Crystal system: orthorhombic
a: | 8.91262 (±0.00019) Å |
b: | 28.7305 (±0.0007) Å |
c: | 9.3578 (±0.0002) Å |
α: | 90° |
β: | 90° |
γ: | 90° |
Starting materials: (S)-(−)-α-methylbenzylamine, (S-MBA, 98%, ee 98%), Tin(IV) oxide (SnO2, 99.9%), hydriodic acid solution (HI, 57% w/w in water, 99.95%, distilled, stabilized by H3PO2), hypophosphorous acid (H3PO2, 50% w/w in water)
Product: Orange, rod-like crystals
Description: SnO2 (0.896 mmol), S-MBA (1.57 mmol), HI (5.5 mL), and H3PO2 (0.5 mL) were mixed. The solution was heated to 120 degrees Celsius and stirred until it became clear and yellow. Its vial was then put in an oil bath at 90 degrees and then underwent slow cooling at the rate of 1 degree per hour, eventually yielding orange rods. The crystals were filtered in a nitrogen atmosphere and were vacuum dried overnight.
Method: single-crystal X-ray diffraction
Description: A Rigaku XtaLAB Synergy-S instrument using Mo Kα radiation (λ = 0.71073 Å) is utilized to collect a full sphere of diffraction data at 250K and multiscan empirical absorption correction was applied. Within the Olex2 software, using direct methods of the SHELXS program to solve the crystal structure, then utilizing the least-squares method of the SHELXL58 program to refine it.
Crystal system: orthorhombic