Crystal system: triclinic
| a: | 33.0253 Å |
| b: | 8.7437 Å |
| c: | 8.7437 Å |
| α: | 89.632° |
| β: | 84.6307° |
| γ: | 84.616° |
Starting materials: HI (Sigma Aldrich, 57% w/w), chloroform (Fisher, HPLC grade), tributylphosphate (Acros Organics, 99+%), PbI2 (Strem, 99.999+%), phenylethylamine (PEA, Sigma-Aldrich, >99.5%), diethyl ether (Fisher, ACS grade, anhydrous, stabilized with BHT)
Product: orange crystals
Description: 7 ml Unstabilized HI was treated with 10% v/v solution of tributylphosphate in chloroform. The aqueous phase (HI) was extracted. PbI2 (.231 g) was dissolved in the HI solution by heating to 100º C under N2 flow. In it, 0.13 ml PEA is added. The reaction is then cooled to room temperature, at a constant rate of 2 ºC/h. Then, the mixture is cooled at 4ºC for 30 minutes, filtered, washed with diethyl ether, and dried overnight under vacuum at 50 °C.
Method: Single crystal X-Ray Diffraction
Description: SCXRD data are collected on a Bruker Kappa APEX II DUO diffractometer with a CCD area detector employing graphite-monochromated Mo Kα radiation (λ = 0.710 73 Å).