Synthesis · Electrically Conducting Redox-Complementary Dual-Ligand 2D Graphitic MOF with Orthogonal Charge Transport Pathways

3 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

p004 / SI p.S3 · Material Synthesis and Characterization

Metal precursorsCu(OAc)2.H2O (22 mg, 0.11 mmol)

Linker precursorsHHTP (3.5 mg, 0.01 mmol); HHTQ (4.5 mg, 0.01 mmol)

SolventsDeionized H2O (8 mL) for Cu(OAc)2.H2O/ethylenediamine; DMF (2 mL) for HHTP/HHTQ

AdditivesEthylenediamine (11.5 uL) modulator

AtmosphereAir / sealed screw-capped vial; atmosphere not otherwise specified

Temperature70

Time24

Work-upSlowly cooled to room temperature; black solid centrifuged and washed thoroughly with H2O, DMF, and acetone; soaked in hot H2O at 60 deg C for 12 h; washed with H2O and acetone.

ActivationDried under vacuum for 24 h.

Scalability context20 mL screw-capped vial laboratory-scale solvothermal batch.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(OAc)2.H2O	22 mg, 0.11 mmol	p004 / SI p.S3 · Material Synthesis and Characterization
Linker	HHTP	3.5 mg, 0.01 mmol	p004 / SI p.S3 · Material Synthesis and Characterization
Linker	HHTQ	4.5 mg, 0.01 mmol	p004 / SI p.S3 · Material Synthesis and Characterization
Additive	ethylenediamine	11.5 uL	p004 / SI p.S3 · Material Synthesis and Characterization
Solvent	deionized H2O	8 mL	p004 / SI p.S3 · Material Synthesis and Characterization
Solvent	DMF	2 mL	p004 / SI p.S3 · Material Synthesis and Characterization

Complete recipeSource: SI

Route 2: Solvothermal

p004 / SI p.S3 · Material Synthesis and Characterization

Metal precursorsCuSO4.5H2O (35.2 mg, 0.141 mmol)

Linker precursorsHHTP ligand (20 mg, 0.062 mmol)

SolventsDeionized H2O (0.8 mL for CuSO4.5H2O; 2 mL for HHTP) and DMF (0.25 mL)

AtmosphereAir / sealed screw-capped vial; atmosphere not otherwise specified

Temperature80

Time16

Work-upCooled to room temperature; dark blue solid centrifuged and washed thoroughly with H2O, EtOH, and acetone.

ActivationDried under vacuum for 24 h.

Scalability context5 mL screw-capped vial laboratory-scale solvothermal batch.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuSO4.5H2O	35.2 mg, 0.141 mmol	p004 / SI p.S3 · Material Synthesis and Characterization
Linker	HHTP ligand	20 mg, 0.062 mmol	p004 / SI p.S3 · Material Synthesis and Characterization
Solvent	deionized H2O	0.8 mL plus 2 mL	p004 / SI p.S3 · Material Synthesis and Characterization
Solvent	DMF	0.25 mL	p004 / SI p.S3 · Material Synthesis and Characterization

Complete recipeSource: SI

Route 3: Solvothermal

p004 / SI p.S3 · Material Synthesis and Characterization

Metal precursorsCuSO4.5H2O (9 mg, 0.036 mmol)

Linker precursorsHHTQ ligand (10 mg, 0.024 mmol)

SolventsDeionized H2O (0.5 mL) and DMF (0.3 mL)

AtmosphereAir / sealed screw-capped vial; atmosphere not otherwise specified

Temperature85

Time16

Work-upCooled to room temperature; black solid centrifuged and washed thoroughly with H2O, DMF, EtOH, and acetone.

ActivationDried under vacuum for 24 h.

Scalability context5 mL screw-capped vial laboratory-scale solvothermal batch.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuSO4.5H2O	9 mg, 0.036 mmol	p004 / SI p.S3 · Material Synthesis and Characterization
Linker	HHTQ ligand	10 mg, 0.024 mmol	p004 / SI p.S3 · Material Synthesis and Characterization
Solvent	deionized H2O	0.5 mL	p004 / SI p.S3 · Material Synthesis and Characterization
Solvent	DMF	0.3 mL	p004 / SI p.S3 · Material Synthesis and Characterization