b: | 15.6934 (±0.0002) Å |
| c: | 44.6446 (±0.0007) 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%)), CH3C(NH2)2I (synthesized from CH3C(NH2)2Cl (95%) and HI)
Product: orange, hexagonal 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 CH3C(NH2)2I (186 mg, 1 mmol) was added to the solution, and the solution was heated to 120º C. Crystals began to grow and were left to grow at this temperature for 2 hours. Finally, the solution was cooled 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.
See all entries for this property (2 total)
Crystal system: hexagonal
| Band gap (optical, diffuse reflectance), eV |
|---|
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), CH3C(NH2)2I (synthesized from CH3C(NH2)2Cl (95%) and HI)
Product: orange, hexagonal 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 CH3C(NH2)2I (186 mg, 1 mmol) was added to the solution, and the solution was heated to 120º C. Crystals began to grow and were left to grow at this temperature for 2 hours. Finally, the solution was cooled to room temperature.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), CH3C(NH2)2I (synthesized from CH3C(NH2)2Cl (95%) and HI)
Product: orange, hexagonal 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 CH3C(NH2)2I (186 mg, 1 mmol) was added to the solution, and the solution was heated to 120º C. Crystals began to grow and were left to grow at this temperature for 2 hours. Finally, the solution was cooled to room temperature.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
Crystal system: monoclinic
| a: | 12.7484 (±0.0005) Å |
| b: | 9.2801 (±0.0004) Å |
| c: | 14.7064 (±0.0006) Å |
| α: | 90° |
| β: | 112.211 (±0.003)° |
| γ: | 90° |
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), CH3C(NH2)2I (synthesized from CH3C(NH2)2Cl (95%) and HI)
Product: red-orange 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 CH3C(NH2)2I (372 mg, 2 mmol) was added to the solution, and crystals began to grow when stirring was discontinued. Solution cooled, and crystals transformed from red-orange needles to yellow hexagonal plates.
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.
See all entries for this property (2 total)
Crystal system: monoclinic
| Band gap (optical, diffuse reflectance), eV |
|---|
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), CH3C(NH2)2I (synthesized from CH3C(NH2)2Cl (95%) and HI)
Product: red-orange 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 CH3C(NH2)2I (372 mg, 2 mmol) was added to the solution, and crystals began to grow when stirring was discontinued. Solution cooled, and crystals transformed from red-orange needles to yellow hexagonal plates.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), CH3C(NH2)2I (synthesized from CH3C(NH2)2Cl (95%) and HI)
Product: red-orange 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 CH3C(NH2)2I (372 mg, 2 mmol) was added to the solution, and crystals began to grow when stirring was discontinued. Solution cooled, and crystals transformed from red-orange needles to yellow hexagonal plates.
Method: UV-vis absorption (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.
Crystal system: monoclinic
| a: | 12.876 (±0.0008) Å |
| b: | 9.4302 (±0.0007) Å |
| c: | 15.1306 (±0.001) Å |
| α: | 90° |
| β: | 114.194 (±0.005)° |
| γ: | 90° |
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), imidazole (99%)
Product: yellow/orange hexagonal plates
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 imidazole (136 mg, 1 mmol) was added to the solution, and the solution was heated to 120º C. Crystals began to grow for 120º C for 2 hours. The solution was then cooled 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: monoclinic
| Band gap (optical, diffuse reflectance), eV |
|---|
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), imidazole (99%)
Product: yellow/orange hexagonal plates
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 imidazole (136 mg, 1 mmol) was added to the solution, and the solution was heated to 120º C. Crystals began to grow for 120º C for 2 hours. The solution was then cooled to room temperature.
Method: UV-vis absorption (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: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnI2 (synthesized from Sn granules, and I2 (99.8%)), imidazole (99%)
Product: yellow/orange hexagonal plates
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 imidazole (136 mg, 1 mmol) was added to the solution, and the solution was heated to 120º C. Crystals began to grow for 120º C for 2 hours. The solution was then cooled to room temperature.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
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.
See all entries for this property (2 total)
Crystal system: orthorhombic
| Band gap (optical, diffuse reflectance), eV |
|---|
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: UV-vis absorption (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.
See all entries for this property (2 total)
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: UV-vis absorption (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.
See all entries for this property (2 total)
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.
See all entries for this property (2 total)
Crystal system: orthorhombic
| Band gap (optical, diffuse reflectance), eV |
|---|
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: UV-vis absorption (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.
See all entries for this property (2 total)
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: UV-vis absorption (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.
See all entries for this property (2 total)
Crystal system: orthorhombic
| a: | 8.7763 (±0.0005) Å |
| b: | 8.8581 (±0.0005) Å |
| c: | 39.497 (±0.003) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnCl2·2H2O (98%), CH3NH3Cl (98%), CH3(CH2)3NH2
Product: cherry-red rectangular plates
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. SnCl2•2H2O powder (2256 mg, 10 mmol) was dissolved in a solution of 57% (w/w) aqueous HI solution (20 mL, 152 mmol) and 50% aqueous H3PO2 (3.4 mL, 31 mmol) by boiling the solution and constantly stirring. This formed a bright yellow solution. Solid CH3(CH2)3NH2 (694 μL, 7 mmol) was neutralized with 57% (w/w) HI (5 mL38 mmol) via an ice bath. This resulted in a clear pale-yellow solution. CH3(CH2)3NH3I solution was added to SnI2 solution and produced a black precipitate. After the solution was boiled, stirring stopped, the solution cooled, and crystals formed for 2 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: orthorhombic
| Band gap (optical, diffuse reflectance), eV |
|---|
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnCl2·2H2O (98%), CH3NH3Cl (98%), CH3(CH2)3NH2
Product: cherry-red rectangular plates
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. SnCl2•2H2O powder (2256 mg, 10 mmol) was dissolved in a solution of 57% (w/w) aqueous HI solution (20 mL, 152 mmol) and 50% aqueous H3PO2 (3.4 mL, 31 mmol) by boiling the solution and constantly stirring. This formed a bright yellow solution. Solid CH3(CH2)3NH2 (694 μL, 7 mmol) was neutralized with 57% (w/w) HI (5 mL38 mmol) via an ice bath. This resulted in a clear pale-yellow solution. CH3(CH2)3NH3I solution was added to SnI2 solution and produced a black precipitate. After the solution was boiled, stirring stopped, the solution cooled, and crystals formed for 2 hours.
Method: UV-vis absorption (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.
See all entries for this property (2 total)
Starting materials: distilled HI (aqueous 99.95%), H3PO2 (50% aqueous), SnCl2·2H2O (98%), CH3NH3Cl (98%), CH3(CH2)3NH2
Product: cherry-red rectangular plates
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. SnCl2•2H2O powder (2256 mg, 10 mmol) was dissolved in a solution of 57% (w/w) aqueous HI solution (20 mL, 152 mmol) and 50% aqueous H3PO2 (3.4 mL, 31 mmol) by boiling the solution and constantly stirring. This formed a bright yellow solution. Solid CH3(CH2)3NH2 (694 μL, 7 mmol) was neutralized with 57% (w/w) HI (5 mL38 mmol) via an ice bath. This resulted in a clear pale-yellow solution. CH3(CH2)3NH3I solution was added to SnI2 solution and produced a black precipitate. After the solution was boiled, stirring stopped, the solution cooled, and crystals formed for 2 hours.
Method: UV-vis absorption (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.
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.
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: HI, H3PO2, SnI2, (CH3)2CHNH3I
Product: yellow 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 (CH3)2CHNH3I (4mmol) was added to the solution, forming a yellow precipitate. Solution was raised to 200°C, were the precipitate changed from yellow to red. Solution was left to cool, leading to the yellow color.
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.