Synthesis · Structure and Electrical Transport Properties of Metal Cate-Cholate Frameworks: The Metal Center Matters†

12 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Liquid Liquid Interface

SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film

Metal precursorscalcium acetate (0.08 mmol) in 50 mL aqueous solution

Linker precursorsHexahydroxytriphenylene (HHTP, 0.04 mmol) in 50 mL ethyl acetate solution

SolventsEthyl acetate organic phase and water aqueous phase

Additives10 uL ammonia water

AtmosphereAmbient atmosphere; biphasic system left undisturbed

Temperatureroom temperature

Time48

Substrate orientationFilm formed at liquid-liquid interface and transferred onto quartz substrate.

Work-upResulting film carefully transferred onto quartz substrate and rinsed with acetone.

Scalability context90 mm crystallization dish; 50 mL organic phase plus 50 mL aqueous phase.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol in 50 mL ethyl acetate	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film
Metal Source	calcium acetate	0.08 mmol · in 50 mL aqueous solution	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	ethyl acetate	50 mL	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	water	50 mL	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film
Additive	ammonia water	10 uL	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film

Complete recipeSource: Both

Route 2: Solvothermal

SI p.S5-S6 · Section 2.2 Synthesis of M-HHTP MOFs

Metal precursorsCalcium acetate (0.08 mmol, 12.7 mg)

Linker precursorsHexahydroxytriphenylene (HHTP) ligand (0.04 mmol, 13 mg)

Solvents1 mL DMF plus 5 mL water in aqueous NaOH solution

AdditivesNaOH solution (10 mg NaOH in 5 mL water)

AtmosphereLoosely capped glass vial; atmosphere not otherwise specified

Temperature85

Time24

Work-upSolid collected by centrifugation, thoroughly washed with water and acetone.

ActivationDried under vacuum at 40 C for 12 h.

Scalability context20 mL glass vial batch synthesis yielding microcrystalline powder.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol, 13 mg	SI p.S5-S6 · Section 2.2 Synthesis of M-HHTP MOFs
Metal Source	Calcium acetate	0.08 mmol, 12.7 mg	SI p.S5-S6 · Section 2.2 Synthesis of M-HHTP MOFs
Solvent	1 mL DMF plus 5 mL water in aqueous NaOH solution	Not specified	SI p.S5-S6 · Section 2.2 Synthesis of M-HHTP MOFs
Base	NaOH	10 mg in 5 mL water	SI p.S5-S6 · Section 2.2 Synthesis of M-HHTP MOFs

Complete recipeSource: Both

Route 3: Liquid Liquid Interface

SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film

Metal precursorscobalt(II) acetate tetrahydrate (0.08 mmol) in 50 mL aqueous solution

Linker precursorsHexahydroxytriphenylene (HHTP, 0.04 mmol) in 50 mL ethyl acetate solution

SolventsEthyl acetate organic phase and water aqueous phase

AtmosphereAmbient atmosphere; biphasic system left undisturbed

Temperatureroom temperature

Time48

Substrate orientationFilm formed at liquid-liquid interface and transferred onto quartz substrate.

Work-upResulting film carefully transferred onto quartz substrate and rinsed with acetone.

Scalability context90 mm crystallization dish; 50 mL organic phase plus 50 mL aqueous phase.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol in 50 mL ethyl acetate	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Metal Source	cobalt(II) acetate tetrahydrate	0.08 mmol · in 50 mL aqueous solution	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	ethyl acetate	50 mL	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	water	50 mL	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film

Complete recipeSource: Both

Route 4: Solvothermal

SI p.S6 · Section 2.2 Synthesis of M-HHTP MOFs

Metal precursorsCobalt(II) acetate tetrahydrate (0.08 mmol, 20 mg)

Linker precursorsHexahydroxytriphenylene (HHTP) ligand (0.04 mmol, 13 mg)

Solvents0.5 mL NMP plus 5 mL ultrapure water

Additivesbrief sonication

AtmosphereLoosely capped glass vial; atmosphere not otherwise specified

Temperature80

Time24

Work-upSolid collected by centrifugation, thoroughly washed with water and acetone.

ActivationDried under vacuum at 40 C for 12 h.

Scalability context20 mL glass vial batch synthesis yielding microcrystalline powder.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol, 13 mg	SI p.S6 · Section 2.2 Synthesis of M-HHTP MOFs
Metal Source	Cobalt(II) acetate tetrahydrate	0.08 mmol, 20 mg	SI p.S6 · Section 2.2 Synthesis of M-HHTP MOFs
Solvent	0.5 mL NMP plus 5 mL ultrapure water	Not specified	SI p.S6 · Section 2.2 Synthesis of M-HHTP MOFs

Complete recipeSource: Both

Route 5: Liquid Liquid Interface

SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film

Metal precursorscopper nitrate trihydrate (0.08 mmol) in 50 mL aqueous solution

Linker precursorsHexahydroxytriphenylene (HHTP, 0.04 mmol) in 50 mL ethyl acetate solution

SolventsEthyl acetate organic phase and water aqueous phase

AtmosphereAmbient atmosphere; biphasic system left undisturbed

Temperatureroom temperature

Time48

Substrate orientationFilm formed at liquid-liquid interface and transferred onto quartz substrate.

Work-upResulting film carefully transferred onto quartz substrate and rinsed with acetone.

Scalability context90 mm crystallization dish; 50 mL organic phase plus 50 mL aqueous phase.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol in 50 mL ethyl acetate	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Metal Source	copper nitrate trihydrate	0.08 mmol · in 50 mL aqueous solution	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	ethyl acetate	50 mL	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	water	50 mL	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film

Complete recipeSource: Both

Route 6: Solvothermal

SI p.S6-S7 · Section 2.2 Synthesis of M-HHTP MOFs

Metal precursorsCopper nitrate trihydrate aqueous solution (725 uL, 20 mg/mL)

Linker precursorsHexahydroxytriphenylene (HHTP) ligand (0.04 mmol, 13 mg)

Solvents1 mL DMF plus 5 mL ultrapure water

Additivesbrief sonication

AtmosphereLoosely capped glass vial; atmosphere not otherwise specified

Temperature85

Time24

Work-upSolid collected by centrifugation, thoroughly washed with water and acetone.

ActivationDried under vacuum at 40 C for 12 h.

Scalability context20 mL glass vial batch synthesis yielding microcrystalline powder.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol, 13 mg	SI p.S6-S7 · Section 2.2 Synthesis of M-HHTP MOFs
Metal Source	Copper nitrate trihydrate aqueous solution	725 uL, 20 mg/mL · 20 mg/mL	SI p.S6-S7 · Section 2.2 Synthesis of M-HHTP MOFs
Solvent	1 mL DMF plus 5 mL ultrapure water	Not specified	SI p.S6-S7 · Section 2.2 Synthesis of M-HHTP MOFs

Complete recipeSource: Both

Route 7: Liquid Liquid Interface

SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film

Metal precursorsmagnesium acetate (0.08 mmol) in 50 mL aqueous solution

Linker precursorsHexahydroxytriphenylene (HHTP, 0.04 mmol) in 50 mL ethyl acetate solution

SolventsEthyl acetate organic phase and water aqueous phase

Additives10 uL ammonia water

AtmosphereAmbient atmosphere; biphasic system left undisturbed

Temperatureroom temperature

Time48

Substrate orientationFilm formed at liquid-liquid interface and transferred onto quartz substrate.

Work-upResulting film carefully transferred onto quartz substrate and rinsed with acetone.

Scalability context90 mm crystallization dish; 50 mL organic phase plus 50 mL aqueous phase.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol in 50 mL ethyl acetate	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film
Metal Source	magnesium acetate	0.08 mmol · in 50 mL aqueous solution	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	ethyl acetate	50 mL	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	water	50 mL	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film
Additive	ammonia water	10 uL	SI p.S7 · Section 2.3 Synthesis of M-HHTP MOF film

Complete recipeSource: Both

Route 8: Solvothermal

SI p.S5 · Section 2.2 Synthesis of M-HHTP MOFs

Metal precursorsMagnesium ethoxide (0.08 mmol, 9.2 mg)

Linker precursorsHexahydroxytriphenylene (HHTP) ligand (0.04 mmol, 13 mg)

Solvents5 mL ultrapure water

AtmosphereLoosely capped glass vial; atmosphere not otherwise specified

Temperature85

Time24

Work-upSolid collected by centrifugation, thoroughly washed with water and acetone.

ActivationDried under vacuum at 40 C for 12 h.

Scalability context20 mL glass vial batch synthesis yielding microcrystalline powder.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol, 13 mg	SI p.S5 · Section 2.2 Synthesis of M-HHTP MOFs
Metal Source	Magnesium ethoxide	0.08 mmol, 9.2 mg	SI p.S5 · Section 2.2 Synthesis of M-HHTP MOFs
Solvent	5 mL ultrapure water	Not specified	SI p.S5 · Section 2.2 Synthesis of M-HHTP MOFs

Complete recipeSource: Both

Route 9: Liquid Liquid Interface

SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film

Metal precursorsnickel acetate tetrahydrate (0.08 mmol) in 50 mL aqueous solution

Linker precursorsHexahydroxytriphenylene (HHTP, 0.04 mmol) in 50 mL ethyl acetate solution

SolventsEthyl acetate organic phase and water aqueous phase

AtmosphereAmbient atmosphere; biphasic system left undisturbed

Temperatureroom temperature

Time48

Substrate orientationFilm formed at liquid-liquid interface and transferred onto quartz substrate.

Work-upResulting film carefully transferred onto quartz substrate and rinsed with acetone.

Scalability context90 mm crystallization dish; 50 mL organic phase plus 50 mL aqueous phase.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol in 50 mL ethyl acetate	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Metal Source	nickel acetate tetrahydrate	0.08 mmol · in 50 mL aqueous solution	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	ethyl acetate	50 mL	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	water	50 mL	SI p.S8 · Section 2.3 Synthesis of M-HHTP MOF film

Complete recipeSource: Both

Route 10: Solvothermal

SI p.S6 · Section 2.2 Synthesis of M-HHTP MOFs

Metal precursorsNickel acetate tetrahydrate (0.08 mmol, 20 mg)

Linker precursorsHexahydroxytriphenylene (HHTP) ligand (0.04 mmol, 13 mg)

Solvents5 mL ultrapure water

AtmosphereLoosely capped glass vial; atmosphere not otherwise specified

Temperature85

Time24

Work-upSolid collected by centrifugation, thoroughly washed with water and acetone.

ActivationDried under vacuum at 40 C for 12 h.

Scalability context20 mL glass vial batch synthesis yielding microcrystalline powder.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol, 13 mg	SI p.S6 · Section 2.2 Synthesis of M-HHTP MOFs
Metal Source	Nickel acetate tetrahydrate	0.08 mmol, 20 mg	SI p.S6 · Section 2.2 Synthesis of M-HHTP MOFs
Solvent	5 mL ultrapure water	Not specified	SI p.S6 · Section 2.2 Synthesis of M-HHTP MOFs

Complete recipeSource: Both

Route 11: Liquid Liquid Interface

SI p.S8-S9 · Section 2.3 Synthesis of M-HHTP MOF film

Metal precursorszinc acetate dihydrate (0.08 mmol) in 50 mL aqueous solution

Linker precursorsHexahydroxytriphenylene (HHTP, 0.04 mmol) in 50 mL ethyl acetate solution

SolventsEthyl acetate organic phase and water aqueous phase

AtmosphereAmbient atmosphere; biphasic system left undisturbed

Temperatureroom temperature

Time48

Substrate orientationFilm formed at liquid-liquid interface and transferred onto quartz substrate.

Work-upResulting film carefully transferred onto quartz substrate and rinsed with acetone.

Scalability context90 mm crystallization dish; 50 mL organic phase plus 50 mL aqueous phase.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol in 50 mL ethyl acetate	SI p.S8-S9 · Section 2.3 Synthesis of M-HHTP MOF film
Metal Source	zinc acetate dihydrate	0.08 mmol · in 50 mL aqueous solution	SI p.S8-S9 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	ethyl acetate	50 mL	SI p.S8-S9 · Section 2.3 Synthesis of M-HHTP MOF film
Solvent	water	50 mL	SI p.S8-S9 · Section 2.3 Synthesis of M-HHTP MOF film

Complete recipeSource: Both

Route 12: Solvothermal

SI p.S7 · Section 2.2 Synthesis of M-HHTP MOFs

Metal precursorsZinc(II) acetylacetonate (0.068 mmol, 18 mg)

Linker precursorsHexahydroxytriphenylene (HHTP) ligand (0.04 mmol, 13 mg)

Solvents1 mL NMP plus 5 mL ultrapure water

Additivesbrief sonication

AtmosphereLoosely capped glass vial; atmosphere not otherwise specified

Temperature85

Time24

Work-upSolid collected by centrifugation, thoroughly washed with water and acetone.

ActivationDried under vacuum at 40 C for 12 h.

Scalability context20 mL glass vial batch synthesis yielding microcrystalline powder.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	hexahydroxytriphenylene (HHTP)	0.04 mmol, 13 mg	SI p.S7 · Section 2.2 Synthesis of M-HHTP MOFs
Metal Source	Zinc(II) acetylacetonate	0.068 mmol, 18 mg	SI p.S7 · Section 2.2 Synthesis of M-HHTP MOFs
Solvent	1 mL NMP plus 5 mL ultrapure water	Not specified	SI p.S7 · Section 2.2 Synthesis of M-HHTP MOFs