Synthesis · Direct Observation of Confined I−⋅⋅⋅I2⋅⋅⋅I− Interactions in a Metal–Organic Framework: Iodine Capture and Sensing

5 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

p005-p006 / SI p.4-5 · Syntheses of the compounds · Figure S3

Metal precursorsG@1 crystals, {[Tb3(Cu4I4)3(ina)9(DMF)4].DMF}n

Linker precursorsina already incorporated in G@1

SolventsDMF removed during evacuation

Additivesnone reported

Atmospherevacuum / evacuated

Temperature160

Time12

Oxidant / reductantnone reported

Work-upEvacuated until colour changed from green-yellow to dark-yellow; no additional washing reported.

ActivationEvacuation at 160 C for 12 h removes free/coordinated DMF to yield [Tb(Cu4I4)(ina)3(DMF)]n.

Scalability contextReported on 1 g crystals of G@1.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	G@1 crystals	1 g	p005-p006 / SI p.4-5 · Syntheses of the compounds · Figure S3

Complete recipeSource: SI

Route 2: Other

p006 / SI p.5 · Syntheses of the compounds

Metal precursorscompound 1 crystals

Linker precursorsina already incorporated in compound 1

Solventsdry ethanol (10 mL)

Additivesnone reported

Atmospherenot specified

Temperatureroom temperature

Time168

Oxidant / reductantnone reported

Work-upSolution decanted and resulting EtOH@1 crystals collected.

Activationnone reported

Scalability contextReported on 100 mg crystals of 1.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 1 crystals	100 mg	p006 / SI p.5 · Syntheses of the compounds
Solvent	dry ethanol	10 mL	p006 / SI p.5 · Syntheses of the compounds

Complete recipeSource: SI

Route 3: Solvothermal

p005 / SI p.4 · Syntheses of the compounds

Metal precursorsTb(NO3)3.6H2O (1.0 mmol); CuI (1 mmol)

Linker precursorsisonicotinic acid (1 mmol)

SolventsDMF (4 mL) and MeCN (2 mL)

Additivesnone reported

Atmospherenot specified

Temperature100

Time12

Oxidant / reductantCuI provides iodide/copper source; no separate oxidant/reductant reported

Work-upCooled to room temperature; yellow crystals washed with DMF and dried in vacuum; yield ca. 87% based on Cu.

Activationnone for G@1; later evacuated to form 1

Scalability contextMillimole-scale slurry recipe; yield ca. 87% based on Cu.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Tb(NO3)3.6H2O	1.0 mmol	p005 / SI p.4 · Syntheses of the compounds
Metal Source	CuI	1 mmol	p005 / SI p.4 · Syntheses of the compounds
Linker	isonicotinic acid	1 mmol	p005 / SI p.4 · Syntheses of the compounds
Solvent	DMF	4 mL	p005 / SI p.4 · Syntheses of the compounds
Solvent	MeCN	2 mL	p005 / SI p.4 · Syntheses of the compounds

Complete recipeSource: Both

Route 4: Other

p006 / SI p.5 · Syntheses of the compounds

Metal precursorscompound 1 crystals

Linker precursorsina already incorporated in compound 1

Solventscyclohexane

AdditivesI2 guest source

Atmospherenot specified

Temperatureroom temperature not explicitly stated

Time2

Oxidant / reductantI2 guest loading; no redox reagent specified

Work-upSoaked until crystals changed from dark-yellow to black; subsequent washing/drying not specified.

ActivationI2 can later be released by heating or soaking I2@1 in ethanol.

Scalability contextReported on 500 mg crystals of 1.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 1 crystals	500 mg	p006 / SI p.5 · Syntheses of the compounds
Other	I2	saturated in cyclohexane	p006 / SI p.5 · Syntheses of the compounds
Solvent	cyclohexane	saturated I2/cyclohexane solution	p006 / SI p.5 · Syntheses of the compounds

Complete recipeSource: SI

Route 5: Other

p006 / SI p.5 · Syntheses of the compounds

Metal precursorscompound 1 crystals

Linker precursorsina already incorporated in compound 1

Solventsdry acetonitrile (10 mL)

Additivesnone reported

Atmospherenot specified

Temperatureroom temperature

Time168

Oxidant / reductantnone reported

Work-upSolution decanted and resulting MeCN@1 crystals collected.

Activationnone reported

Scalability contextReported on 100 mg crystals of 1.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 1 crystals	100 mg	p006 / SI p.5 · Syntheses of the compounds
Solvent	dry acetonitrile	10 mL	p006 / SI p.5 · Syntheses of the compounds