cMOF Evidence Base

Synthesis evidence

Charge-Transfer-Induced Electrical Conductivity in a Tetrathiafulvalene-Based Metal-Organic Framework

Ukaj D., Bunzen H., Berger J. et al. · Chemistry of Materials · 2021 · 2532-2542

12 structured synthesis routes

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

Vague recipeSource: Main

Route 1: Unknown

p008 / 2539 · Experimental Section - Synthesis

SolventsDMF wash; EtOH solvent exchange
Work-upAs-synthesised MOFs washed with DMF three times by leaving them in solvent overnight and replacing the supernatant, then solvent-exchanged with EtOH three times.
ActivationActivated overnight at 230 deg C for Cd2TTFTB.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
SolventDMFNot specifiedp008 / 2539 · Experimental Section - Synthesis
SolventEtOHNot specifiedp008 / 2539 · Experimental Section - Synthesis
Complete recipeSource: Main

Route 2: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Cd2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature200
Time720
Oxidant / reductantTCNE electron-accepting guest, 28.3 mg, 0.22 mmol, 1.0 equiv
Work-upAfter cooling, excess TCNE was found at the colder end of the ampule for TCNE equivalents higher than 0.5; ampule opened in glovebox and product stored under Ar.
ActivationStarting Cd2TTFTB was activated overnight at 230 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Cd2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE28.3 mg; 0.22 mmol; 1.0 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 3: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Zn2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature200
Time240
Oxidant / reductantTCNE electron-accepting guest, 15.8 mg, 0.13 mmol, 0.5 equiv
Work-upAfter cooling, ampule opened in glovebox and product stored under Ar.
ActivationStarting Zn2TTFTB was activated overnight at 200 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Zn2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE15.8 mg; 0.13 mmol; 0.5 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 4: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Zn2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature200
Time240
Oxidant / reductantTCNE electron-accepting guest, 31.6 mg, 0.25 mmol, 1.0 equiv
Work-upAfter cooling, excess TCNE was found at the colder end of the ampule for TCNE equivalents higher than 0.5; ampule opened in glovebox and product stored under Ar.
ActivationStarting Zn2TTFTB was activated overnight at 200 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Zn2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE31.6 mg; 0.25 mmol; 1.0 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 5: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Zn2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature200
Time720
Oxidant / reductantTCNE electron-accepting guest, 15.8 mg, 0.13 mmol, 0.5 equiv
Work-upAfter cooling, ampule opened in glovebox and product stored under Ar.
ActivationStarting Zn2TTFTB was activated overnight at 200 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Zn2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE15.8 mg; 0.13 mmol; 0.5 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 6: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Zn2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature200
Time720
Oxidant / reductantTCNE electron-accepting guest, 31.6 mg, 0.25 mmol, 1.0 equiv
Work-upAfter cooling, excess TCNE was found at the colder end of the ampule for TCNE equivalents higher than 0.5; ampule opened in glovebox and product stored under Ar.
ActivationStarting Zn2TTFTB was activated overnight at 200 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Zn2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE31.6 mg; 0.25 mmol; 1.0 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 7: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Zn2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature300
Time720
Oxidant / reductantTCNE electron-accepting guest, 15.8 mg, 0.13 mmol, 0.5 equiv
Work-upAfter cooling, ampule opened in glovebox and product stored under Ar.
ActivationStarting Zn2TTFTB was activated overnight at 200 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Zn2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE15.8 mg; 0.13 mmol; 0.5 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 8: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Zn2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature300
Time720
Oxidant / reductantTCNE electron-accepting guest, 31.6 mg, 0.25 mmol, 1.0 equiv
Work-upAfter cooling, excess TCNE was found at the colder end of the ampule for TCNE equivalents higher than 0.5; ampule opened in glovebox and product stored under Ar.
ActivationStarting Zn2TTFTB was activated overnight at 200 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Zn2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE31.6 mg; 0.25 mmol; 1.0 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 9: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Cd2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature200
Time240
Oxidant / reductantTCNE electron-accepting guest, 14.2 mg, 0.11 mmol, 0.5 equiv
Work-upAfter cooling, ampule opened in glovebox and product stored under Ar.
ActivationStarting Cd2TTFTB was activated overnight at 230 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Cd2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE14.2 mg; 0.11 mmol; 0.5 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 10: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Cd2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature200
Time240
Oxidant / reductantTCNE electron-accepting guest, 28.3 mg, 0.22 mmol, 1.0 equiv
Work-upAfter cooling, excess TCNE was found at the colder end of the ampule for TCNE equivalents higher than 0.5; ampule opened in glovebox and product stored under Ar.
ActivationStarting Cd2TTFTB was activated overnight at 230 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Cd2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE28.3 mg; 0.22 mmol; 1.0 equivp009 / 2540 · Experimental Section · Table 2
Complete recipeSource: Main

Route 11: Other

p009 / 2540 · Experimental Section · Table 2

Metal precursorsActivated Cd2TTFTB host, 200 mg
SolventsNone; solvent-free vapour-phase infiltration
AtmosphereArgon glovebox; evacuated borosilicate ampule, ca. 3 x 10^-2 mbar before flame sealing
Temperature200
Time720
Oxidant / reductantTCNE electron-accepting guest, 14.2 mg, 0.11 mmol, 0.5 equiv
Work-upAfter cooling, ampule opened in glovebox and product stored under Ar.
ActivationStarting Cd2TTFTB was activated overnight at 230 deg C.
Scalability contextMain recipe scale was 200 mg MOF.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Cd2TTFTB200 mgp009 / 2540 · Experimental Section · Table 2
OxidantTCNE14.2 mg; 0.11 mmol; 0.5 equivp009 / 2540 · Experimental Section · Table 2
Vague recipeSource: Main

Route 12: Unknown

p008 / 2539 · Experimental Section - Synthesis

SolventsDMF wash; EtOH solvent exchange
Work-upAs-synthesised MOFs washed with DMF three times by leaving them in solvent overnight and replacing the supernatant, then solvent-exchanged with EtOH three times.
ActivationActivated overnight at 200 deg C for Zn2TTFTB.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
SolventDMFNot specifiedp008 / 2539 · Experimental Section - Synthesis
SolventEtOHNot specifiedp008 / 2539 · Experimental Section - Synthesis