Crystal system: monoclinic
| a: | 8.693 (±0.005) Å |
| b: | 8.911 (±0.005) Å |
| c: | 16.338 (±0.01) Å |
| α: | 90° |
| β: | 94.85 (±0.03)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.628 (±0.004) Å |
| b: | 8.854 (±0.004) Å |
| c: | 16.107 (±0.007) Å |
| α: | 90° |
| β: | 92.27 (±0.03)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.622 (±0.004) Å |
| b: | 8.829 (±0.004) Å |
| c: | 16.108 (±0.007) Å |
| α: | 90° |
| β: | 92.25 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.617 (±0.003) Å |
| b: | 8.818 (±0.003) Å |
| c: | 16.085 (±0.004) Å |
| α: | 90° |
| β: | 92.31 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.62 (±0.003) Å |
| b: | 8.81 (±0.003) Å |
| c: | 16.068 (±0.005) Å |
| α: | 90° |
| β: | 92.29 (±0.03)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.614 (±0.002) Å |
| b: | 8.811 (±0.003) Å |
| c: | 16.064 (±0.004) Å |
| α: | 90° |
| β: | 92.28 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.621 (±0.003) Å |
| b: | 8.818 (±0.003) Å |
| c: | 16.077 (±0.006) Å |
| α: | 90° |
| β: | 92.26 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.618 (±0.003) Å |
| b: | 8.82 (±0.003) Å |
| c: | 16.082 (±0.004) Å |
| α: | 90° |
| β: | 92.3 (±0.2)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.618 (±0.004) Å |
| b: | 8.821 (±0.004) Å |
| c: | 16.09 (±0.07) Å |
| α: | 90° |
| β: | 92.26 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.621 (±0.004) Å |
| b: | 8.829 (±0.004) Å |
| c: | 16.106 (±0.007) Å |
| α: | 90° |
| β: | 92.24 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.625 (±0.004) Å |
| b: | 8.836 (±0.004) Å |
| c: | 16.113 (±0.007) Å |
| α: | 90° |
| β: | 92.24 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.627 (±0.003) Å |
| b: | 8.845 (±0.004) Å |
| c: | 16.111 (±0.007) Å |
| α: | 90° |
| β: | 92.19 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.636 (±0.003) Å |
| b: | 8.859 (±0.004) Å |
| c: | 16.117 (±0.007) Å |
| α: | 90° |
| β: | 92.18 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.652 (±0.004) Å |
| b: | 8.877 (±0.004) Å |
| c: | 16.129 (±0.007) Å |
| α: | 90° |
| β: | 92.12 (±0.02)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.678 (±0.004) Å |
| b: | 8.895 (±0.004) Å |
| c: | 16.264 (±0.008) Å |
| α: | 90° |
| β: | 93.56 (±0.03)° |
| γ: | 90° |
Crystal system: monoclinic
| a: | 8.702 (±0.004) Å |
| b: | 8.92 (±0.05) Å |
| c: | 16.345 (±0.009) Å |
| α: | 90° |
| β: | 94.93 (±0.03)° |
| γ: | 90° |
Starting materials: HI, HA (C6H13NH3), Et2O, PbI2
Product: Powder of (C6H13NH3)2PbI4
Description: Prepare hexylammonium iodide salts via neutralization of HI with HA. Remove unreacted species by evaporation. Purify product by recrystallization in minimal diethyl ether/excess hexane and isolate via vacuum filtration. Prepare films by spin-coating or drop-casting solutions (prepared by dissolving HAI and PbI2 powders at a 2.5:1 molar ratio in a 1:0.34 volume ratio mixture of THF and methanol). To prepare powder for XRD, drop-cast thin film from 200 mg/mL solutions and anneal at 70 °C for 15 min.
Method: Powder X-ray diffraction
Description: Bruker X-ray D8 Advance diffractometer with Cu Kα1,2 radiation (λ = 1.541 Å). Spectra were collected with an angular range of 5 < 2θ < 60° and step size of 0.01022 ° over 60 minutes. Rietveld analysis was carried out using the TOPAS program. Low-temperature measurements were made on cooling between 300−12K using an Oxford Cyrosytem PheniX stage.
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Crystal system: orthorhombic
| 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), pentylamine 99%, H3PO2 (50 wt. % in H2O)
Product: orange 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. 1159 μL (10 mmol) of pentylamine in 50% aqueous H3PO2 (2 mL) was slowly added. The solution was slowly cooled to room temperature.
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.
See all entries for this property (2 total)
Crystal system: orthorhombic
| Photoluminescence peak position, eV |
|---|
Starting materials: Lead(II) oxide (PbO, <10 μm, ReagentPlus®, ≥99.9% trace metals basis ), HI (57 wt. % in H2O), hexylamine 99%, H3PO2 (50 wt. % in H2O)
Product: orange 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. 1000 μL (7.52 mmol) of hexylamine in 50% aqueous H3PO2 (2 mL) was slowly added. The solution was slowly cooled to room temperature.
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.
See all entries for this property (2 total)
Starting materials: Lead(II) oxide (PbO, <10 μm, ReagentPlus®, ≥99.9% trace metals basis ), HI (57 wt. % in H2O), hexylamine 99%, H3PO2 (50 wt. % in H2O)
Product: orange 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. 1000 μL (7.52 mmol) of hexylamine in 50% aqueous H3PO2 (2 mL) was slowly added. The solution was slowly cooled to room temperature.
Comment: Note that the n=1 C6N1 compound is specifically mentioned as crystallizing in an orthorhombic spacegroup in the reference, with associated PXRD data shown in Figure S10. In contrast, the n>1 C6N1 compounds crystallize in a monoclinic spacegroup.
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.