Crystal system: cubic
| a: | 5.675 Å |
| b: | 5.675 Å |
| c: | 5.675 Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: lead (II) acetate, CH3NH3+ (by adding a 40% solution of CH3NH2 in water), concentrated HCl
Product: Colorless MAPbCl3 crystals
Description: CH3NH3PbCI3 was synthesized from lead (II) acetate and CH3NH3+ dissolved in concentrated HCl solution. The aqueous solution was cooled from l00°C to room temperature to obtain the colorless crystals.
Method: Temperature-dependent Guinier-Simon photograph
Description: Not specified.
Crystal system: tetragonal
| a: | 5.656 Å |
| b: | 5.656 Å |
| c: | 5.63 Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: lead (II) acetate, CH3NH3+ (by adding a 40% solution of CH3NH2 in water), concentrated HCl
Product: Colorless MAPbCl3 crystals
Description: CH3NH3PbCI3 was synthesized from lead (II) acetate and CH3NH3+ dissolved in concentrated HCl solution. The aqueous solution was cooled from l00°C to room temperature to obtain the colorless crystals.
Method: Temperature-dependent Guinier-Simon photograph
Description: Not specified.
Crystal system: orthorhombic
| a: | 5.673 Å |
| b: | 5.628 Å |
| c: | 11.182 Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: lead (II) acetate, CH3NH3+ (by adding a 40% solution of CH3NH2 in water), concentrated HCl
Product: Colorless MAPbCl3 crystals
Description: CH3NH3PbCI3 was synthesized from lead (II) acetate and CH3NH3+ dissolved in concentrated HCl solution. The aqueous solution was cooled from l00°C to room temperature to obtain the colorless crystals.
Method: Temperature-dependent Guinier-Simon photograph
Description: Not specified.
Crystal system: cubic
| a: | 5.68415 (±6e-05) Å |
| b: | 5.68415 (±6e-05) Å |
| c: | 5.68415 (±6e-05) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: Lead(II) acetate (Chemical Reagents, Sigma), concentrated aqueous HCl, CH3NH2 (40% soluble in water, Merck)
Product: Colorless MAPbCl3 Single crystal ~1mm
Description: Precipitate polycrystalline MAPbCl3 from a halogenated acid solution using the method of [1]. Dissolve 1.88 g of lead(II) acetate in 40 ml concentrated aquous HCl solution (37 wt%) warmed (~90 °C) in a water bath. Then add an excess of HCl to prevent the co-precipitation of PbCl2 in agreement with previous work [2], along with 0.45 g CH3NH2. Crystallize by cooling the solution from 90 °C to room temperature over 3 hours. Wash product with acetone and dry overnight at 100 °C in a vacuum oven. Obtain larger crystals via slow cooling from 90 to 50 °C over 3 days.
Comment: Synthesis references: [1] A. Poglitsch and D. Weber, J. Chem. Phys., 1987, 87, 6373–6378. [2] Q. Xu, T. Eguchi, H. Nakayama, N. Nakamura and M. Kishita, Z. Naturforsch., A: Phys. Sci., 1991, 46, 240–246.
Method: Powder X-ray diffraction
Description: Bruker D8 Advance diffractometer (Bragg–Brentano geometry) equipped with a Cu-Ka X-ray tube operated at 40 kV and 40 mA. Refer to Page 9300 Section 3.1 Paragraph 2.
Crystal system: cubic
| a: | 5.657 (±0.002) Å |
| b: | 5.657 (±0.002) Å |
| c: | 5.657 (±0.002) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: HCl, CH3NH2, PbCl2
Product: MAPbCl3 Single-crystal
Description: Primarily referenced the methods of [1] and [2]. The synthesis of MAPbBr3 in ref [2] was modified to prepare MAPbCl3.
Comment: Synthesis references: [1] Canadian Journal of Chemistry, 1987, 65(5): 1042-1046 https://doi.org/10.1139/v87-176 [2] D. WEBER. Z. Naturforsch. 33b, 1443 (1978).
Method: Single crystal X-ray diffraction
Description: CAD-4 four-circle diffractometer; Mo Kα, λ = 0.70926 Å (graphite monochromator); T = 18 °C. Lorentz, polarization, and absorption corrections applied. Refer to page 413 Experimental.
Crystal system: cubic
| a: | 5.714 (±0.003) Å |
| b: | 5.714 (±0.003) Å |
| c: | 5.714 (±0.003) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: MACl (TCI, >98.0%), PbCl2 (Aldrich, 98.0%), dimethyl sulfoxide (DMSO) (Wako), and N, N-dimethylformamide (DMF) (Wako)
Product: Single crystalline colorless MAPbCl3 with the size of several hundred micrometers
Description: Optical trapping induced crystallization: 1:1 MACl/PbCl2 (1.0 M) were dissolved in DMSO: DMF solvent mixture (1:1, v-v) to prepare the precursor solution. The solution was centrifuged at 10,000 r.p.m for 5 min; the supernatant was used for further experiments. 10 μL of the supernatant solution was used to prepare a thin layer (100-200 um thickness) in a laboratory-built sample chamber. A near-infrared (NIR) laser (Spectron Laser System, λ = 1064 nm) was focused onto the solution surface through an objective lens at 60 times magnification (Olympus UPlanFLN with a numerical aperture of 0.90).
Comment: Details of the sample chamber can be found on Page 2 of the publication.
Method: Single crystal X-ray diffraction
Description: The crystal was mounted on the glass capillary and fixed with epoxy resin. Crystallographic data were collected using a Rigaku RAXIS-RAPID diffractometer with Mo-Kα (λ = 0.71073 Å) radiation from a graphite monochromator. Structural refinements were performed using the full-matrix least-squares method on F2. The calculations were carried out with the Yadokari-XG software.
Crystal system: cubic
| a: | 5.68 Å |
| b: | 5.68 Å |
| c: | 5.68 Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: Presumably (by analogy with MAPbBr3 synthesis description in same reference): 40% aqueous CH3NH2 solution; concentrated HCl(aq); Pb(NO3)2 (aq; 0.021 molar)
Product: colorless crystals
Description: Adapted from synthesis description of CH3NH3PbBr3 as indicated by the author. Neutralize 20g of 40% aq. CH3NH2 solution with concentrated aq. HCl. At 100 deg. C, add aq. (0.021 mol) solution of Pb(NO3)2 by slow dripping while stirring vigorously. Crystals begin to form while stirring. Solution is filtrated after cooling to room temperature. The crystals are washed with n-butanol and subsequently benzene and are finally dried in vacuum. Nominal stoichiometry: C 3.47 wt.% H 1.75 wt.% N 4.05 wt.% Pb(II) 59.95 wt.% Cl 30.77 wt.% Actual stoichiometry: C 3.17 wt.% H 1.63 wt.% N 3.71 wt.% Pb(II) 60.9 wt.% Cl 31.8 wt.%
Method: Powder X-ray diffraction (PXRD)
Description: X-ray powder diagrams collected with a Debye-Scherrer camera using Cu K-alpha radiation (wave length 1.54178 Angstrom).
Comment: Miss Leonhardt recorded the PXRD diagrams.
Crystal system: orthorhombic
| a: | 11.157 (±0.001) Å |
| b: | 11.157 (±0.001) Å |
| c: | 11.157 (±0.001) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Crystal system: orthorhombic
| a: | 11.146 (±0.002) Å |
| b: | 11.338 (±0.002) Å |
| c: | 11.263 (±0.002) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Crystal system: orthorhombic
| a: | 11.164 (±0.001) Å |
| b: | 11.164 (±0.001) Å |
| c: | 11.164 (±0.001) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Crystal system: orthorhombic
| a: | 11.163 (±0.001) Å |
| b: | 11.345 (±0.001) Å |
| c: | 11.292 (±0.001) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Crystal system: orthorhombic
| a: | 11.165 (±0.003) Å |
| b: | 11.345 (±0.003) Å |
| c: | 11.275 (±0.003) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Crystal system: orthorhombic
| a: | 11.187 (±0.003) Å |
| b: | 11.343 (±0.003) Å |
| c: | 11.282 (±0.003) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Crystal system: orthorhombic
| a: | 11.193 (±0.003) Å |
| b: | 11.347 (±0.003) Å |
| c: | 11.287 (±0.003) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Crystal system: orthorhombic
| a: | 11.331 (±0.002) Å |
| b: | 11.318 (±0.002) Å |
| c: | 11.29 (±0.002) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |