Synthesis evidence

A New Electrically Conducting Metal–Organic Framework Featuring U-Shaped cis-Dipyridyl Tetrathiafulvalene Ligands

Gordillo M.A., Benavides P.A., Spalding K. et al. · Frontiers in Chemistry · 2021 · 726544

4 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

1-2 · MOF Pellets for Electrochemical Impedance and Electrical Conductivity Measurements

Metal precursorspreformed I2-treated sine-MOF powder
Linker precursorspreformed iodine-treated sine-MOF framework containing Z-DPTTF and TCPB
Additivessilver paint/coated stainless-steel rod tips as electrode contact material
Atmosphereambient for I-V measurement; pressing atmosphere not specified
Work-upPressed under 200 MPa in a Teflon tube between two silver-coated stainless-steel rods.
ActivationNot reported during pellet pressing.
Scalability contextDevice-scale pressed pellet made from 3.0 mg powder.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherI2-treated sine-MOF powder3.0 mg1-2 · MOF Pellets for Electrochemical Impedance and Electrical Conductivity Measurements
AdditiveAg-coated stainless-steel electrodes/rod tipstwo rods, diameter 2.7 mm1-2 · MOF Pellets for Electrochemical Impedance and Electrical Conductivity Measurements
Complete recipeSource: SI

Route 2: Other

1-2 · MOF Pellets for Electrochemical Impedance and Electrical Conductivity Measurements

Metal precursorspreformed pristine sine-MOF powder
Linker precursorspreformed sine-MOF framework containing Z-DPTTF and TCPB
Additivessilver paint/coated stainless-steel rod tips as electrode contact material
Atmosphereambient for I-V measurement; pressing atmosphere not specified
Work-upPressed under 200 MPa in a Teflon tube between two silver-coated stainless-steel rods.
ActivationNot reported during pellet pressing.
Scalability contextDevice-scale pressed pellet made from 3.0 mg powder.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otherpristine sine-MOF powder3.0 mg1-2 · MOF Pellets for Electrochemical Impedance and Electrical Conductivity Measurements
AdditiveAg-coated stainless-steel electrodes/rod tipstwo rods, diameter 2.7 mm1-2 · MOF Pellets for Electrochemical Impedance and Electrical Conductivity Measurements
Partial recipeSource: Both

Route 3: Other

2 · Preparation of I2 Doped sine-MOF

Metal precursorspreformed evacuated sine-MOF powder
Linker precursorspreformed sine-MOF framework containing Z-DPTTF and TCPB
Solventshexane for post-treatment washing
Atmosphereiodine vapour in sealed screw-capped vial
Time72
Oxidant / reductantI2 chips / iodine vapour oxidant
Work-upRemoved from I2 chamber, left open overnight, then washed thoroughly with hexane until wash solution was colourless.
ActivationNo additional activation reported after hexane washing.
Scalability contextSmall open vial inside larger screw-capped vial; iodine amount stated only as 'few I2 chips'.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherevacuated sine-MOF powdernot reported2 · Preparation of I2 Doped sine-MOF
OxidantI2 chipsfew I2 chips2 · Preparation of I2 Doped sine-MOF
Solventhexanewashed thoroughly until colourless2 · Preparation of I2 Doped sine-MOF
Partial recipeSource: Both

Route 4: Solvothermal

2 · Preparation of sine-MOF

Metal precursorsZn(NO3)2*6H2O (11.9 mg, 0.04 mmol)
Linker precursorsZ-DPTTF ligand (7.2 mg, 0.02 mmol); TCPB (11.2 mg, 0.02 mmol)
SolventsDMAc (2 mL for Z-DPTTF solution); 2:1 DMAc/H2O mixture (1.5 mL for Zn/TCPB solution); ethanolic HNO3 solution additive
Additives1 M HNO3 ethanolic solution (20 uL)
Atmospherenot reported
Temperature80
Time24
Work-upDark-red crystals obtained in 48% yield and used for SXRD; no detailed pristine washing conditions reported.
ActivationCorresponding evacuated powder used for electrical and optical measurements; evacuation temperature/time not reported in main text or supplied SI text.
Scalability contextSmall screw-capped vial synthesis on milligram scale; no scale-up reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2*6H2O11.9 mg, 0.04 mmol2 · Preparation of sine-MOF
LinkerZ-DPTTF ligand7.2 mg, 0.02 mmol2 · Preparation of sine-MOF
LinkerTCPB11.2 mg, 0.02 mmol2 · Preparation of sine-MOF
SolventDMAc2 mL plus part of 1.5 mL 2:1 DMAc/H2O mixture2 · Preparation of sine-MOF
SolventH2Opart of 1.5 mL 2:1 DMAc/H2O mixture · DMAc/H2O = 2:12 · Preparation of sine-MOF
AcidHNO3 ethanolic solution20 uL · 1 M2 · Preparation of sine-MOF