Crystal system: orthorhombic
| a: | 9.1437 (±0.0002) Å |
| b: | 8.6684 (±0.0002) Å |
| c: | 28.5984 (±0.0005) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: Benzylamine (BzA), PbI2, Aq. HI (57%), H3PO2 (50 %)
Product: Orange (BzA)2PbI4 crystals
Description: BzA (214.45 mg) was dissolved in Aq.HI (4.5 ml) treated with hypophosphorous acid (0.5 ml) as a stabilizer. A stoichiometric amount of PbI2 (461.01) was added to the above solution, stirred at 90 °C for 2 h, and cooled to room temperature at a rate of 1 K/hr to induce crystallization. All synthesis was performed at ambient conditions. The as-formed crystals were collected by suction, washed with diethyl ether and dried under vacuum.
Method: single crystal X-ray diffraction
Description: Single crystal X-ray data were collected on a Nonius Kappa CCD single-crystal diffractometer (MoKα, λ = 0.71073 Å) at 180 K.
Crystal system: orthorhombic
| a: | 9.1561 (±0.0005) Å |
| b: | 8.6894 (±0.0003) Å |
| c: | 28.7762 (±0.0015) Å |
| α: | 90° |
| β: | 90 (±0.004)° |
| γ: | 90° |
Starting materials: PbO, HI, H3PO2, benzylamine hydrochloride
Product: Orange plate-like crystals
Description: PbO powder was dissolved in a solution with HI and H3PO2 and heated while stirring for 20 minutes at 120 degrees Celsius. The solution became bright yellow. Benzylamine hydrochloride was then dissolved into another HI solution and also heated (2:1 molar ratio to PbO). Then the latter solution was carefully layered on top of the PbI2 solution and dark orange crystals precipitated upon cooling.
Method: Single-crystal X-ray diffraction
Description: Either a STOE IPDS 2 or IPDS 2T diffractometer with Mo Kalpha radiation operated at 50 kV and 40 mA in a nitrogen atmosphere was used. Integration and absorption corrections were made with the STOE X-AREA programs. Structure was solved directly and refined with full-matrix least-squares on F2 with the OLEX2 program package.