Synthesis · Two-dimensional conductive metal-organic frameworks with dual metal sites toward the electrochemical 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: Main

Route 1: Drop Cast

1628 · Electrochemical measurements

Solvents0.5 mL DMF and 0.5 mL ultrapure water

Additives2 mg acetylene black; 5 uL Nafion, 0.5 wt% in ethanol

AtmosphereO2-saturated 1 M KOH during electrochemical testing

Temperature298

Time1

Substrate orientationpre-polished glassy carbon electrode

Work-upultrasonicated for 60 min; 10 uL catalyst ink drop-cast; dried at 298 K; Nafion dropped evenly

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NiPc-Ni MOF sample	2 mg	1628 · Electrochemical measurements
Additive	acetylene black	2 mg	1628 · Electrochemical measurements
Solvent	DMF	0.5 mL	1628 · Electrochemical measurements
Solvent	ultrapure water	0.5 mL	1628 · Electrochemical measurements
Additive	Nafion in ethanol	5 uL · 0.5 wt%	1628 · Electrochemical measurements

Complete recipeSource: Main

Route 2: Solvothermal

1627 · General procedure for the synthesis of NiPc-Ni

Metal precursorsnickel(II) acetate tetrahydrate aqueous solution, 24.88 mg, 0.1 mmol

Linker precursorsNiPc, 28 mg, 0.04 mmol

Solvents5 mL DMF; 6 mL H2O; 2 mL aqueous metal-salt solution

Additives2.2 mL NH3.H2O, about 22 wt%

Atmospherenot specified for MOF solvothermal step

Temperature120

Time48

Work-upfiltered, washed with DMF and acetone

Activationdried under vacuum at room temperature

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	NiPc	28 mg, 0.04 mmol	1627 · General procedure for the synthesis of NiPc-Ni
Solvent	DMF	5 mL	1627 · General procedure for the synthesis of NiPc-Ni
Base	NH3.H2O	2.2 mL · ~22 wt%	1627 · General procedure for the synthesis of NiPc-Ni
Solvent	H2O	6 mL	1627 · General procedure for the synthesis of NiPc-Ni
Metal Source	nickel(II) acetate tetrahydrate aqueous solution	2 mL solution containing 24.88 mg, 0.1 mmol	1627 · General procedure for the synthesis of NiPc-Ni

Partial recipeSource: Main

Route 3: Solvothermal

1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn

Metal precursorszinc(II) acetate dihydrate; amount not explicitly reported for analogue

Linker precursorsNiPc, inferred same as NiPc-Ni route

SolventsDMF, H2O and aqueous metal-salt solution, by analogy to NiPc-Ni

AdditivesNH3.H2O, about 22 wt%, by analogy to NiPc-Ni

Atmospherenot specified

Temperature120

Time48

Work-upfiltered, washed with DMF and acetone, by analogy to NiPc-Ni

Activationdried under vacuum at room temperature

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	NiPc	not separately specified; analogous to 28 mg, 0.04 mmol	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Metal Source	zinc(II) acetate dihydrate	not explicitly reported	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Solvent	DMF/H2O	by analogy to NiPc-Ni	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Base	NH3.H2O	by analogy to NiPc-Ni · ~22 wt%	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn

Partial recipeSource: Main

Route 4: Solvothermal

1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn

Metal precursorsnickel(II) acetate tetrahydrate aqueous solution, inferred same as NiPc-Ni route

Linker precursorsZnPc; amount not explicitly reported for analogue

SolventsDMF, H2O and aqueous metal-salt solution, by analogy to NiPc-Ni

AdditivesNH3.H2O, about 22 wt%, by analogy to NiPc-Ni

Atmospherenot specified

Temperature120

Time48

Work-upfiltered, washed with DMF and acetone, by analogy to NiPc-Ni

Activationdried under vacuum at room temperature

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	ZnPc	not explicitly reported	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Metal Source	nickel(II) acetate tetrahydrate aqueous solution	by analogy to NiPc-Ni	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Solvent	DMF/H2O	by analogy to NiPc-Ni	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Base	NH3.H2O	by analogy to NiPc-Ni · ~22 wt%	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn

Partial recipeSource: Main

Route 5: Solvothermal

1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn

Metal precursorszinc(II) acetate dihydrate; amount not explicitly reported for analogue

Linker precursorsZnPc; amount not explicitly reported for analogue

SolventsDMF, H2O and aqueous metal-salt solution, by analogy to NiPc-Ni

AdditivesNH3.H2O, about 22 wt%, by analogy to NiPc-Ni

Atmospherenot specified

Temperature120

Time48

Work-upfiltered, washed with DMF and acetone, by analogy to NiPc-Ni

Activationdried under vacuum at room temperature

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	ZnPc	not explicitly reported	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Metal Source	zinc(II) acetate dihydrate	not explicitly reported	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Solvent	DMF/H2O	by analogy to NiPc-Ni	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn
Base	NH3.H2O	by analogy to NiPc-Ni · ~22 wt%	1627 · General procedure for the synthesis of NiPc-Zn, ZnPc-Ni, and ZnPc-Zn