Synthesis · Li + Ion-Conducting Sulfonate-Based Neutral Metal-Organic Framework

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: Other

SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts

Solvents1 M Bu4NClO4/MeCN solution (5 mL); CHCl3 wash.

AdditivesBu4NClO4

AtmosphereAir/vacuum drying after solution treatment; treatment atmosphere not specified.

Temperatureroom temperature

Time60 h in SI; main text describes similar treatment but does not give a separate time in that passage

Work-upDecanted salt solution; washed with CHCl3 (3 x 5 mL); dried under air and vacuum.

ActivationDried under air and vacuum after washing.

Scalability contextNo measurable weight gain after treatment.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Dried [Cu2(BPY)2(NDIDS)] MOF powder	10 mg, ~9.9 umol	SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts
Electrolyte	Bu4NClO4	5 mL solution · 1 M in MeCN	SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts
Solvent	MeCN	5 mL solution	SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts
Solvent	CHCl3 wash	3 x 5 mL	SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts

Complete recipeSource: Both

Route 2: Other

SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts

Solvents1 M LiClO4/MeCN solution (5 mL); wash solvent CHCl3 in main/SI method, with SI parenthetical noting CH2Cl2 for the weighed LiClO4-treated MOF.

AdditivesLiClO4

AtmosphereAir/vacuum drying after solution treatment; treatment atmosphere not specified.

Temperatureroom temperature

Time72 h in main text; 60 h in SI

Work-upDecanted salt solution; washed with CHCl3 (3 x 5 mL) to remove physisorbed salt; dried under air and vacuum.

ActivationDried under air and vacuum after washing.

Scalability context10 mg dried MOF gave 12 mg LiClO4-treated material, 20 wt% uptake.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Dried [Cu2(BPY)2(NDIDS)] MOF powder	10 mg, ~9.9 umol	SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts
Electrolyte	LiClO4	5 mL solution; 2 mg or 18.8 umol uptake reported · 1 M in MeCN	SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts
Solvent	MeCN	5 mL solution	SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts
Solvent	CHCl3 wash	3 x 5 mL	SI p.S-4 · Treatment of Cu(I)-sulfonate MOF with LiClO4 and Bu4NClO4 salts

Complete recipeSource: Both

Route 3: Hydrothermal

SI p.S-4 · Synthesis of Cu(I)-sulfonate MOF

Metal precursorsCu(NO3)2.3H2O (17 mg, 0.07 mmol)

Linker precursorsNDIDS (42.4 mg, 0.07 mmol) and 4,4'-bipyridine, BPY (11 mg, 0.07 mmol)

SolventsH2O (6 mL)

AtmosphereSealed Teflon-lined autoclave; atmosphere not otherwise specified.

Temperature175

Time60

Work-upCooled to room temperature; crystals filtered, washed thoroughly with H2O and MeOH, dried under air and vacuum to give free-flowing crystalline MOF powder.

ActivationFor sorption, washed with H2O then MeOH, dried under air, activated under high vacuum first at room temperature and then at 150 deg C for 24 h.

Scalability contextReported yield 50 mg, 67% based on Cu.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.3H2O	17 mg, 0.07 mmol	SI p.S-4 · Synthesis of Cu(I)-sulfonate MOF
Linker	NDIDS	42.4 mg, 0.07 mmol	SI p.S-4 · Synthesis of Cu(I)-sulfonate MOF
Linker	4,4'-bipyridine (BPY)	11 mg, 0.07 mmol	SI p.S-4 · Synthesis of Cu(I)-sulfonate MOF
Solvent	H2O	6 mL	SI p.S-4 · Synthesis of Cu(I)-sulfonate MOF

Complete recipeSource: SI

Route 4: Other

SI p.S-4 · Preparation of pellets for ac impedance measurements

AdditivesSilver paint on steel electrodes.

AtmosphereAmbient measurement conditions after pressing.

Temperatureroom temperature

Time0.0167

Work-up3 mg material placed in Teflon tube between silver-coated steel rods and pressed at 200 MPa for 1 min.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	MOF or control material	3 mg	SI p.S-4 · Preparation of pellets for ac impedance measurements
Additive	silver paint	thin coating on steel rods	SI p.S-4 · Preparation of pellets for ac impedance measurements