Starting materials: PbO, FA acetate, HI, BA, H3PO2

Product: red plate-shaped crystals

Description: First, PbO (223 mg, 1 mmol) and FA acetate (52.1 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 (89.1 μL, 0.9 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.

X. Li, Y. Fu, L. Pedesseau, P. Guo, S. Cuthriell, I. Hadar, J. Even, C. Katan, C. C. Stoumpos, R. D. Schaller, E. Harel, and M. G. Kanatzidis, Negative Pressure Engineering with Large Cage Cations in 2D Halide Perovskites Causes Lattice Softening, Journal of the American Chemical Society 142, 11486‑11496 (2020). doi: 10.1021/jacs.0c03860.

Extraction method: Manual entry
Entry added on: Dec. 15, 2020, 9:26 p.m.
Entry added by: Rebecca Lau Duke University
Last updated on: Dec. 15, 2020, 9:26 p.m.
Last updated by: Rebecca Lau Duke University

Starting materials: PbO, FA acetate, HI, BA, H3PO2

Product: red plate-shaped crystals

Description: First, PbO (223 mg, 1 mmol) and FA acetate (52.1 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 (89.1 μL, 0.9 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.

X. Li, Y. Fu, L. Pedesseau, P. Guo, S. Cuthriell, I. Hadar, J. Even, C. Katan, C. C. Stoumpos, R. D. Schaller, E. Harel, and M. G. Kanatzidis, Negative Pressure Engineering with Large Cage Cations in 2D Halide Perovskites Causes Lattice Softening, Journal of the American Chemical Society 142, 11486‑11496 (2020). doi: 10.1021/jacs.0c03860.

Extraction method: Manual entry
Entry added on: Dec. 15, 2020, 9:27 p.m.
Entry added by: Rebecca Lau Duke University
Last updated on: Dec. 15, 2020, 9:27 p.m.
Last updated by: Rebecca Lau Duke University