Partial recipeSource: SI
Route 1: Unknown
S3-S4 · Methods
Synthesis evidence
Mechanistic Evidence for Ligand-Centered Electrocatalytic Oxygen Reduction with the Conductive MOF Ni3(hexaiminotriphenylene)2
Miner E.M., Gul S., Ricke N.D. et al. · ACS Catalysis · 2017 · 7726-7731
5 structured synthesis routes
Completeness describes how fully the route could be reconstructed from the main article and supporting information.
Complete recipeSource: SI
Route 2: Other
S6 · Synthesis and purification of Ni3(HITP)2 film on the interdigitated electrode
Metal precursorsnickel(II) chloride hexahydrate (10 mg)
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene.6HCl (HATP) salt (10 mg)
Solventsdeionized water; methanol used during purification
Additivesconcentrated aqueous ammonium hydroxide (0.60 mL)
Atmospherereaction atmosphere not specified; stored under N2 for 12 h after drying
Temperature65
Time2
Substrate orientationgold interdigitated electrode taped with Kapton tape and submerged in reaction vial
Work-upheated in deionized water 30 min at 60 degC, then methanol 30 min at 60 degC
Activationdried under dynamic vacuum and stored under N2 for 12 h
Scalability contextFilm grows on electrode while black flaky solid also settles at vial bottom.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | nickel(II) chloride hexahydrate | 10 mg | S6 · Synthesis and purification of Ni3(HITP)2 film on the interdigitated electrode |
| Linker | 2,3,6,7,10,11-hexaaminotriphenylene.6HCl (HATP) salt | 10 mg | S6 · Synthesis and purification of Ni3(HITP)2 film on the interdigitated electrode |
| Solvent | deionized water | 4 mL for HATP solution; 4 mL for NiCl2 solution | S6 · Synthesis and purification of Ni3(HITP)2 film on the interdigitated electrode |
| Base | concentrated aqueous ammonium hydroxide | 0.60 mL | S6 · Synthesis and purification of Ni3(HITP)2 film on the interdigitated electrode |
| Solvent | methanol | 30 min wash/heating at 60 degC | S6 · Synthesis and purification of Ni3(HITP)2 film on the interdigitated electrode |
Complete recipeSource: SI
Route 3: Other
S8 · Synthesis of Ni3(HITP)2 film on the ITO-coated PET electrode
Metal precursorsnickel(II) chloride hexahydrate (10 mg)
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene.6HCl (HATP) salt (10 mg)
Solventsdeionized water; methanol used during purification
Additivesconcentrated aqueous ammonium hydroxide (0.60 mL)
Atmospherereaction atmosphere not specified; packed under argon for shipment after drying
Temperature65
Time2
Substrate orientationtwo ITO-coated PET electrodes (1 x 2 cm) submerged in reaction vial
Work-upheated in deionized water 30 min at 60 degC, then methanol 30 min at 60 degC
Activationdried under dynamic vacuum and packed under argon
Scalability contextBlack flaky solid also settled at vial bottom.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | nickel(II) chloride hexahydrate | 10 mg | S8 · Synthesis of Ni3(HITP)2 film on the ITO-coated PET electrode |
| Linker | 2,3,6,7,10,11-hexaaminotriphenylene.6HCl (HATP) salt | 10 mg | S8 · Synthesis of Ni3(HITP)2 film on the ITO-coated PET electrode |
| Solvent | deionized water | 4 mL for HATP solution; 4 mL for NiCl2 solution | S8 · Synthesis of Ni3(HITP)2 film on the ITO-coated PET electrode |
| Base | concentrated aqueous ammonium hydroxide | 0.60 mL | S8 · Synthesis of Ni3(HITP)2 film on the ITO-coated PET electrode |
| Solvent | methanol | 30 min wash/heating at 60 degC | S8 · Synthesis of Ni3(HITP)2 film on the ITO-coated PET electrode |
Complete recipeSource: SI
Route 4: Drop Cast
S12 · Deposition of Ni(ISQ)2 onto the working electrodes
Solventsacetone
Substrate orientationdropcast onto glassy carbon and ITO
Work-upsonicated 20 min before dropcasting
Show 2 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | Ni(ISQ)2 | 2 mg | S12 · Deposition of Ni(ISQ)2 onto the working electrodes |
| Solvent | acetone | 0.2 mL | S12 · Deposition of Ni(ISQ)2 onto the working electrodes |
Complete recipeSource: SI
Route 5: Other
S11 · Synthesis of Ni(ISQ)2
Metal precursorsnickel chloride hexahydrate (0.33 g)
Linker precursorso-phenylenediamine (0.2 g)
Solventswater; acetone wash
Additivesconcentrated aqueous ammonia (1.0 mL)
Atmosphereopen beaker during synthesis; stored under N2 for 12 h
Temperature65
Time24
Work-upcentrifugation; water wash while stirring at 65 degC for 30 min; acetone wash at 23 degC; centrifugation
Activationdried under dynamic vacuum; stored under N2 for 12 h
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | nickel chloride hexahydrate | 0.33 g | S11 · Synthesis of Ni(ISQ)2 |
| Linker | o-phenylenediamine | 0.2 g | S11 · Synthesis of Ni(ISQ)2 |
| Base | concentrated aqueous ammonia | 1.0 mL | S11 · Synthesis of Ni(ISQ)2 |
| Solvent | water | 1.0 mL for Ni solution; 200 mL warm water for ligand solution | S11 · Synthesis of Ni(ISQ)2 |
| Solvent | acetone | wash at 23 degC | S11 · Synthesis of Ni(ISQ)2 |