Crystal system: orthorhombic
| a: | 9.0894 (±4e-06) Å |
| b: | 39.262 (±2e-05) Å |
| c: | 8.9518 (±6e-06) Å |
| α: | 90 (±0)° |
| β: | 90 (±0)° |
| γ: | 90 (±0)° |
Starting materials: PbO (99.9%), guanidinium chloride (99%), hydroiodic acid (HI, 57 wt % in H2O, distilled, stabilized, 99.95%), butylamine, hypophosphorous acid solution (H3PO2, 50 wt % in H2O)
Product: red plate-shaped crystals
Description: First, PbO (223 mg, 1 mmol) and GA chloride (47.8 mg, 0.5 mmol) were added to 1.5 mL of concentrated HI solution. These substances were dissolved under constant stirring and heating. Then, BA (49.6 μL, 0.5 mmol) was added to 0.25 mL of concentrated aqueous H3PO2 in a separate vial. This solution was stirred and was soon added to the initial solution. The temperature was lowered to 125º C until crystals began to form. The temperature was lowered again to 80ºC, the hot plate was turned off after 60 minutes, and after 30 minutes thereafter, the crystals were collected.
Method: Powder X-ray diffraction
Description: A Rigaku Miniflex600 powder X-ray diffractometer (Cu Kα graphite, λ = 1.5406 Å) was used. Operating settings included 40 kV/15 mA with Kβ foil filter.
Crystal system: orthorhombic
| a: | 39.262 (±5e-05) Å |
| b: | 9.0894 (±1e-05) Å |
| c: | 8.9518 (±9e-06) Å |
| α: | 90 (±0)° |
| β: | 90 (±0)° |
| γ: | 90 (±0)° |
Starting materials: PbO, GA chloride, HI, BA, H3PO2
Product: red plate-shaped crystals
Description: First, PbO (223 mg, 1 mmol) and GA chloride (47.8 mg, 0.5 mmol) were added to 1.5 mL of concentrated HI solution. These substances were dissolved under constant stirring and heating. Then, BA (49.6 μL, 0.5 mmol) was added to 0.25 mL of concentrated aqueous H3PO2 in a separate vial. This solution was stirred and was soon added to the initial solution. The temperature was lowered to 125º C until crystals began to form. The temperature was lowered again to 80ºC, the hot plate was turned off after 60 minutes, and after 30 minutes thereafter, the crystals were collected.
Method: Powder X-ray diffraction
Description: A Rigaku Miniflex600 powder X-ray diffractometer (Cu Kα graphite, λ = 1.5406 Å) was used. Operating settings included 40 kV/15 mA with Kβ foil filter.