Synthesis evidence

Experimental manifestation of redox-conductivity in metal-organic frameworks and its implication for semiconductor/insulator switching

Li J., Kumar A., Johnson B.A. et al. · Nature Communications · 2023 · 4388

3 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

8 · Methods: Synthesis of UU-100(Co) thin-film on FTO surface

Metal precursorsZrCl4, 26 mg, 0.11 mmol; Co already present in cobaloxime linker
Linker precursorscobaloxime linker, 30 mg, 0.038 mmol; SAM from 1 mM cobaloxime linker in anhydrous DMF
SolventsAnhydrous DMF, 8 mL; DMF for SAM and washing; 50 uL H2O
AdditivesAnhydrous acetic acid, 35 uL, 0.61 mmol
Atmospheresealed vial; no inert atmosphere reported for synthesis
Temperature80
Time120
Substrate orientationSAM-modified FTO transferred with FTO side facing down
Work-upAfter solvothermal growth, slowly cool to room temperature; wash with DMF; remove unwanted growth on glass side with DMF-wetted Kimtech paper.
ActivationSoaked in DMF for future analysis; no dry activation reported.
Scalability contextIncludes a 2 h 80 degC pre-heating step to form Zr cluster solution before adding cobaloxime linker and growing for 5 days.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrCl426 mg, 0.11 mmol8 · Methods: Synthesis of UU-100(Co) thin-film on FTO surface
Linkercobaloxime linker30 mg, 0.038 mmol · 1 mM for SAM pretreatment8 · Methods: Synthesis of UU-100(Co) thin-film on FTO surface
Acidanhydrous acetic acid35 uL, 0.61 mmol8 · Methods: Synthesis of UU-100(Co) thin-film on FTO surface
SolventDMF8 mL8 · Methods: Synthesis of UU-100(Co) thin-film on FTO surface
AdditiveH2O50 uL8 · Methods: Synthesis of UU-100(Co) thin-film on FTO surface
OtherSAM-modified FTO1 x 2 cm8 · Methods: Synthesis of UU-100(Co) thin-film on FTO surface
Complete recipeSource: Both

Route 2: Solvothermal

8 · Methods: Synthesis of Zn(pyrazol-NDI) thin-film on FTO surface

Metal precursorsZn(NO3)2.6H2O, 4.8 mM
Linker precursorspyrazol-NDI linker, 4.3 mM; linker synthesis followed previous protocol and was checked by 1H NMR
SolventsDMF, 10 mL; FTO cleaning in DI water, ethanol and acetone
Atmospheresealed vial; no inert atmosphere reported for synthesis
Temperature135
Time3
Substrate orientationCleaned FTO slides, 1 x 2 cm, conductive side facing down
Work-upSlow cooling to room temperature at 2 degC/min; wash with DMF; remove unwanted growth on glass side with DMF-wetted Kimtech paper; sonicate in DMF for 1 min; thoroughly wash with DMF.
ActivationStored in DMF for future use; no dry activation reported.
Scalability contextPrepared on 1 x 2 cm FTO slides in 20 mL scintillation vial.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O4.8 mM8 · Methods: Synthesis of Zn(pyrazol-NDI) thin-film on FTO surface
Linkerpyrazol-NDI linker4.3 mM8 · Methods: Synthesis of Zn(pyrazol-NDI) thin-film on FTO surface
SolventDMF10 mL8 · Methods: Synthesis of Zn(pyrazol-NDI) thin-film on FTO surface
OtherFTO slide1 x 2 cm8 · Methods: Synthesis of Zn(pyrazol-NDI) thin-film on FTO surface
Complete recipeSource: Both

Route 3: Solvothermal

8 · Methods: Synthesis of Zr(dcphOH-NDI) thin-film on FTO surface

Metal precursorsZrCl4, 23.3 mg, 0.1 mmol
Linker precursorsdcphOH-NDI linker, 53.8 mg, 0.1 mmol; SAM from 1 mM dcphOH-NDI in anhydrous DMF
SolventsAnhydrous DMF, 8 mL; DMF for SAM and washing
AdditivesAnhydrous acetic acid, 286 uL, 5 mmol
Atmospheresealed vial; no inert atmosphere reported for synthesis
Temperature120
Time72
Substrate orientationSAM-modified FTO placed with FTO side facing down
Work-upSlow cooling to room temperature; wash with DMF; remove unwanted growth on glass side with DMF-wetted Kimtech paper.
ActivationSoaked in DMF for future analysis; no dry activation reported.
Scalability contextPrepared on 1 x 2 cm FTO in a 20 mL vial after 12 h SAM pretreatment.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrCl423.3 mg, 0.1 mmol8 · Methods: Synthesis of Zr(dcphOH-NDI) thin-film on FTO surface
LinkerdcphOH-NDI linker53.8 mg, 0.1 mmol · 1 mM for SAM pretreatment8 · Methods: Synthesis of Zr(dcphOH-NDI) thin-film on FTO surface
Acidanhydrous acetic acid286 uL, 5 mmol8 · Methods: Synthesis of Zr(dcphOH-NDI) thin-film on FTO surface
SolventDMF8 mL8 · Methods: Synthesis of Zr(dcphOH-NDI) thin-film on FTO surface
OtherSAM-modified FTO1 x 2 cm8 · Methods: Synthesis of Zr(dcphOH-NDI) thin-film on FTO surface