cMOF Evidence Base

Synthesis evidence

A family of lanthanide metal-organic frameworks based on a redox-active tetrathiafulvalene-dicarboxylate ligand showing slow relaxation of magnetisation and electronic conductivity

Hu J.-J., Li Y.-G., Wen H.-R. et al. · Dalton Transactions · 2021 · 14714-14723

8 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Solvothermal

14715 · Synthesis and characterization · Scheme 1

Metal precursorsDy(NO3)3.6H2O, 90 mg
Linker precursors(TTF-TC)H4, 56 mg; in situ decomposes to TTF-DC
Solvents10 mL DMF/H2O, v/v = 7:3
AdditivesO-fluorobenzoic acid, 105 mg
Atmospherenot specified
Temperature120
Time72
Work-upcooled to room temperature; red transparent crystals filtered and washed with DMF
Activationnot specified
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceDy(NO3)3.6H2O90 mg14715 · Synthesis and characterization · Scheme 1
Linker(TTF-TC)H456 mg14715 · Synthesis and characterization · Scheme 1
AcidO-fluorobenzoic acid105 mg14715 · Synthesis and characterization · Scheme 1
SolventDMF/H2O (v/v = 7:3)10 mL14715 · Synthesis and characterization · Scheme 1
Complete recipeSource: Main

Route 2: Solvothermal

14715 · Synthesis and characterization · Scheme 1

Metal precursorsEr(NO3)3.6H2O, 90 mg
Linker precursors(TTF-TC)H4, 56 mg; in situ decomposes to TTF-DC
Solvents10 mL DMF/H2O, v/v = 7:3
AdditivesO-fluorobenzoic acid, 105 mg
Atmospherenot specified
Temperature120
Time72
Work-upcooled to room temperature; red transparent crystals filtered and washed with DMF
Activationnot specified
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceEr(NO3)3.6H2O90 mg14715 · Synthesis and characterization · Scheme 1
Linker(TTF-TC)H456 mg14715 · Synthesis and characterization · Scheme 1
AcidO-fluorobenzoic acid105 mg14715 · Synthesis and characterization · Scheme 1
SolventDMF/H2O (v/v = 7:3)10 mL14715 · Synthesis and characterization · Scheme 1
Complete recipeSource: Main

Route 3: Solvothermal

14715 · Synthesis and characterization · Scheme 1

Metal precursorsGd(NO3)3.6H2O, 90 mg
Linker precursors(TTF-TC)H4, 56 mg; in situ decomposes to TTF-DC
Solvents10 mL DMF/H2O, v/v = 7:3
AdditivesO-fluorobenzoic acid, 105 mg
Atmospherenot specified
Temperature120
Time72
Work-upcooled to room temperature; red transparent crystals filtered and washed with DMF
Activationnot specified
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceGd(NO3)3.6H2O90 mg14715 · Synthesis and characterization · Scheme 1
Linker(TTF-TC)H456 mg14715 · Synthesis and characterization · Scheme 1
AcidO-fluorobenzoic acid105 mg14715 · Synthesis and characterization · Scheme 1
SolventDMF/H2O (v/v = 7:3)10 mL14715 · Synthesis and characterization · Scheme 1
Complete recipeSource: Main

Route 4: Solvothermal

14715 · Synthesis and characterization · Scheme 1

Metal precursorsTb(NO3)3.6H2O, 90 mg
Linker precursors(TTF-TC)H4, 56 mg; in situ decomposes to TTF-DC
Solvents10 mL DMF/H2O, v/v = 7:3
AdditivesO-fluorobenzoic acid, 105 mg
Atmospherenot specified
Temperature120
Time72
Work-upcooled to room temperature; red transparent crystals filtered and washed with DMF
Activationnot specified
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceTb(NO3)3.6H2O90 mg14715 · Synthesis and characterization · Scheme 1
Linker(TTF-TC)H456 mg14715 · Synthesis and characterization · Scheme 1
AcidO-fluorobenzoic acid105 mg14715 · Synthesis and characterization · Scheme 1
SolventDMF/H2O (v/v = 7:3)10 mL14715 · Synthesis and characterization · Scheme 1
Complete recipeSource: Main

Route 5: Other

14715-14716 · Syntheses of 2-Ln

Metal precursors1-Dy
Linker precursorsTTF-DC framework in 1-Dy
Solventscyclohexane
Atmospherenot specified
Temperatureroom temperature
Time48
Oxidant / reductantiodine, 0.1 M in cyclohexane
Work-upseparated and washed with cyclohexane to remove excess/surface iodine
Activationnot specified
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other1-DyNot specified14715-14716 · Syntheses of 2-Ln
Oxidantiodine0.1 M14715-14716 · Syntheses of 2-Ln
SolventcyclohexaneNot specified14715-14716 · Syntheses of 2-Ln
Complete recipeSource: Main

Route 6: Other

14715-14716 · Syntheses of 2-Ln

Metal precursors1-Er
Linker precursorsTTF-DC framework in 1-Er
Solventscyclohexane
Atmospherenot specified
Temperatureroom temperature
Time48
Oxidant / reductantiodine, 0.1 M in cyclohexane
Work-upseparated and washed with cyclohexane to remove excess/surface iodine
Activationnot specified
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other1-ErNot specified14715-14716 · Syntheses of 2-Ln
Oxidantiodine0.1 M14715-14716 · Syntheses of 2-Ln
SolventcyclohexaneNot specified14715-14716 · Syntheses of 2-Ln
Complete recipeSource: Both

Route 7: Other

14715 · Syntheses of 2-Ln · Table S3

Metal precursors1-Gd
Linker precursorsTTF-DC framework in 1-Gd
Solventscyclohexane
Atmospherenot specified
Temperatureroom temperature
Time48
Oxidant / reductantiodine, 0.1 M in cyclohexane
Work-upseparated and washed with cyclohexane to remove excess/surface iodine
Activationnot specified
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other1-GdNot specified14715 · Syntheses of 2-Ln · Table S3
Oxidantiodine0.1 M14715 · Syntheses of 2-Ln · Table S3
SolventcyclohexaneNot specified14715 · Syntheses of 2-Ln · Table S3
Complete recipeSource: Main

Route 8: Other

14715-14716 · Syntheses of 2-Ln

Metal precursors1-Tb
Linker precursorsTTF-DC framework in 1-Tb
Solventscyclohexane
Atmospherenot specified
Temperatureroom temperature
Time48
Oxidant / reductantiodine, 0.1 M in cyclohexane
Work-upseparated and washed with cyclohexane to remove excess/surface iodine
Activationnot specified
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other1-TbNot specified14715-14716 · Syntheses of 2-Ln
Oxidantiodine0.1 M14715-14716 · Syntheses of 2-Ln
SolventcyclohexaneNot specified14715-14716 · Syntheses of 2-Ln