cMOF Evidence Base

Synthesis evidence

Topochemical conversion of a dense metal-organic framework from a crystalline insulator to an amorphous semiconductor

Tominaka S., Hamoudi H., Suga T. et al. · Chemical Science · 2015 · 1465-1473

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

2 · Experimental - Synthesis

Metal precursorsCuCl (95%, Aldrich), 0.50 mmol
Linker precursorstrithiocyanuric acid, ttcH3 (>98%, TCI), 0.5 mmol
Solventsacetonitrile (99.9%, Fisher), 20 mL
Temperature60 deg C overnight, then 80 deg C
Timeovernight at 60 deg C plus 48 h at 80 deg C
Work-upReddish orange octahedral crystals collected by vacuum filtration and rinsed with ethanol.
Scalability contextReported yield 95%; crystals 10-200 um.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuCl (95%, Aldrich)0.50 mmol2 · Experimental - Synthesis
LinkerttcH3 (>98%, TCI)0.5 mmol2 · Experimental - Synthesis
Solventacetonitrile (99.9%, Fisher)20 mL2 · Experimental - Synthesis
Complete recipeSource: Main

Route 2: Other

2 · Experimental - Synthesis

Metal precursorsCompound 1 CuCl(ttcH3) crystals
Linker precursorsttcH3 framework already present in compound 1
Solventsdistilled water
Additives0.43% aqueous ammonia, pH 11.4, prepared from 35% NH3 aq. and distilled water
Atmosphereambient/room-temperature solution treatment
Temperatureroom temperature
Time48 h
Oxidant / reductantammonia base; dehydrochlorination/deprotonation treatment
Work-upRinsed with distilled water; colour darkened to black.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1 crystalsNot specified2 · Experimental - Synthesis
Baseaqueous ammonia (35% NH3 aq. + distilled water)0.43%, pH 11.42 · Experimental - Synthesis
Solventdistilled waterNot specified2 · Experimental - Synthesis
Partial recipeSource: Both

Route 3: Other

2 · Experimental - Synthesis

Metal precursorsCompound 1 CuCl(ttcH3) crystals
Linker precursorsttcH3 framework already present in compound 1
Solventsdistilled water
Additives0.43% aqueous ammonia, pH 11.4
Atmosphereambient solution treatment followed by vacuum drying
Temperatureroom temperature treatment; vacuum drying temperature not restated for 5-day replicate
Time120 h treatment
Oxidant / reductantammonia base
ActivationDried under vacuum, as indicated for time-dependent FTIR samples.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1 crystalsNot specified2 · Experimental - Synthesis
Baseaqueous ammonia0.43%, pH 11.42 · Experimental - Synthesis
Complete recipeSource: Main

Route 4: Other

2 · Experimental - Synthesis

Metal precursorsCompound 2 ammonia-treated Cu-trithiocyanurate monolith
Linker precursorstrithiocyanurate framework in compound 2
Atmospherevacuum
Temperature130
Time>6
ActivationVacuum drying at 130 deg C for >6 h to remove H2O/NH3 and form compound 3.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Othercompound 2Not specified2 · Experimental - Synthesis