Synthesis · Dissecting π-conjugated covalent-coupling over conductive MOFs toward efficient two-electron oxygen reduction

3 structured synthesis routes

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

Complete recipeSource: Both

Preparation of Cu-HHTP sample

Metal precursors0.4 mmol Cu(Ac)2.H2O

Linker precursors0.2 mmol HHTP

Solvents10 mL mixed DMF and DI water, DMF:H2O = 1:1; distilled water and ethanol for washing

AtmosphereNot reported; heated under stirring in oil bath

Temperature85

Time24

Work-upNatural cooling to room temperature; centrifugation; washed with distilled water and ethanol several times

ActivationNo separate activation reported

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(Ac)2.H2O	0.4 mmol	Preparation of Cu-HHTP sample
Linker	HHTP	0.2 mmol	Preparation of Cu-HHTP sample
Solvent	DMF	part of 10 mL mixed solution · DMF:H2O = 1:1	Preparation of Cu-HHTP sample
Solvent	DI water	part of 10 mL mixed solution · DMF:H2O = 1:1	Preparation of Cu-HHTP sample
Solvent	distilled water and ethanol	several washes	Preparation of Cu-HHTP sample

Complete recipeSource: Both

Synthesis of Ni-HITP and Cu-HITP samples

Metal precursors0.2 mmol Cu(Ac)2.H2O

Linker precursors2 mg HITP

Solvents20 mL dimethyl sulfoxide; aqueous metal solution; distilled water and ethanol for washing

Additives100 uL NH3.H2O, by same procedure as Ni-HITP

AtmosphereNot reported; heated under stirring in oil bath

Temperature50 then 60

Time0.167 at 50 deg C after metal addition; 12 at 60 deg C after NH3.H2O addition; dried overnight

Work-upInferred from the identical Ni-HITP procedure: centrifugation; washed with distilled water and ethanol several times

ActivationInferred from the identical Ni-HITP procedure: dried at 60 deg C overnight

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HITP	2 mg, inherited from Ni-HITP recipe	Synthesis of Ni-HITP and Cu-HITP samples
Solvent	dimethyl sulfoxide	20 mL, inherited from Ni-HITP recipe	Synthesis of Ni-HITP and Cu-HITP samples
Metal Source	Cu(Ac)2.H2O	0.2 mmol	Synthesis of Ni-HITP and Cu-HITP samples
Base	NH3.H2O	100 uL, inherited from Ni-HITP recipe	Synthesis of Ni-HITP and Cu-HITP samples
Solvent	distilled water and ethanol	several washes, inherited from Ni-HITP recipe	Synthesis of Ni-HITP and Cu-HITP samples

Complete recipeSource: Both

Synthesis of Ni-HITP and Cu-HITP samples

Metal precursors0.2 mmol Ni(Ac)2.H2O in 4 mL aqueous solution

Linker precursors2 mg HITP

Solvents20 mL dimethyl sulfoxide; aqueous metal solution; distilled water and ethanol for washing

Additives100 uL NH3.H2O

AtmosphereNot reported; heated under stirring in oil bath

Temperature50 then 60

Time0.167 at 50 deg C after metal addition; 12 at 60 deg C after NH3.H2O addition; dried overnight

Work-upCentrifugation; washed with distilled water and ethanol several times

ActivationDried at 60 deg C overnight

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HITP	2 mg	Synthesis of Ni-HITP and Cu-HITP samples
Solvent	dimethyl sulfoxide	20 mL	Synthesis of Ni-HITP and Cu-HITP samples
Metal Source	Ni(Ac)2.H2O	0.2 mmol in 4 mL aqueous solution	Synthesis of Ni-HITP and Cu-HITP samples
Base	NH3.H2O	100 uL	Synthesis of Ni-HITP and Cu-HITP samples
Solvent	distilled water and ethanol	several washes	Synthesis of Ni-HITP and Cu-HITP samples