Synthesis · Engineering defective trimetallic metal-organic framework nanosheets for advanced water oxidation electrocatalysis

10 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

2 · Experimental section 2.1

Metal precursorsFeSO4*7H2O

Linker precursors1,4-H2BDC

SolventsDI water; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upas for Ni-MOF: centrifugation; washed with water and ethanol; dried 12 h at 60 deg C

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*FeSO47H2O replacing Ni(OAc)24H2O*	not explicitly restated	2 · Experimental section 2.1
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	2 · Experimental section 2.1
Solvent	DI water	6.0 mL	2 · Experimental section 2.1
Solvent	DMAC	6 mL	2 · Experimental section 2.1

Complete recipeSource: Both

Route 2: Solvothermal

2 · Experimental section 2.1

Metal precursorsNi(OAc)2*4H2O

Linker precursors1,4-H2BDC

SolventsDI water; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcooled to room temperature; precipitate collected by centrifugation; washed with water and ethanol; dried 12 h at 60 deg C

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.0248 g · in 6.0 mL DI water	2 · Experimental section 2.1
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	2 · Experimental section 2.1
Solvent	DI water	6.0 mL	2 · Experimental section 2.1
Solvent	N,N-dimethylacetamide (DMAC)	6 mL	2 · Experimental section 2.1

Complete recipeSource: Both

Route 3: Solvothermal

2 · Experimental section 2.2

Metal precursorsNi(OAc)2*4H2O; FeSO4*7H2O

Linker precursors1,4-H2BDC

Solventswater; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcollected via centrifugation, washed with ethanol and water, dried at 60 deg C for 12 h

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.1 mmol, 0.0248 g	2 · Experimental section 2.2
Metal Source	*FeSO47H2O**	0.03 mmol	2 · Experimental section 2.2
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	2 · Experimental section 2.2
Solvent	water	6 mL	2 · Experimental section 2.2
Solvent	DMAC	6 mL	2 · Experimental section 2.2

Complete recipeSource: Both

Route 4: Solvothermal

2 · Experimental section 2.3

Metal precursorsNi(OAc)2*4H2O; FeSO4*7H2O; CdSO4*3H2O

Linker precursors1,4-H2BDC

Solventswater; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcollected via centrifugation, washed with ethanol and water, dried at 60 deg C for 12 h

Activationelectrochemical activation by cyclic voltammetry for 60 cycles before OER testing

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.1 mmol, 0.0248 g	2 · Experimental section 2.3
Metal Source	*FeSO47H2O**	0.015 mmol	2 · Experimental section 2.3
Metal Source	*CdSO43H2O**	0.015 mmol	2 · Experimental section 2.3
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	2 · Experimental section 2.3
Solvent	water	6 mL	2 · Experimental section 2.3
Solvent	DMAC	6 mL	2 · Experimental section 2.3

Partial recipeSource: Main

Route 5: Solvothermal

2 · Experimental section 2.3

Metal precursorsNi(OAc)2*4H2O; FeSO4*7H2O; CuSO4 (hydrate not specified)

Linker precursors1,4-H2BDC

Solventswater; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcollected via centrifugation, washed with ethanol and water, dried at 60 deg C for 12 h

Activationelectrochemical activation by cyclic voltammetry for 60 cycles before OER testing

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.1 mmol, 0.0248 g	2 · Experimental section 2.3
Metal Source	*FeSO47H2O**	0.015 mmol	2 · Experimental section 2.3
Metal Source	CuSO4 (hydrate not specified)	0.015 mmol	2 · Experimental section 2.3
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	2 · Experimental section 2.3
Solvent	water	6 mL	2 · Experimental section 2.3
Solvent	DMAC	6 mL	2 · Experimental section 2.3

Complete recipeSource: Both

Route 6: Solvothermal

2 · Experimental section 2.3

Metal precursorsNi(OAc)2*4H2O; FeSO4*7H2O; MnSO4*H2O

Linker precursors1,4-H2BDC

Solventswater; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcollected via centrifugation, washed with ethanol and water, dried at 60 deg C for 12 h

Activationelectrochemical activation by cyclic voltammetry for 60 cycles before OER testing

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.1 mmol, 0.0248 g	2 · Experimental section 2.3
Metal Source	*FeSO47H2O**	0.015 mmol	2 · Experimental section 2.3
Metal Source	*MnSO4H2O**	0.015 mmol	2 · Experimental section 2.3
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	2 · Experimental section 2.3
Solvent	water	6 mL	2 · Experimental section 2.3
Solvent	DMAC	6 mL	2 · Experimental section 2.3

Partial recipeSource: Main

Route 7: Solvothermal

4 · Results and discussion 3.1

Metal precursorsNi(OAc)2*4H2O; FeSO4*7H2O; Pb salt not specified

Linker precursors1,4-H2BDC

Solventswater; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcollected via centrifugation, washed with ethanol and water, dried at 60 deg C for 12 h

Activationelectrochemical activation by cyclic voltammetry for 60 cycles before OER testing

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.1 mmol, 0.0248 g	4 · Results and discussion 3.1
Metal Source	*FeSO47H2O**	0.015 mmol	4 · Results and discussion 3.1
Metal Source	Pb salt not specified in route	not specified	4 · Results and discussion 3.1
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	4 · Results and discussion 3.1
Solvent	water	6 mL	4 · Results and discussion 3.1
Solvent	DMAC	6 mL	4 · Results and discussion 3.1

Complete recipeSource: Both

Route 8: Solvothermal

3 · Results and discussion 3.1

Metal precursorsNi(OAc)2*4H2O; FeSO4*7H2O; ZnSO4*7H2O

Linker precursors1,4-H2BDC

Solventswater; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcollected via centrifugation, washed with ethanol and water, dried at 60 deg C for 12 h

Activationelectrochemical activation by cyclic voltammetry for 60 cycles before OER testing

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.1 mmol, 0.0248 g	3 · Results and discussion 3.1
Metal Source	*FeSO47H2O**	0.015 mmol	3 · Results and discussion 3.1
Metal Source	*ZnSO47H2O**	1 mM	3 · Results and discussion 3.1
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	3 · Results and discussion 3.1
Solvent	water	6 mL	3 · Results and discussion 3.1
Solvent	DMAC	6 mL	3 · Results and discussion 3.1

Complete recipeSource: Both

Route 9: Solvothermal

3 · Results and discussion 3.1

Metal precursorsNi(OAc)2*4H2O; FeSO4*7H2O; ZnSO4*7H2O

Linker precursors1,4-H2BDC

Solventswater; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcollected via centrifugation, washed with ethanol and water, dried at 60 deg C for 12 h

Activationelectrochemical activation by cyclic voltammetry for 60 cycles before OER testing

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.1 mmol, 0.0248 g	3 · Results and discussion 3.1
Metal Source	*FeSO47H2O**	0.015 mmol	3 · Results and discussion 3.1
Metal Source	*ZnSO47H2O**	5 mM	3 · Results and discussion 3.1
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	3 · Results and discussion 3.1
Solvent	water	6 mL	3 · Results and discussion 3.1
Solvent	DMAC	6 mL	3 · Results and discussion 3.1

Complete recipeSource: Both

Route 10: Solvothermal

2 · Experimental section 2.3

Metal precursorsNi(OAc)2*4H2O; FeSO4*7H2O; ZnSO4*7H2O

Linker precursors1,4-H2BDC

Solventswater; DMAC

Atmospheresealed Teflon-lined stainless-steel vessel/autoclave; atmosphere not otherwise specified

Temperature150

Time3

Work-upcollected via centrifugation, washed with ethanol and water, dried at 60 deg C for 12 h

Activationelectrochemical activation by cyclic voltammetry for 60 cycles before OER testing

Scalability contextAuthors describe the method as universal/facile for trimetallic NiFeM MOF nanosheets, but no scale-up mass or batch yield is reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	*Ni(OAc)24H2O**	0.1 mmol, 0.0248 g	2 · Experimental section 2.3
Metal Source	*FeSO47H2O**	0.015 mmol	2 · Experimental section 2.3
Metal Source	*ZnSO47H2O**	0.015 mmol · reported elsewhere as 3 mM baseline	2 · Experimental section 2.3
Linker	1,4-H2BDC	0.0083 g · in 6 mL DMAC	2 · Experimental section 2.3
Solvent	water	6 mL	2 · Experimental section 2.3
Solvent	DMAC	6 mL	2 · Experimental section 2.3