Synthesis evidence

An Electrically Conducting Three-Dimensional Iron–Catecholate Porous Framework

Mähringer et al. · Angewandte Chemie International Edition · 2021 · 18065-18072

2 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

SI p.4 · Preparation of pellets

AtmosphereAmbient conditions for electrical measurements.
Temperatureroom temperature
Work-upPressed as a 1 cm diameter pellet from several batches.
ActivationEvacuated MOF bulk material used before pressing.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otherevacuated Fe-HHTP-MOF bulk material100 mgSI p.4 · Preparation of pellets
Complete recipeSource: Both

Route 2: Solvothermal

SI p.4 · Synthesis of Fe-HHTP-MOF

Metal precursorsFe(BF4)2 . 6 H2O, 42.4 mg
Linker precursorsHHTP (hexahydroxytriphenylene), 20 mg
Solvents3.5 mL DMF; 250 uL NMP; deionized water; methanol
AdditivesNBu4NO3, 20 mg crystallisation additive
AtmosphereInert conditions in an Ar-filled glovebox; sealed vial / argon atmosphere.
Temperature120
Time48
Work-upReaction mixture washed with 30 mL dimethylformamide, 30 mL methanol, and 30 mL water to obtain a black powder.
ActivationActivation under dynamic vacuum; main text says degassed under dynamic vacuum prior to analysis.
Scalability contextSI reports 50 mg Fe-HHTP-MOF obtained from the stated batch.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP (hexahydroxtriphenylene)20 mgSI p.4 · Synthesis of Fe-HHTP-MOF
Metal SourceFe(BF4)2 . 6 H2O42.4 mgSI p.4 · Synthesis of Fe-HHTP-MOF
AdditiveNBu4NO320 mgSI p.4 · Synthesis of Fe-HHTP-MOF
SolventDMF3.5 mLSI p.4 · Synthesis of Fe-HHTP-MOF
SolventNMP (N-methyl-2-pyrrolidone)250 uLSI p.4 · Synthesis of Fe-HHTP-MOF
Solventdeionized waterNot specifiedSI p.4 · Synthesis of Fe-HHTP-MOF
SolventmethanolNot specifiedSI p.4 · Synthesis of Fe-HHTP-MOF