Synthesis · Conductive Metal-Organic Frameworks Bearing M−O4 Active Sites as Highly Active Biomass Valorization Electrocatalysts

10 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

2 · 1.2 Synthesis and characterization of M-CAT

Metal precursorsCobalt(II) acetate tetrahydrate, 5 mg

Linker precursorsHHTP, 3.5 mg

Solventsdeionised water:n-propanol = 1 mL:1 mL

Atmospherenot specified; capped culture tube

Temperature85

Time18

Substrate orientationCarbon paper put into dark-blue precursor solution before heating

Work-upFilm rinsed with water, acetone and ethylene; samples scanned for two CV cycles before characterisation.

Scalability contextHigh-surface-area carbon paper electrode growth.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cobalt(II) acetate tetrahydrate	5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Linker	HHTP	3.5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	deionized water	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	n-propanol	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Other	carbon paper	substrate	2 · 1.2 Synthesis and characterization of M-CAT

Complete recipeSource: Both

Route 2: Solvothermal

2 · 1.2 Synthesis and characterization of M-CAT

Metal precursorsCobalt(II) acetate tetrahydrate, 5 mg

Linker precursorsHHTP, 3.5 mg

Solventsdeionised water:n-propanol = 1 mL:1 mL

Atmospherenot specified; capped culture tube

Temperature85

Time18

Substrate orientationFTO substrate put into dark-blue precursor solution before heating

Work-upFilm rinsed with water, acetone and ethylene; samples scanned for two CV cycles before characterisation.

Scalability contextDirect surface growth on conductive substrate; no scale-up reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cobalt(II) acetate tetrahydrate	5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Linker	HHTP	3.5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	deionized water	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	n-propanol	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Other	FTO	substrate	2 · 1.2 Synthesis and characterization of M-CAT

Vague recipeSource: Main

Route 3: Drop Cast

5 · Results and Discussion · Figure 3f

Substrate orientationCo-CAT powder deposited directly on glassy carbon disk

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co-CAT powder	Not specified	5 · Results and Discussion · Figure 3f
Other	glassy carbon disk	substrate	5 · Results and Discussion · Figure 3f

Complete recipeSource: Both

Route 4: Solvothermal

2 · 1.2 Synthesis and characterization of M-CAT

Metal precursorsCobalt(II) acetate tetrahydrate, 5 mg

Linker precursorsHHTP, 3.5 mg

Solventsdeionised water:n-propanol = 1 mL:1 mL

Atmospherenot specified; capped culture tube

Temperature85

Time18

Work-upWashed three times with dry acetone; collected by centrifugation for 30 min.

ActivationDried in dynamic vacuum at 50 C prior to characterisation.

Scalability contextPerformed in 5 mL culture tube; no scale-up reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cobalt(II) acetate tetrahydrate	5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Linker	2,3,6,7,10,11-Hexahydroxytriphenylene Hydrate (HHTP)	3.5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	deionized water	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	n-propanol	1 mL	2 · 1.2 Synthesis and characterization of M-CAT

Partial recipeSource: SI

Route 5: Solvothermal

4 · 1.4 Operando spectroscopy

Metal precursorsCobalt(II) acetate tetrahydrate

Linker precursorsHHTP

Solventsdeionised water and n-propanol

Atmospherenot specified

Temperature85

Time18

Substrate orientationFlexible carbon cloth selected as working electrode

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cobalt(II) acetate tetrahydrate	Not specified	4 · 1.4 Operando spectroscopy
Linker	HHTP	Not specified	4 · 1.4 Operando spectroscopy
Other	flexible carbon cloth	substrate	4 · 1.4 Operando spectroscopy

Partial recipeSource: SI

Route 6: Solvothermal

4 · 1.4 Operando spectroscopy

Metal precursorsNickel(II) acetate tetrahydrate

Linker precursorsHHTP

Solventsdeionised water and n-propanol

Atmospherenot specified

Temperature85

Time18

Substrate orientationFlexible carbon cloth selected as working electrode

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Nickel(II) acetate tetrahydrate	Not specified	4 · 1.4 Operando spectroscopy
Linker	HHTP	Not specified	4 · 1.4 Operando spectroscopy
Other	flexible carbon cloth	substrate	4 · 1.4 Operando spectroscopy

Complete recipeSource: Both

Route 7: Solvothermal

2 · 1.2 Synthesis and characterization of M-CAT

Metal precursorsNickel(II) acetate tetrahydrate, 5 mg

Linker precursorsHHTP, 3.5 mg

Solventsdeionised water:n-propanol = 1 mL:1 mL

Atmospherenot specified; capped culture tube

Temperature85

Time18

Substrate orientationCarbon paper put into dark-blue precursor solution before heating

Work-upFilm rinsed with water, acetone and ethylene; samples scanned for two CV cycles before characterisation.

Scalability contextHigh-surface-area carbon paper electrode growth.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Nickel(II) acetate tetrahydrate	5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Linker	HHTP	3.5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	deionized water	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	n-propanol	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Other	carbon paper	substrate	2 · 1.2 Synthesis and characterization of M-CAT

Complete recipeSource: Both

Route 8: Solvothermal

2 · 1.2 Synthesis and characterization of M-CAT

Metal precursorsNickel(II) acetate tetrahydrate, 5 mg

Linker precursorsHHTP, 3.5 mg

Solventsdeionised water:n-propanol = 1 mL:1 mL

Atmospherenot specified; capped culture tube

Temperature85

Time18

Substrate orientationFTO substrate put into dark-blue precursor solution before heating

Work-upFilm rinsed with water, acetone and ethylene; samples scanned for two CV cycles before characterisation.

Scalability contextDirect surface growth on conductive substrate; no scale-up reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Nickel(II) acetate tetrahydrate	5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Linker	HHTP	3.5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	deionized water	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	n-propanol	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Other	FTO	substrate	2 · 1.2 Synthesis and characterization of M-CAT

Vague recipeSource: Main

Route 9: Drop Cast

5 · Results and Discussion · Figure 3f

Substrate orientationNi-CAT powder deposited directly on glassy carbon disk

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-CAT powder	Not specified	5 · Results and Discussion · Figure 3f
Other	glassy carbon disk	substrate	5 · Results and Discussion · Figure 3f

Complete recipeSource: Both

Route 10: Solvothermal

2 · 1.2 Synthesis and characterization of M-CAT

Metal precursorsNickel(II) acetate tetrahydrate, 5 mg

Linker precursorsHHTP, 3.5 mg

Solventsdeionised water:n-propanol = 1 mL:1 mL

Atmospherenot specified; capped culture tube

Temperature85

Time18

Work-upWashed three times with dry acetone; collected by centrifugation for 30 min.

ActivationDried in dynamic vacuum at 50 C prior to characterisation.

Scalability contextPerformed in 5 mL culture tube; no scale-up reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Nickel(II) acetate tetrahydrate	5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Linker	2,3,6,7,10,11-Hexahydroxytriphenylene Hydrate (HHTP)	3.5 mg	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	deionized water	1 mL	2 · 1.2 Synthesis and characterization of M-CAT
Solvent	n-propanol	1 mL	2 · 1.2 Synthesis and characterization of M-CAT