Synthesis · Ultrathin two-dimensional conjugated metal-organic framework single-crystalline nanosheets enabled by surfactant-assisted synthesis

6 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

SI p.2 · Synthesis of bulk HHB-Cu

Metal precursorsCu(OAc)2 (480 mg, 2.61 mmol)

Linker precursorsTetrahydroxy-1,4-quinone (THQ, 300 mg, 1.74 mmol)

Solvents300 mL aqueous NaOH solution; water and ethanol washes.

AdditivesNaOH (150 mg, 3.75 mmol) as base; no SDS.

AtmosphereAmbient atmosphere.

Temperature50 deg C sonication; 25 deg C undisturbed reaction; 80 deg C vacuum drying.

Time0.5 h sonication; 10 h undisturbed; 12 h drying.

Work-upPrecipitate collected and washed with water and ethanol.

ActivationDried under vacuum for 12 h at 80 deg C.

Scalability contextReported 77.5% isolated yield; SI says reaction is scalable by equivalently increasing monomers, SDS and base, but this sentence likely carried over despite the no-SDS route.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(OAc)2	480 mg, 2.61 mmol	SI p.2 · Synthesis of bulk HHB-Cu
Linker	Tetrahydroxy-1,4-quinone (THQ)	300 mg, 1.74 mmol	SI p.2 · Synthesis of bulk HHB-Cu
Base	NaOH	150 mg, 3.75 mmol · in 300 mL aqueous solution	SI p.2 · Synthesis of bulk HHB-Cu
Solvent	Water	300 mL	SI p.2 · Synthesis of bulk HHB-Cu

Complete recipeSource: Both

Route 2: Other

SI p.2 · Synthesis of HHB-Cu NSs

Metal precursorsCu(OAc)2 (480 mg, 2.61 mmol)

Linker precursorsTetrahydroxy-1,4-quinone (THQ, 300 mg, 1.74 mmol)

SolventsWater, 150 mL for Cu(OAc)2/SDS plus 150 mL for NaOH; water and ethanol washes.

AdditivesSodium dodecyl sulfate (SDS, 150 mg, 0.51 mmol); NaOH (150 mg, 3.75 mmol) as base.

AtmosphereAmbient atmosphere.

Temperature50 deg C sonication; 25 deg C undisturbed reaction; 80 deg C vacuum drying.

Time0.5 h sonication; 10 h undisturbed; 0.5 h ultrasonic ice-bath wash; 24 h settling; 12 h drying; repeated sonication of precipitated large particles until fully exfoliated.

Work-upPrecipitate collected, washed with water and ethanol in an ultrasonic ice bath, dispersions settled for 24 h, upper colloidal suspension collected; large particles further sonicated.

ActivationDried under vacuum for 12 h at 80 deg C.

Scalability contextReported 87.5% yield; reaction scalable by equivalently increasing monomers, SDS and base.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(OAc)2	480 mg, 2.61 mmol	SI p.2 · Synthesis of HHB-Cu NSs
Linker	Tetrahydroxy-1,4-quinone (THQ)	300 mg, 1.74 mmol	SI p.2 · Synthesis of HHB-Cu NSs
Additive	Sodium dodecyl sulfate (SDS)	150 mg, 0.51 mmol	SI p.2 · Synthesis of HHB-Cu NSs
Base	NaOH	150 mg, 3.75 mmol	SI p.2 · Synthesis of HHB-Cu NSs
Solvent	Water	300 mL total	SI p.2 · Synthesis of HHB-Cu NSs

Complete recipeSource: SI

Route 3: Drop Cast

SI p.2 · Preparation of organic cathodes

SolventsWater

AdditivesSuper P conductive additive; sodium alginate binder.

AtmosphereCoin cells assembled in Ar-filled glovebox with oxygen and water below 0.1 ppm.

TemperatureRoom temperature drying; 80 deg C vacuum drying before coin-cell assembly.

Time30 min mortar grinding; vacuum drying for 8 h.

Substrate orientationSlurry cast onto Cu thin foil.

Work-upPunched into 1 cm diameter discs.

ActivationVacuum oven drying at 80 deg C for 8 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	HHB-Cu NSs	60 mass parts	SI p.2 · Preparation of organic cathodes
Additive	super P	30 mass parts	SI p.2 · Preparation of organic cathodes
Additive	alginate sodium	10 mass parts	SI p.2 · Preparation of organic cathodes
Solvent	Water	Not specified	SI p.2 · Preparation of organic cathodes

Complete recipeSource: SI

Route 4: Other

SI p.2 · Synthesis of HHB-Ni nanosheets

Metal precursorsNi(OAc)2 (460 mg, 2.61 mmol)

Linker precursorsTetrahydroxy-1,4-quinone (THQ, 300 mg, 1.74 mmol)

SolventsWater, 150 mL for Ni(OAc)2/SDS plus 150 mL for NaOH; water and ethanol washes.

AdditivesSodium dodecyl sulfate (SDS, 150 mg, 0.51 mmol); NaOH (150 mg, 3.75 mmol) as base.

AtmosphereAmbient atmosphere.

Temperature50 deg C sonication; 25 deg C undisturbed reaction; 80 deg C vacuum drying.

Time0.5 h sonication; 10 h undisturbed; 0.5 h ultrasonic ice-bath wash; 24 h settling; 12 h drying; repeated sonication of precipitated large particles until fully exfoliated.

Work-upPrecipitate collected, washed with water and ethanol in an ultrasonic ice bath, dispersions settled for 24 h, upper colloidal suspension collected; large particles further sonicated.

ActivationDried under vacuum for 12 h at 80 deg C.

Scalability contextReported 85.5% yield; reaction scalable by equivalently increasing monomers, SDS and base.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2	460 mg, 2.61 mmol	SI p.2 · Synthesis of HHB-Ni nanosheets
Linker	Tetrahydroxy-1,4-quinone (THQ)	300 mg, 1.74 mmol	SI p.2 · Synthesis of HHB-Ni nanosheets
Additive	Sodium dodecyl sulfate (SDS)	150 mg, 0.51 mmol	SI p.2 · Synthesis of HHB-Ni nanosheets
Base	NaOH	150 mg, 3.75 mmol	SI p.2 · Synthesis of HHB-Ni nanosheets
Solvent	Water	300 mL total	SI p.2 · Synthesis of HHB-Ni nanosheets

Vague recipeSource: Both

Route 5: Other

SI p.20 · Figure S14 caption · Fig. S14E-H

AdditivesNo surfactant.

Complete recipeSource: SI

Route 6: Other

SI p.2 · Synthesis of HHTP-Cu nanosheets

Metal precursorsCu(OAc)2 (254 mg, 1.395 mmol)

Linker precursorsHHTP (300 mg, 0.93 mmol)

SolventsWater, 150 mL for Cu(OAc)2/SDS plus 150 mL for NaOH; water and ethanol washes.

AdditivesSodium dodecyl sulfate (SDS, 150 mg, 0.51 mmol); NaOH (150 mg, 3.75 mmol) as base.

AtmosphereAmbient atmosphere.

Temperature50 deg C sonication; 25 deg C undisturbed reaction; 80 deg C vacuum drying.

Time0.5 h sonication; 10 h undisturbed; 0.5 h ultrasonic ice-bath wash; 24 h settling; 12 h drying; repeated sonication of precipitated large particles until fully exfoliated.

Work-upPrecipitate collected, washed with water and ethanol in an ultrasonic ice bath, dispersions settled for 24 h, upper colloidal suspension collected; large particles further sonicated.

ActivationDried under vacuum for 12 h at 80 deg C.

Scalability contextReported 80.5% yield; reaction scalable by equivalently increasing monomers, SDS and base.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(OAc)2	254 mg, 1.395 mmol	SI p.2 · Synthesis of HHTP-Cu nanosheets
Linker	HHTP	300 mg, 0.93 mmol	SI p.2 · Synthesis of HHTP-Cu nanosheets
Additive	Sodium dodecyl sulfate (SDS)	150 mg, 0.51 mmol	SI p.2 · Synthesis of HHTP-Cu nanosheets
Base	NaOH	150 mg, 3.75 mmol	SI p.2 · Synthesis of HHTP-Cu nanosheets
Solvent	Water	300 mL total	SI p.2 · Synthesis of HHTP-Cu nanosheets