Crystal system: orthorhombic
| a: | 8.8632 (±0.0021) Å |
| b: | 8.6816 (±0.0008) Å |
| c: | 27.57 (±0.002) Å |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: PbI2, HI, C4H9NH2
Product: Orange-yellow sheetlike crystals
Description: Grow the crystals under slowly-cooled aqueous hydriodic acid solutions. Perform all synthetic steps and crystal manipulations after synthesis in an inert atmosphere to prevent oxidation. Dissolve 0.534 g (1.16 mmol) of PbI2 in 2 mL of concentrated (57 wt %) aqueous HI solvent under flowing argon at 90 °C. In a separate tube, dissolve 2.32 mmol of (C4H9NH2).HI in 3 mL of concentrated HI solution and add to the metal halide solution. Ramp the solution temperature at 2 °C/h from 90 to -10 °C, filter the crystals formed under argon or nitrogen and dry in argon at 80 °C.
Method: Single crystal X-ray diffraction
Description: Select suitable single crystals in an argon-filled drybox (<1 ppm O2 and H2O) under a microscope and seal in quartz capillaries. Collect data at room temperature on an Enraf-Nonius CAD4 diffractometer with graphite-monochromatized Mo Ka radiation. Obtain unitcell parameters and the crystal orientation matrix by a least-squares fit of 25 reflections with 18° < 2θ < 30°. Monitor intensity control reflections every 5000s during the data collection. Little to no degradation was observed for the compounds. Use the NRCVAX 386 PC version program for structural solution and refinement.
Crystal system: orthorhombic
| a: | 8.8764 |
| b: | 8.6925 |
| c: | 27.6014 |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: PbI2; HI; C4H9NH2
Product: Orange single crystal
Description: PbI2 (0.217 g, 0.471 mmol) was dissolved in 3 ml of 47% HI in a sample vial. Thereafter, 0.074 g of C4H9NH2 (1.01 mmol) was added and the precipitate dissolved by refluxing for 2 h at 363 K. The solution was slowly cooled at 2 K h 1 to room temperature
Comment: Billing D G, Lemmerer A. Synthesis, characterization and phase transitions in the inorganic–organic layered perovskite-type hybrids [(CnH2n+ 1NH3) 2PbI4], n= 4, 5 and 6[J]. Acta Crystallographica Section B: Structural Science, 2007, 63(5): 735-747.
Method: X-ray diffraction analysis
Description: Diffraction data were collected using a Bruker Apex II CCD diffractometer (Bruker, 2005) equipped with graphite-monochromated Mo Kα radiation (lambda = 0.71073 Å). For experiments conducted at non-ambient temperatures, an Oxford Cryostream 700 was employed. Data reduction and unit cell refinement were performed using SAINT-PLUS (Bruker, 2004), and space groups were determined through systematic absences analyzed with XPREP (Bruker, 2004) and further validated by refinement results. Absorption corrections based on face-indexed data were applied to all crystals using XPREP (Bruker, 2004).
Comment: Billing D G, Lemmerer A. Synthesis, characterization and phase transitions in the inorganic–organic layered perovskite-type hybrids [(CnH2n+ 1NH3) 2PbI4], n= 4, 5 and 6[J]. Acta Crystallographica Section B: Structural Science, 2007, 63(5): 735-747.
Code: FHI-aims
Level of theory: Density Functional Theory (DFT)
Exchange-correlation functional: PBE-TS
K-point grid: 5X5X2
Level of relativity: atomic ZORA
Basis set definition: intermediate
Crystal system: orthorhombic
| a: | 8.428 |
| b: | 8.986 |
| c: | 26.233 |
| α: | 90° |
| β: | 90° |
| γ: | 90° |
Starting materials: PbI2; HI; C4H9NH2
Product: Orange single crystal
Description: PbI2 (0.217 g, 0.471 mmol) was dissolved in 3 ml of 47% HI in a sample vial. Thereafter, 0.074 g of C4H9NH2 (1.01 mmol) was added and the precipitate dissolved by refluxing for 2 h at 363 K. The solution was slowly cooled at 2 K h 1 to room temperature
Comment: Billing D G, Lemmerer A. Synthesis, characterization and phase transitions in the inorganic–organic layered perovskite-type hybrids [(CnH2n+ 1NH3) 2PbI4], n= 4, 5 and 6[J]. Acta Crystallographica Section B: Structural Science, 2007, 63(5): 735-747.
Method: X-ray diffraction analysis
Description: Diffraction data were collected using a Bruker Apex II CCD diffractometer (Bruker, 2005) equipped with graphite-monochromated Mo Kα radiation (lambda = 0.71073 Å). For experiments conducted at non-ambient temperatures, an Oxford Cryostream 700 was employed. Data reduction and unit cell refinement were performed using SAINT-PLUS (Bruker, 2004), and space groups were determined through systematic absences analyzed with XPREP (Bruker, 2004) and further validated by refinement results. Absorption corrections based on face-indexed data were applied to all crystals using XPREP (Bruker, 2004).
Comment: Billing D G, Lemmerer A. Synthesis, characterization and phase transitions in the inorganic–organic layered perovskite-type hybrids [(CnH2n+ 1NH3) 2PbI4], n= 4, 5 and 6[J]. Acta Crystallographica Section B: Structural Science, 2007, 63(5): 735-747.
Code: FHI-aims
Level of theory: Density Functional Theory (DFT)
Exchange-correlation functional: PBE-TS
K-point grid: 5X5X2
Level of relativity: atomic ZORA
Basis set definition: intermediate