cMOF Evidence Base

Synthesis evidence

Wavy Two-Dimensional Conjugated Metal-Organic Framework with Metallic Charge Transport

Zhang J., Zhou G., Un H.-I. et al. · Journal of the American Chemical Society · 2023 · 23630-23638

5 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

5 · Preparation of the Cu3(HFcHBC)2 electrode

Metal precursorsCu3(HFcHBC)2 powder component
Solventsacetonitrile
Additivesacetylene black, PVDF
Atmospherevacuum oven drying
Temperature80
Timeovernight
Substrate orientationcoated on carbon cloth
Work-upMixed into slurry and coated on carbon cloth.
Activationdried at 80 C overnight in a vacuum oven
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HFcHBC)2 powder8 parts by weight5 · Preparation of the Cu3(HFcHBC)2 electrode
Additiveacetylene black1 part by weight5 · Preparation of the Cu3(HFcHBC)2 electrode
Additivepolyvinylidene difluoride (PVDF)1 part by weight5 · Preparation of the Cu3(HFcHBC)2 electrode
SolventacetonitrileNot specified5 · Preparation of the Cu3(HFcHBC)2 electrode
Othercarbon clothNot specified5 · Preparation of the Cu3(HFcHBC)2 electrode
Complete recipeSource: Both

Route 2: Liquid Liquid Interface

6 · Cu3(HFcHBC)2 film synthesis · Figure S6

Metal precursorsCu(OAc)2 aqueous solution
Linker precursorsHFcHBC solution in DMF
SolventsDCM, DMF, Milli-Q water
Atmospherenot specified for MOF film synthesis
Temperatureroom temperature
Time3
Substrate orientationfilms deposited/transferred onto SiO2/Si, Si, or quartz
Work-upAs-prepared films deposited on substrate and rinsed with water, DMF, and acetone.
Activationdried under vacuum at 90 C for 24 h
Scalability contextMain text reports a continuous film with lateral area about 28 cm2 at the water/DCM interface.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
SolventDCM20 mL6 · Cu3(HFcHBC)2 film synthesis · Figure S6
LinkerHFcHBC solution in DMF0.7 mL · 1 mg ml-16 · Cu3(HFcHBC)2 film synthesis · Figure S6
SolventMilli-Q water10 ml6 · Cu3(HFcHBC)2 film synthesis · Figure S6
Metal SourceCu(OAc)2 aqueous solution10 ml · 2 mg ml-16 · Cu3(HFcHBC)2 film synthesis · Figure S6
Solventwater, DMF and acetone rinseNot specified6 · Cu3(HFcHBC)2 film synthesis · Figure S6
Complete recipeSource: SI

Route 3: Liquid Liquid Interface

6 · Cu3(HFcHBC)2 powder synthesis

Metal precursorsCu(OAc)2 aqueous solution as in film synthesis
Linker precursorsHFcHBC solution in DMF as in film synthesis
SolventsDCM, DMF, water, acetone
Atmospherenot specified
Temperatureroom temperature synthesis; 90 C drying
Time3 h synthesis; 3 d acetone exchange; 24 h vacuum drying
Work-upFilm products filtered at oil/water interface and washed with water, DMF, and acetone.
Activationsolvent exchanged with 10 ml dry acetone each day for 3 d; dried under vacuum at 90 C for 24 h
Scalability contextPowder collected from film samples from multiple beakers.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HFcHBC)2 film samples from multiple beakersNot specified6 · Cu3(HFcHBC)2 powder synthesis
Solventwater, DMF, and acetone washNot specified6 · Cu3(HFcHBC)2 powder synthesis
Solventdry acetone10 ml each day for 3 d6 · Cu3(HFcHBC)2 powder synthesis
Complete recipeSource: SI

Route 4: Other

6 · Cu3(HFcHBC)2 single crystal isolation

Solventsethanol; water, DMF, acetone washes
Atmospherevacuum drying after isolation
Temperatureice bath sonication; 90 C drying
Time15 min sonication; 24 h drying
Substrate orientationSuspension drops onto Si/SiO2 substrates or TEM grids
Work-upSmall piece of Cu3(HFcHBC)2 film sonicated in ethanol; suspension placed on substrates/TEM grids and washed.
Activationdried under vacuum at 90 C for 24 h before analysis
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othersmall piece of Cu3(HFcHBC)2 film sampleNot specified6 · Cu3(HFcHBC)2 single crystal isolation
Solventethanol0.5 ml6 · Cu3(HFcHBC)2 single crystal isolation
Solventwater, DMF, and acetone washNot specified6 · Cu3(HFcHBC)2 single crystal isolation
Partial recipeSource: Both

Route 5: Other

6 · Synthesis of HFcHBC ligand · Scheme S1

Linker precursorsHFcHBC-OMe precursor
Solventsanhydrous dichloromethane; cold methanol quench; water and dichloromethane wash
AdditivesBBr3
AtmosphereAr
Temperature-78 C addition, then room temperature
Time24
Oxidant / reductantBBr3 demethylation reagent
Work-upReaction quenched by slow addition of cold methanol, washed with water and dichloromethane to give green precipitate.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHFcHBC-OMe100 mg, 0.112 mmol6 · Synthesis of HFcHBC ligand · Scheme S1
Additiveboron tribromide solution in anhydrous dichloromethane1.34 ml · 1.0 M6 · Synthesis of HFcHBC ligand · Scheme S1
Solventanhydrous dichloromethaneNot specified6 · Synthesis of HFcHBC ligand · Scheme S1
Solventcold methanol2 ml6 · Synthesis of HFcHBC ligand · Scheme S1