Crystal system: monoclinic
| a: | 45.3552 (±0.0008) Å |
| b: | 8.9209 (±0.0002) Å |
| c: | 8.8062 (±0.0002) Å |
| α: | 90° |
| β: | 98.2088 (±0.0008)° |
| γ: | 90° |
Starting materials: Lead(II) oxide (PbO, <10 μm, ReagentPlus®, ≥99.9% trace metals basis ), HI (57 wt. % in H2O), methylamine hydrochloride (≥98%), hexylamine 99%, H3PO2 (50 wt. % in H2O)
Product: red plate-like crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in 57% w/w aqueous HI solution (16 mL) in a 50 mL glass flask by heating to boiling under stirring. A bright yellow solution resulted. Solid methylamine hydrochloride (338 mg, 5 mmol, DRY) was added to the hot yellow solution, and a black powder precipitated. This dissolved under stirring and resulted in a bright yellow solution. 580 μL (4.39 mmol) of hexylamine in 50% aqueous H3PO2 (2 mL) was slowly added. The solution was slowly cooled to room temperature. After two hours, crystals were completely formed.
Method: Single crystal X-Ray diffraction
Description: A Bruker Molly or Duo instrument with MoKα IμS microfocus source (λ=0.71073 Å) and MX Optics was used. All samples were collected at 293 K. Data was integrated and corrected for absorption with APEX3 software.
See all entries for this property (2 total)
Crystal system: monoclinic
| Band gap (optical, diffuse reflectance), eV |
|---|
Starting materials: Lead(II) oxide (PbO, <10 μm, ReagentPlus®, ≥99.9% trace metals basis ), HI (57 wt. % in H2O), methylamine hydrochloride (≥98%), hexylamine 99%, H3PO2 (50 wt. % in H2O)
Product: red plate-like crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in 57% w/w aqueous HI solution (16 mL) in a 50 mL glass flask by heating to boiling under stirring. A bright yellow solution resulted. Solid methylamine hydrochloride (338 mg, 5 mmol, DRY) was added to the hot yellow solution, and a black powder precipitated. This dissolved under stirring and resulted in a bright yellow solution. 580 μL (4.39 mmol) of hexylamine in 50% aqueous H3PO2 (2 mL) was slowly added. The solution was slowly cooled to room temperature. After two hours, crystals were completely formed.
Method: UV-vis absorption (diffused reflectance)
Description: Optical diffuse-reflectance measurements were conducted at room temperature. A Shimadzu UV-2600 PC double-beam, double-monochromator spectrophotometer was operating from 200 to 2500 nm. BaS4 was used as a non-absorbing reflectance reference. Reflectance v. wavelength data was collected and used to estimate the band gap by converting reflectance to absorbance via the Kubelka-Munk equation: α/S = (1-R)^{2}/2R. Band gap energy was calculated based on the absorption edge and exciton peak of the optical absorption spectra.
Crystal system: monoclinic
| Photoluminescence peak position, eV |
|---|
Starting materials: Lead(II) oxide (PbO, <10 μm, ReagentPlus®, ≥99.9% trace metals basis ), HI (57 wt. % in H2O), methylamine hydrochloride (≥98%), hexylamine 99%, H3PO2 (50 wt. % in H2O)
Product: red plate-like crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in 57% w/w aqueous HI solution (16 mL) in a 50 mL glass flask by heating to boiling under stirring. A bright yellow solution resulted. Solid methylamine hydrochloride (338 mg, 5 mmol, DRY) was added to the hot yellow solution, and a black powder precipitated. This dissolved under stirring and resulted in a bright yellow solution. 580 μL (4.39 mmol) of hexylamine in 50% aqueous H3PO2 (2 mL) was slowly added. The solution was slowly cooled to room temperature. After two hours, crystals were completely formed.
Method: Photoluminescence microscopy
Description: Data was collected with a Horiba LabRam Evolution high-resolution confocal Raman microscope spectrometer (600g/mm diffraction grating, with a diode continuous wave laser (473 nm, 25 mW) and a Synapse charge-coupled device camera. PL energy was calculated by the PL peak position of the optical emission spectra.
Starting materials: Lead(II) oxide (PbO, <10 μm, ReagentPlus®, ≥99.9% trace metals basis ), HI (57 wt. % in H2O), methylamine hydrochloride (≥98%), pentylamine 99%, H3PO2 (50 wt. % in H2O)
Product: red plate-like crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in 57% w/w aqueous HI solution (16 mL) in a 50 mL glass flask by heating to boiling under stirring. A bright yellow solution resulted. Solid methylamine hydrochloride (338 mg, 5 mmol, DRY) was added to the hot yellow solution, and a black powder precipitated. This dissolved under stirring and resulted in a bright yellow solution. 580 μL (4.39 mmol) of hexylamine in 50% aqueous H3PO2 (2 mL) was slowly added. The solution was slowly cooled to room temperature. After two hours, crystals were completely formed.
Method: Photoluminescence microscopy
Description: Data was collected with a Horiba LabRam Evolution high-resolution confocal Raman microscope spectrometer (600g/mm diffraction grating, with a diode continuous wave laser (473 nm, 25 mW) and a Synapse charge-coupled device camera. PL energy was calculated by the PL peak position of the optical emission spectra.
Starting materials: Lead(II) oxide (PbO, <10 μm, ReagentPlus®, ≥99.9% trace metals basis ), HI (57 wt. % in H2O), methylamine hydrochloride (≥98%), pentylamine 99%, H3PO2 (50 wt. % in H2O)
Product: red plate-like crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in 57% w/w aqueous HI solution (16 mL) in a 50 mL glass flask by heating to boiling under stirring. A bright yellow solution resulted. Solid methylamine hydrochloride (338 mg, 5 mmol, DRY) was added to the hot yellow solution, and a black powder precipitated. This dissolved under stirring and resulted in a bright yellow solution. 580 μL (4.39 mmol) of hexylamine in 50% aqueous H3PO2 (2 mL) was slowly added. The solution was slowly cooled to room temperature. After two hours, crystals were completely formed.
Method: UV-vis absorption (diffused reflectance)
Description: Optical diffuse-reflectance measurements were conducted at room temperature. A Shimadzu UV-2600 PC double-beam, double-monochromator spectrophotometer was operating from 200 to 2500 nm. BaS4 was used as a non-absorbing reflectance reference. Reflectance v. wavelength data was collected and used to estimate the band gap by converting reflectance to absorbance via the Kubelka-Munk equation: α/S = (1-R)^{2}/2R.