Vague recipeSource: SI
Route 1: Unknown
S4 · Materials
Linker precursorsHHTP
Show 1 structured reagent record
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | HHTP | Not specified | S4 · Materials |
Synthesis evidence
Acid-Dependent Charge Transport in a Solution-Processed 2D Conductive Metal-Organic Framework
Park G., Demuth M.C., Hendon C.H. et al. · Journal of the American Chemical Society · 2024
5 structured synthesis routes
Completeness describes how fully the route could be reconstructed from the main article and supporting information.
Complete recipeSource: Both
Route 2: Hydrothermal
S4-S5 · Synthesis of Cu3(HHTATP)2
Metal precursorsCu(NO3)2.3H2O (63.5 mg, 0.239 mmol)
Linker precursorsHHTATP.3HBr (97.3 mg, 0.159 mmol)
Solventswater: 4.2 mL for linker; 1 mL deionized water for copper solution
Additives0.4145 mL of 28% aqueous ammonia solution
Atmosphereair; capped vial
Temperature80
Time24
Work-upSlow-cooled to room temperature over 5 h; precipitate centrifuged and washed with DMF (35 mL x 3), DCM (20 mL x 2), hexane (20 mL x 2).
ActivationDried at 80 C under vacuum; transferred to N2 glovebox.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | HHTATP.3HBr | 97.3 mg, 0.159 mmol | S4-S5 · Synthesis of Cu3(HHTATP)2 |
| Metal Source | Cu(NO3)2.3H2O | 63.5 mg, 0.239 mmol | S4-S5 · Synthesis of Cu3(HHTATP)2 |
| Solvent | water | 4.2 mL + 1 mL | S4-S5 · Synthesis of Cu3(HHTATP)2 |
| Base | aqueous ammonia | 0.4145 mL · 28% | S4-S5 · Synthesis of Cu3(HHTATP)2 |
Complete recipeSource: Both
Route 3: Solvothermal
S5 · Synthesis of Cu3(HHTATP)2
Metal precursorsCuSO4.5H2O (9.0 mg, 0.0361 mmol)
Linker precursorsHHTATP.3HBr (8.7 mg, 0.0142 mmol)
Solvents2.0 mL DMF for linker; 3.5 mL deionized water for copper solution
Atmosphereair; capped vial
Temperature65
Time12
Work-upSlow-cooled to room temperature over 3 h; precipitate centrifuged and washed with DMF (35 mL x 3), DCM (20 mL x 3), hexane (20 mL x 2).
ActivationDried at 80 C under vacuum; transferred to N2 glovebox.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | HHTATP.3HBr | 8.7 mg, 0.0142 mmol | S5 · Synthesis of Cu3(HHTATP)2 |
| Metal Source | CuSO4.5H2O | 9.0 mg, 0.0361 mmol | S5 · Synthesis of Cu3(HHTATP)2 |
| Solvent | DMF | 2.0 mL | S5 · Synthesis of Cu3(HHTATP)2 |
| Solvent | deionized water | 3.5 mL | S5 · Synthesis of Cu3(HHTATP)2 |
Complete recipeSource: SI
Route 4: Other
S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method
Metal precursorspreformed Cu3(HHTATP)2 powder (53.8 mg)
Solvents0.8 mL anhydrous DMSO; acetone and hexane washes
Additives30 uL trifluoroacetic acid (TFA)
Atmospheresolution nitrogen-bubbled 5 min; final anneal under N2
Temperature80 for substrate piranha treatment and final anneal
Time12 h solution stirring; 6 h spin-coating evaporation; 5 min anneal
Substrate orientation1.5 cm x 1.5 cm SiO2/Si wafer, p-type highly doped, 200 nm SiO2
Oxidant / reductantpiranha substrate treatment H2SO4:30% H2O2 = 3:1
Work-upSubstrate sonicated in acetone, IPA, and water; piranha-treated, washed and vacuum dried. Spin-coated solution at 400 rpm until solvent evaporated; protonated sample washed without Et3N/THF.
ActivationAnnealed at 80 C for 5 min on a hot plate in N2 before electrical measurements.
Scalability contextMain text describes fabrication of large-area thin films through spin-coating.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | Cu3(HHTATP)2 | 53.8 mg | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |
| Solvent | anhydrous DMSO | 0.8 mL | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |
| Acid | TFA | 30 uL | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |
| Solvent | acetone | soak 5 min | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |
| Solvent | hexane | soak 5 min | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |
Complete recipeSource: SI
Route 5: Other
S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method
Metal precursorspreformed Cu3(HHTATP)2 powder (53.8 mg)
Solvents0.8 mL anhydrous DMSO; acetone, Et3N/THF, and hexane washes
Additives30 uL TFA for solution formation; 0.1 M Et3N/THF for proton removal
Atmospheresolution nitrogen-bubbled 5 min; final anneal under N2
Temperature80 for substrate piranha treatment and final anneal
Time12 h solution stirring; 6 h spin-coating evaporation; 5 min anneal
Substrate orientation1.5 cm x 1.5 cm SiO2/Si wafer, p-type highly doped, 200 nm SiO2
Oxidant / reductantpiranha substrate treatment H2SO4:30% H2O2 = 3:1
Work-upSpin-coated at 400 rpm until solvent fully evaporated, then soaked in acetone, 0.1 M Et3N/THF, and hexane, each for 5 min.
ActivationAnnealed at 80 C for 5 min on a hot plate in N2 before electrical measurements.
Scalability contextMain text describes large-area thin-film fabrication by spin-coating the viscous DMSO/TFA solution.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | Cu3(HHTATP)2 | 53.8 mg | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |
| Solvent | anhydrous DMSO | 0.8 mL | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |
| Acid | TFA | 30 uL | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |
| Base | Et3N/THF | soak 5 min · 0.1 M | S5 · Fabrication of Cu3(HHTATP)2 thin-film by a spin-coating method |