cMOF Evidence Base

Synthesis evidence

Asymmetrical Substitution Manipulates Stacking Modes in 2D Conductive MOF Crystals

Liu Y., Yao H., Zhang H. et al. · Journal of the American Chemical Society · 2025 · 48127-48135

5 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Solvothermal

12 · Synthesis of Cu3F2HHTP2

Metal precursorscopper(II) trifluoroacetylacetonate (Cu(C5H4F3O2)2)
Linker precursorsF2HHTP
Solventswater and NMP
Atmospherecapped vial; atmosphere not specified
Temperature85
Time24
Work-upcentrifuged and washed twice with water, ethanol, and acetone
Scalability context5 mL vial scale.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper(II) trifluoroacetylacetonate (Cu(C5H4F3O2)2)14.4 mg (0.039 mmol)12 · Synthesis of Cu3F2HHTP2
LinkerF2HHTP7.9 mg (0.022 mmol)12 · Synthesis of Cu3F2HHTP2
Solventwater0.9 mL12 · Synthesis of Cu3F2HHTP2
SolventNMP0.6 mL12 · Synthesis of Cu3F2HHTP2
Complete recipeSource: SI

Route 2: Solvothermal

12 · Synthesis of Cu3FHHTP2

Metal precursorscopper nitrate hydrate (Cu(NO3)2.2.5H2O)
Linker precursorsFHHTP
Solventswater and DMF
Atmospherecapped vial; atmosphere not specified
Temperature85
Time24
Work-upcentrifuged and washed twice with water, ethanol, and acetone
Scalability context5 mL vial scale.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper nitrate hydrate (Cu(NO3)2.2.5H2O)9.1 mg (0.039 mmol)12 · Synthesis of Cu3FHHTP2
LinkerFHHTP7.5 mg (0.022 mmol)12 · Synthesis of Cu3FHHTP2
Solventwater1.5 mL12 · Synthesis of Cu3FHHTP2
SolventDMF0.15 mL12 · Synthesis of Cu3FHHTP2
Partial recipeSource: Both

Route 3: Solvothermal

3 · Results and Discussion

Metal precursorscupric acetate
Linker precursorsHHTP
SolventsDMF/H2O
Temperature80
Time6
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecupric acetateNot specified3 · Results and Discussion
LinkerHHTPNot specified3 · Results and Discussion
SolventDMF/H2ONot specified3 · Results and Discussion
Partial recipeSource: SI

Route 4: Other

11 · Synthesis of F2HHTP · Scheme S1

Linker precursors1,2-dibromo-3,6-difluoro-4,5-dimethoxybenzene; 3,4-dimethoxyphenylboronic acid pinacol ester
Solventssame sequence as FHHTP; DCM for demethylation
AdditivesSPhos Pd G2, K2CO3, TFA, DDQ, BBr3
Atmospherenitrogen for air/water-sensitive steps
Temperaturemulti-step; similar to FHHTP
Timemulti-step; similar to FHHTP
Oxidant / reductantbromine; DDQ; BBr3 demethylation reagent
Work-upsimilar to FHHTP
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
LinkerF2HHTP precursor 13Not specified11 · Synthesis of F2HHTP · Scheme S1
OtherBBr3Not specified11 · Synthesis of F2HHTP · Scheme S1
Complete recipeSource: SI

Route 5: Other

9-11 · Synthesis of FHHTP · Scheme S1

Linker precursors1-fluoro-2,3-dimethoxybenzene; 3,4-dimethoxyphenylboronic acid pinacol ester
Solventsacetic acid, THF/H2O, DCM, methanol/chloroform
Additivessodium acetate, SPhos Pd G2, K2CO3, TFA, BBr3
Atmospherenitrogen for air/water-sensitive steps
Temperaturemulti-step: 75, 70, 0 to room temperature
Timemulti-step: until complete, 18 h, 3 h
Oxidant / reductantbromine; DDQ; BBr3 demethylation reagent
Work-upquench, extraction, drying, silica chromatography, recrystallisation
Scalability contextPrecursor amounts are reported for the characterised synthetic sequence.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkercompound 60.30 g (0.703 mmol)9-11 · Synthesis of FHHTP · Scheme S1
Solventanhydrous dichloromethane10 mL9-11 · Synthesis of FHHTP · Scheme S1
OtherBBr32.12 g (8.40 mmol)9-11 · Synthesis of FHHTP · Scheme S1