Synthesis · Trimetallic conductive metal-organic frameworks as precatalysts for the oxygen evolution reaction with enhanced activity

11 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

2 · Synthesis of CoxNi1-x-CATs

Metal precursorsCo(OAc)2.4H2O and Ni(OAc)2.4H2O at varied molar ratios; fixed total metal ions 0.2 mmol

Linker precursorsHHTP, typical amount 32.4 mg, 0.1 mmol

Solvents10 mL water/DMF solvent mixture, v:v = 7:3

Atmospherenot reported

Temperature85

Time12

Work-upCentrifugation; washed with deionized water and methanol.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	varied; total Co+Ni 0.2 mmol	2 · Synthesis of CoxNi1-x-CATs
Metal Source	Ni(OAc)2.4H2O	varied; total Co+Ni 0.2 mmol	2 · Synthesis of CoxNi1-x-CATs
Linker	HHTP	typical 32.4 mg, 0.1 mmol	2 · Synthesis of CoxNi1-x-CATs

Complete recipeSource: Main

Route 2: Solvothermal

2 · Synthesis of CoxNi1-x-CATs

Metal precursorsCo(OAc)2.4H2O (30 mg, 0.12 mmol); Ni(OAc)2.4H2O (20 mg, 0.08 mmol)

Linker precursorsHHTP (32.4 mg, 0.1 mmol)

Solvents10 mL water/DMF solvent mixture, v:v = 7:3

Atmospherenot reported

Temperature85

Time12

Work-upCooled to room temperature; collected by centrifugation; washed several times with deionized water and methanol separately.

ActivationNo synthesis activation reported; catalyst ink ultrasonicated before electrode preparation.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	32.4 mg, 0.1 mmol	2 · Synthesis of CoxNi1-x-CATs
Metal Source	Co(OAc)2.4H2O	30 mg, 0.12 mmol	2 · Synthesis of CoxNi1-x-CATs
Metal Source	Ni(OAc)2.4H2O	20 mg, 0.08 mmol	2 · Synthesis of CoxNi1-x-CATs
Solvent	water/DMF	10 mL · v:v = 7:3	2 · Synthesis of CoxNi1-x-CATs

Partial recipeSource: Main

Route 3: Solvothermal

2 · Synthesis of CoxNi1-x-CATs

Metal precursorsCo(OAc)2.4H2O and Ni(OAc)2.4H2O at varied molar ratios; fixed total metal ions 0.2 mmol

Linker precursorsHHTP, typical amount 32.4 mg, 0.1 mmol

Solvents10 mL water/DMF solvent mixture, v:v = 7:3

Atmospherenot reported

Temperature85

Time12

Work-upCentrifugation; washed with deionized water and methanol.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	varied; total Co+Ni 0.2 mmol	2 · Synthesis of CoxNi1-x-CATs
Metal Source	Ni(OAc)2.4H2O	varied; total Co+Ni 0.2 mmol	2 · Synthesis of CoxNi1-x-CATs
Linker	HHTP	typical 32.4 mg, 0.1 mmol	2 · Synthesis of CoxNi1-x-CATs

Partial recipeSource: Main

Route 4: Solvothermal

2 · Synthesis of CoxNi1-x-CATs

Metal precursorsCo(OAc)2.4H2O; fixed total metal ions 0.2 mmol

Linker precursorsHHTP, amount inferred from similar route but exact Co-CAT amount not separately stated

Solventswater/DMF, v:v = 7:3

Atmospherenot reported

Temperature85

Time12

Work-upCentrifugation; washed with deionized water and methanol.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	fixed total metal ions 0.2 mmol	2 · Synthesis of CoxNi1-x-CATs
Linker	HHTP	not separately stated for Co-CAT	2 · Synthesis of CoxNi1-x-CATs
Solvent	water/DMF	not separately stated for Co-CAT · v:v = 7:3	2 · Synthesis of CoxNi1-x-CATs

Complete recipeSource: Main

Route 5: Other

3 · Results and discussion

Metal precursorsCo0.4Ni0.6-CAT (10 mg); Fe(OAc)2 methanolic solution, typically 1 mM

Linker precursorsHHTP already present in parent Co0.4Ni0.6-CAT

Solvents10 mL methanol

Atmospherenot reported

Temperatureroom temperature

Time12

Oxidant / reductantFe(OAc)2 as cation-exchange Fe source

Work-upCollected by centrifugation, washed several times with MeOH.

ActivationVacuum dried at room temperature.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co0.4Ni0.6-CAT	10 mg	3 · Results and discussion
Metal Source	Fe(OAc)2	typically 1 mM	3 · Results and discussion
Solvent	methanol	10 mL	3 · Results and discussion

Complete recipeSource: Main

Route 6: Other

2 · Synthesis of FeCoxNi1-x-CATs

Metal precursorsCo0.6Ni0.4-CAT (10 mg); Fe(OAc)2 methanolic solution, typically 1 mM

Linker precursorsHHTP already present in parent Co0.6Ni0.4-CAT

Solvents10 mL methanol

Atmospherenot reported

Temperatureroom temperature

Time12

Oxidant / reductantFe(OAc)2 as cation-exchange Fe source

Work-upCollected by centrifugation, washed several times with MeOH.

ActivationVacuum dried at room temperature.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co0.6Ni0.4-CAT	10 mg	2 · Synthesis of FeCoxNi1-x-CATs
Metal Source	Fe(OAc)2	typically 1 mM	2 · Synthesis of FeCoxNi1-x-CATs
Solvent	methanol	10 mL	2 · Synthesis of FeCoxNi1-x-CATs

Complete recipeSource: Main

Route 7: Other

4 · Results and discussion

Metal precursorsCo0.6Ni0.4-CAT; Fe(OAc)2 methanolic solutions of 0.25, 0.5, 1.0, and 2.0 mM

Linker precursorsHHTP already present in parent Co0.6Ni0.4-CAT

Solventsmethanol

Atmospherenot reported

Temperatureroom temperature

Time12

Oxidant / reductantFe(OAc)2 as cation-exchange Fe source

Work-upCentrifugation, MeOH wash, vacuum drying at room temperature; exact series workup assumed from the general route.

ActivationVacuum dried at room temperature.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co0.6Ni0.4-CAT	10 mg in typical route	4 · Results and discussion
Metal Source	Fe(OAc)2	0.25, 0.5, 1.0, and 2.0 mM	4 · Results and discussion
Solvent	methanol	10 mL in typical route	4 · Results and discussion

Complete recipeSource: Main

Route 8: Other

3 · Results and discussion

Metal precursorsCo0.8Ni0.2-CAT (10 mg); Fe(OAc)2 methanolic solution, typically 1 mM

Linker precursorsHHTP already present in parent Co0.8Ni0.2-CAT

Solvents10 mL methanol

Atmospherenot reported

Temperatureroom temperature

Time12

Oxidant / reductantFe(OAc)2 as cation-exchange Fe source

Work-upCollected by centrifugation, washed several times with MeOH.

ActivationVacuum dried at room temperature.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co0.8Ni0.2-CAT	10 mg	3 · Results and discussion
Metal Source	Fe(OAc)2	typically 1 mM	3 · Results and discussion
Solvent	methanol	10 mL	3 · Results and discussion

Complete recipeSource: Main

Route 9: Other

2 · Synthesis of FeCoxNi1-x-CATs

Metal precursorsCo-CAT (10 mg); Fe(OAc)2 methanolic solution, typically 1 mM

Linker precursorsHHTP already present in parent Co-CAT

Solvents10 mL methanol

Atmospherenot reported

Temperatureroom temperature

Time12

Oxidant / reductantFe(OAc)2 as cation-exchange Fe source

Work-upCollected by centrifugation, washed several times with MeOH.

ActivationVacuum dried at room temperature.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co-CAT	10 mg	2 · Synthesis of FeCoxNi1-x-CATs
Metal Source	Fe(OAc)2	typically 1 mM	2 · Synthesis of FeCoxNi1-x-CATs
Solvent	methanol	10 mL	2 · Synthesis of FeCoxNi1-x-CATs

Complete recipeSource: Main

Route 10: Other

2 · Synthesis of FeCoxNi1-x-CATs

Metal precursorsNi-CAT (10 mg); Fe(OAc)2 methanolic solution, typically 1 mM

Linker precursorsHHTP already present in parent Ni-CAT

Solvents10 mL methanol

Atmospherenot reported

Temperatureroom temperature

Time12

Oxidant / reductantFe(OAc)2 as cation-exchange Fe source

Work-upCollected by centrifugation, washed several times with MeOH.

ActivationVacuum dried at room temperature.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-CAT	10 mg	2 · Synthesis of FeCoxNi1-x-CATs
Metal Source	Fe(OAc)2	typically 1 mM	2 · Synthesis of FeCoxNi1-x-CATs
Solvent	methanol	10 mL	2 · Synthesis of FeCoxNi1-x-CATs

Partial recipeSource: Main

Route 11: Solvothermal

2 · Synthesis of CoxNi1-x-CATs

Metal precursorsNi(OAc)2.4H2O; fixed total metal ions 0.2 mmol

Linker precursorsHHTP, amount inferred from similar route but exact Ni-CAT amount not separately stated

Solventswater/DMF, v:v = 7:3

Atmospherenot reported

Temperature85

Time12

Work-upCentrifugation; washed with deionized water and methanol.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	fixed total metal ions 0.2 mmol	2 · Synthesis of CoxNi1-x-CATs
Linker	HHTP	not separately stated for Ni-CAT	2 · Synthesis of CoxNi1-x-CATs
Solvent	water/DMF	not separately stated for Ni-CAT · v:v = 7:3	2 · Synthesis of CoxNi1-x-CATs