Crystal system: orthorhombic
| a: | 8.689 (±0.005) Å |
| b: | 28.78 (±0.01) Å |
| c: | 9.162 (±0.004) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: PbI2 (Johnson Matthey, 976204), PbO (Ferak 01-881), hydroiodic acid 57% (Merck 341), H3PO2 50% (Fluka 9421), benzylamine (Fluka 13180)
Product: Orange plate crystals
Description: To prepare C6H5CH2NH3I, treat benzylamine with aq.HI 57% in the presence of H3PO2 and recrystallize the precipitate from acetonitrile. Treat C6H5CH2NH3I and PbI2 in molar ratio 2:1 in CH3CN or DMF to obtain small crystals. Dissolve C6H5CH2NH2 (107 mg, 1 mmol) and PbO (111.5 mg, 0.5 mmol) in aq. HI (57%) in the presence of H3PO2 at reflux temperature to obtain large crystals. Slowly cool the solution and obtain the crystals several hours later, filter and dry in air.
Method: X-ray diffraction
Description: Collect on a Crystal Logic dual goniometer using graphite monochromated MoKa radiation. Unit cell dimensions were determined and refined by using the angular setting of 24 automatically centered reflections in the range 11° < 29 < 24°. Intensity data were recorded using a Theta-2theta scan. Refer to page 1406 for details.
Crystal system: tetragonal
| a: | 28.53445007 Å |
| b: | 9.199474154 Å |
| c: | 8.532616549 Å |
| α: | 90.0000136° |
| β: | 90.00078387° |
| γ: | 90.00100703° |
Code: FHI-aims
Level of theory: Density Functional Theory (DFT)
Exchange-correlation functional: PBE+TS
K-point grid: 2x5x5
Level of relativity: atomic ZORA
Basis set definition: intermediate