Vague recipeSource: SI
Route 1: Unknown
2 · Materials and Methods
Synthesis evidence
Ligand-Insertion Strategy for Constructing 2D Conjugated Metal–Organic Framework with Large Pore Size for Electrochemical Analytics
Wang X.-Z., Chen Y., Cao X.-M. et al. · Angewandte Chemie - International Edition · 2025 · e202413115
4 structured synthesis routes
Completeness describes how fully the route could be reconstructed from the main article and supporting information.
Complete recipeSource: SI
Route 2: Drop Cast
3 · Electrochemical Measurements
SolventsWater/ethanol mixed solvent (v/v = 1/1)
AdditivesNafion, 50 uL
AtmosphereAir drying; electrochemical cell atmosphere not specified
Temperatureroom temperature drying
Time1.5 h sonication; drying time not specified
Substrate orientationPolished 3 mm diameter GCE
Work-upGCE polished with 1 and 0.3 um alumina slurries, rinsed with ethanol and deionized water in ultrasonic bath, dried in air; 5 uL MOF suspension drop-cast and dried naturally.
Scalability contextElectrode-preparation protocol uses 4 mg MOF and 5 uL aliquots for each 3 mm GCE.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | Cu3(HHTP)(DHBQ)1.5(3-) powder | 4 mg | 3 · Electrochemical Measurements |
| Additive | Nafion | 50 uL | 3 · Electrochemical Measurements |
| Solvent | water/ethanol (v/v = 1/1) | 400 uL | 3 · Electrochemical Measurements |
| Other | GCE | 3 mm diameter | 3 · Electrochemical Measurements |
Complete recipeSource: Both
Route 3: Liquid Liquid Interface
2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2
Metal precursorsCopper acetate (22 mg, 0.1 mmol)
Linker precursorsHHTP (10 mg, 0.03 mmol); DHBQ (16 mg, 0.11 mmol)
Solvents6 mL distilled water; 2 mL n-butanol interface layer; 3 mL n-butanol ligand solution
AdditivesEthylenediamine (en, 13 uL, 0.2 mmol) as modulator/base
AtmosphereSealed glass vial; atmosphere not otherwise specified
Temperature65
Time24
Oxidant / reductantDHBQ can act as a reductant at high concentration; successful route physically separates Cu2+ from excess DHBQ in a liquid-liquid interface.
Work-upCool to room temperature; separate black solid by centrifugation; wash with water (5 mL x 3) and acetone (5 mL x 3); dry at 85 deg C for 12 h.
ActivationFor N2 sorption, samples were degassed under vacuum at 120 deg C for 12 h before measurement.
Scalability contextSmall sealed-vial interfacial synthesis using commercially available ligands; SI recipe uses milligram-scale reagents in a 20 mL vial.
Show 8 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Copper acetate | 22 mg, 0.1 mmol | 2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2 |
| Base | ethylenediamine (en) | 13 uL, 0.2 mmol | 2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2 |
| Solvent | distilled water | 6 mL | 2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2 |
| Solvent | n-butanol | 2 mL interface layer plus 3 mL ligand solution | 2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2 |
| Linker | 2,3,6,7,10,11-hexahydrotriphenylene (HHTP) | 10 mg, 0.03 mmol | 2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2 |
| Linker | 2,5-dihydroxybenzoquinone (DHBQ) | 16 mg, 0.11 mmol | 2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2 |
| Solvent | water wash | 5 mL x 3 | 2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2 |
| Solvent | acetone wash | 5 mL x 3 | 2 · Synthesis of Cu3(HHTP)(DHBQ)1.5(3-) · Table S2; Figure S2 |
Partial recipeSource: Both
Route 4: Solvothermal
12 · Table S1 · Table S1; Figure S1
Metal precursorsCu(OAc)2 fixed at 22 mg in Table S1
Linker precursorsHHTP fixed at 10 mg; DHBQ varied; HHTP/DHBQ ratios 1/1.5 or 1/3.7
SolventsDMF/H2O = 1/1, H2O, DMF, or DMF/H2O = 2/1; total 11 mL mixed solvent
Additivesen (13 uL) or NH4OH (29 uL)
AtmosphereNot specified
Temperature65-120
Time24
Oxidant / reductantHigh DHBQ concentration gave products with Cu impurity, attributed to DHBQ reducing Cu2+ ions.
Work-upNot reported for screening attempts
Scalability contextScreening routes did not provide the high-crystallinity target and motivated liquid-liquid interface synthesis.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Cu(OAc)2 | 22 mg | 12 · Table S1 · Table S1; Figure S1 |
| Linker | HHTP | 10 mg | 12 · Table S1 · Table S1; Figure S1 |
| Linker | DHBQ | changed; HHTP/DHBQ = 1/1.5 or 1/3.7 | 12 · Table S1 · Table S1; Figure S1 |
| Solvent | DMF/H2O, H2O, or DMF | 11 mL mixed solvent | 12 · Table S1 · Table S1; Figure S1 |
| Base | en or NH4OH | 13 uL en or 29 uL NH4OH | 12 · Table S1 · Table S1; Figure S1 |