Crystal system: monoclinic
| a: | 16.5278 (±0.0009) Å |
| b: | 8.562 (±0.0004) Å |
| c: | 8.7273 (±0.0005) Å |
| α: | 90° |
| β: | 99.531 (±0.003)° |
| γ: | 90° |
Starting materials: Hydroiodic acid (55-57% w/w containing 1.5% hypophosphorous acid as stabilizer), 4-fluorophenethylamine, PbI2, acetone, nitromethane, NaI
Product: orange, plate-shaped crystals
Description: (FPEA)I was first synthesized by adding concentrated hydroiodic acid (2.4 mL) to 4-fluorphenethylamine (2.0 mL) at 0º C. A colorless precipitate formed, and the solid was filtered and washed with dethyl ether. A 60º C, saturated isopropanol solution was cooled to -10º C and (FPEA)I resulted. The perovskite crystals were formed by dissolving solid (FPEA)I (12 mg, 0.043 mmol) and PbI2 (10 mg, 0.022 mmol) in acetone (10 mL) and nitromethane (5mL). To enhance solubility, solid NaI (6.5 mg, 0.043 mmol) was added and orange, plate-shaped crystals formed over 6 days from slow solvent evaporation.
Method: Single crystal X-Ray Diffraction
Description: Conducted on Beamline 11.3.1. Crystals were coated with Paratone-N oil, placed on a MiTeGen sample mount, and then mounted on the goniometer head of Bruker d85 diffractometer with Photon 100 CMOS detector. Data were corrected for Lorentz and polarization effects via SAINT v8.34A and for absorption effects via TWINABS V2012/I4. The incident radiation was 0.7749 Å.
Comment: All were solved using APEX3 and refined using SHELXTL and OLEX2 software