cMOF Evidence Base

Synthesis evidence

Porous lanthanide metal–organic frameworks with metallic conductivity

Skorupskii G., Le K.N., Cordova D.L.M. et al. · Proceedings of the National Academy of Sciences of the United States of America · 2022 · e2205127119

2 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

p005-p006 · Materials and Methods · Typical Synthesis

Metal precursorsLa(NO3)3 . 6 H2O
Linker precursorsH6HOTP; commercial recrystallized twice from hot DMA or synthesized in-house if commercial quality was unsatisfactory
SolventsN,N-dimethylacetamide; deoxygenated water; workup/washes with deoxygenated water and methanol, optionally dichloromethane or diethyl ether
AdditivesSanded borosilicate glass rods used as nucleation sites; DMA hydrolysis produces base in situ
AtmosphereN2-filled glovebox; deoxygenated solvents; pressure tube sealed before heating
Temperature90 degC dissolution; 135 degC reaction
Time72 h at 135 degC; cool to room temperature over 8 h; water washes include at least one 24 h soak
Substrate orientationSanded borosilicate glass rods as nucleation surfaces, not oriented substrates
Oxidant / reductantNo deliberate oxidant/reductant; N2 atmosphere used to prevent linker overoxidation and cation deficiency
Work-upOpened in N2 glovebox; mother liquor removed; crystals transferred into deoxygenated water; four water soaks, then methanol and sometimes dichloromethane or diethyl ether soaks
ActivationFor elemental analysis, samples activated at 90 degC for 24 h in vacuo; conductivity samples measured after solvent washes and stored under solvent
Scalability contextReaction uses commercially available precursors and accessible conditions; single-crystal growth relies on pressure tubes and nucleation rods.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLa(NO3)3 . 6 H2O4,156.9 mg; 9.600 mmol; 160 equivp005-p006 · Materials and Methods · Typical Synthesis
LinkerH6HOTP19.5 mg · 0.060 mmol, 1 equivp005-p006 · Materials and Methods · Typical Synthesis
SolventN,N-dimethylacetamide (DMA)0.7 mLp005-p006 · Materials and Methods · Typical Synthesis
Solventdeoxygenated water6 mLp005-p006 · Materials and Methods · Typical Synthesis
Additivesanded borosilicate glass rodsnot specified · nucleation sitesp005-p006 · Materials and Methods · Typical Synthesis
Complete recipeSource: Both

Route 2: Solvothermal

p005-p006 · Materials and Methods · Typical Synthesis

Metal precursorsNd(NO3)3 . 6 H2O
Linker precursorsH6HOTP; commercial recrystallized twice from hot DMA or synthesized in-house if commercial quality was unsatisfactory
SolventsN,N-dimethylacetamide; deoxygenated water; workup/washes with deoxygenated water and methanol, optionally dichloromethane or diethyl ether
AdditivesSanded borosilicate glass rods used as nucleation sites; DMA hydrolysis produces base in situ
AtmosphereN2-filled glovebox; deoxygenated solvents; pressure tube sealed before heating
Temperature90 degC dissolution; 135 degC reaction
Time72 h at 135 degC; cool to room temperature over 8 h; water washes include at least one 24 h soak
Substrate orientationSanded borosilicate glass rods as nucleation surfaces, not oriented substrates
Oxidant / reductantNo deliberate oxidant/reductant; N2 atmosphere used to prevent linker overoxidation and cation deficiency
Work-upOpened in N2 glovebox; mother liquor removed; crystals transferred into deoxygenated water; four water soaks, then methanol and sometimes dichloromethane or diethyl ether soaks
ActivationFor elemental analysis, samples activated at 90 degC for 24 h in vacuo; conductivity samples measured after solvent washes and stored under solvent
Scalability contextReaction uses commercially available precursors and accessible conditions; single-crystal growth relies on pressure tubes and nucleation rods.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNd(NO3)3 . 6 H2O4,208.1 mg; 9.600 mmol; 160 equivp005-p006 · Materials and Methods · Typical Synthesis
LinkerH6HOTP19.5 mg · 0.060 mmol, 1 equivp005-p006 · Materials and Methods · Typical Synthesis
SolventN,N-dimethylacetamide (DMA)0.7 mLp005-p006 · Materials and Methods · Typical Synthesis
Solventdeoxygenated water6 mLp005-p006 · Materials and Methods · Typical Synthesis
Additivesanded borosilicate glass rodsnot specified · nucleation sitesp005-p006 · Materials and Methods · Typical Synthesis