Synthesis evidence

Turning 2D MOFs into Mixed Ionic-Electronic Conductors via Side Chain Engineering

Roh H., Su A.Y., Oh C. et al. · Journal of the American Chemical Society · 2025 · 38419-38427

9 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: Both

Route 1: Solvothermal

p017 · Synthesis Details · Supplementary Figure 10

Metal precursorsCu(SO)4·5H2O
Linker precursorsHA1EG3-TAT
SolventsDMF, DMA, aqueous Na(OAc)
AdditivesNa(OAc) modulator/base
Atmosphereambient / not specified unless noted
Temperature65
Timeovernight
Work-upblack powder washed with water and MeOH
Activationnot reported
Scalability context20 mL vial scale; milligram quantities reported
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(SO)4·5H2O / Cu(SO4)2·5H2O as printed10.135 mg (or 10.15 mg in earlier SI sentence)p017 · Synthesis Details · Supplementary Figure 10
LinkerHAR3-TAT ligand, R=nBu/1EG/2EG20 mgp017 · Synthesis Details · Supplementary Figure 10
SolventDMF3 mLp017 · Synthesis Details · Supplementary Figure 10
SolventDMA3 mLp017 · Synthesis Details · Supplementary Figure 10
AdditiveNa(OAc)4 mL aqueous solution · 4 Mp017 · Synthesis Details · Supplementary Figure 10
Complete recipeSource: Both

Route 2: Solvothermal

p008 · Synthesis Details · MOF synthesis

Metal precursorsCu(SO)4·5H2O
Linker precursorsHA2EG3-TAT
SolventsDMF, DMA, aqueous Na(OAc)
AdditivesNa(OAc) modulator/base
Atmosphereambient / not specified unless noted
Temperature65
Timeovernight
Work-upblack powder washed with water and MeOH
Activationnot reported
Scalability context20 mL vial scale; milligram quantities reported
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(SO)4·5H2O / Cu(SO4)2·5H2O as printed10.135 mg (or 10.15 mg in earlier SI sentence)p008 · Synthesis Details · MOF synthesis
LinkerHAR3-TAT ligand, R=nBu/1EG/2EG20 mgp008 · Synthesis Details · MOF synthesis
SolventDMF3 mLp008 · Synthesis Details · MOF synthesis
SolventDMA3 mLp008 · Synthesis Details · MOF synthesis
AdditiveNa(OAc)4 mL aqueous solution · 4 Mp008 · Synthesis Details · MOF synthesis
Complete recipeSource: Both

Route 3: Solvothermal

p017 · Synthesis Details · Supplementary Figure 10

Metal precursorsCu(SO)4·5H2O
Linker precursorsHABu3-TAT
SolventsDMF, DMA, aqueous Na(OAc)
AdditivesNa(OAc) modulator/base
Atmosphereambient / not specified unless noted
Temperature65
Timeovernight
Work-upblack powder washed with water and MeOH
Activationnot reported
Scalability context20 mL vial scale; milligram quantities reported
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(SO)4·5H2O / Cu(SO4)2·5H2O as printed10.135 mg (or 10.15 mg in earlier SI sentence)p017 · Synthesis Details · Supplementary Figure 10
LinkerHAR3-TAT ligand, R=nBu/1EG/2EG20 mgp017 · Synthesis Details · Supplementary Figure 10
SolventDMF3 mLp017 · Synthesis Details · Supplementary Figure 10
SolventDMA3 mLp017 · Synthesis Details · Supplementary Figure 10
AdditiveNa(OAc)4 mL aqueous solution · 4 Mp017 · Synthesis Details · Supplementary Figure 10
Partial recipeSource: Both

Route 4: Other

p004 · Synthesis Details · Figure 3

Metal precursorsNi-1EG powder
Linker precursorsnot applicable
Solventspropylene carbonate
AdditivesLiTFSI
Atmosphereambient / not specified unless noted
Temperatureroom temperature
Time72
Work-upfilter-washing and drying
ActivationMOF powders vacuum-dried overnight before EIS assembly
Scalability context20 mL vial scale; milligram quantities reported
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Electrolytelithium bis(trifluoromethylsulfonyl)imide (LiTFSI) in propylene carbonatenot reported · 1 Mp004 · Synthesis Details · Figure 3
OtherNi-MOF powdernot reportedp004 · Synthesis Details · Figure 3
Partial recipeSource: Both

Route 5: Other

p004 · Synthesis Details · Figure 3

Metal precursorsNi-2EG powder
Linker precursorsnot applicable
Solventspropylene carbonate
AdditivesLiTFSI
Atmosphereambient / not specified unless noted
Temperatureroom temperature
Time72
Work-upfilter-washing and drying
ActivationMOF powders vacuum-dried overnight before EIS assembly
Scalability context20 mL vial scale; milligram quantities reported
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Electrolytelithium bis(trifluoromethylsulfonyl)imide (LiTFSI) in propylene carbonatenot reported · 1 Mp004 · Synthesis Details · Figure 3
OtherNi-MOF powdernot reportedp004 · Synthesis Details · Figure 3
Partial recipeSource: Both

Route 6: Other

p005 · Synthesis Details · Figure 3

Metal precursorsNi-nBu powder
Linker precursorsnot applicable
Solventspropylene carbonate
AdditivesLiTFSI
Atmosphereambient / not specified unless noted
Temperatureroom temperature
Time72
Work-upfilter-washing and drying
ActivationMOF powders vacuum-dried overnight before EIS assembly
Scalability context20 mL vial scale; milligram quantities reported
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Electrolytelithium bis(trifluoromethylsulfonyl)imide (LiTFSI) in propylene carbonatenot reported · 1 Mp005 · Synthesis Details · Figure 3
OtherNi-MOF powdernot reportedp005 · Synthesis Details · Figure 3
Complete recipeSource: Both

Route 7: Solvothermal

p008 · Synthesis Details · MOF synthesis

Metal precursorsNi(OAc)2·4H2O
Linker precursorsHA1EG3-TAT
SolventsDMF, DMA, aqueous Na(OAc)
AdditivesNa(OAc) modulator/base
Atmosphereambient / not specified unless noted
Temperature65
Timeovernight / about 12
Work-upblack powder washed with water and MeOH
Activationnot reported for synthesis; N2 samples later activated under dynamic vacuum
Scalability context20 mL vial scale; milligram quantities reported
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2·4H2O10.1 mgp008 · Synthesis Details · MOF synthesis
LinkerHAR3-TAT ligand, R=1EG/2EG/3EG20 mgp008 · Synthesis Details · MOF synthesis
SolventDMF3 mLp008 · Synthesis Details · MOF synthesis
SolventDMA3 mLp008 · Synthesis Details · MOF synthesis
Solventaqueous Na(OAc) solution4 mL · 4 Mp008 · Synthesis Details · MOF synthesis
AdditiveNa(OAc)4 mL aqueous solution · 4 Mp008 · Synthesis Details · MOF synthesis
Complete recipeSource: Both

Route 8: Solvothermal

p008 · Synthesis Details · MOF synthesis

Metal precursorsNi(OAc)2·4H2O
Linker precursorsHA2EG3-TAT
SolventsDMF, DMA, aqueous Na(OAc)
AdditivesNa(OAc) modulator/base
Atmosphereambient / not specified unless noted
Temperature65
Timeovernight / about 12
Work-upblack powder washed with water and MeOH
Activationnot reported for synthesis; N2 samples later activated under dynamic vacuum
Scalability context20 mL vial scale; milligram quantities reported
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2·4H2O10.1 mgp008 · Synthesis Details · MOF synthesis
LinkerHAR3-TAT ligand, R=1EG/2EG/3EG20 mgp008 · Synthesis Details · MOF synthesis
SolventDMF3 mLp008 · Synthesis Details · MOF synthesis
SolventDMA3 mLp008 · Synthesis Details · MOF synthesis
Solventaqueous Na(OAc) solution4 mL · 4 Mp008 · Synthesis Details · MOF synthesis
AdditiveNa(OAc)4 mL aqueous solution · 4 Mp008 · Synthesis Details · MOF synthesis
Complete recipeSource: SI

Route 9: Solvothermal

p008 · Synthesis Details · MOF synthesis

Metal precursorsNi(OAc)2·4H2O
Linker precursorsHABu3-TAT
SolventsDMF, DMA, water
AdditivesNa(OAc) modulator
Atmosphereambient / not specified unless noted
Temperature65
Timeovernight / about 12
Work-upblack powder washed with water and MeOH
Activationnot reported for synthesis; N2 samples later activated under dynamic vacuum
Scalability context20 mL vial scale; milligram quantities reported
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(OAc)2·4H2O10.1 mgp008 · Synthesis Details · MOF synthesis
LinkerHABu3-TAT ligand10 mgp008 · Synthesis Details · MOF synthesis
SolventDMF3 mLp008 · Synthesis Details · MOF synthesis
SolventDMA3 mLp008 · Synthesis Details · MOF synthesis
Solventwater1.5 mL ligand suspension plus 2 mL aqueous Na(OAc)p008 · Synthesis Details · MOF synthesis
AdditiveNa(OAc)2 mL aqueous solution · 2 Mp008 · Synthesis Details · MOF synthesis