Crystal system: triclinic
| a: | 8.7389 (±0.0002) Å |
| b: | 8.7403 (±0.0002) Å |
| c: | 32.9952 (±0.0006) Å |
| α: | 84.646 (±0.001)° |
| β: | 84.657 (±0.001)° |
| γ: | 89.643 (±0.001)° |
Starting materials: PbI2 (99.999% trace metal basis), HI (57 wt % in H2O, with hypophosphorous acid as stabilizer, assay 99.95%), CH3OH (>99.9%), 2-phenylethylamine (PEA, 99%)
Product: Red and laminar crystals.
Description: Dissolve PbI2 (54.6 mg) in 0.5 mL of HI (57%). Place CH3OH (1 ml) on the top of the PbI2 solution. Add 0.030 mL of PEA liquid into the CH3OH layer. Crystals would form in the solution overnight.
Method: Single-crystal X-ray diffraction
Description: Single-crystal X-ray diffraction data were collected using a Bruker D8 ADVANCE Series II at room temperature. The crystal structures were solved and refined by Shelxl and Olex software.
Comment: This is the experimentally resolved structure, which contains a statistical (disordered) representation of the equatorial iodine atoms in the original refinement. This structure is our recommended "best" published experimental structure for phenethylammonium lead iodide at room temperature, supported by a computational comparison of the total energies of various published structures after full structure optimization in Chemistry of Materials, Vol. 34, issue 7, 3109-3122 (2022), https://doi.org/10.1021/acs.chemmater.1c04213. The computationally relaxed (PEA)2PbI4 structure with resolved disorder (i.e., no overlapping iodine positions), optimized using the PBE+Tkatchenko-Scheffler approach, is also available in the HybriD3 database (see datasets linked to the present one.)