Crystal system: cubic
a: | 6.2397 (±0.0005) Å |
b: | 6.2397 (±0.0005) Å |
c: | 6.2397 (±0.0005) Å |
α: | 90° |
β: | 90° |
γ: | 90° |
Starting materials: Tin (II) oxide, HI (aq), ethylene glycol, argon, nitrogen
Product: Black-green powder.
Description: Dissolve Tin (II) oxide (10.40 g, 27.9 mmole) in 20 ml of a concentrate (57% by weight) HI (aq) in a test tube under flowing argon. Add another 8.0 ml of aqueous HI to a test tube containing CH3NH3-HI (4.44g, 27.9 mmole). Gently heat solution to 90.0 °C in a water/ethylene glycol bath to facilitate dissolution. Mix warm CH3NH2-HI and SNI2 solutions and cool the resulting yellow solution to room temperature. Filter the black-green precipitate that forms under flowing nitrogen and dry under flowing argon at 100 °C for 5 hr. Yield is typically 76 %. CH3NH3SnI3 is air sensitive and decomposes in air within several hours. All samples are stored and manipulated for the various measurements in an argon-filled glove box with oxygen and water levels below 1 ppm.
Method: Powder X-ray diffraction
Description: Not specified. Refer to Page 160 Experimental paragraph 1.
Comment: The reference for the assignment of the PXRD peaks is not available.
Crystal system: cubic
a: | 6.2 Å |
b: | 6.2 Å |
c: | 6.2 Å |
α: | 90° |
β: | 90° |
γ: | 90° |
Starting materials: Tin (II) oxide, HI (aq), ethylene glycol, argon, nitrogen
Product: Black single crystal
Description: Dissolve Tin (II) oxide (10.40 g, 27.9 mmole) in 20 ml of a concentrate (57% by weight) HI (aq) in a test tube under flowing argon. Add another 8.0 ml of aqueous HI to a test tube containing CH3NH3-HI (4.44g, 27.9 mmole). Gently heat solution to 90.0 °C in a water/ethylene glycol bath to facilitate dissolution. Mix warm CH3NH2-HI and SNI2 solutions and cool the resulting yellow solution to room temperature. Filter the black-green precipitate that forms under flowing nitrogen and dry under flowing argon at 100 °C for 5 hr. Yield is typically 76 %. CH3NH3SnI3 is air sensitive and decomposes in air within several hours. All samples are stored and manipulated for the various measurements in an argon-filled glove box with oxygen and water levels below 1 ppm. Use 2.0 g of CH3NH3SnI3 and equilibrate at 90.0 °C in a water/ethylene glycol bath. Add sufficient HI under flowing argon to dissolve the entire charge (about 11 ml). Cool the solution to -10.0 °C at 2 °C/hr. The small black crystals grow in a rhombic dodecahedral habit.
Method: X-ray diffraction
Description: Not specified. Refer to Page 160 Experimental paragraph 1,3.
Crystal system: cubic
a: | 6.242 (±0.001) Å |
b: | 6.242 (±0.001) Å |
c: | 6.242 (±0.001) Å |
α: | 90° |
β: | 90° |
γ: | 90° |
Starting materials: Tin (II) iodide, methylammonium iodide, HI (aq), argon, nitrogen
Product: Powder
Description: Dissolve tin(II) iodide (2.235 g, 6 mmol) in flowing argon at 70°C in 4 ml of a concentrated (57% by weight) aqueous HI solution. Dissolve methylammonium iodide (6 mmol) at room temperature in 1.0 ml of concentrated aqueous hydriodic acid and immediately add to the tin(II) iodide solution (after allowing it to cool). Rinse the methylammonium tube using two additional 0.5-ml portions of hydriodic acid and add to the test tube containing the product, which at all times was kept in an inert atmosphere of flowing argon. Maintain the product in the hydriodic acid solution for 15 min at room temperature, with periodic agitation of the solution, and filter under flowing dry nitrogen gas. Dry powder under vacuum at room temperature and store in an argon-filled glovebox, with oxygen and water levels maintained below 1 ppm.
Comment: Similar procedure as MASnI3 in D. B. Mitzi, C. A. Feild, Z. Schlesinger, and R. B. Laibowitz, J. Solid State Chem. 114, 159 (1995).
Method: Powder X-ray diffraction
Description: Siemens D5000 CuKα radiation, refined using Siemens WIN-METRIC program. Refer to Page 377 X-ray diffraction section.
Crystal system: tetragonal
a: | 6.2302 (±0.0001) Å |
b: | 6.2302 (±0.0001) Å |
c: | 6.2316 (±0.0011) Å |
α: | 90° |
β: | 90° |
γ: | 90° |
Starting materials: CH3NH3I [from synthesis], SnI2 [from synthesis], distilled HI (57% aqueous) (99.95%), H3PO2 (50% aqueous)
Product: Black MASnI3 crystals
Description: Charge 100 ml 2-necked round bottom flask with a mixture of aqueous HI (6.8 ml, 7.58M) and aqueous H3PO2 (1.7 ml, 9.14M). The liquid was degassed by passing a stream of nitrogen through it for 1 min and keeping it under a nitrogen atmosphere throughout the experiment. Dissolve SnI2 (372 mg, 1 mmol) in the mixture upon heating the flask to 120 °C using an oil bath, under constant magnetic stirring, forming a bright yellow solution. Add solid CH3NH3I (159 mg, 1 mmol). Evaporate solution to approximately half its original volume by heating at 120 °C. Discontinue stirring and leave the solution to cool back to room temperature. Upon cooling, black, elongated, rhombic dodecahedral (12 faces) crystals of the title compound were precipitated. Leave crystals to grow for a further 24 h under a nitrogen atmosphere before filtering and washing copiously with degassed EtOH.
Method: Single crystal X-ray diffraction
Description: Single-crystal X-ray diffraction experiments were performed using either a STOE IPDS II or IPDS 2T diffractometer using Mo Kα radiation (λ = 0.71073 Å) and operating at 50 kV and 40 mA. Integration and numerical absorption corrections were performed using the X-AREA, X-RED, and X-SHAPE programs. Refer to Page 9025 Table 1.
Crystal system: tetragonal
a: | 8.7577 (±0.0015) Å |
b: | 8.7577 (±0.0015) Å |
c: | 12.429 (±0.003) Å |
α: | 90° |
β: | 90° |
γ: | 90° |
Starting materials: CH3NH3I [from synthesis], SnI2 [from synthesis], distilled HI (57% aqueous) (99.95%), H3PO2 (50% aqueous)
Product: Black MAPbI3 crystals
Description: Charge 100 ml 2-necked round bottom flask with a mixture of aqueous HI (6.8 ml, 7.58M) and aqueous H3PO2 (1.7 ml, 9.14M). The liquid was degassed by passing a stream of nitrogen through it for 1 min and keeping it under a nitrogen atmosphere throughout the experiment. Dissolve SnI2 (372 mg, 1 mmol) in the mixture upon heating the flask to 120 °C using an oil bath, under constant magnetic stirring, forming a bright yellow solution. Add solid CH3NH3I (159 mg, 1 mmol). Evaporate the solution to approximately half its original volume by heating at 120 °C. Discontinue stirring and leave the solution to cool back to room temperature. Upon cooling, black, elongated, rhombic dodecahedral (12 faces) crystals of the title compound were precipitated. Leave crystals to grow for a further 24 h under a nitrogen atmosphere before filtering and washing copiously with degassed EtOH. Yield 70-90%.
Method: Single crystal X-ray diffraction
Description: Single-crystal X-ray diffraction experiments were performed using either an STOE IPDS II or IPDS 2T diffractometer using Mo Kα radiation (λ = 0.71073 Å) and operating at 50 kV and 40 mA. Integration and numerical absorption corrections were performed using the X-AREA, X-RED, and X-SHAPE programs. Refer to Page 9025 Table 2.