| Initial crystal system | tetragonal |
| Final crystal system | cubic |
| Initial space group | I4/mcm |
| Final space group | Pm-3m |
| Direction | Heating |
| Phase transition temperature | 330.0 K |
Hysteresis: 15
| Initial crystal system | cubic |
| Final crystal system | tetragonal |
| Initial space group | Pm-3m |
| Final space group | I4/mcm |
| Direction | Cooling |
| Phase transition temperature | 315.0 K |
Hysteresis: 15
| Initial crystal system | orthorhombic |
| Final crystal system | tetragonal |
| Initial space group | Pnma |
| Final space group | I4/mcm |
| Direction | Heating |
| Phase transition temperature | 172.0 K |
Hysteresis: 9
| Initial crystal system | tetragonal |
| Final crystal system | orthorhombic |
| Initial space group | I4/mcm |
| Final space group | Pnma |
| Direction | Cooling |
| Phase transition temperature | 163.0 K |
Hysteresis: 9
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: Neutron diffraction
Description: Samples were loaded into 8mm diameter vanadium cans in a helium glove- box for analysis on the POWGEN diffractometer situated at the Spallation Neutron Source, Oak Ridge National Laboratory. The analyses of the POWGEN data were carried out using the TOPAS refinement package for Rietveld. Heating and cooling rates were 1K/min. Refer to Page 10 Table 2.