| Initial crystal system | tetragonal |
| Final crystal system | cubic |
| Initial space group | I4/mcm |
| Final space group | Pm-3m |
| Direction | Heating |
| Phase transition temperature | 332.0 K |
Hysteresis: 0
| Initial crystal system | cubic |
| Final crystal system | tetragonal |
| Initial space group | Pm-3m |
| Final space group | I4/mcm |
| Direction | Cooling |
| Phase transition temperature | 332.0 K |
Hysteresis: 0
| Initial crystal system | tetragonal |
| Final crystal system | orthorhombic |
| Initial space group | I4/mcm |
| Final space group | Pnma |
| Direction | Cooling |
| Phase transition temperature | 162.5 K |
Hysteresis: 2.5
Starting materials: CD3ND2DCl (Sigma-Aldrich, 98 atom % D), DI, D2O, PbI2 (Acros Organics)
Product: Black d6-MAPbI3 Powder
Description: Dissolve 1.0 g of CD3ND2DCl in 15 g of 16% DI in D2O (made by dissolving 5 g DI gas in 25 g D2O) and pump to dryness to yield CD3ND2DI. Add material to 6 g of lead iodide and mix in ~25mL of DMF. Upon stirring, obtain pale yellow clear solution. Warm resulting solution and stir overnight in a N2 glove box. Evaporate solution to dryness under vacuum and wash the resulting black solution with dichloromethane and n-propanol. Isolate using suction drying. Anneal solid in nitrogen in the glove box at 140 °C for 1hr to remove residual solvent. Expect to yield 7.95 g of d6-MAPbI3 (97% yield).
Comment: MAPbI3 (d6-CD3ND3PbI3)
Method: Synchrotron X-ray powder diffraction
Description: The X-ray powder diffraction measurements were performed on the bending magnet station at DND-CAT sector 5 of the Advanced Photon Source. The X-ray wavelength used was 0.40012(2) Å, selected to reduce X-ray absorption by the sample to an acceptable level. Temperatures were equilibrated for ~10 min after 1 K changes. Refer to Page 10 Table 2.