Complete recipeSource: Both
Route 1: Liquid Liquid Interface
2 · Suppl. Note 2
Metal precursorsCuCl2 aqueous solution, 2 x 10^-2 mol/L, 200 mL
Linker precursorsBHT, 100 mg (0.37 mmol), dissolved in 200 mL hot toluene; BHT itself prepared from 1,2,3,4,5,6-hexakis(benzylthio)benzene and BBr3
SolventsWater, toluene, DMF, methanol, acetone, ethyl ether; BHT synthesis used dry fluorobenzene and methanol
AtmosphereMain methods state solvents were freeze-thaw degassed and air-/water-sensitive reactions were performed under nitrogen; SI chamber synthesis uses an oven and does not explicitly state nitrogen during the interface reaction.
Temperature75
Time168
Oxidant / reductantCu2+ is proposed to be partly reduced to Cu+ while BHT is oxidised to an anionic charge state of -4 during framework formation.
Work-upRemove remaining solvent by filtration; wash Cu3BHT film sequentially with DMF, methanol, acetone, and ethyl ether.
ActivationDry the film in a vacuum oven for 24 h; isolated crystals obtained by sonicating the film in methanol.
Scalability context500 mL flask recipe gives multicrystalline film containing microcrystals; higher temperature improves crystallinity, CuCl2 is most effective among Cu salts, and longer reaction time promotes larger crystals.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | CuCl2 | 200 ml copper solution · 2 x 10-2 mol/L | 2 · Suppl. Note 2 |
| Linker | BHT | 100 mg (0.37 mmol) · 1.85 mmol/L in toluene | 2 · Suppl. Note 2 |
| Solvent | toluene | 100 ml buffer layer plus 200 ml hot toluene for BHT | 2 · Suppl. Note 2 |
| Solvent | water | aqueous copper solution | 2 · Suppl. Note 2 |
| Solvent | DMF, methanol, acetone, ethyl ether | sequential washes | 2 · Suppl. Note 2 |