cMOF Evidence Base

Synthesis evidence

Cation-dependent intrinsic electrical conductivity in isostructural tetrathiafulvalene-based microporous metal-organic frameworks

Park S.S., Hontz E.R., Sun L. et al. · Journal of the American Chemical Society · 2015 · 1774-1777

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

p003 / SI p.S3 · Synthesis of Cd2(TTFTB)

Metal precursorsCd(NO3)2·4H2O (172 mg, 0.558 mmol)
Linker precursorsH4TTFTB (103 mg, 0.154 mmol)
Solvents1:1 water/ethanol (12 ml) for metal solution; 3:1 DMF/ethanol (8.4 ml) for linker solution; DMF and ethanol washes
Atmospherenot specified; 20 mL scintillation vial
Temperature75
Time72
Work-upCollected by filtration and washed with DMF (30 ml) and ethanol (30 ml)
ActivationEvacuated at 220 C for 24 h at 4 mtorr for activated elemental-analysis/desolvated sample
Scalability contextReaction afforded 122 mg product, 73% yield; no scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2·4H2O172 mg, 0.558 mmolp003 / SI p.S3 · Synthesis of Cd2(TTFTB)
LinkerH4TTFTB103 mg, 0.154 mmolp003 / SI p.S3 · Synthesis of Cd2(TTFTB)
Solventwater/ethanol12 ml, 1:1p003 / SI p.S3 · Synthesis of Cd2(TTFTB)
SolventDMF/ethanol8.4 ml, 3:1p003 / SI p.S3 · Synthesis of Cd2(TTFTB)
SolventDMF30 ml washp003 / SI p.S3 · Synthesis of Cd2(TTFTB)
Solventethanol30 ml washp003 / SI p.S3 · Synthesis of Cd2(TTFTB)
Complete recipeSource: Both

Route 2: Solvothermal

p003 / SI p.S3 · Synthesis of Co2(TTFTB)

Metal precursorsCo(NO3)2·6H2O (77 mg, 0.27 mmol)
Linker precursorsH4TTFTB (50. mg, 0.073 mmol)
Solvents1:1 water/ethanol (8 ml) for metal solution; 3:1 DMF/ethanol (8 ml) for linker solution; DMF and ethanol washes
Atmospherenot specified; 20 mL scintillation vial
Temperature75
Time72
Work-upCollected by filtration and washed with DMF (20 ml) and ethanol (20 ml)
ActivationEvacuated at 200 C for 12 h at 4 mtorr for activated elemental-analysis/desolvated sample
Scalability contextReaction afforded 55 mg product, 75% yield; no scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)2·6H2O77 mg, 0.27 mmolp003 / SI p.S3 · Synthesis of Co2(TTFTB)
LinkerH4TTFTB50. mg, 0.073 mmolp003 / SI p.S3 · Synthesis of Co2(TTFTB)
Solventwater/ethanol8 ml, 1:1p003 / SI p.S3 · Synthesis of Co2(TTFTB)
SolventDMF/ethanol8 ml, 3:1p003 / SI p.S3 · Synthesis of Co2(TTFTB)
SolventDMF20 ml washp003 / SI p.S3 · Synthesis of Co2(TTFTB)
Solventethanol20 ml washp003 / SI p.S3 · Synthesis of Co2(TTFTB)
Complete recipeSource: Both

Route 3: Solvothermal

p003 / SI p.S3 · Synthesis of Mn2(TTFTB)

Metal precursorsMn(NO3)2·xH2O (67 mg, 0.27 mmol)
Linker precursorsH4TTFTB (50. mg, 0.073 mmol)
Solvents1:1 water/ethanol (8 ml) for metal solution; 3:1 DMF/ethanol (8 ml) for linker solution; DMF and ethanol washes
Atmospherenot specified; 20 mL scintillation vial
Temperature75
Time72
Work-upCollected by filtration and washed with DMF (20 ml) and ethanol (20 ml)
ActivationEvacuated at 200 C for 12 h at 4 mtorr for activated elemental-analysis/desolvated sample
Scalability contextReaction afforded 56 mg product, 84% yield; no scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMn(NO3)2·xH2O67 mg, 0.27 mmolp003 / SI p.S3 · Synthesis of Mn2(TTFTB)
LinkerH4TTFTB50. mg, 0.073 mmolp003 / SI p.S3 · Synthesis of Mn2(TTFTB)
Solventwater/ethanol8 ml, 1:1p003 / SI p.S3 · Synthesis of Mn2(TTFTB)
SolventDMF/ethanol8 ml, 3:1p003 / SI p.S3 · Synthesis of Mn2(TTFTB)
SolventDMF20 ml washp003 / SI p.S3 · Synthesis of Mn2(TTFTB)
Solventethanol20 ml washp003 / SI p.S3 · Synthesis of Mn2(TTFTB)
Partial recipeSource: Both

Route 4: Unknown

p003 / SI p.S3 · Materials

Metal precursorsZn(NO3)2; exact hydrate/amount not reproduced in this paper
Linker precursorsH4TTFTB; exact amount not reproduced in this paper
Solventsnot reproduced in this paper
Atmospherenot reproduced in this paper
Work-upnot reproduced in this paper
Activationnot reproduced in this paper; Zn reference surface area cited as 537 m2/mmol
Scalability contextSI notes Zn2(TTFTB) crystals are commonly shorter than 300 um in this study.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2not specifiedp003 / SI p.S3 · Materials
LinkerH4TTFTBnot specifiedp003 / SI p.S3 · Materials