Synthesis · Extension of charge separation distance over isolated dual-metal sites in metal-organic frameworks for efficient CO2 photoreduction

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

p003 · 2.1 Synthesis of Cu-THQ

Metal precursorsCu(NO3)2.2.5H2O (532 mg) in H2O (100 mL)

Linker precursorstetrahydroxyquinone (THQ, 300 mg) in H2O (100 mL)

SolventsH2O

Additivesethylenediamine (230 uL)

AtmosphereN2 protection; THQ solution degassed

Temperatureroom temperature synthesis; dried at 60

Time12 h stirring; 24 h drying

Work-upsolid washed three times with H2O

Activationdried at 60 deg C for 24 h

Scalability contextNo scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.2.5H2O	532 mg · in 100 mL aqueous solution	p003 · 2.1 Synthesis of Cu-THQ
Linker	Tetrahydroxyquinone (THQ)	300 mg · in 100 mL H2O	p003 · 2.1 Synthesis of Cu-THQ
Additive	ethylenediamine	230 uL	p003 · 2.1 Synthesis of Cu-THQ
Solvent	H2O	200 mL total	p003 · 2.1 Synthesis of Cu-THQ

Complete recipeSource: Main

Route 2: Hydrothermal

p003 · 2.2 Synthesis of CuCo-THQ

Metal precursorsCu(NO3)2.2.5H2O (444 mg) and Co(NO3)2.6H2O (111 mg) in 100 mL metal salt solution

Linker precursorsdegassed THQ (300 mg) aqueous solution (100 mL)

SolventsH2O

Additivesethylenediamine (230 uL)

AtmosphereN2 protection; THQ solution degassed

Temperatureroom temperature synthesis; vacuum dried at 60

Time12 h stirring; 24 h drying

Work-upsolid washed three times with deionized H2O

Activationdried in vacuum at 60 deg C for 24 h

Scalability contextNo scale-up data reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.2.5H2O	444 mg · in 100 mL metal salt solution	p003 · 2.2 Synthesis of CuCo-THQ
Metal Source	Co(NO3)2.6H2O	111 mg · in 100 mL metal salt solution	p003 · 2.2 Synthesis of CuCo-THQ
Linker	THQ	300 mg · in 100 mL degassed aqueous solution	p003 · 2.2 Synthesis of CuCo-THQ
Additive	ethylenediamine	230 uL	p003 · 2.2 Synthesis of CuCo-THQ
Solvent	H2O	200 mL total	p003 · 2.2 Synthesis of CuCo-THQ

Complete recipeSource: Main

Route 3: Hydrothermal

p003 · 2.4 Synthesis of CuFe-THQ

Metal precursorsCu(NO3)2.2.5H2O (444 mg) and Fe(NO3)3.9H2O (154 mg) in 100 mL metal salt solution

Linker precursorsdegassed THQ (300 mg) aqueous solution (100 mL)

SolventsH2O

Additivesethylenediamine (230 uL)

AtmosphereN2 protection; THQ solution degassed

Temperatureroom temperature synthesis; vacuum dried at 60

Time12 h stirring; 24 h drying

Work-upsolid washed three times with deionized H2O

Activationdried in vacuum at 60 deg C for 24 h

Scalability contextNo scale-up data reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.2.5H2O	444 mg · in 100 mL metal salt solution	p003 · 2.4 Synthesis of CuFe-THQ
Metal Source	Fe(NO3)3.9H2O	154 mg · in 100 mL metal salt solution	p003 · 2.4 Synthesis of CuFe-THQ
Linker	THQ	300 mg · in 100 mL degassed aqueous solution	p003 · 2.4 Synthesis of CuFe-THQ
Additive	ethylenediamine	230 uL	p003 · 2.4 Synthesis of CuFe-THQ
Solvent	H2O	200 mL total	p003 · 2.4 Synthesis of CuFe-THQ

Complete recipeSource: Main

Route 4: Hydrothermal

p003 · 2.3 Synthesis of CuNi-THQ

Metal precursorsCu(NO3)2.2.5H2O (444 mg) and Ni(NO3)2.6H2O (111 mg) in 100 mL metal salt solution

Linker precursorsdegassed THQ (300 mg) aqueous solution (100 mL)

SolventsH2O

Additivesethylenediamine (230 uL)

AtmosphereN2 protection; THQ solution degassed

Temperatureroom temperature synthesis; vacuum dried at 60

Time12 h stirring; 24 h drying

Work-upsolid washed three times with deionized H2O

Activationdried in vacuum at 60 deg C for 24 h

Scalability contextNo scale-up data reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.2.5H2O	444 mg · in 100 mL metal salt solution	p003 · 2.3 Synthesis of CuNi-THQ
Metal Source	Ni(NO3)2.6H2O	111 mg · in 100 mL metal salt solution	p003 · 2.3 Synthesis of CuNi-THQ
Linker	THQ	300 mg · in 100 mL degassed aqueous solution	p003 · 2.3 Synthesis of CuNi-THQ
Additive	ethylenediamine	230 uL	p003 · 2.3 Synthesis of CuNi-THQ
Solvent	H2O	200 mL total	p003 · 2.3 Synthesis of CuNi-THQ