Crystal system: monoclinic
| a: | 39.741 (±0.002) Å |
| b: | 5.842 (±0.003) Å |
| c: | 11.5734 (±0.0006) Å |
| α: | 90° |
| β: | 92.36 (±0.01)° |
| γ: | 90° |
Starting materials: AEQT.2HBr, PbBr2, ethylene glycol, HBr (48% in water)
Product: Yellow (AEQT)PbBr4 crystals
Description: Prepare the starting AEQT.2HBr salt using a technique similar to that described in detail for the synthesis of AMQT.2HCl [1]. Grow (AEQT)PbBr4 crystals from a slowly cooled, saturated, aqueous solution containing the organic and inorganic salts. First, weigh 14.5 mg (0.025 mmol) of AEQT.2HBr and 18.3 mg (0.050 mmol) of PbBr2 and add to a test tube under an inert atmosphere. Dissolve the contents in the sealed tube at 120 °C in a solvent mixture of 22 mL of deionized water, 1 mL of ethylene glycol, and 2 drops of 48% aqueous HBr, forming a nominally saturated yellow solution. Slow cool at 2 °C/h to 0 °C, to form small, yellow, sheetlike crystals of the desired (AEQT)PbBr4 compound. To prevent deforming the thin crystals, remove the product from the reaction tube using a pipet and deposit on filter paper to absorb the solution.
Comment: References: [1] (a) Muguruma, H.; Saito, T.; Sasaki, S.; Hotta, S.; Karube, I. J. Heterocycl. Chem. 1996, 33, 173. (b) Muguruma, H.; Saito, T.; Hiratsuka, A.; Karube, I.; Hotta, S. Langmuir 1996, 12, 5451.
Method: Single-crystal X-ray diffraction
Description: An (AEQT)PbBr4 crystal, with the approximate dimensions 0.01 mm X 0.27 mm X 0.30 mm, was selected under a microscope and attached to the end of a quartz fiber with 5 min epoxy. 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 Ka radiation). Refer to Page 6247 for details.
Comment: Refer to Table 2 for Positional and Thermal Parameters.
Crystal system: triclinic
| a: | 39.95010996 Å |
| b: | 11.60299493 Å |
| c: | 11.48001227 Å |
| α: | 89.98225306° |
| β: | 91.24294626° |
| γ: | 90.02085902° |
Code: FHI-aims
Level of theory: density functional theory
Exchange-correlation functional: HSE06 α = 0.25, ω = 0.11/bohr
Level of relativity: with spin-orbit coupling
Comment: Using the experimental structure of AE4TPbBr4 [1], also in Dataset ID 217. [1] D. B. Mitzi, K. Chondroudis, and C. R. Kagan, Inorg. Chem. 38, 6246 (1999).