Synthesis · A tribenzocoronene-based 2D conductive metal-organic framework for efficient energy storage

5 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

S7 · Section 2. Synthesis of 6OH-TBC · Scheme S1

Metal precursorsnone

Linker precursors6OCH3-TBC (200 mg, 0.37 mmol); precursor itself was synthesised according to literature S1

Solventsdry CH2Cl2 (20 mL)

AdditivesBBr3 (2 mmol)

Atmospherenitrogen

Temperature0 degC addition, then room temperature

Time12

Oxidant / reductantBBr3 demethylation reagent

Work-upquenched with distilled water; solid collected by filtration and washed with water

Activationnone reported

Scalability context200 mg precursor scale; 135 mg product; precursor preparation not reproduced in this paper.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	6OCH3-TBC	200 mg, 0.37 mmol	S7 · Section 2. Synthesis of 6OH-TBC · Scheme S1
Solvent	dry CH2Cl2	20 mL	S7 · Section 2. Synthesis of 6OH-TBC · Scheme S1
Additive	BBr3	2 mmol	S7 · Section 2. Synthesis of 6OH-TBC · Scheme S1
Other	distilled water	not specified · quench/wash	S7 · Section 2. Synthesis of 6OH-TBC · Scheme S1

Complete recipeSource: SI

Route 2: Other

S9-S10 · Section 3. Preparation of Two-electrode Asymmetrical MOF//AC device

Metal precursorsCu-TBC electrode on Ti mesh

Linker precursorsnot applicable

Solvents0.1 M H2SO4 aqueous electrolyte (50 uL)

Additivesactivated carbon cathode; NKK-MPF30AC-100 membrane separator

Atmospherenot specified

Temperatureroom temperature assembly implied

Timenot specified

Substrate orientationtwo round titanium mesh electrodes

Oxidant / reductantnone

Work-upassemble Cu-TBC anode, AC cathode, separator and electrolyte

Activationnone reported

Scalability contextCu-TBC active mass approx. 0.53 mg cm-2; AC active mass approx. 5.3 mg cm-2.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-TBC loaded round titanium mesh	active mass approx. 0.53 mg cm-2 · anode	S9-S10 · Section 3. Preparation of Two-electrode Asymmetrical MOF//AC device
Other	AC loaded round titanium mesh	active mass approx. 5.3 mg cm-2 · cathode	S9-S10 · Section 3. Preparation of Two-electrode Asymmetrical MOF//AC device
Electrolyte	H2SO4 aqueous solution	50 uL · 0.1 M	S9-S10 · Section 3. Preparation of Two-electrode Asymmetrical MOF//AC device
Other	NKK-MPF30AC-100 membrane	not specified · separator	S9-S10 · Section 3. Preparation of Two-electrode Asymmetrical MOF//AC device

Complete recipeSource: SI

Route 3: Drop Cast

S9 · Section 3. Standard three-electrode system measurements

Metal precursorsCu-TBC powder already synthesised

Linker precursorsnot applicable

Solventsdry ethanol (577.0 uL)

Additivesconductive carbon black (3.0 mg); Nafion (23.0 uL, 5 wt%, dispersed in water)

Atmosphereair drying after deposition

Temperatureroom temperature

Time0.5 h ultrasonic mixing plus 1 h drying

Substrate orientationpre-polished glassy carbon electrode, area 0.07 cm2

Oxidant / reductantnone

Work-up8 uL slurry pipetted/spread on GCE and dried in air for 1 h

Activationnone reported before electrochemical test

Scalability contextElectrode loading reported as 1.14 mg cm-2.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	as-prepared MOF powder	6.0 mg · 60 wt% in electrode solids	S9 · Section 3. Standard three-electrode system measurements
Additive	conductive carbon black	3.0 mg · 30 wt%	S9 · Section 3. Standard three-electrode system measurements
Additive	Nafion	23.0 uL · 5 wt%, dispersed in water; 10 wt% binder	S9 · Section 3. Standard three-electrode system measurements
Solvent	dry ethanol	577.0 uL	S9 · Section 3. Standard three-electrode system measurements

Complete recipeSource: Both

Route 4: Solvothermal

S8 · Section 2. Preparation of Cu-TBC

Metal precursorsbis(1,1,1-trifluoropentane-2,4-dionato-O,O')copper (29.5 mg, 0.08 mmol)

Linker precursors6OH-TBC ligand (11.0 mg, 0.02 mmol)

SolventsDMAc/MeOH/water = 0.5 mL/1 mL/1 mL

Additivesnone reported

Atmospheresealed Pyrex tube; gas atmosphere not specified

Temperature120

Time72

Oxidant / reductantnone reported

Work-upcool; filter precipitate; thoroughly wash with DMAc, MeOH and acetone

Activationdried under vacuum; porosity sample degassed at 80 degC for 10 h under vacuum (10^-5 bar) before N2 sorption

Scalability context10 mL Pyrex tube; 8.9 mg black powder isolated; 70.0% yield.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	6OH-TBC ligand	11.0 mg, 0.02 mmol	S8 · Section 2. Preparation of Cu-TBC
Metal Source	bis(1,1,1-trifluoropentane-2,4-dionato-O,O')copper	29.5 mg, 0.08 mmol	S8 · Section 2. Preparation of Cu-TBC
Solvent	DMAc	0.5 mL	S8 · Section 2. Preparation of Cu-TBC
Solvent	MeOH	1 mL	S8 · Section 2. Preparation of Cu-TBC
Solvent	water	1 mL	S8 · Section 2. Preparation of Cu-TBC
Solvent	acetone	not specified · wash	S8 · Section 2. Preparation of Cu-TBC

Complete recipeSource: SI

Route 5: Drop Cast

S9 · Section 3. Preparation of the MOF and AC film electrode

Metal precursorsCu-TBC powder already synthesised

Linker precursorsnot applicable

Solventsdry ethanol (1.15 mL)

Additivesconductive carbon black (6.0 mg); Nafion binder solution (46 uL, 5 wt%, dispersed in water)

Atmospherevacuum drying

Temperature80

Time0.5 h stirring plus overnight drying

Substrate orientationpre-polished round titanium mesh electrode, r = 0.6 cm

Oxidant / reductantnone

Work-up60 uL slurry spread onto titanium mesh; dried at 80 degC under vacuum overnight

Activationnone beyond vacuum drying

Scalability contextComposition reported as 60 wt% MOF, 30 wt% carbon black, 10 wt% Nafion.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF powder	12.0 mg · 60 wt% in electrode solids	S9 · Section 3. Preparation of the MOF and AC film electrode
Additive	conductive carbon black	6.0 mg · 30 wt%	S9 · Section 3. Preparation of the MOF and AC film electrode
Additive	Nafion binder solution	46 uL · 5 wt%, dispersed in water; 10 wt% binder	S9 · Section 3. Preparation of the MOF and AC film electrode
Solvent	dry ethanol	1.15 mL	S9 · Section 3. Preparation of the MOF and AC film electrode