cMOF Evidence Base

Synthesis evidence

Nanopore-induced host-guest charge transfer phenomena in a metal-organic framework

Yamamoto S., Pirillo J., Hijikata Y. et al. · Chemical Science · 2018 · 3282-3289

7 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

p.4 · Physical measurements

Linker precursorsAQDC ligand
SolventsHot DMF
AdditivesTMPDA donor molecule
AtmosphereNot specified
Temperature120
Time1
Oxidant / reductantTMPDA donor and AQDC acceptor
Work-upSolid-state products collected by evacuating all DMF solvent.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerAQDC ligand1 : 1 molar ratio with TMPDAp.4 · Physical measurements
AdditiveTMPDA1 : 1 molar ratio with AQDCp.4 · Physical measurements
SolventDMFNot specifiedp.4 · Physical measurements
Partial recipeSource: Main

Route 2: Other

p.4 · Physical measurements

Linker precursorsAQDC ligand
SolventsHot DMF
AdditivesTTF donor molecule
AtmosphereNot specified
Temperature120
Time1
Oxidant / reductantTTF donor and AQDC acceptor
Work-upSolid-state products collected by evacuating all DMF solvent.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerAQDC ligand1 : 1 molar ratio with TTFp.4 · Physical measurements
AdditiveTTF1 : 1 molar ratio with AQDCp.4 · Physical measurements
SolventDMFNot specifiedp.4 · Physical measurements
Vague recipeSource: SI

Route 3: Other

SI p.7 · S6. Selective impregnation · Fig. S7

Metal precursorsMn-MOF crystals
Linker precursorsAQDC/DMA host
SolventsNot specified
AdditivesBEDT-TTF donor
AtmosphereNot specified
Oxidant / reductantBEDT-TTF electron donor
Work-upNot specified; SEM-EDX used to examine doped crystals.
Scalability contextNo phase-pure material isolated.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMn-MOF crystalsNot specifiedSI p.7 · S6. Selective impregnation · Fig. S7
AdditiveBEDT-TTFNot specifiedSI p.7 · S6. Selective impregnation · Fig. S7
Blocked Missing Si recipeSource: Main

Route 4: Solvothermal

p.3 · Preparation of the materials

Metal precursorsNot specified in this paper; host preparation cited to prior report.
Linker precursorsNot specified in this paper; host preparation cited to prior report.
SolventsDMF wash
Work-upCrystals collected from product of solvothermal reactions and washed with hot DMF.
ActivationUsed without solvent exchange and activation.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
SolventDMFhot DMF washp.3 · Preparation of the materials
Partial recipeSource: Main

Route 5: Other

p.3 · Preparation of the materials

Metal precursorsAs-prepared Mn-MOF crystals
Linker precursorsMn-MOF host containing AQDC linkers
Solvents5 mL dichloromethane solution
AdditivesTMPDA guest donor
AtmosphereNeedle-pierced capped vial left in fume hood; ambient air during slow solvent evaporation
Temperature140 sublimation workup
Time48-72 loading
Oxidant / reductantTMPDA electron donor; AQDC anthraquinone acceptor in host
Work-upDried after 2-3 days; vial placed in larger flask, evacuated and heated to remove excess guest by sublimation.
ActivationVacuum heating at 140 degC to sublime excess free TMPDA.
Scalability contextSmall-vial 5 mg crystal-sponge loading; no scale-up demonstrated.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-prepared Mn-MOF crystals5 mgp.3 · Preparation of the materials
Solventdichloromethane5 mLp.3 · Preparation of the materials
AdditiveTMPDAapproximately 10 mg · in 5 mL dichloromethanep.3 · Preparation of the materials
Partial recipeSource: Main

Route 6: Other

p.3 · Preparation of the materials

Metal precursorsAs-prepared Mn-MOF crystals
Linker precursorsMn-MOF host containing AQDC linkers
Solvents5 mL dichloromethane solution
AdditivesTTF guest donor
AtmosphereNeedle-pierced capped vial left in fume hood; ambient air during slow solvent evaporation
Temperature140 sublimation workup
Time48-72 loading
Oxidant / reductantTTF electron donor; AQDC anthraquinone acceptor in host
Work-upDried after 2-3 days; vial placed in larger flask, evacuated and heated to remove excess guest by sublimation.
ActivationVacuum heating at 140 degC to sublime excess free TTF.
Scalability contextSmall-vial 5 mg crystal-sponge loading; no scale-up demonstrated.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-prepared Mn-MOF crystals5 mgp.3 · Preparation of the materials
Solventdichloromethane5 mLp.3 · Preparation of the materials
AdditiveTTFapproximately 10 mg · in 5 mL dichloromethanep.3 · Preparation of the materials
Vague recipeSource: SI

Route 7: Other

SI p.7 · S6. Selective impregnation · Fig. S7

Metal precursorsMn-MOF crystals
Linker precursorsAQDC/DMA host
SolventsNot specified
AdditivesTMTSF donor
AtmosphereNot specified
Oxidant / reductantTMTSF electron donor
Work-upNot specified; SEM-EDX used to examine doped crystals.
Scalability contextNo phase-pure material isolated.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMn-MOF crystalsNot specifiedSI p.7 · S6. Selective impregnation · Fig. S7
AdditiveTMTSFNot specifiedSI p.7 · S6. Selective impregnation · Fig. S7