cMOF Evidence Base

Synthesis evidence

Highly Electroconductive Metal-Organic Framework: Tunable by Metal Ion Sorption Quantity

Rouhani F., Rafizadeh-Masuleh F., Morsali A. · Journal of the American Chemical Society · 2019 · 11173-11182

7 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

7 · Study of the Effect of Other Metal Ions on TMU-60 Conductivity · Table S5

Metal precursorsZn(II), Co(II), Cu(II), or Pb(II) aqueous solutions
Solventswater
Atmosphereambient aqueous
Time3 times longer exposure than Cd test
ActivationUses activated TMU-60.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Metal SourceZn(II), Co(II), Cu(II), Pb(II) solutions10 times Cd concentration7 · Study of the Effect of Other Metal Ions on TMU-60 Conductivity · Table S5
Complete recipeSource: Both

Route 2: Other

8 · Methods - Activation of TMU-60

SolventsCH2Cl2
Atmosphereair for solvent exchange; alternative vacuum treatment
Temperature120 C; alternative 200 C
Time48 h CH2Cl2 exchange; 24 h at 120 C; alternative 4 h at 200 C under vacuum
Work-upFiltered after CH2Cl2 exchange.
ActivationCrystals immersed in CH2Cl2 for 48 h; solvent refreshed every 12 h; filtered; kept at 120 C for 24 h.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
SolventCH2Cl2Not specified8 · Methods - Activation of TMU-60
Complete recipeSource: Main

Route 3: Other

7 · Direct Current I-V Measurement · Figure 9

Atmospheredry pellet; ambient four-probe measurement
Temperature200 C post-preparation storage
Time4 h
Work-upPressed Cd2+-adsorbed MOF pellet, 1 cm diameter and 0.2 mm thickness.
ActivationUses TMU-60-Cd prepared by Cd(II) sorption.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherTMU-60-CdNot specified7 · Direct Current I-V Measurement · Figure 9
Complete recipeSource: Both

Route 4: Other

3 · Sorption Studies

Metal precursorsCd(NO3)2 aqueous solution
Solventswater
Atmosphereambient aqueous
Temperatureroom temperature / ambient
Time10 min for reported sorption preparation; kinetic studies varied 1-120 min
Work-upCentrifuged, washed with water to remove unsorbed Cd(II).
ActivationUses activated TMU-60.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2 aqueous solution50 mL · 50 ppm3 · Sorption Studies
Otheractivated TMU-6015 mg3 · Sorption Studies
Solventwater50 mL solution3 · Sorption Studies
Complete recipeSource: Both

Route 5: Other

4 · Sorption Studies · Figure S5

AdditivesPVDF binder
Atmosphereambient
Work-upGround activated TMU-60 mixed with PVDF and compressed into paste-electrode hole.
ActivationUses activated TMU-60.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othergrinded activated TMU-6010 mg4 · Sorption Studies · Figure S5
AdditivePVDF1 mg4 · Sorption Studies · Figure S5
Complete recipeSource: Main

Route 6: Other

7 · Direct Current I-V Measurement · Figure 9

Atmospheredry pellet; ambient four-probe measurement
Temperature200 C post-preparation storage
Time4 h
Work-upPressed polycrystalline pellet, 1 cm diameter and 0.2 mm thickness.
ActivationActivated dry TMU-60 pellet.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otheractivated pristine TMU-60Not specified7 · Direct Current I-V Measurement · Figure 9
Partial recipeSource: Both

Route 7: Solvothermal

8 · Methods - Synthesis of TMU-60 [Zn(OBA)(L*).DMF]

Metal precursorsZn(NO3)2.4H2O
Linker precursors4,4'-oxybis(benzoic acid) (H2OBA); N1,N2-bis(pyridin-4-ylmethylene)ethane-1,2-diamine (L) as pillar precursor to in situ L*
SolventsDMF (reported as 15 mg in main text; likely volume/amount as printed)
Atmospheresealed Teflon autoclave; absence of oxygen in autoclave discussed
Temperature60 C dissolution, then 120 C solvothermal
Time72 h at 120 C; cooled to ambient over 24 h
Work-upRed crystals filtered, washed with DMF and three times with ethanol, dried in air; yield about 20%.
ActivationSeparate solvent exchange/thermal activation route before sorption and measurements.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.4H2Oequivalent molar ratio8 · Methods - Synthesis of TMU-60 [Zn(OBA)(L*).DMF]
Linker4,4'-oxybis(benzoic acid) (H2OBA)equivalent molar ratio8 · Methods - Synthesis of TMU-60 [Zn(OBA)(L*).DMF]
LinkerN1,N2-bis(pyridin-4-ylmethylene)ethane-1,2-diamine (L)equivalent molar ratio8 · Methods - Synthesis of TMU-60 [Zn(OBA)(L*).DMF]
SolventDMF15 mg8 · Methods - Synthesis of TMU-60 [Zn(OBA)(L*).DMF]