Crystal system: monoclinic
| a: | 64.191 (±0.006) Å |
| b: | 6.0936 (±0.0005) Å |
| c: | 12.2111 (±0.0009) Å |
| α: | 90° |
| β: | 97.773 (±0.004)° |
| γ: | 90° |
Starting materials: As-synthesized 4Tm, PbI2, anhydrous dimethyl formamide (DMF) ((CH3)2NCH), anhydrous chlorobenzene (CB) (C6H5Cl), Si/SiO2
Product: orange plate-like crystals
Description: Solution and thin film growth experiments were prepared and executed inside of a nitrogen-filled glove box with oxygen and water levels less than 1 ppm. Inside a 4 mL vial, as-synthesized 4Tm (10.6 mg, 20 µmol) and PbI2(4.6 mg, 10 µmol) were dissolved in a mixture of DMF (1 mL) and CB (1 mL). To obtain single crystals, the solution in DMF was diffused with chloroform and chlorobenzene vapor. This resulted in thin orange-red plates.
Method: Single Crystal X-Ray Diffraction
Description: Data were collected using a Bruker AXS D8 Quest CMOS diffractometer, an I-mu-S microsource X-ray tube with Cu Kα radiation (λ = 1.54178 Å), Goebel mirror, and a Photon2 CMOS area detector. Data was collected and analyzed at 150 K. Files were scaled and corrected using APEX3.
Crystal system: monoclinic
| a: | 64.191 (±0.006) Å |
| b: | 6.0936 (±0.0005) Å |
| c: | 12.2111 (±0.0009) Å |
| α: | 90° |
| β: | 97.773 (±0.004)° |
| γ: | 90° |
Starting materials: 4Tm•HI(4Tm: quaterthiophenylethylammonium), lead iodide (PbI2), dimethylformide (DMF), anhydrous chlorobenzene (CB)
Product: sheet-like crystals
Description: 10 μmol of PbI2 and 20 μmol of 4Tm•HI were dissolved in 2 mL of DMF/CB co-solvent (1:1 ration). This resulted in 5 mM of stock solution. This solution was diluted 240 times by CB/An/DCB cosolvent (3.9:1:0.01 volume ratio). Only 5-10 μmol was placed on a growth substrate SiO2, at the bottom of a glass vial and was later transferred to another vial with 3 mL of CB. This was placed on a 90º hot plate. Growth took 10-30 minutes.
Method: Single Crystal X-Ray Diffraction
Description: Bruker AXS D8 Quest CMOS diffractometer with kappa geometry, an I-μ-S microsource X-ray tube, multilayer Göbel mirror, and Photon2 CMOS was used. Data was collected with Cu Kα radiation (λ = 1.54178 Å).