Synthesis · Multimetal Incorporation into 2D Conductive Metal-Organic Framework Nanowires Enabling Excellent Electrocatalytic Oxidation of Benzylamine to Benzonitrile

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: Hydrothermal

3 · Synthesis of Ni-CAT Nanowire

Metal precursorsNickel(II) acetate tetrahydrate, Ni(CH3COO)2.4H2O (10 mg, 0.04 mmol)

Linker precursors2,3,6,7,10,11-hexahydroxytriphenylene hydrate/CAT (10 mg, 0.04 mmol)

SolventsDeionized water, 4 mL; ethanol used in wash

AtmosphereNot specified

Temperature90

Time72 reaction; 2 drying

Work-upCool to room temperature, centrifuge, wash with H2O three times and ethanol once.

ActivationDried at 90 deg C for 2 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	10 mg, 0.04 mmol	3 · Synthesis of Ni-CAT Nanowire
Linker	CAT	10 mg, 0.04 mmol	3 · Synthesis of Ni-CAT Nanowire
Solvent	deionized water (H2O)	4 mL	3 · Synthesis of Ni-CAT Nanowire
Solvent	ethanol	wash once	3 · Synthesis of Ni-CAT Nanowire

Complete recipeSource: Main

Route 2: Hydrothermal

3 · Synthesis of NiCo-CAT Nanowire

Metal precursorsNi(CH3COO)2.4H2O (10 mg, 0.04 mmol); Co(CH3COO)2.4H2O (10 mg, 0.04 mmol)

Linker precursorsCAT (10 mg, 0.04 mmol)

SolventsDeionized water, 4 mL; same purification as Ni-CAT

AtmosphereNot specified

Temperature90

Time72 reaction; 2 drying

Work-upReaction and purification similar to Ni-CAT nanowires: cool, centrifuge, wash with water and ethanol.

ActivationDried at 90 deg C for 2 h by analogy to Ni-CAT route.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	10 mg, 0.04 mmol	3 · Synthesis of NiCo-CAT Nanowire
Metal Source	Co(CH3COO)2.4H2O	10 mg, 0.04 mmol	3 · Synthesis of NiCo-CAT Nanowire
Linker	CAT	10 mg, 0.04 mmol	3 · Synthesis of NiCo-CAT Nanowire
Solvent	deionized water (H2O)	4 mL	3 · Synthesis of NiCo-CAT Nanowire

Complete recipeSource: Main

Route 3: Hydrothermal

3 · Synthesis of NiCoFe-CAT Nanowire

Metal precursorsNi(CH3COO)2.4H2O (10 mg, 0.04 mmol); Co(CH3COO)2.4H2O (10 mg, 0.04 mmol); ferrocene (Fe(C5H5)2, 7 mg, 0.04 mmol)

Linker precursorsCAT (10 mg, 0.04 mmol)

SolventsDeionized water, 4 mL; same purification as Ni-CAT

AtmosphereNot specified

Temperature90

Time72 reaction; 2 drying

Oxidant / reductantFerrocene used as stable Fe(II) precursor.

Work-upReaction and purification similar to Ni-CAT nanowires.

ActivationDried at 90 deg C for 2 h by analogy to Ni-CAT route.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	10 mg, 0.04 mmol	3 · Synthesis of NiCoFe-CAT Nanowire
Metal Source	Co(CH3COO)2.4H2O	10 mg, 0.04 mmol	3 · Synthesis of NiCoFe-CAT Nanowire
Metal Source	ferrocene (Fe(C5H5)2)	7 mg, 0.04 mmol	3 · Synthesis of NiCoFe-CAT Nanowire
Linker	CAT	10 mg, 0.04 mmol	3 · Synthesis of NiCoFe-CAT Nanowire
Solvent	deionized water (H2O)	4 mL	3 · Synthesis of NiCoFe-CAT Nanowire

Complete recipeSource: Main

Route 4: Hydrothermal

3 · Synthesis of NiFe-CAT Nanowire

Metal precursorsNi(CH3COO)2.4H2O (10 mg, 0.04 mmol); ferrocene (Fe(C5H5)2, 7 mg, 0.04 mmol)

Linker precursorsCAT (10 mg, 0.04 mmol)

SolventsDeionized water, 4 mL; same purification as Ni-CAT

AtmosphereNot specified

Temperature90

Time72 reaction; 2 drying

Oxidant / reductantFerrocene used as stable Fe(II) precursor; authors avoid readily oxidised ferrous salts.

Work-upReaction and purification similar to Ni-CAT nanowires.

ActivationDried at 90 deg C for 2 h by analogy to Ni-CAT route.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	10 mg, 0.04 mmol	3 · Synthesis of NiFe-CAT Nanowire
Metal Source	ferrocene (Fe(C5H5)2)	7 mg, 0.04 mmol	3 · Synthesis of NiFe-CAT Nanowire
Linker	CAT	10 mg, 0.04 mmol	3 · Synthesis of NiFe-CAT Nanowire
Solvent	deionized water (H2O)	4 mL	3 · Synthesis of NiFe-CAT Nanowire

Complete recipeSource: Main

Route 5: Drop Cast

3 · Synthesis of the Working Electrode (WE)

Metal precursorsPre-synthesised M-CAT catalyst powder

SolventsAlcohol, 1 mL; deionised water and acetone for carbon cloth washing

AdditivesAcetylene black (2 mg); PVDF binder (2 mg)

AtmosphereAmbient, not otherwise specified

Temperature90 carbon-cloth drying and final electrode drying

Time1 HCl treatment; 12 carbon-cloth drying; 1 ink ultrasonication; 0.5 final drying

Substrate orientationCarbon cloth, available space about 1 cm x 1 cm

Work-upCarbon cloth pretreated with 3 M HCl, washed with deionised water and acetone; 300 uL catalyst suspension dropped onto treated cloth.

ActivationElectrochemical activation by 20 CV cycles before LSV testing.

Scalability contextMOF catalyst loading about 3.0 mg cm-2.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF catalyst	10 mg	3 · Synthesis of the Working Electrode (WE)
Additive	acetylene black (AB)	2 mg	3 · Synthesis of the Working Electrode (WE)
Additive	poly(vinylidene fluoride) (PVDF)	2 mg	3 · Synthesis of the Working Electrode (WE)
Solvent	alcohol	1 mL	3 · Synthesis of the Working Electrode (WE)
Acid	HCl	carbon cloth immersed for 1 h · 3 M	3 · Synthesis of the Working Electrode (WE)