Compound 2
4PE(benzaldehyde)4
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Compound data: CIF
Compound data: FCF
Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.
In an argon atmosphere, dry benzaldehyde (53 mg, 0.5 mmol, 5 equiv.) was added to a suspension of 1 (39.2 mg, 0.10 mmol, 1 equiv.) in anhydrous 1,4-dioxane (0.5 mL) and CHCl3 (2 mL). After addition of 5 beads of 3 Å molecular sieve, the reaction mixture was heated at 70 °C for 16 h. Upon slow cooling yellow needles formed, which were isolated by filtration and dried under reduced pressure. Crystals suitable for X-ray structure analysis were grown from a THF/1,2-dichloroethane (1:1 v:v) solution.
