Crystal system: monoclinic
| a: | 8.9159 (±0.0007) Å |
| b: | 20.0335 (±0.0015) Å |
| c: | 8.9925 (±0.0006) Å |
| α: | 90° |
| β: | 91.875 (±0.006)° |
| γ: | 90° |
Starting materials: PbO, HI, H3PO2, histamine dihydrochloride
Product: Dark 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. Histamine dihydrochloride was then dissolved into another HI solution and also heated (1:1 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.
Crystal system: monoclinic
| a: | 8.8952 (±0.0002) Å |
| b: | 19.7237 (±0.0005) Å |
| c: | 8.925 (±0.0002) Å |
| α: | 90° |
| β: | 92.2131 (±0.0007)° |
| γ: | 90° |
Starting materials: histamine dihydrochloride, HI, PbI2
Product: red block
Description: Histamine dihydrochloride was purchased from Sigma Aldrich. Then, stoichiometric amounts of PbI2 (purchased from Sigma Aldrich) and HA were added to concentrated stabilized aqueous HI. The concentration of the solution was maintained at 0.25-0.30M of Pb2+. The solution was heated at 140ºC and stirred for an hour. The resulting clear solution was cooled slowly to room temperature.
Method: Single Crystal X-ray Diffraction
Description: Data was collected with a BrukerX8 CCD area detector diffractometer, with Mo Kα radiation (0.71073Å) at 100 K. SAINT and SADABS packages were used for data reduction and absorption corrections, respectively.