Synthesis · Paramagnetic Conducting Metal–Organic Frameworks with Three-Dimensional Structure

3 structured synthesis routes

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

Complete recipeSource: SI

2 · Experimental Section - Synthesis of Co-THBQ

Metal precursorsCo(CH3COO)2.4H2O (98%), 129.5 mg, 0.52 mmol

Linker precursorstetrahydroxy-1,4-benzoquinone hydrate / THBQ, 45 mg, 0.26 mmol

Solvents20 ml degassed water

Atmospherenitrogen-filled glovebox; solvents degassed by freeze-thaw

Temperature120

Time48

Work-upAutoclave cooled to room temperature in the oven; powder filtered and washed with deionized water (3 x 100 ml) and EtOH (2 x 50 ml).

ActivationWell-crystallized powder dried at 45 deg C in a vacuum oven.

Scalability contextYield 51 mg (60%).

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(CH3COO)2.4H2O	129.5 mg, 0.52 mmol	2 · Experimental Section - Synthesis of Co-THBQ
Linker	THBQ	45 mg, 0.26 mmol	2 · Experimental Section - Synthesis of Co-THBQ
Solvent	degassed water	20 ml	2 · Experimental Section - Synthesis of Co-THBQ

Complete recipeSource: SI

2 · Experimental Section - Synthesis of Fe-THBQ

Metal precursorsFeSO4.7H2O (99%), 278 mg, 1 mmol

Linker precursorstetrahydroxy-1,4-benzoquinone hydrate / THBQ, 86 mg, 0.5 mmol

Solvents35 ml degassed water and 5 ml diethylene glycol

Atmospherenitrogen conditions; solvents degassed by freeze-thaw

Temperature120

Time48

Work-upCool to room temperature, filter, wash with deionized water (3 x 100 ml) and EtOH (2 x 50 ml).

ActivationDried at 45 deg C in a vacuum oven.

Scalability contextYield 50 mg (61%).

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	FeSO4.7H2O	278 mg, 1 mmol	2 · Experimental Section - Synthesis of Fe-THBQ
Linker	THBQ	86 mg, 0.5 mmol	2 · Experimental Section - Synthesis of Fe-THBQ
Solvent	water	35 ml	2 · Experimental Section - Synthesis of Fe-THBQ
Solvent	diethylene glycol	5 ml	2 · Experimental Section - Synthesis of Fe-THBQ

Partial recipeSource: SI

2 · Experimental Section - Synthesis of Mn-THBQ

Metal precursorsMn(CH3COO)2.4H2O (99.99%); exact amount not stated, same method as Co-THBQ

Linker precursorstetrahydroxy-1,4-benzoquinone hydrate / THBQ; exact amount not restated, same method as Co-THBQ

Solventsdegassed water; same method as Co-THBQ

Atmospherenitrogen-filled glovebox inferred from same method as Co-THBQ; solvents degassed by freeze-thaw

Temperature120

Time48

Work-upSame method as Co-THBQ: cool in oven, filter, wash with deionized water and EtOH.

ActivationSame method as Co-THBQ: dried at 45 deg C in a vacuum oven.

Scalability contextYield 43 mg (53%).

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Mn(CH3COO)2.4H2O	not stated; same method as Co-THBQ	2 · Experimental Section - Synthesis of Mn-THBQ
Linker	THBQ	not restated; same method as Co-THBQ	2 · Experimental Section - Synthesis of Mn-THBQ
Solvent	degassed water	not restated; same method as Co-THBQ	2 · Experimental Section - Synthesis of Mn-THBQ