cMOF Evidence Base

Synthesis evidence

Redox-Active Two-Dimensional Tetrathiafulvalene-Copper Metal-Organic Framework with Boosted Electrochemical Performances for Supercapatteries

Zhang Z.-R., Ren Z.-H., Luo C.-Y. et al. · Inorganic Chemistry · 2023 · 4672-4679

5 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

p006 / 4677 · 4.1. Preparation of Compounds

Metal precursorspreformed crystals of 1 (5 mg)
Atmospheresealed large screw-capped vial containing iodine vapour
Temperatureroom temperature
Time48
Oxidant / reductantiodine chips; iodine vapour oxidation
Work-upblack crystals kept under vacuum overnight
Activationvacuum overnight
Scalability contextMass increased from 5 mg to ca. 9 mg.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercrystals of 15 mgp006 / 4677 · 4.1. Preparation of Compounds
Oxidantiodine chipssome iodine chipsp006 / 4677 · 4.1. Preparation of Compounds
Complete recipeSource: Main

Route 2: Other

p006 / 4677 · 4.1. Preparation of Compounds

Metal precursors1-ox black crystals
Solventshexane wash
Atmospherevacuum drying
Temperature60
Timeovernight
Oxidant / reductantiodine retained as I3-; excess physisorbed iodine removed
Work-uprepeatedly washed with hexane and kept overnight under vacuum at 60 C
Activationvacuum at 60 C overnight
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Other1-ox black crystalsNot specifiedp006 / 4677 · 4.1. Preparation of Compounds
Solventhexanerepeated washingp006 / 4677 · 4.1. Preparation of Compounds
Complete recipeSource: Main

Route 3: Solvothermal

p006 / 4677 · 4.1. Preparation of Compounds

Metal precursorsCuSCN (0.6 mg, 0.005 mmol)
Linker precursorsTTF(py)4 (1.3 mg, 0.0025 mmol)
SolventsDMF (0.80 mL), CH3CN (0.80 mL), MeOH (0.05 mL); volume ratio 16/16/1
Additivesmaleic acid (0.6 mg, 0.005 mmol)
Atmospheresealed thick glass tube; atmosphere not otherwise specified
Temperature120
Time168
Work-upcooled to room temperature; maroon crystals hand-picked under a microscope
Scalability contextYield 0.8 mg, 46.2% based on py-TTF-py; alternative CuI or Cu(ClO4)2 gave very low yield.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSCN0.6 mg, 0.005 mmolp006 / 4677 · 4.1. Preparation of Compounds
LinkerTTF(py)41.3 mg, 0.0025 mmolp006 / 4677 · 4.1. Preparation of Compounds
Acidmaleic acid0.6 mg, 0.005 mmolp006 / 4677 · 4.1. Preparation of Compounds
SolventDMF0.80 mLp006 / 4677 · 4.1. Preparation of Compounds
SolventCH3CN0.80 mLp006 / 4677 · 4.1. Preparation of Compounds
SolventMeOH0.05 mLp006 / 4677 · 4.1. Preparation of Compounds
Complete recipeSource: SI

Route 4: Drop Cast

p005-p006 / SI · 1.3 Electrochemical measurements

Metal precursorsprepared MOF sample (1, 1-ox or 1-ox')
Solventsethanol
AdditivesSuper P and PTFE
Atmosphereroom temperature; drying under vacuum
Temperatureroom temperature
Time12 h vacuum drying after coating
Substrate orientationnickel foam, 1.0 cm x 1.0 cm area for three-electrode tests; 0.5 cm x 0.5 cm for two-electrode tests
Work-upnickel foam ultrasonicated in acetone, then 0.1 M HCl, vacuum dried; electrode compacted at 10 MPa
Activationvacuum dried for 12 h
Scalability contextMOF loading controlled to 2.5 mg cm^-2.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Otherprepared MOFloading mass controlled to 2.5 mg cm^-2p005-p006 / SI · 1.3 Electrochemical measurements
AdditiveSuper Pweight ratio MOF:Super P:PTFE = 8:1:1p005-p006 / SI · 1.3 Electrochemical measurements
AdditivePTFEweight ratio MOF:Super P:PTFE = 8:1:1p005-p006 / SI · 1.3 Electrochemical measurements
SolventethanolNot specifiedp005-p006 / SI · 1.3 Electrochemical measurements
Othernickel foam1.5 cm x 1.0 cm cut piecep005-p006 / SI · 1.3 Electrochemical measurements
Partial recipeSource: SI

Route 5: Other

p006 / SI · 1.3 Electrochemical measurements · Eq. S1

Metal precursors1-ox or 1-ox' positive electrode
Solvents6.0 M KOH electrolyte
Additivesactivated carbon negative electrode; fibre paper separator
Atmosphereroom temperature electrochemical assembly
Temperatureroom temperature
Work-upmass ratio of positive and negative electrodes selected to maintain charge equilibrium q+ = q-
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Other1-ox or 1-ox' positive electrodeNot specifiedp006 / SI · 1.3 Electrochemical measurements · Eq. S1
Otheractivated carbonNot specifiedp006 / SI · 1.3 Electrochemical measurements · Eq. S1
ElectrolyteKOH6.0 Mp006 / SI · 1.3 Electrochemical measurements · Eq. S1
Otherfibre paper separatorNot specifiedp006 / SI · 1.3 Electrochemical measurements · Eq. S1