Complete recipeSource: Both
Route 1: Hydrothermal
p003 / SI p.S3 · Synthesis of single crystals of 1
Metal precursorsCuI (38 mg, 0.2 mmol)
Linker precursors3,3',5,5'-tetramethyl-4,4'-bipyrazol/TMBP (38 mg, 0.2 mmol)
SolventsH2O (10 mL)
AdditivesKI (830 mg, 5.0 mmol), large excess
AtmosphereStirred in air before sealing in a Teflon-lined autoclave; hydrothermal step conducted sealed.
Temperature140
Time48
Oxidant / reductantAir oxidation of KI proposed to generate I2 in situ.
Work-upCooled to room temperature at 5 C/h; black needle-like crystals collected by suction filtration, washed several times with distilled water, and dried in air.
ActivationNo activation reported.
Scalability contextMilligram-scale single-crystal synthesis; yield 82.5 mg, 65% based on TMBP.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | 3,3',5,5'-tetramethyl-4,4'-bipyrazol (TMBP) | 38 mg, 0.2 mmol | p003 / SI p.S3 · Synthesis of single crystals of 1 |
| Metal Source | CuI | 38 mg, 0.2 mmol | p003 / SI p.S3 · Synthesis of single crystals of 1 |
| Additive | KI | 830 mg, 5.0 mmol | p003 / SI p.S3 · Synthesis of single crystals of 1 |
| Solvent | H2O | 10 mL | p003 / SI p.S3 · Synthesis of single crystals of 1 |
| Oxidant | air/O2, proposed in situ oxidation of KI | Not specified | p003 / SI p.S3 · Synthesis of single crystals of 1 |