cMOF Evidence Base

Synthesis evidence

Heterometallic Actinide-Containing Photoresponsive Metal-Organic Frameworks: Dynamic and Static Tuning of Electronic Properties

Martin C.R., Leith G.A., Kittikhunnatham P. et al. · Angewandte Chemie - International Edition · 2021 · 8072-8080

8 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

S10 · Preparation of iodine-loaded frameworks

Metal precursorsfiltered MOF host
Linker precursorshost framework linkers
SolventsDMF wash
Additivesiodine crystals
Atmospheresealed 20 mL vial with iodine vapour
Temperatureroom temperature
Time72
Oxidant / reductantiodine
Work-upfiltered and washed with 2.0 mL DMF to remove surface iodine
Activationfiltered MOF in uncapped 0.5-dram vial
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherfiltered MOF8.0 mgS10 · Preparation of iodine-loaded frameworks
Oxidantiodine crystals0.10 g, 0.39 mmolS10 · Preparation of iodine-loaded frameworks
SolventDMF2.0 mL washS10 · Preparation of iodine-loaded frameworks
Complete recipeSource: SI

Route 2: Other

S11 · Preparation of tetracyanoquinodimethane-loaded frameworks

Metal precursorsfiltered MOF host
Linker precursorshost framework linkers
SolventsDMF
AdditivesTCNQ
Atmospheresealed vial
Temperature75
Time72
Oxidant / reductantTCNQ electron acceptor
Work-upfiltered and washed with 2.0 mL DMF to remove residual TCNQ
Activationfiltered MOF powder
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherfiltered MOF powder8.0 mgS11 · Preparation of tetracyanoquinodimethane-loaded frameworks
AdditiveTCNQ1.0 mL solution · 100 mMS11 · Preparation of tetracyanoquinodimethane-loaded frameworks
SolventDMF1.0 mL solution; 2.0 mL washS11 · Preparation of tetracyanoquinodimethane-loaded frameworks
Complete recipeSource: SI

Route 3: Drop Cast

S12-S13 · MOF-based field-effect transistor preparation · Scheme 1b

Metal precursorsTCNQ@Zr-65% MOF crystals
Linker precursorsMe2BPDC and TNDA2- in MOF
SolventsDMF
Substrate orientationheavily boron-doped Si wafer with 285 nm SiO2; Ti/Au electrodes
Work-upcontact confirmed by optical microscopy
ActivationSi wafer rinsed with isopropyl alcohol and water, dried with nitrogen, heated at 180 deg C for 5 min; Ti/Au electrodes fabricated by electron-beam evaporation
Scalability contextDevice demonstration only; radioactive Th/U frameworks were avoided for FET due to safety limitations.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMOF crystalssuspension in DMFS12-S13 · MOF-based field-effect transistor preparation · Scheme 1b
SolventDMFNot specifiedS12-S13 · MOF-based field-effect transistor preparation · Scheme 1b
OtherTi/Au electrodes on boron-doped Si/SiO2Ti 30 nm / Au 70 nmS12-S13 · MOF-based field-effect transistor preparation · Scheme 1b
Complete recipeSource: SI

Route 4: Other

S10 · Preparation of Th5U-MOF

Metal precursorsfreshly synthesized U-MOF; Th(NO3)4.H2O
Linker precursorsMe2BPDC in U-MOF
SolventsDMF
Temperatureroom temperature
Time48
Work-upwashed with DMF (5.0 mL); portion Soxhlet washed 3 d in DMF before ICP-MS
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceU-MOF36.0 mgS10 · Preparation of Th5U-MOF
Metal SourceTh(NO3)4.H2O1.00 mL · 0.170 MS10 · Preparation of Th5U-MOF
SolventDMFwash 5.0 mL; Soxhlet 3 dS10 · Preparation of Th5U-MOF
Partial recipeSource: Main

Route 5: Solvothermal

8074 · Results and Discussion

Metal precursorsTh(NO3)4
Linker precursorsH2Me2BPDC
SolventsDMF
Additivestrifluoroacetic acid
Temperature120
Time72
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceTh(NO3)4Not specified8074 · Results and Discussion
LinkerH2Me2BPDCNot specified8074 · Results and Discussion
SolventDMFNot specified8074 · Results and Discussion
Acidtrifluoroacetic acidNot specified8074 · Results and Discussion
Complete recipeSource: Both

Route 6: Other

S10 · Linker installation procedure

Metal precursorsfreshly synthesized Th-MOF, Zr-MOF, or Th5U-MOF
Linker precursorsH2TNDA
SolventsDMF
Atmosphereair dry before reaction; sealed/vial atmosphere not specified
Temperature75 for Zr-33% and Th-34%; 85 for Zr-65%, Th-65%, and Th5U-50%
Time72
Work-upcooled to room temperature, filtered, washed with DMF (5.0 mL)
Activationhost washed with DMF (1.0 mL) and dried in air 10 min before linker installation
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherfreshly synthesized Th-MOF, Zr-MOF, or Th5U-MOF8.0 mgS10 · Linker installation procedure
LinkerH2TNDA1.0 mL solution; 0.030 mmol · 0.030 MS10 · Linker installation procedure
SolventDMF1.0 mL reaction solution; 5.0 mL washS10 · Linker installation procedure
Vague recipeSource: SI

Route 7: Other

S6 · Materials

Metal precursorsuranium tetrachloride listed in materials; exact U-MOF recipe not reproduced
Linker precursorsH2Me2BPDC
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceuranium tetrachlorideNot specifiedS6 · Materials
LinkerH2Me2BPDCNot specifiedS6 · Materials
Vague recipeSource: SI

Route 8: Other

S6 · Materials

Metal precursorszirconium chloride listed in materials; exact parent Zr-MOF recipe not reproduced
Linker precursorsH2Me2BPDC
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezirconium chlorideNot specifiedS6 · Materials
LinkerH2Me2BPDCNot specifiedS6 · Materials