cMOF Evidence Base

Synthesis evidence

Efficient and tunable one-dimensional charge transport in layered lanthanide metal–organic frameworks

Skorupskii G., Trump B.A., Kasel T.W. et al. · Nature Chemistry · 2020 · 131-136

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

main p.134 · Methods - Synthesis of LnHHTP

Metal precursorsHo(NO3)3.6H2O
Linker precursorsH6HHTP, 0.063 mmol (1.0 equiv., 20 mg), recrystallised before use
Solvents3.0 ml deionised water for metal nitrate; 0.4 ml DMI for H6HHTP; 0.6 ml deionised water for sodium acetate
AdditivesAnhydrous sodium acetate, 0.189 mmol (3.0 equiv., 15 mg)
AtmosphereReaction assembled in air; workup and storage in dry N2-filled glove box with degassed wash solvents.
Temperature80
Time16
Oxidant / reductantNo discrete oxidant/reductant reported; acetate used as additive/base.
Work-upCollect precipitate by centrifugation; transfer to N2-filled glove box containing water vapour; soak four times for at least 30 min in degassed deionised water and four times for at least 30 min in degassed acetone.
ActivationDry in vacuo on Schlenk line for 1 h at 90 deg C; for elemental analysis and N2 adsorption dry overnight under same conditions.
Scalability context20 ml scintillation-vial batch using 20 mg linker; no scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceHo(NO3)3.6H2O0.629 mmol (10.0 equiv.) · in 3.0 ml deionised watermain p.134 · Methods - Synthesis of LnHHTP
LinkerH6HHTP0.063 mmol (1.0 equiv., 20 mg) · in 0.4 ml DMImain p.134 · Methods - Synthesis of LnHHTP
Solventdeionised water3.0 ml + 0.6 mlmain p.134 · Methods - Synthesis of LnHHTP
SolventN,N'-dimethylimidazolidinone (DMI)0.4 mlmain p.134 · Methods - Synthesis of LnHHTP
Baseanhydrous sodium acetate0.189 mmol (3.0 equiv., 15 mg) · in 0.6 ml deionised watermain p.134 · Methods - Synthesis of LnHHTP
Solventacetonefour soaking washes, at least 30 min each · degassedmain p.134 · Methods - Synthesis of LnHHTP
Complete recipeSource: Both

Route 2: Solvothermal

main p.134 · Methods - Synthesis of LnHHTP

Metal precursorsLa(NO3)3.6H2O
Linker precursorsH6HHTP, 0.063 mmol (1.0 equiv., 20 mg), recrystallised before use
Solvents3.0 ml deionised water for metal nitrate; 0.4 ml DMI for H6HHTP; 0.6 ml deionised water for sodium acetate
AdditivesAnhydrous sodium acetate, 0.189 mmol (3.0 equiv., 15 mg)
AtmosphereReaction assembled in air; workup and storage in dry N2-filled glove box with degassed wash solvents.
Temperature80
Time16
Oxidant / reductantNo discrete oxidant/reductant reported; acetate used as additive/base.
Work-upCollect precipitate by centrifugation; transfer to N2-filled glove box containing water vapour; soak four times for at least 30 min in degassed deionised water and four times for at least 30 min in degassed acetone.
ActivationDry in vacuo on Schlenk line for 1 h at 90 deg C; for elemental analysis and N2 adsorption dry overnight under same conditions.
Scalability context20 ml scintillation-vial batch using 20 mg linker; no scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLa(NO3)3.6H2O0.629 mmol (10.0 equiv.) · in 3.0 ml deionised watermain p.134 · Methods - Synthesis of LnHHTP
LinkerH6HHTP0.063 mmol (1.0 equiv., 20 mg) · in 0.4 ml DMImain p.134 · Methods - Synthesis of LnHHTP
Solventdeionised water3.0 ml + 0.6 mlmain p.134 · Methods - Synthesis of LnHHTP
SolventN,N'-dimethylimidazolidinone (DMI)0.4 mlmain p.134 · Methods - Synthesis of LnHHTP
Baseanhydrous sodium acetate0.189 mmol (3.0 equiv., 15 mg) · in 0.6 ml deionised watermain p.134 · Methods - Synthesis of LnHHTP
Solventacetonefour soaking washes, at least 30 min each · degassedmain p.134 · Methods - Synthesis of LnHHTP
Complete recipeSource: Both

Route 3: Solvothermal

main p.134 · Methods - Synthesis of LnHHTP

Metal precursorsNd(NO3)3.6H2O
Linker precursorsH6HHTP, 0.063 mmol (1.0 equiv., 20 mg), recrystallised before use
Solvents3.0 ml deionised water for metal nitrate; 0.4 ml DMI for H6HHTP; 0.6 ml deionised water for sodium acetate
AdditivesAnhydrous sodium acetate, 0.189 mmol (3.0 equiv., 15 mg)
AtmosphereReaction assembled in air; workup and storage in dry N2-filled glove box with degassed wash solvents.
Temperature80
Time16
Oxidant / reductantNo discrete oxidant/reductant reported; acetate used as additive/base.
Work-upCollect precipitate by centrifugation; transfer to N2-filled glove box containing water vapour; soak four times for at least 30 min in degassed deionised water and four times for at least 30 min in degassed acetone.
ActivationDry in vacuo on Schlenk line for 1 h at 90 deg C; for elemental analysis and N2 adsorption dry overnight under same conditions.
Scalability context20 ml scintillation-vial batch using 20 mg linker; no scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNd(NO3)3.6H2O0.629 mmol (10.0 equiv.) · in 3.0 ml deionised watermain p.134 · Methods - Synthesis of LnHHTP
LinkerH6HHTP0.063 mmol (1.0 equiv., 20 mg) · in 0.4 ml DMImain p.134 · Methods - Synthesis of LnHHTP
Solventdeionised water3.0 ml + 0.6 mlmain p.134 · Methods - Synthesis of LnHHTP
SolventN,N'-dimethylimidazolidinone (DMI)0.4 mlmain p.134 · Methods - Synthesis of LnHHTP
Baseanhydrous sodium acetate0.189 mmol (3.0 equiv., 15 mg) · in 0.6 ml deionised watermain p.134 · Methods - Synthesis of LnHHTP
Solventacetonefour soaking washes, at least 30 min each · degassedmain p.134 · Methods - Synthesis of LnHHTP
Complete recipeSource: Both

Route 4: Solvothermal

main p.134 · Methods - Synthesis of LnHHTP

Metal precursorsYb(NO3)3.6H2O
Linker precursorsH6HHTP, 0.063 mmol (1.0 equiv., 20 mg), recrystallised before use
Solvents3.0 ml deionised water for metal nitrate; 0.4 ml DMI for H6HHTP; 0.6 ml deionised water for sodium acetate
AdditivesAnhydrous sodium acetate, 0.189 mmol (3.0 equiv., 15 mg)
AtmosphereReaction assembled in air; workup and storage in dry N2-filled glove box with degassed wash solvents.
Temperature80
Time16
Oxidant / reductantNo discrete oxidant/reductant reported; acetate used as additive/base.
Work-upCollect precipitate by centrifugation; transfer to N2-filled glove box containing water vapour; soak four times for at least 30 min in degassed deionised water and four times for at least 30 min in degassed acetone.
ActivationDry in vacuo on Schlenk line for 1 h at 90 deg C; for elemental analysis and N2 adsorption dry overnight under same conditions.
Scalability context20 ml scintillation-vial batch using 20 mg linker; no scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceYb(NO3)3.6H2O0.629 mmol (10.0 equiv.) · in 3.0 ml deionised watermain p.134 · Methods - Synthesis of LnHHTP
LinkerH6HHTP0.063 mmol (1.0 equiv., 20 mg) · in 0.4 ml DMImain p.134 · Methods - Synthesis of LnHHTP
Solventdeionised water3.0 ml + 0.6 mlmain p.134 · Methods - Synthesis of LnHHTP
SolventN,N'-dimethylimidazolidinone (DMI)0.4 mlmain p.134 · Methods - Synthesis of LnHHTP
Baseanhydrous sodium acetate0.189 mmol (3.0 equiv., 15 mg) · in 0.6 ml deionised watermain p.134 · Methods - Synthesis of LnHHTP
Solventacetonefour soaking washes, at least 30 min each · degassedmain p.134 · Methods - Synthesis of LnHHTP