Synthesis · Conductive Lanthanide Metal-Organic Frameworks with Exceptionally High Stability

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

15 · MnO4 anion exchange studies · Figure S27

Metal precursorsas-synthesised Gd4-MOF crystals, 3 mg

Linker precursorsnot applicable; post-synthetic anion exchange

Solvents21 mL aqueous solution

Additivespotassium permanganate, 50 ppm

Atmosphere30 mL amber bottle; atmosphere not specified

Temperatureroom temperature not explicitly stated

Time168

Substrate orientationnot applicable

Oxidant / reductantKMnO4 / MnO4- oxidising medium

Work-upcentrifuged and washed with deionized water three times

Activationnone reported

Scalability contextanalytical post-synthetic exchange on 3 mg crystals

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Gd4-MOF crystals	3 mg	15 · MnO4 anion exchange studies · Figure S27
Oxidant	potassium permanganate	21 mL solution · 50 ppm	15 · MnO4 anion exchange studies · Figure S27
Solvent	water	21 mL	15 · MnO4 anion exchange studies · Figure S27

Complete recipeSource: Both

Route 2: Solvothermal

1-2 · 2.1 Synthesis of compound Gd4-MOF

Metal precursorsGd(CF3SO3)3 (gadolinium trifluoromethanesulfonate), 241.8 mg, 0.4 mmol

Linker precursorsisonicotinic acid 123.1 mg, 1.0 mmol; glycolic acid 38.0 mg, 0.5 mmol

Solvents4 mL deionized water, 5 mL anhydrous ethanol, 6 mL acetonitrile

Additivesnone stated

Atmospheresealed 25 mL Teflon-lined stainless steel container; atmosphere not otherwise specified

Temperature150

Time48

Substrate orientationnot applicable for crystal synthesis

Oxidant / reductantnone stated

Work-upcooled to 30 C at 4 C/h; isolation/washing not specified

Activationnone reported for synthesis; crystals used as obtained

Scalability contextabout 30% yield based on Gd

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Gd(CF3SO3)3 (Gadolinium trifluoromethanesulfonate)	241.8 mg, 0.4 mmol	1-2 · 2.1 Synthesis of compound Gd4-MOF
Linker	Isonicotinic acid	123.1 mg, 1.0 mmol	1-2 · 2.1 Synthesis of compound Gd4-MOF
Linker	glycolic acid	38.0 mg, 0.5 mmol	1-2 · 2.1 Synthesis of compound Gd4-MOF
Solvent	deionized water	4 mL	1-2 · 2.1 Synthesis of compound Gd4-MOF
Solvent	anhydrous ethanol	5 mL	1-2 · 2.1 Synthesis of compound Gd4-MOF
Solvent	acetonitrile	6 mL	1-2 · 2.1 Synthesis of compound Gd4-MOF

Complete recipeSource: SI

Route 3: Solvothermal

2 · 2.3 Synthesis of compound Lu4-MOF

Metal precursorsLu(CF3SO3)3 (lutetium trifluoromethanesulfonate), 124.4 mg, 0.2 mmol

Linker precursorsisonicotinic acid 61.6 mg, 0.5 mmol; glycolic acid 19.0 mg, 0.25 mmol

Solvents4 mL deionized water, 5 mL anhydrous ethanol, 6 mL acetonitrile

Additivesnone stated

Atmospheresealed 25 mL Teflon-lined stainless steel container; atmosphere not otherwise specified

Temperature150

Time48

Substrate orientationnot applicable for crystal synthesis

Oxidant / reductantnone stated

Work-upcooled to 30 C at 4 C/h; isolation/washing not specified

Activationnone reported for synthesis; crystals used as obtained

Scalability contextabout 30% yield based on Lu

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Lu(CF3SO3)3 (Lutetium trifluoromethanesulfonate)	124.4 mg, 0.2 mmol	2 · 2.3 Synthesis of compound Lu4-MOF
Linker	Isonicotinic acid	61.6 mg, 0.5 mmol	2 · 2.3 Synthesis of compound Lu4-MOF
Linker	glycolic acid	19.0 mg, 0.25 mmol	2 · 2.3 Synthesis of compound Lu4-MOF
Solvent	deionized water	4 mL	2 · 2.3 Synthesis of compound Lu4-MOF
Solvent	anhydrous ethanol	5 mL	2 · 2.3 Synthesis of compound Lu4-MOF
Solvent	acetonitrile	6 mL	2 · 2.3 Synthesis of compound Lu4-MOF

Complete recipeSource: SI

Route 4: Solvothermal

2 · 2.2 Synthesis of compound Tm4-MOF

Metal precursorsTm(CF3SO3)3 (thulium trifluoromethanesulfonate), 123.2 mg, 0.2 mmol

Linker precursorsisonicotinic acid 61.6 mg, 0.5 mmol; glycolic acid 19.0 mg, 0.25 mmol

Solvents4 mL deionized water, 5 mL anhydrous ethanol, 6 mL acetonitrile

Additivesnone stated

Atmospheresealed 25 mL Teflon-lined stainless steel container; atmosphere not otherwise specified

Temperature150

Time48

Substrate orientationnot applicable for crystal synthesis

Oxidant / reductantnone stated

Work-upcooled to 30 C at 4 C/h; isolation/washing not specified

Activationnone reported for synthesis; crystals used as obtained

Scalability contextabout 30% yield based on Tm

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Tm(CF3SO3)3 (Thulium trifluoromethanesulfonate)	123.2 mg, 0.2 mmol	2 · 2.2 Synthesis of compound Tm4-MOF
Linker	Isonicotinic acid	61.6 mg, 0.5 mmol	2 · 2.2 Synthesis of compound Tm4-MOF
Linker	glycolic acid	19.0 mg, 0.25 mmol	2 · 2.2 Synthesis of compound Tm4-MOF
Solvent	deionized water	4 mL	2 · 2.2 Synthesis of compound Tm4-MOF
Solvent	anhydrous ethanol	5 mL	2 · 2.2 Synthesis of compound Tm4-MOF
Solvent	acetonitrile	6 mL	2 · 2.2 Synthesis of compound Tm4-MOF