Crystal system: triclinic
| a: | 11.1463 (±0.0003) Å |
| b: | 11.2181 (±0.0003) Å |
| c: | 17.6966 (±0.0005) Å |
| α: | 99.173 (±0.001)° |
| β: | 104.634 (±0.001)° |
| γ: | 89.999 (±0.001)° |
Starting materials: PbCl2, HCl, methanol, phenethylamine
Product: Small block-like crystals to larger plate-like crystals
Description: Layered solution approach. Grow crystals within a long, straight, glass tube (Refer to Fig. 1). First dissolve 1.0 mmol (0.278 g) of freshly sublimed PbCl2 (Aldrich; 99.999%) in 7.5 ml concentrated (37 wt %) aqueous HCl (Aldrich; 99.999%). Weigh and add PbCl2 to the tube in an argon-filled glove box, with oxygen and water levels maintained below 1 ppm. Cover the tube with a septum before removing the glove box and adding HCl with a syringe. Create a second layer in the crystal tube by gently syringing 15 ml of methanol (Aldrich; anhydrous, 99.8%) on top of the HCl/PbCl2 solution. A relatively sharp interface can be created between the solvent layers due to density differences. On top of the column, add a stoichiometric amount (2 mmol or approximately 0.25 ml) of phenethylamine with a syringe. In the experiment, the phenethylamine rapidly dispersed in the methanol but, because of the sharp interface with the HCl solution, formation of the final (C6H5C2H4NH3)2PbCl4 product was very slow. The crystals were isolated after approximately one year by removing the solvent with a syringe and drying the crystals under vacuum at room temperature and later stored in an argon glove box.
Method: Single-crystal X-ray diffraction
Description: A colorless single crystal of dimensions 0.09 mm X 0.18 mm X 0.27 mm was used. A full sphere of data was collected at room temperature on a Bruker SMART CCD diffractometer, equipped with a normal focus 2.4 kW sealed tube X-ray source (Mo Kα radiation, λ = 0.71073 Å). Refer to page 695 for details.
Comment: Refer to Table 2 for the positional data