Crystal system: orthorhombic
| a: | 8.9274 Å |
| b: | 64.383 Å |
| c: | 8.8816 Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: Lead Oxide (PbO), HI (57% w/w aqueous), H3PO2 (50% aqueous), butylammonium iodide (n-CH3(CH2)3NH3I) , solid CH3NH3Cl
Product: Black plate-like (BA)2(MA)3Pb4I13 crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in a mixture of HI solution (10.0 mL, 76 mmol) and H3PO2 (1.7 mL, 15.5 mmol) by heating to boiling under constant magnetic stirring for about 5 min, which formed a bright yellow solution. Subsequent addition of solid CH3NH3Cl (507 mg, 7.5 mmol) to the hot yellow solution initially caused the precipitation of a black powder, which rapidly redissolved under stirring to afford a clear bright yellow solution. In a separate beaker, n-CH3(CH2)3NH2 (248 μL, 2.5 mmol) was neutralized with HI 57% w/w (5 mL, 38 mmol) in an ice bath resulting in a clear pale yellow solution. Addition of the n-CH3(CH2)3NH3I solution to the PbI2 solution initially produced a black precipitate, which subsequently dissolved under heating the combined solution to boiling. The stirring was then discontinued, and the solution was left to cool to room temperature during which time black rectangular-shaped plates started to crystallize. The precipitation was deemed to be complete after ∼2 h. The crystals were isolated by suction filtration and thoroughly dried under reduced pressure.
Method: Single Crystal X-ray diffraction
Description: Single-crystal X-ray diffraction data were collected using an image plate STOE IPDS II diffractometer using Mo Kα radiation (λ = 0.71073 Å), operating at 50 kV and 40 mA. Data reduction and numerical absorption corrections were performed using the X-AREA suite
Starting materials: Lead Oxide (PbO), HI (57% w/w aqueous), H3PO2 (50% aqueous), butylammonium iodide (n-CH3(CH2)3NH3I) , solid CH3NH3Cl
Product: Dark red plate-like (BA)2(MA)2Pb3I10 crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in a mixture of HI solution (10.0 mL, 76 mmol) and H3PO2 (1.7 mL, 15.5 mmol) by heating to boiling under constant magnetic stirring for about 5 min, which formed a bright yellow solution. Subsequent addition of solid CH3NH3Cl (450 mg, 6.67 mmol) to the hot yellow solution initially caused the precipitation of a black powder, which rapidly redissolved under stirring to afford a clear bright yellow solution. In a separate beaker, n-CH3(CH2)3NH2 (327 μL, 3.33 mmol) was neutralized with HI 57% w/w (5 mL, 38 mmol) in an ice bath resulting in a clear pale yellow solution. Addition of the n-CH3(CH2)3NH3I solution to the PbI2 solution initially produced a black precipitate, which was subsequently dissolved under heating the combined solution to boiling. The stirring was then discontinued, and the solution was left to cool to room temperature during which time deep-red/purple rectangular-shaped plates started to crystallize. The precipitation was deemed to be complete after ∼2 h. The crystals were isolated by suction filtration and thoroughly dried under reduced pressure.
Method: Single Crystal X-ray diffraction
Description: Single-crystal X-ray diffraction data were collected using an image plate STOE IPDS II diffractometer using Mo Kα radiation (λ = 0.71073 Å), operating at 50 kV and 40 mA. Data reduction and numerical absorption corrections were performed using the X-AREA suite
See all entries for this property (2 total)
Starting materials: Lead Oxide (PbO), aqueous HI, aqueous H3PO2, n-CH3(CH2)3NH3I , solid CH3NH3Cl
Product: Black plate-like (BA)2(MA)3Pb4I13 crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in a mixture of 57% w/w aqueous HI solution (10.0 mL, 76 mmol) and 50% aqueous H3PO2 (1.7 mL, 15.5 mmol) by heating to boiling under constant magnetic stirring for about 5 min, which formed a bright yellow solution. Subsequent addition of solid CH3NH3Cl (507 mg, 7.5 mmol) to the hot yellow solution initially caused the precipitation of a black powder, which rapidly redissolved under stirring to afford a clear bright yellow solution. In a separate beaker, n-CH3(CH2)3NH2 (248 μL, 2.5 mmol) was neutralized with HI 57% w/w (5 mL, 38 mmol) in an ice bath resulting in a clear pale yellow solution. Addition of the n-CH3(CH2)3NH3I solution to the PbI2 solution initially produced a black precipitate, which subsequently dissolved under heating the combined solution to boiling. The stirring was then discontinued, and the solution was left to cool to room temperature during which time black rectangular-shaped plates started to crystallize. The precipitation was deemed to be complete after ∼2 h. The crystals were isolated by suction filtration and thoroughly dried under reduced pressure.
Method: Photoluminescence spectroscopy
Description: Oriented rectangular crystals were used in the collection of photoluminescence spectra. Crystals of type (BA)2(MA)3Pb4I13 provided data for the material with n=4. A Horiba LabRam Evolution Raman microscope spectrometer with a diode CW laser (600 g/mm diffraction grating; 473 m, 25 mW) and a Synapse CCD camera carried out measurements. The laser beam was focused at about 1 µm spot size was made parallel to the 010 orientation of the crystals. The power output of the laser source was limited to 0.1% of the maximum power output.
See all entries for this property (2 total)
Starting materials: Lead Oxide (PbO), HI (57% w/w aqueous), H3PO2 (50% aqueous), butylammonium iodide (n-CH3(CH2)3NH3I) , solid CH3NH3Cl
Product: Dark red plate-like (BA)2(MA)2Pb3I10 crystals
Description: PbO powder (2232 mg, 10 mmol) was dissolved in a mixture of HI solution (10.0 mL, 76 mmol) and H3PO2 (1.7 mL, 15.5 mmol) by heating to boiling under constant magnetic stirring for about 5 min, which formed a bright yellow solution. Subsequent addition of solid CH3NH3Cl (450 mg, 6.67 mmol) to the hot yellow solution initially caused the precipitation of a black powder, which rapidly redissolved under stirring to afford a clear bright yellow solution. In a separate beaker, n-CH3(CH2)3NH2 (327 μL, 3.33 mmol) was neutralized with HI 57% w/w (5 mL, 38 mmol) in an ice bath resulting in a clear pale yellow solution. Addition of the n-CH3(CH2)3NH3I solution to the PbI2 solution initially produced a black precipitate, which was subsequently dissolved under heating the combined solution to boiling. The stirring was then discontinued, and the solution was left to cool to room temperature during which time deep-red/purple rectangular-shaped plates started to crystallize. The precipitation was deemed to be complete after ∼2 h. The crystals were isolated by suction filtration and thoroughly dried under reduced pressure.
Method: Photoluminescence spectroscopy
Description: Oriented rectangular crystals were used in the collection of photoluminescence spectra. Crystals of type (BA)2(MA)2Pb3I10 provided data for the material with n=3. A Horiba LabRam Evolution Raman microscope spectrometer with a diode CW laser (600 g/mm diffraction grating; 473 m, 25 mW) and a Synapse CCD camera carried out measurements. The laser beam was focused at about 1 µm spot size was made parallel to the 010 orientation of the crystals. The power output of the laser source was limited to 0.1% of the maximum power output.