Synthesis · Regulating Electronic Structure of Bimetallic NiFe-THQ Conductive Metal–Organic Frameworks to Boost Catalytic Activity for Oxygen Evolution Reaction

5 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

p003 · S1.2 Synthesis

Metal precursorsFeSO4.7H2O only; 0.27 mmol total Fe

Linker precursors0.29 mmol THQ

Solventsdeionized water

Additives40 uL ethylenediamine

Atmospheresealed glass vial; atmosphere not specified

Temperature85

Time12

Work-upcooled naturally, centrifuged at 10000 rpm, washed with deionized water three times

Activationdried in a 60 °C oven for 24 h

Scalability context50 mL sealed glass vial; powder isolated by centrifugation.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	varied; total metal ions fixed at 0.27 mmol	p003 · S1.2 Synthesis
Metal Source	FeSO4.7H2O	varied; total metal ions fixed at 0.27 mmol	p003 · S1.2 Synthesis
Linker	tetrahydroxy-1,4-quinone (THQ)	0.29 mmol · dissolved in 16 mL deionized water	p003 · S1.2 Synthesis
Solvent	deionized water	16 mL for metal solution + 16 mL for THQ solution	p003 · S1.2 Synthesis
Base	ethylenediamine	40 uL	p003 · S1.2 Synthesis

Complete recipeSource: Both

Route 2: Hydrothermal

p003 · S1.2 Synthesis

Metal precursorsNi(OAc)2.4H2O and FeSO4.7H2O at x=0.2; 0.27 mmol total metal ions

Linker precursors0.29 mmol THQ

Solventsdeionized water

Additives40 uL ethylenediamine

Atmospheresealed glass vial; atmosphere not specified

Temperature85

Time12

Work-upcooled naturally, centrifuged at 10000 rpm, washed with deionized water three times

Activationdried in a 60 °C oven for 24 h

Scalability context50 mL sealed glass vial; powder isolated by centrifugation.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	varied; total metal ions fixed at 0.27 mmol	p003 · S1.2 Synthesis
Metal Source	FeSO4.7H2O	varied; total metal ions fixed at 0.27 mmol	p003 · S1.2 Synthesis
Linker	tetrahydroxy-1,4-quinone (THQ)	0.29 mmol · dissolved in 16 mL deionized water	p003 · S1.2 Synthesis
Solvent	deionized water	16 mL for metal solution + 16 mL for THQ solution	p003 · S1.2 Synthesis
Base	ethylenediamine	40 uL	p003 · S1.2 Synthesis

Complete recipeSource: Both

Route 3: Hydrothermal

p003 · S1.2 Synthesis

Metal precursors0.135 mmol Ni(OAc)2.4H2O and 0.135 mmol FeSO4.7H2O

Linker precursors0.29 mmol THQ

Solventsdeionized water

Additives40 uL ethylenediamine

Atmospheresealed glass vial; atmosphere not specified

Temperature85

Time12

Work-upcooled naturally, centrifuged at 10000 rpm, washed with deionized water three times

Activationdried in a 60 °C oven for 24 h

Scalability context50 mL sealed glass vial; powder isolated by centrifugation.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	0.135 mmol	p003 · S1.2 Synthesis
Metal Source	FeSO4.7H2O	0.135 mmol	p003 · S1.2 Synthesis
Linker	tetrahydroxy-1,4-quinone (THQ)	0.29 mmol · dissolved in 16 mL deionized water	p003 · S1.2 Synthesis
Solvent	deionized water	16 mL for metal solution + 16 mL for THQ solution	p003 · S1.2 Synthesis
Base	ethylenediamine	40 uL	p003 · S1.2 Synthesis

Complete recipeSource: Both

Route 4: Hydrothermal

p003 · S1.2 Synthesis

Metal precursorsNi(OAc)2.4H2O and FeSO4.7H2O at x=0.8; 0.27 mmol total metal ions

Linker precursors0.29 mmol THQ

Solventsdeionized water

Additives40 uL ethylenediamine

Atmospheresealed glass vial; atmosphere not specified

Temperature85

Time12

Work-upcooled naturally, centrifuged at 10000 rpm, washed with deionized water three times

Activationdried in a 60 °C oven for 24 h

Scalability context50 mL sealed glass vial; powder isolated by centrifugation.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	varied; total metal ions fixed at 0.27 mmol	p003 · S1.2 Synthesis
Metal Source	FeSO4.7H2O	varied; total metal ions fixed at 0.27 mmol	p003 · S1.2 Synthesis
Linker	tetrahydroxy-1,4-quinone (THQ)	0.29 mmol · dissolved in 16 mL deionized water	p003 · S1.2 Synthesis
Solvent	deionized water	16 mL for metal solution + 16 mL for THQ solution	p003 · S1.2 Synthesis
Base	ethylenediamine	40 uL	p003 · S1.2 Synthesis

Complete recipeSource: Both

Route 5: Hydrothermal

p003 · S1.2 Synthesis

Metal precursorsNi(OAc)2.4H2O only; 0.27 mmol total Ni

Linker precursors0.29 mmol THQ

Solventsdeionized water

Additives40 uL ethylenediamine

Atmospheresealed glass vial; atmosphere not specified

Temperature85

Time12

Work-upcooled naturally, centrifuged at 10000 rpm, washed with deionized water three times

Activationdried in a 60 °C oven for 24 h

Scalability context50 mL sealed glass vial; powder isolated by centrifugation.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	varied; total metal ions fixed at 0.27 mmol	p003 · S1.2 Synthesis
Metal Source	FeSO4.7H2O	varied; total metal ions fixed at 0.27 mmol	p003 · S1.2 Synthesis
Linker	tetrahydroxy-1,4-quinone (THQ)	0.29 mmol · dissolved in 16 mL deionized water	p003 · S1.2 Synthesis
Solvent	deionized water	16 mL for metal solution + 16 mL for THQ solution	p003 · S1.2 Synthesis
Base	ethylenediamine	40 uL	p003 · S1.2 Synthesis