Partial recipeSource: Main
Route 1: Other
p005 · Solvent removal in Ni6HHTT3 · Fig. S14
AtmosphereNot specified
Temperature90
ActivationHeat treatment at 90 deg C for PXRD comparison.
Synthesis evidence
Continuous and reversible tuning of inter-layer spacings in two-dimensional conductive metal organic frameworks
Dontireddy G.M.R., Suman S.P., Merino-Gardea J.L. et al. · Journal of Materials Chemistry A · 2025 · 8734-8741
8 structured synthesis routes
Completeness describes how fully the route could be reconstructed from the main article and supporting information.
Complete recipeSource: SI
Route 2: Hydrothermal
p002 · Synthesis of Ga9HHTP4
Metal precursorsGa(NO3)3.6H2O; Ga2(SO4)3.H2O
Linker precursors2,3,6,7,10,11-hexahydroxytriphenylene hydrate
SolventsWater; acetone for washing
AdditivesGallium(III) sulfate hydrate supplies sulfate anions
AtmosphereAmbient conditions; sealed vial heated in oven
Temperature80
Time24
Work-upCool to room temperature; collect dark blue precipitate by centrifugation; wash three times with water and three times with acetone.
Scalability contextSmall-batch vial synthesis using 20 mg linker.
Show 5 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | 2,3,6,7,10,11-hexahydroxytriphenylene hydrate | 20.0 mg (0.056 mmol; 1 equiv) | p002 · Synthesis of Ga9HHTP4 |
| Metal Source | Ga(NO3)3.6H2O | 65.8 mg (0.181 mmol; 3.2 equiv) | p002 · Synthesis of Ga9HHTP4 |
| Metal Source | Ga2(SO4)3.H2O | 10.0 mg (0.022 mmol; 0.4 equiv) | p002 · Synthesis of Ga9HHTP4 |
| Solvent | water | 1 mL for linker suspension; 2 mL for gallium salts | p002 · Synthesis of Ga9HHTP4 |
| Solvent | acetone | wash three times | p002 · Synthesis of Ga9HHTP4 |
Complete recipeSource: SI
Route 3: Other
p003 · Procedures for heating and soaking samples
AtmosphereDynamic vacuum using a Schlenk line
Temperature90
Time12
ActivationHeat-treatment in Chemglass vacuum chamber on Heidolph heating plate.
Scalability contextPost-synthetic treatment applied to milligram quantities.
Complete recipeSource: SI
Route 4: Other
p003 · Procedures for heating and soaking samples
SolventsWater; acetonitrile; ethanol; N,N-dimethylformamide; propylene carbonate; chloroform; dichloromethane; dimethyl sulfoxide
AtmosphereNot specified for soaking; final brief heating in air oven
Temperature60
Timeovernight soak; 0.033 h oven step
Work-upFilter solids with no additional solvent during filtration; heat collected powders in 60 deg C air oven for 2 min.
ActivationStarts from heat-treated Ga9HHTP4 prepared under dynamic vacuum.
Scalability context~3 mg heat-treated samples soaked in ~2 mL solvent.
Show 2 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Solvent | desired solvents | ~2 mL | p003 · Procedures for heating and soaking samples |
| Other | heat-treated Ga9HHTP4 | ~3 mg | p003 · Procedures for heating and soaking samples |
Complete recipeSource: SI
Route 5: Other
p003 · Synthesis of 2,3,7,8,12,13-Hexahydroxytricycloquinazoline (HHTT)
Linker precursors5,6-dimethyoxyanthranil; 2,3,7,8,12,13-hexamethoxytricycloquinazoline intermediate
SolventsSulfolane; glacial acetic acid; water; methanol
AdditivesAmmonium acetate; pyridine hydrochloride
AtmosphereAir for intermediate drying; vacuum drying after demethylation
Temperaturereflux; 240
Time96; 3
Work-upAdd water, suction filter, wash with water and methanol, dry under air; then demethylate with pyridine hydrochloride, add water, suction filter, wash with water, dry under vacuum.
Scalability contextLinker synthesis scale: 4 g anthranil precursor; final HHTT yield reported as 320 mg (50%).
Show 6 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | 5,6-dimethyoxyanthranil 2 | 4 g (22.33 mmol) | p003 · Synthesis of 2,3,7,8,12,13-Hexahydroxytricycloquinazoline (HHTT) |
| Additive | ammonium acetate | 12 g (156 mmol) | p003 · Synthesis of 2,3,7,8,12,13-Hexahydroxytricycloquinazoline (HHTT) |
| Acid | glacial acetic acid | 25 mL | p003 · Synthesis of 2,3,7,8,12,13-Hexahydroxytricycloquinazoline (HHTT) |
| Solvent | sulfolane | 100 mL | p003 · Synthesis of 2,3,7,8,12,13-Hexahydroxytricycloquinazoline (HHTT) |
| Additive | pyridine hydrochloride | 27 g (234 mmol) | p003 · Synthesis of 2,3,7,8,12,13-Hexahydroxytricycloquinazoline (HHTT) |
| Other | 2,3,7,8,12,13-hexamethoxytricycloquinazoline | 800 mg (1.6 mmol) | p003 · Synthesis of 2,3,7,8,12,13-Hexahydroxytricycloquinazoline (HHTT) |
Complete recipeSource: SI
Route 6: Hydrothermal
p002 · Synthesis of Ni6HHTT3 MOF
Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTT
SolventsDeionized water; water, DMF, ethanol and acetone for washing
AtmosphereAir; closed 20 mL scintillation vial
Temperature85
Time12
Work-upCentrifuge black powder; wash twice each with water, DMF, ethanol and acetone.
Scalability contextSmall-batch vial synthesis using 8.0 mg HHTT.
Show 4 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Linker | HHTT | 0.019 mmol (1.0 equiv, 8.0 mg) · in 3.0 mL deionized water | p002 · Synthesis of Ni6HHTT3 MOF |
| Metal Source | Ni(OAc)2.4H2O | 0.048 mmol (2.5 equiv, 12.0 mg) · in 1.0 mL deionized water | p002 · Synthesis of Ni6HHTT3 MOF |
| Solvent | deionized water | 4.0 mL total | p002 · Synthesis of Ni6HHTT3 MOF |
| Solvent | DMF, ethanol, acetone | washed twice for each solvent | p002 · Synthesis of Ni6HHTT3 MOF |
Complete recipeSource: SI
Route 7: Other
p003 · Procedures for heating and soaking samples
AtmosphereDynamic vacuum using a Schlenk line
Temperature90
Time12
ActivationHeat-treatment in Chemglass vacuum chamber.
Scalability contextPost-synthetic treatment applied to milligram quantities.
Complete recipeSource: SI
Route 8: Other
p003 · Procedures for heating and soaking samples
SolventsWater
AtmosphereNot specified for soaking; final brief heating in air oven
Temperature60
Timeovernight soak; 0.033 h oven step
Work-upFilter solids with no additional solvent during filtration; heat collected powders in 60 deg C air oven for 2 min.
ActivationStarts from heat-treated Ni6HHTT3.
Scalability context~3 mg heat-treated samples soaked in ~2 mL solvent.
Show 2 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Solvent | water | ~2 mL | p003 · Procedures for heating and soaking samples |
| Other | heat-treated Ni6HHTT3 | ~3 mg | p003 · Procedures for heating and soaking samples |