cMOF Evidence Base

Synthesis evidence

Electrical conductivity through π–π stacking in a two-dimensional porous gallium catecholate metal–organic framework

Skorupskii G., Chanteux G., Le K.N. et al. · Annals of the New York Academy of Sciences · 2022 · 226-230

3 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

SI p.2 · Typical synthesis of Ga9(HOTP)4

Metal precursors65.8 mg (0.181 mmol; 3.2 equiv) Ga(NO3)3.6H2O and 10.0 mg (0.022 mmol; 0.4 equiv) Ga2(SO4)3.H2O
Linker precursors20.0 mg (0.056 mmol; 1 equiv) 2,3,6,7,10,11-hexahydroxytriphenylene hydrate
SolventsWater only: 1 ml water for linker suspension and 2 ml water for gallium salts; work-up with water and acetone
AdditivesGallium nitrate also used to control solution pH and improve crystallinity; sulfate anions incorporated into the product
AtmosphereAmbient conditions during setup; sealed scintillation vial during heating
Temperature80
Time24
Work-upCool to room temperature; collect dark blue precipitate by centrifugation; wash three times with water and three times with acetone.
ActivationNone for as-made powder.
Scalability contextMild aqueous synthesis without organic solvent during framework formation; no yield or scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate20.0 mg (0.056 mmol; 1 equiv)SI p.2 · Typical synthesis of Ga9(HOTP)4
Metal SourceGa(NO3)3.6H2O65.8 mg (0.181 mmol; 3.2 equiv)SI p.2 · Typical synthesis of Ga9(HOTP)4
Metal SourceGa2(SO4)3.H2O10.0 mg (0.022 mmol; 0.4 equiv)SI p.2 · Typical synthesis of Ga9(HOTP)4
Solventwater1 ml for linker suspension; 2 ml for metal salt solutionSI p.2 · Typical synthesis of Ga9(HOTP)4
Solventacetonewashed three timesSI p.2 · Typical synthesis of Ga9(HOTP)4
Partial recipeSource: SI

Route 2: Other

SI p.2 · Elemental and thermogravimetric analysis · Figure S2

Metal precursorsAs-made Ga9(HOTP)4 powder from aqueous synthesis
Linker precursorsAs-made Ga9(HOTP)4 powder from aqueous synthesis
AtmosphereVacuum
Temperature90
ActivationAttempted activation by heating at 90 C under vacuum; reported to significantly reduce crystallinity.
Complete recipeSource: SI

Route 3: Other

SI p.3 · Elemental and thermogravimetric analysis · Figure S2

Metal precursorsAs-made Ga9(HOTP)4 powder from aqueous synthesis
Linker precursorsAs-made Ga9(HOTP)4 powder from aqueous synthesis
SolventsEthanol exchange followed by liquid/supercritical CO2
AtmosphereCO2 during supercritical drying; brief air exposure; dry N2-filled glovebox after evacuation
Temperature40 during supercritical CO2 hold; 45 during overnight evacuation
Time0.5 h liquid CO2 exchange; 0.5 h hold above critical point; 8 h CO2 vent; overnight evacuation
Work-upSuspend powder in ethanol on aluminium foil boat, exchange ethanol with liquid CO2 using 5-minute soaks and vents, vent CO2, transfer to screwcap vacuum adapter vial.
ActivationSupercritical CO2 drying at approximately 40 C and about 1300 psi followed by 8 h venting and overnight evacuation at 45 C; final transfer to dry N2 glovebox.
Scalability contextActivation requires supercritical CO2 drying equipment; no scale-up data reported.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Solventethanolsample powder was suspended in ethanolSI p.3 · Elemental and thermogravimetric analysis · Figure S2
Otherliquid CO2 / supercritical CO2exchanged over 30 minutes; held 30 minutes above critical point · about 1300 psi at approximately 40 CSI p.3 · Elemental and thermogravimetric analysis · Figure S2