Synthesis evidence

Diffusional Electron Transport Coupled to Thermodynamically Driven Electron Transfers in Redox-Conductive Multivariate Metal-Organic Frameworks

Li J., Kumar A., Ott S. · Journal of the American Chemical Society · 2024 · 12000-12010

5 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Solvothermal

12008 · Experimental Section

Metal precursorsZn(NO3)2·6H2O in DMF, 6.65 mmol L-1
Linker precursorsPredissolved NDI linker and/or PMDI linker in DMF, each 2.75 mmol L-1; NDI/PMDI feeding ratio 20/80
SolventsDMF; FTO cleaning used deionised water, ethanol, and acetone
AdditivesNone reported
AtmosphereSealed 20 mL scintillation vial; electrochemical measurements in Ar-saturated DMF but synthesis atmosphere not otherwise specified
Temperature135
Time3.5
Substrate orientationCleaned 1 cm x 2 cm FTO plate, conductive side facing down
Oxidant / reductantNone reported
Work-upSlow cool to room temperature; wash thin films with DMF; remove glass-side growth with DMF-wetted Kimtech paper; sonicate in DMF for 10 s; wash thoroughly with DMF; store in DMF
ActivationNo drying/thermal activation reported for these DMF-stored electrochemical thin-film samples
Scalability contextPrepared on 1 cm x 2 cm FTO plates in 20 mL scintillation vials; linker ratio tuned by solution volumes.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2·6H2O6.65 mmol L-1 in DMF12008 · Experimental Section
LinkerNDI linkervolume adjusted for NDI/PMDI 20/80 · 2.75 mmol L-1 in DMF12008 · Experimental Section
LinkerPMDI linkervolume adjusted for NDI/PMDI 20/80 · 2.75 mmol L-1 in DMF12008 · Experimental Section
SolventDMFNot specified12008 · Experimental Section
OtherFTO substrate1 cm x 2 cm plate12008 · Experimental Section
Complete recipeSource: Main

Route 2: Solvothermal

12008 · Experimental Section

Metal precursorsZn(NO3)2·6H2O in DMF, 6.65 mmol L-1
Linker precursorsPredissolved NDI linker and/or PMDI linker in DMF, each 2.75 mmol L-1; NDI/PMDI feeding ratio 50/50
SolventsDMF; FTO cleaning used deionised water, ethanol, and acetone
AdditivesNone reported
AtmosphereSealed 20 mL scintillation vial; electrochemical measurements in Ar-saturated DMF but synthesis atmosphere not otherwise specified
Temperature135
Time3.5
Substrate orientationCleaned 1 cm x 2 cm FTO plate, conductive side facing down
Oxidant / reductantNone reported
Work-upSlow cool to room temperature; wash thin films with DMF; remove glass-side growth with DMF-wetted Kimtech paper; sonicate in DMF for 10 s; wash thoroughly with DMF; store in DMF
ActivationNo drying/thermal activation reported for these DMF-stored electrochemical thin-film samples
Scalability contextPrepared on 1 cm x 2 cm FTO plates in 20 mL scintillation vials; linker ratio tuned by solution volumes.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2·6H2O6.65 mmol L-1 in DMF12008 · Experimental Section
LinkerNDI linkervolume adjusted for NDI/PMDI 50/50 · 2.75 mmol L-1 in DMF12008 · Experimental Section
LinkerPMDI linkervolume adjusted for NDI/PMDI 50/50 · 2.75 mmol L-1 in DMF12008 · Experimental Section
SolventDMFNot specified12008 · Experimental Section
OtherFTO substrate1 cm x 2 cm plate12008 · Experimental Section
Complete recipeSource: Main

Route 3: Solvothermal

12008 · Experimental Section

Metal precursorsZn(NO3)2·6H2O in DMF, 6.65 mmol L-1
Linker precursorsPredissolved NDI linker and/or PMDI linker in DMF, each 2.75 mmol L-1; NDI/PMDI feeding ratio 80/20
SolventsDMF; FTO cleaning used deionised water, ethanol, and acetone
AdditivesNone reported
AtmosphereSealed 20 mL scintillation vial; electrochemical measurements in Ar-saturated DMF but synthesis atmosphere not otherwise specified
Temperature135
Time3.5
Substrate orientationCleaned 1 cm x 2 cm FTO plate, conductive side facing down
Oxidant / reductantNone reported
Work-upSlow cool to room temperature; wash thin films with DMF; remove glass-side growth with DMF-wetted Kimtech paper; sonicate in DMF for 10 s; wash thoroughly with DMF; store in DMF
ActivationNo drying/thermal activation reported for these DMF-stored electrochemical thin-film samples
Scalability contextPrepared on 1 cm x 2 cm FTO plates in 20 mL scintillation vials; linker ratio tuned by solution volumes.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2·6H2O6.65 mmol L-1 in DMF12008 · Experimental Section
LinkerNDI linkervolume adjusted for NDI/PMDI 80/20 · 2.75 mmol L-1 in DMF12008 · Experimental Section
LinkerPMDI linkervolume adjusted for NDI/PMDI 80/20 · 2.75 mmol L-1 in DMF12008 · Experimental Section
SolventDMFNot specified12008 · Experimental Section
OtherFTO substrate1 cm x 2 cm plate12008 · Experimental Section
Complete recipeSource: Main

Route 4: Solvothermal

12008 · Experimental Section

Metal precursorsZn(NO3)2·6H2O in DMF, 6.65 mmol L-1
Linker precursorsPredissolved NDI linker and/or PMDI linker in DMF, each 2.75 mmol L-1; NDI/PMDI feeding ratio 100/0
SolventsDMF; FTO cleaning used deionised water, ethanol, and acetone
AdditivesNone reported
AtmosphereSealed 20 mL scintillation vial; electrochemical measurements in Ar-saturated DMF but synthesis atmosphere not otherwise specified
Temperature135
Time3.5
Substrate orientationCleaned 1 cm x 2 cm FTO plate, conductive side facing down
Oxidant / reductantNone reported
Work-upSlow cool to room temperature; wash thin films with DMF; remove glass-side growth with DMF-wetted Kimtech paper; sonicate in DMF for 10 s; wash thoroughly with DMF; store in DMF
ActivationNo drying/thermal activation reported for these DMF-stored electrochemical thin-film samples
Scalability contextPrepared on 1 cm x 2 cm FTO plates in 20 mL scintillation vials; linker ratio tuned by solution volumes.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2·6H2O6.65 mmol L-1 in DMF12008 · Experimental Section
LinkerNDI linkervolume adjusted for NDI/PMDI 100/0 · 2.75 mmol L-1 in DMF12008 · Experimental Section
LinkerPMDI linkervolume adjusted for NDI/PMDI 100/0 · 2.75 mmol L-1 in DMF12008 · Experimental Section
SolventDMFNot specified12008 · Experimental Section
OtherFTO substrate1 cm x 2 cm plate12008 · Experimental Section
Complete recipeSource: Main

Route 5: Solvothermal

12008 · Experimental Section

Metal precursorsZn(NO3)2·6H2O in DMF, 6.65 mmol L-1
Linker precursorsPredissolved NDI linker and/or PMDI linker in DMF, each 2.75 mmol L-1; NDI/PMDI feeding ratio 0/100
SolventsDMF; FTO cleaning used deionised water, ethanol, and acetone
AdditivesNone reported
AtmosphereSealed 20 mL scintillation vial; electrochemical measurements in Ar-saturated DMF but synthesis atmosphere not otherwise specified
Temperature135
Time3.5
Substrate orientationCleaned 1 cm x 2 cm FTO plate, conductive side facing down
Oxidant / reductantNone reported
Work-upSlow cool to room temperature; wash thin films with DMF; remove glass-side growth with DMF-wetted Kimtech paper; sonicate in DMF for 10 s; wash thoroughly with DMF; store in DMF
ActivationNo drying/thermal activation reported for these DMF-stored electrochemical thin-film samples
Scalability contextPrepared on 1 cm x 2 cm FTO plates in 20 mL scintillation vials; linker ratio tuned by solution volumes.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2·6H2O6.65 mmol L-1 in DMF12008 · Experimental Section
LinkerNDI linkervolume adjusted for NDI/PMDI 0/100 · 2.75 mmol L-1 in DMF12008 · Experimental Section
LinkerPMDI linkervolume adjusted for NDI/PMDI 0/100 · 2.75 mmol L-1 in DMF12008 · Experimental Section
SolventDMFNot specified12008 · Experimental Section
OtherFTO substrate1 cm x 2 cm plate12008 · Experimental Section