Synthesis · Tri-Metallic Catalyst for Oxygen Evolution Reaction Enables Continuous Operation of Anion Exchange Membrane Electrolyzer at 1A cm−2 for Hundreds of Hours

18 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.045 g; Co(NO3)2.6H2O 0.01 g; FeSO4.7H2O 0.045 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Scalability contextScaling up performed by multiplying concentrations of metals/ligand and solvent amounts; main text reports reproducible multi-gram batches and states one 5 g batch is enough to fabricate 2500 cm2 of MEA.

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.045 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.01 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.045 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 2: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0 g; Co(NO3)2.6H2O 0.05 g; FeSO4.7H2O 0.05 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.05 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.05 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 3: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.025 g; Co(NO3)2.6H2O 0.05 g; FeSO4.7H2O 0.025 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.025 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.05 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.025 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 4: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0 g; Co(NO3)2.6H2O 0.08 g; FeSO4.7H2O 0.02 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.08 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.02 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 5: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.005 g; Co(NO3)2.6H2O 0.09 g; FeSO4.7H2O 0.005 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.005 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.09 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.005 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 6: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.045 g; Co(NO3)2.6H2O 0.045 g; FeSO4.7H2O 0.01 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.045 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.045 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.01 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 7: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.04 g; Co(NO3)2.6H2O 0.04 g; FeSO4.7H2O 0.02 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.04 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.04 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.02 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 8: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.025 g; Co(NO3)2.6H2O 0.025 g; FeSO4.7H2O 0.05 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.025 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.025 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.05 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 9: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.01 g; Co(NO3)2.6H2O 0.01 g; FeSO4.7H2O 0.08 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.01 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.01 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.08 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: SI

Route 10: Other

2 · MEA Fabrication

Metal precursorsFe10Ni45Co45 MOF-74 catalyst powder from solvothermal route

Linker precursorsnot applicable to electrode fabrication; MOF already synthesised

Solventssolution ink solvent not specified

Additivesionomer/binder implied for MEA fabrication but composition not specified; no carbon black added to anode catalyst

AtmosphereN2 gas flow during airbrush spraying

Temperatureroom temperature spray; brief heating temperature not specified

Substrate orientationporous transport layer / Ni foam anode support

Work-upMOF catalyst ground, deagglomerated, fed as solution ink, sprayed on PTL, then heated for 20 s to evaporate ink solvent

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF catalyst	0.7 mg/cm2 anode catalyst loading	2 · MEA Fabrication
Other	Ni foam porous transport layer/anode support	Not specified	2 · MEA Fabrication
Other	commercial Pt-Ni cathode catalyst on non-wetproofing carbon fiber paper	1.2 mg/cm2 cathode catalyst loading	2 · MEA Fabrication

Partial recipeSource: Both

Route 11: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O, Co(NO3)2.6H2O and FeSO4.7H2O in sample-specific masses listed in SI Table S1

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0-0.08 g depending on Table S1 composition	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0-0.09 g depending on Table S1 composition	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0-0.08 g depending on Table S1 composition	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	DMF:water:ethanol	15:1:1 ratio	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 12: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.01 g; Co(NO3)2.6H2O 0.045 g; FeSO4.7H2O 0.045 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.01 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.045 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.045 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 13: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.033 g; Co(NO3)2.6H2O 0.033 g; FeSO4.7H2O 0.033 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.033 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.033 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.033 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 14: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.050 g; Co(NO3)2.6H2O 0.025 g; FeSO4.7H2O 0.025 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.050 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.025 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.025 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 15: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.05 g; Co(NO3)2.6H2O 0.05 g; FeSO4.7H2O 0 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.05 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.05 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 16: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.05 g; Co(NO3)2.6H2O 0 g; FeSO4.7H2O 0.05 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.05 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.05 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 17: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.005 g; Co(NO3)2.6H2O 0.0475 g; FeSO4.7H2O 0.0475 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.005 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.0475 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.0475 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1

Partial recipeSource: Both

Route 18: Solvothermal

1-2 · Synthesis and Table S1 · Table S1

Metal precursorsNi(NO3)2.6H2O 0.08 g; Co(NO3)2.6H2O 0.01 g; FeSO4.7H2O 0.01 g

Linker precursors0.05 g DOBDC / 2,5-dihydroxyterephthalic acid ligand; approximately 3:2 total metals:ligand

Solvents15:1:1 dimethylformamide (DMF):water:ethanol solvent mixture

Atmospherenot specified

Temperature130

Time48

Substrate orientationnot applicable; powder synthesis in Teflon autoclave

Oxidant / reductantFeSO4.7H2O used as Fe source; main text states FeSO4 stabilises Fe2+ and avoids iron oxide impurities

Work-upcooled; washed with DMF and ethanol; methanol solvent exchange for three days, twice per day; powder collected by vacuum filtration

ActivationMicromeritics Smart VacPrep station at 150 C for 12 h

Show 8 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	0.08 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	Co(NO3)2.6H2O	0.01 g	1-2 · Synthesis and Table S1 · Table S1
Metal Source	FeSO4.7H2O	0.01 g	1-2 · Synthesis and Table S1 · Table S1
Linker	dobdc ligand / 2,5-dihydroxyterephthalic acid	0.05 g · approximately 3:2 total metals:ligand	1-2 · Synthesis and Table S1 · Table S1
Solvent	dimethylformamide (DMF)	15 parts by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	water	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	ethanol	1 part by volume in 15:1:1 DMF:water:ethanol mixture	1-2 · Synthesis and Table S1 · Table S1
Solvent	methanol	solvent exchange for three days, two times/day	1-2 · Synthesis and Table S1 · Table S1