Crystal system: monoclinic
| a: | 8.67739964 Å |
| b: | 9.01430035 Å |
| c: | 26.41200065 Å |
| α: | 90° |
| β: | 92.49199677° |
| γ: | 90° |
Starting materials: PbI2, 47% HI, C14H29NH2, ethyl acetate
Product: Red plate-like crystal
Description: 0.015 g PbI2 (0.104 mmol) was added into 1 mL 47% HI. Then, 0.010 g C14H29NH2 (0.047 mmol) was added to the above solution. The formed precipitation was then dissolved into 5 mL ethyl acetate. The yellow single crystals were obtained by slow evaporation over a number of days. The crystals undergo a phase transition at a higher temperature to obtain the red monoclinic phase.
Method: Single crystal X-ray diffraction
Description: A Bruker Apex II CCD diffractometer with graphite-monochromated Mo-Ka radiation (λ = 0.71073 Å) was used to get diffraction data. SAINT-NT16 was used to do data reduction and cell refinement. XPREP16 was used to determine space groups. WinGx17 Suite by direct methods using SHELXS9718 was used to resolve structure and the structure refinement was done by full-matrix least squares/difference Fourier techniques using SHELXL97.
Code: FHI-aims
Level of theory: Density Functional Theory (DFT)
Exchange-correlation functional: PBE-TS
K-point grid: 5X5X2
Level of relativity: atomic ZORA
Basis set definition: intermediate