cMOF Evidence Base

Synthesis evidence

Size-Dependent Properties of Solution-Processable Conductive MOF Nanocrystals

Marshall C.R., Dvorak J.P., Twight L.P. et al. · Journal of the American Chemical Society · 2022 · 5784-5794

6 structured synthesis routes

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

Vague recipeSource: SI

Route 1: Solvothermal

10 · S2 Discussion of Fe(TA)2 nanoparticle syntheses · Figure S7

Metal precursorscobalt precursor not specified in supplied text
Linker precursorstriazolate linker inferred from CoTA2
Additives1-methylimidazole, varied equivalents
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt sourcenot specified10 · S2 Discussion of Fe(TA)2 nanoparticle syntheses · Figure S7
Linkertriazolate linkernot specified10 · S2 Discussion of Fe(TA)2 nanoparticle syntheses · Figure S7
Additive1-methylimidazolevaried equivalents10 · S2 Discussion of Fe(TA)2 nanoparticle syntheses · Figure S7
Complete recipeSource: Main

Route 2: Solution Shearing

5792 · Preparation of Fe(TA)2 Nanoparticle Thin Films

SolventsDMF
Additives5 wt% carbon black and 5 wt% poly(vinylidene difluoride)
AtmosphereAir for the reported composite conductivity sample
Substrate orientationDoctor-bladed onto glass microscope slides.
Work-upDried overnight.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Other84 nm Fe(TA)2 nanoparticle suspensionoverall concentration 20 mg/mL5792 · Preparation of Fe(TA)2 Nanoparticle Thin Films
Additivecarbon black5 wt%5792 · Preparation of Fe(TA)2 Nanoparticle Thin Films
Additivepoly(vinylidene difluoride)5 wt%5792 · Preparation of Fe(TA)2 Nanoparticle Thin Films
SolventDMFNot specified5792 · Preparation of Fe(TA)2 Nanoparticle Thin Films
Complete recipeSource: Both

Route 3: Solvothermal

5791 · Experimental Methods

Metal precursorsanhydrous iron(II) chloride in DMF, same base conditions as 1-mIm route
Linker precursors1,2,3-triazole, typically 3 equiv
SolventsDMF
Additives5-bromo-1-methylimidazole, 1-benzyl-2-methylimidazole, n-butylamine or sodium formate; bromo and benzyl varied over the 1-mIm equivalent series; initial exploratory nBA and sodium formate used 1 equiv.
AtmosphereN2 unless stated otherwise
Temperature120
Time1.5
Work-upCentrifuged and washed with DMF as for standard route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous iron(II) chloride0.805 mmol in the standard scaled route · 0.0575 M5791 · Experimental Methods
Linker1,2,3-triazole2.42 mmol, 140 uL, 3 equiv5791 · Experimental Methods
Additive5-bromo-1-methylimidazole; 1-benzyl-2-methylimidazole; n-butylamine; sodium formatevaried; initial nBA and sodium formate 1 equiv · equivalents relative to FeCl25791 · Experimental Methods
SolventDMFNot specified5791 · Experimental Methods
Partial recipeSource: SI

Route 4: Solvothermal

7 · S2 Synthesis of Fe(TA)2 under different conditions

Metal precursorsiron(II) chloride
Linker precursors1,2,3-triazole
SolventsDMF
Additivesnone for bulk/no-modulator comparison
AtmosphereN2 unless stated otherwise
Temperature120
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceiron(II) chloride0.0575 M FeCl2 for the no-modulator comparison7 · S2 Synthesis of Fe(TA)2 under different conditions
Linker1,2,3-triazoleNot specified7 · S2 Synthesis of Fe(TA)2 under different conditions
SolventDMFNot specified7 · S2 Synthesis of Fe(TA)2 under different conditions
Complete recipeSource: Both

Route 5: Solvothermal

5791 · Experimental Methods

Metal precursorsanhydrous iron(II) chloride, 0.805 mmol, 0.0575 M in DMF
Linker precursors1,2,3-triazole, 2.42 mmol, 140 uL, 3 equiv
SolventsDMF, 14 mL
Additives1-methylimidazole, 3.5 uL (0.044 mmol, 0.055 equiv) to 700 uL (8.78 mmol, 10.9 equiv) relative to FeCl2
AtmosphereN2 glovebox; air-free conditions
Temperature120
Time1.5
Work-upImmediately centrifuged and washed twice with DMF after heating.
ActivationFor sorption only: washed with DMF, MeCN and DCM, dried under vacuum and degassed at 120 C for 24-48 h.
Scalability contextExploratory syntheses were on 2 mL scale; suitable conditions were scaled to 14 mL with no observed changes in crystallite or SEM sizes.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous iron(II) chloride0.805 mmol · 0.0575 M5791 · Experimental Methods
Linker1,2,3-triazole2.42 mmol, 140 uL, 3 equiv5791 · Experimental Methods
SolventN,N-dimethylformamide (DMF)14 mL5791 · Experimental Methods
Additive1-methylimidazole3.5 uL to 700 uL; 0.044 to 8.78 mmol · 0.055 to 10.9 equiv vs FeCl25791 · Experimental Methods
Complete recipeSource: Main

Route 6: Solution Shearing

5792 · Preparation of Fe(TA)2 Nanoparticle Thin Films

SolventsDMF
Additivesnone for pristine films
AtmosphereFilms made both in N2-filled glovebox and in air
Substrate orientationGlass microscope slides taped with electrical tape; 200 uL aliquot doctor-bladed.
Work-upSamples dried overnight; N2-fabricated samples additionally dried under vacuum for at least 1 h.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherFe(TA)2 nanoparticle or bulk powder dispersion200 uL aliquot · initial tests 20 mg/mL; most slightly diluted5792 · Preparation of Fe(TA)2 Nanoparticle Thin Films
SolventDMFNot specified5792 · Preparation of Fe(TA)2 Nanoparticle Thin Films