Synthesis · Enhancing One-Dimensional Charge Transport in Metal-organic Framework Hexagonal Nanorods for Electrocatalytic Oxygen Evolution

6 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Hydrothermal

SI p. 2 · 1.1 Synthesis of NiFe-HXR

Metal precursorsFeSO4.7H2O (same procedure as NiFe-HXR; Ni(NO3)2.6H2O omitted)

Linker precursors4,4'-bipyridine, 2.23 mmol

Solvents16.7 mL deionised water

AdditivesNa2S, 2.53 mmol

Atmosphereairtight 20 mL autoclave; sealed glass bottle for crystallisation

Temperature150; then 70

Time72; then 12

Oxidant / reductantNa2S additive/reductant or sulphide source

Work-upPink solution transferred to sealed glass bottle; metal salts added; followed by filtration; clear solution crystallised at 70 C.

Activationnone reported

Scalability context20 mL autoclave batch; no scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	4,4'-bipyridine	2.23 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Additive	Na2S	2.53 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Solvent	deionized water	16.7 mL	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Metal Source	FeSO4.7H2O	same procedure as NiFe-HXR; Ni(NO3)2.6H2O omitted	SI p. 2 · 1.1 Synthesis of NiFe-HXR

Complete recipeSource: SI

Route 2: Hydrothermal

SI p. 2 · 1.1 Synthesis of NiFe-HXR

Metal precursorsNi(NO3)2.6H2O (Ni/Fe = 0.2:0.8); FeSO4.7H2O (Ni/Fe = 0.2:0.8)

Linker precursors4,4'-bipyridine, 2.23 mmol

Solvents16.7 mL deionised water

AdditivesNa2S, 2.53 mmol

Atmosphereairtight 20 mL autoclave; sealed glass bottle for crystallisation

Temperature150; then 70

Time72; then 12

Oxidant / reductantNa2S additive/reductant or sulphide source

Work-upPink solution transferred to sealed glass bottle; metal salts added; followed by filtration; clear solution crystallised at 70 C.

Activationnone reported

Scalability context20 mL autoclave batch; no scale-up data reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	4,4'-bipyridine	2.23 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Additive	Na2S	2.53 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Solvent	deionized water	16.7 mL	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Metal Source	Ni(NO3)2.6H2O	Ni/Fe = 0.2:0.8	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Metal Source	FeSO4.7H2O	Ni/Fe = 0.2:0.8	SI p. 2 · 1.1 Synthesis of NiFe-HXR

Complete recipeSource: SI

Route 3: Hydrothermal

SI p. 2 · 1.1 Synthesis of NiFe-HXR

Metal precursorsNi(NO3)2.6H2O (Ni/Fe = 0.8:0.2); FeSO4.7H2O (Ni/Fe = 0.8:0.2)

Linker precursors4,4'-bipyridine, 2.23 mmol

Solvents16.7 mL deionised water

AdditivesNa2S, 2.53 mmol

Atmosphereairtight 20 mL autoclave; sealed glass bottle for crystallisation

Temperature150; then 70

Time72; then 12

Oxidant / reductantNa2S additive/reductant or sulphide source

Work-upPink solution transferred to sealed glass bottle; metal salts added; followed by filtration; clear solution crystallised at 70 C.

Activationnone reported

Scalability context20 mL autoclave batch; no scale-up data reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	4,4'-bipyridine	2.23 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Additive	Na2S	2.53 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Solvent	deionized water	16.7 mL	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Metal Source	Ni(NO3)2.6H2O	Ni/Fe = 0.8:0.2	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Metal Source	FeSO4.7H2O	Ni/Fe = 0.8:0.2	SI p. 2 · 1.1 Synthesis of NiFe-HXR

Complete recipeSource: SI

Route 4: Hydrothermal

SI p. 2 · 1.1 Synthesis of NiFe-HXR

Metal precursorsNi(NO3)2.6H2O (same procedure as NiFe-HXR; FeSO4.7H2O omitted)

Linker precursors4,4'-bipyridine, 2.23 mmol

Solvents16.7 mL deionised water

AdditivesNa2S, 2.53 mmol

Atmosphereairtight 20 mL autoclave; sealed glass bottle for crystallisation

Temperature150; then 70

Time72; then 12

Oxidant / reductantNa2S additive/reductant or sulphide source

Work-upPink solution transferred to sealed glass bottle; metal salts added; followed by filtration; clear solution crystallised at 70 C.

Activationnone reported

Scalability context20 mL autoclave batch; no scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	4,4'-bipyridine	2.23 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Additive	Na2S	2.53 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Solvent	deionized water	16.7 mL	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Metal Source	Ni(NO3)2.6H2O	same procedure as NiFe-HXR; FeSO4.7H2O omitted	SI p. 2 · 1.1 Synthesis of NiFe-HXR

Complete recipeSource: Both

Route 5: Hydrothermal

SI p. 2 · 1.1 Synthesis of NiFe-HXR

Metal precursorsNi(NO3)2.6H2O (part of 2.25 mmol total metal salts; Ni/Fe = 1/1); FeSO4.7H2O (part of 2.25 mmol total metal salts; Ni/Fe = 1/1)

Linker precursors4,4'-bipyridine, 2.23 mmol

Solvents16.7 mL deionised water

AdditivesNa2S, 2.53 mmol

Atmosphereairtight 20 mL autoclave; sealed glass bottle for crystallisation

Temperature150; then 70

Time72; then 12

Oxidant / reductantNa2S additive/reductant or sulphide source

Work-upPink solution transferred to sealed glass bottle; metal salts added; followed by filtration; clear solution crystallised at 70 C.

Activationnone reported

Scalability context20 mL autoclave batch; no scale-up data reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	4,4'-bipyridine	2.23 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Additive	Na2S	2.53 mmol	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Solvent	deionized water	16.7 mL	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Metal Source	Ni(NO3)2.6H2O	part of 2.25 mmol total metal salts; Ni/Fe = 1/1	SI p. 2 · 1.1 Synthesis of NiFe-HXR
Metal Source	FeSO4.7H2O	part of 2.25 mmol total metal salts; Ni/Fe = 1/1	SI p. 2 · 1.1 Synthesis of NiFe-HXR

Complete recipeSource: SI

Route 6: Other

SI p. 2 · 1.1 Synthesis of NiFe-HXR · Figure S3

Metal precursorsNiFe-HXR precursor

Atmosphereair

Temperature500

Time2

Oxidant / reductantair oxidation during heating

Work-upHeating NiFe-HXR at 500 C for 2 h with a heating rate of 2 C min-1.

Activationpyrolysis/calcination

Scalability contextNo scale-up data reported.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	NiFe-HXR	not reported	SI p. 2 · 1.1 Synthesis of NiFe-HXR · Figure S3