Crystal system: orthorhombic
| a: | 8.837 (±0.0005) Å |
| b: | 8.6191 (±0.0004) Å |
| c: | 27.562 (±0.002) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: SnI2, HI, C4H9NH2
Product: Dark red sheetlike crystals
Description: Grow the crystals under slowly-cooled aqueous hydriodic acid solutions. Perform all synthetic steps and crystal manipulations after synthesis in an inert atmosphere to prevent oxidation. Dissolve 0.481 g (1.29 mmol) of SnI2 in 2 mL of concentrated (57 wt %) aqueous HI solvent under flowing argon at 90 °C. In a separate tube, dissolve 2.58 mmol of (C4H9NH2).HI in 3 mL of concentrated HI solution and add to the metal halide solution. Ramp the solution temperature at 2 °C/h from 90 to -10 °C, filter the crystals formed under argon or nitrogen and dry in argon at 80 °C.
Method: Single crystal X-ray diffraction
Description: Select suitable single crystals in an argon-filled drybox (<1 ppm O2 and H2O) under a microscope and seal in quartz capillaries. Collect data at room temperature on an Enraf-Nonius CAD4 diffractometer with graphite-monochromatized Mo Ka radiation. Obtain unitcell parameters and the crystal orientation matrix by a least-squares fit of 25 reflections with 18° < 2θ < 30°. Monitor intensity control reflections every 5000s during the data collection. Little to no degradation was observed for the compounds. Use the NRCVAX 386 PC version program for structural solution and refinement.
Crystal system: orthorhombic
| a: | 8.9315 (±0.0007) Å |
| b: | 26.023 (±0.003) Å |
| c: | 8.4082 (±0.0007) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: HI, H3PO2, Ethanol, SnI2, butylammonium iodide (BAI)
Product: dark purple plate-like crystals
Description: In an inert atmosphere, stoichiometric quantities of BAI and SnI2 were added to HI. The solution was heated to 75°C to dissolve the solids and subsequently cooled to 5 °C at a rate of 1.5 °C/hour.
Method: Single-crystal X-ray diffraction
Description: Data were recorded using a Rigaku R-AXIS rapid imaging plate diffractometer with graphite-monochromated Mo Kα radiation (λ = 0.71069 Å).
Crystal system: orthorhombic
| a: | 8.4372 (±0.0009) Å |
| b: | 8.9376 (±0.001) Å |
| c: | 26.167 (±0.003) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: BAI, 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 0.45mmol BAI, 0.40mmol 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.