Synthesis · Vapor-Induced Superionic Conduction of Magnesium Ions in a Metal-Organic Framework

3 structured synthesis routes

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

Complete recipeSource: Main

p002 / article p.21125 · Materials and Methods - Synthesis of Mg-MOF-74

Metal precursorsMg(NO3)2.6H2O (12.6 g, 49.1 mmol)

Linker precursors2,5-dihydroxyterephthalic acid (H4dobdc) (2.95 g, 14.9 mmol)

SolventsDMF/ethanol/deionized water = 15:1:1 mixed solvent (1320 mL)

Temperature100; then 250 drying

Time21 h heating; 3 d reflux in each solvent; 6 h vacuum drying

Work-upprecipitate separated by decantation; washed by reflux in DMF and MeOH for 3 d for each solvent; solvent replaced three times; filtered

Activationdried at 250 deg C for 6 h under vacuum

Scalability contextReported yield 3.06 g, 56%; elemental analysis reported for Mg2(C8H2O6)(H2O)7.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Mg(NO3)2.6H2O	12.6 g, 49.1 mmol	p002 / article p.21125 · Materials and Methods - Synthesis of Mg-MOF-74
Linker	2,5-dihydroxyterephthalic acid (H4dobdc)	2.95 g, 14.9 mmol	p002 / article p.21125 · Materials and Methods - Synthesis of Mg-MOF-74
Solvent	DMF/ethanol/deionized water = 15:1:1	1320 mL	p002 / article p.21125 · Materials and Methods - Synthesis of Mg-MOF-74

Complete recipeSource: Main

p002 / article p.21125 · Materials and Methods - Synthesis of Mg-MOF-74 superset {(MgTFSI)2}x · Figure 1a

Metal precursorsMg-MOF-74 (300 mg, 0.813 mmol); Mg(TFSI)2.8H2O (0, 28.9, 59.8, 103, or 127 mg)

Linker precursorsMg-MOF-74 preformed framework

Solventsethanol solution, 20 mL

AdditivesMg(TFSI)2.8H2O salt

Temperature85

Time168

Work-upsolution heated in a test tube to evaporate EtOH solvent by slow evaporation

Activationconductivity/adsorption samples later dehydrated at 130 deg C under N2 or vacuum for a night before measurements

Scalability contextBatch used 300 mg Mg-MOF-74 per loading; compositions estimated by ICP-AES.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Mg-MOF-74	300 mg, 0.813 mmol	p002 / article p.21125 · Materials and Methods - Synthesis of Mg-MOF-74 superset {(MgTFSI)2}x · Figure 1a
Electrolyte	Mg(TFSI)2.8H2O	0, 28.9, 59.8, 103, and 127 mg for x = 0, 0.07, 0.13, 0.15, and 0.17	p002 / article p.21125 · Materials and Methods - Synthesis of Mg-MOF-74 superset {(MgTFSI)2}x · Figure 1a
Solvent	ethanol	20 mL	p002 / article p.21125 · Materials and Methods - Synthesis of Mg-MOF-74 superset {(MgTFSI)2}x · Figure 1a

Complete recipeSource: Main

p002 / article p.21125 · Materials and Methods - Synthesis of Mg(TFSI)2.8H2O

Metal precursorsMg powder (0.965 g, 39.7 mmol)

Solventsdeionized water (100 mL)

Additivesbis(trifluoromethane)sulfonamide / HTFSI (22.5 g, 80.0 mmol)

TemperatureRT for reaction; 160 deg C drying

Time1 h stirring; 5 h drying

Work-upunreacted Mg removed by filtration; solution concentrated by rotary evaporation to collect white powder

Activationdried at 160 deg C under vacuum for 5 h

Scalability contextReported isolated yield 22.3 g, 77%.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Mg powder	0.965 g, 39.7 mmol	p002 / article p.21125 · Materials and Methods - Synthesis of Mg(TFSI)2.8H2O
Acid	bis(trifluoromethane)sulfonamide (HTFSI)	22.5 g, 80.0 mmol	p002 / article p.21125 · Materials and Methods - Synthesis of Mg(TFSI)2.8H2O
Solvent	deionized water	100 mL	p002 / article p.21125 · Materials and Methods - Synthesis of Mg(TFSI)2.8H2O