Synthesis · Chemical structure modulation in conductive MOFs by adjusting the oxidation state of the ligand and introducing alkali metal ions

3 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Solvothermal

p. 2 · Experimental section, Synthesis of MnCsTHBQ

Metal precursorsMn(CH3COO)2·4H2O, 127.4 mg (0.52 mmol); CsCl, 437.7 mg (2.6 mmol)

Linker precursorsTHBQ, 45 mg (0.26 mmol)

Solvents20 ml total degassed water

AdditivesCsCl

AtmosphereNitrogen conditions

Temperature120

Time48

Oxidant / reductantNo separate oxidant or reductant specified; THBQ ligand oxidation state and Cs+ inclusion define route.

Work-upFilter powder; wash with water (3 x 50 ml) and EtOH (2 x 50 ml).

ActivationDried at 45 deg C in a vacuum oven for about 6 h.

Scalability contextSmall-batch Teflon-vessel solvothermal synthesis; yield 36 mg (41%).

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	THBQ	45 mg (0.26 mmol)	p. 2 · Experimental section, Synthesis of MnCsTHBQ
Metal Source	Mn(CH3COO)2·4H2O	127.4 mg (0.52 mmol)	p. 2 · Experimental section, Synthesis of MnCsTHBQ
Additive	CsCl	437.7 mg (2.6 mmol)	p. 2 · Experimental section, Synthesis of MnCsTHBQ
Solvent	degassed water	20 ml total	p. 2 · Experimental section, Synthesis of MnCsTHBQ

Complete recipeSource: SI

Route 2: Solvothermal

p. 1 · Experimental section, Synthesis of MnHHB

Metal precursorsMn(CH3COO)2·4H2O, 127.4 mg (0.52 mmol)

Linker precursorsHHB, 46 mg (0.26 mmol)

Solvents20 ml degassed water

AtmosphereNitrogen conditions

Temperature120

Time48

Oxidant / reductantNo separate oxidant or reductant specified; ligand oxidation state controlled by using HHB.

Work-upCool to room temperature; filter powder; wash with water (3 x 50 ml) and EtOH (2 x 50 ml).

ActivationDried at 45 deg C in a vacuum oven for 6 h.

Scalability contextSmall-batch Teflon-vessel solvothermal synthesis; yield 50 mg (79%).

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHB	46 mg (0.26 mmol)	p. 1 · Experimental section, Synthesis of MnHHB
Metal Source	Mn(CH3COO)2·4H2O	127.4 mg (0.52 mmol)	p. 1 · Experimental section, Synthesis of MnHHB
Solvent	degassed water	20 ml	p. 1 · Experimental section, Synthesis of MnHHB

Complete recipeSource: SI

Route 3: Solvothermal

p. 1 · Experimental section, Synthesis of MnRbTHBQ

Metal precursorsMn(CH3COO)2·4H2O, 127.4 mg (0.52 mmol); RbCl, 628.68 mg (5.2 mmol)

Linker precursorsTHBQ, 45 mg (0.26 mmol)

Solvents20 ml total degassed water

AdditivesRbCl

AtmosphereNitrogen-filled glovebox

Temperature120

Time48

Oxidant / reductantNo separate oxidant or reductant specified; THBQ ligand oxidation state and Rb+ inclusion define route.

Work-upCool to room temperature; filter powder; wash with water (3 x 60 ml) and EtOH (2 x 50 ml).

ActivationDried at 45 deg C in a vacuum oven for about 6 h.

Scalability contextSmall-batch Teflon-vessel solvothermal synthesis; yield 40 mg (52%).

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	THBQ	45 mg (0.26 mmol)	p. 1 · Experimental section, Synthesis of MnRbTHBQ
Metal Source	Mn(CH3COO)2·4H2O	127.4 mg (0.52 mmol)	p. 1 · Experimental section, Synthesis of MnRbTHBQ
Additive	RbCl	628.68 mg (5.2 mmol)	p. 1 · Experimental section, Synthesis of MnRbTHBQ
Solvent	degassed water	20 ml total	p. 1 · Experimental section, Synthesis of MnRbTHBQ