cMOF Evidence Base

Synthesis evidence

Tuning Electrical- and Photo-Conductivity by Cation Exchange within a Redox-Active Tetrathiafulvalene-Based Metal–Organic Framework

Zhou Y., Yu F., Su J. et al. · Angewandte Chemie - International Edition · 2020 · 18763-18767

6 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Drop Cast

S4 · Photo-electrochemical sample preparation

SolventsEthanol, 1.0 mL
AdditivesNafion D-520 dispersion, 10 uL, 5.0%
AtmosphereAmbient; dried at room temperature
Temperatureroom temperature
Time0.5 h sonication; drying time not specified
Substrate orientationITO glass plate, 1 x 2 cm2
Work-up200 uL slurry transferred and coated onto ITO glass, then dried at room temperature.
Scalability contextElectrode preparation uses 2 mg powder batch.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMe2NH2@1 powder2 mgS4 · Photo-electrochemical sample preparation
Solventethanol1.0 mLS4 · Photo-electrochemical sample preparation
AdditiveNafion D-520 dispersion10 uL · 5.0%S4 · Photo-electrochemical sample preparation
Vague recipeSource: SI

Route 2: Unknown

S2 · Methods

Linker precursorsH4TTFTB mentioned as synthesised as described in literature.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Linkertetrathiafulvalene-tetrabenzoic acid (H4TTFTB)Not specifiedS2 · Methods
Complete recipeSource: SI

Route 3: Other

S2 · Experimental Section

Metal precursorsMe2NH2@1 framework provides In(III) nodes.
Linker precursorsTTFTB linker already present in Me2NH2@1.
SolventsDMF, 10 mL
Additives(MV)Cl2, 3 mg, as MV2+ source
AtmosphereNot specified
Temperatureroom temperature
Time48 (same method as TTF@1)
Work-upSame method as TTF@1; after cation exchange crystals were collected by filtration, washed with DMF and dried in air.
ActivationDried in air after cation exchange (from SI Figure S18 general workup).
Scalability contextReported on 5 mg crystal scale.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMe2NH2@1 crystals5 mgS2 · Experimental Section
SolventDMF10 mLS2 · Experimental Section
Additive(MV)Cl23 mgS2 · Experimental Section
Complete recipeSource: SI

Route 4: Drop Cast

S4 · Photo-electrochemical sample preparation

SolventsEthanol, 1.0 mL
AdditivesNafion D-520 dispersion, 10 uL, 5.0%
AtmosphereAmbient; dried at room temperature
Temperatureroom temperature
Time0.5 h sonication; drying time not specified
Substrate orientationITO glass plate, 1 x 2 cm2
Work-up200 uL slurry transferred and coated onto ITO glass, then dried at room temperature.
Scalability contextElectrode preparation uses 2 mg powder batch.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMV@1 powder2 mgS4 · Photo-electrochemical sample preparation
Solventethanol1.0 mLS4 · Photo-electrochemical sample preparation
AdditiveNafion D-520 dispersion10 uL · 5.0%S4 · Photo-electrochemical sample preparation
Complete recipeSource: SI

Route 5: Other

S2 · Experimental Section

Metal precursorsMe2NH2@1 framework provides In(III) nodes.
Linker precursorsTTFTB linker already present in Me2NH2@1.
SolventsDMF, 10 mL
Additives(TTF)3(BF4)2, 8 mg, as TTF*+ source
AtmosphereNot specified
Temperatureroom temperature
Time48
Oxidant / reductant(TTF)3(BF4)2
Work-upCrystals separated and washed with DMF to remove excess and surface (TTF)3(BF4)2; SI Figure S18 text also states collected by filtration, washed with DMF and dried in air.
ActivationDried in air after cation exchange (from SI Figure S18 general workup).
Scalability contextReported on 5 mg crystal scale.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMe2NH2@1 crystals5 mgS2 · Experimental Section
SolventDMF10 mLS2 · Experimental Section
Oxidant(TTF)3(BF4)28 mgS2 · Experimental Section
Complete recipeSource: SI

Route 6: Drop Cast

S4 · Photo-electrochemical sample preparation

SolventsEthanol, 1.0 mL
AdditivesNafion D-520 dispersion, 10 uL, 5.0%
AtmosphereAmbient; dried at room temperature
Temperatureroom temperature
Time0.5 h sonication; drying time not specified
Substrate orientationITO glass plate, 1 x 2 cm2
Work-up200 uL slurry transferred and coated onto ITO glass, then dried at room temperature.
Scalability contextElectrode preparation uses 2 mg powder batch.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherTTF@1 powder2 mgS4 · Photo-electrochemical sample preparation
Solventethanol1.0 mLS4 · Photo-electrochemical sample preparation
AdditiveNafion D-520 dispersion10 uL · 5.0%S4 · Photo-electrochemical sample preparation