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
| a: | 39.315 (±0.005) Å |
| b: | 8.8503 (±0.0012) Å |
| c: | 8.7792 (±0.0013) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: BAI, MAI, SnI2, HI, H3PO2
Product: Single crystals of 2D tin halide perovskites. Thin flakes were then exfoliated from the single crystals.
Description: Single crystals synthesized by slow cooling method. Growth solution prepared with 0.43mmol BAI, 0.2mmol MAI, 0.59mmol SnI2, 1mL HI, and 0.1mL H3PO2 in a sealed glass vial and placed in a muffle furnace and heated until completely dissolved. Solution cooled to room temperature at a rate of 2°C/hour. Crystals were then dried and stored in a nitrogen glove box.
Method: Single crystal X-ray diffraction
Description: Phase purity of as synthesized BA2MA(n-1)Sn(n)I(3n+1) crystals were confirmed by PXRD. No impurity signals observed. PXRD performed by Bruker D8 Advance instrument scanning at 0.02° per step with a copper target. All single crystals were analyzed using a Bruker AXS D8 Venture diffractometer with a high-intensity diamond Cu/Mo hybrid dual-microfocal x-ray tube. All data collecting and processing was completed using APEX4 software. Full matrix least squares against F2 method was used for further refinement of structures.