Synthesis · Copper(i) iodide coordination polymers with triazole substituted pyridine ligands: photophysical and electrical conductivity properties

6 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

5 · Synthesis of 1D [Cu2I2(L1)2]n CP1

Metal precursorsCuI (65 mg, 0.34 mmol)

Linker precursorsL1 = 2-(1H-1,2,4-triazol-1-yl)pyridine (50 mg, 0.34 mmol)

SolventsCH3CN/acetonitrile, 3 mL for CuI plus 2 mL for L1

AtmosphereN2/Schlenk line for reactions according to SI general information

Temperatureroom temperature

Time0.75

Work-upWhite precipitate filtered; washed with dichloromethane and CH3CN (1 mL) 2-3 times; dried under vacuum

Activationdried under vacuum

Scalability contextOverall yield 80%

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	65 mg, 0.34 mmol	5 · Synthesis of 1D [Cu2I2(L1)2]n CP1
Linker	L1	50 mg, 0.34 mmol	5 · Synthesis of 1D [Cu2I2(L1)2]n CP1
Solvent	CH3CN	3 mL + 2 mL	5 · Synthesis of 1D [Cu2I2(L1)2]n CP1

Partial recipeSource: SI

Route 2: Other

5 · Synthesis of 1D [Cu2I2(L1)2]n CP1

Metal precursorsCP1 bulk powder

Solventshot CH3CN

Temperaturehot CH3CN, then room temperature crystallisation

Time168

Work-upLeft to grow crystals; colourless needle-shaped crystals obtained

Scalability contextCrystal growth used about 20 mg of CP1

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	CP1	about 20 mg	5 · Synthesis of 1D [Cu2I2(L1)2]n CP1
Solvent	hot CH3CN	Not specified	5 · Synthesis of 1D [Cu2I2(L1)2]n CP1

Partial recipeSource: Both

Route 3: Other

5 · Synthesis of 1D [Cu2I2(L2)2]n CP2

Metal precursorsCuI, as in CP1 procedure

Linker precursorsL2 = 3-(1H-1,2,4-triazol-1-yl)pyridine

SolventsCH3CN/acetonitrile

AtmosphereN2/Schlenk line for reactions according to SI general information

Temperatureroom temperature

Time0.75, inferred from 'manner like CP1'

Work-upPrepared in a manner like CP1; filtration/washing/drying details implied by CP1 procedure

Activationdried under vacuum, inferred from CP1 procedure

Scalability contextOverall yield 49%

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	not restated for CP2; prepared like CP1	5 · Synthesis of 1D [Cu2I2(L2)2]n CP2
Linker	L2	not restated for CP2	5 · Synthesis of 1D [Cu2I2(L2)2]n CP2
Solvent	CH3CN	not restated for CP2	5 · Synthesis of 1D [Cu2I2(L2)2]n CP2

Partial recipeSource: SI

Route 4: Other

5 · Synthesis of 1D [Cu2I2(L2)2]n CP2

Metal precursorsCP2 bulk powder

Solventshot CH3CN

Temperaturehot CH3CN, then room temperature crystallisation

Timea few days

Work-upLeft to grow crystals; yellow crystals obtained

Scalability contextCrystal growth used about 20 mg of CP2

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	CP2	20 mg	5 · Synthesis of 1D [Cu2I2(L2)2]n CP2
Solvent	hot CH3CN	Not specified	5 · Synthesis of 1D [Cu2I2(L2)2]n CP2

Partial recipeSource: Both

Route 5: Other

5 · Synthesis of 1D [CuI(L3)]n CP3

Metal precursorsCuI, as in CP1 procedure

Linker precursorsL3 = 4-(1H-1,2,4-triazol-1-yl)pyridine

SolventsCH3CN/acetonitrile

AtmosphereN2/Schlenk line for reactions according to SI general information

Temperatureroom temperature

Time0.75, inferred from 'same procedure as CP1'

Work-upPrepared following the same procedure as CP1 except L3; CP1 filtration/washing/drying procedure implied

Activationdried under vacuum, inferred from CP1 procedure

Scalability contextOverall yield up to 60%

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	not restated for CP3; prepared like CP1	5 · Synthesis of 1D [CuI(L3)]n CP3
Linker	L3	not restated for CP3	5 · Synthesis of 1D [CuI(L3)]n CP3
Solvent	CH3CN	not restated for CP3	5 · Synthesis of 1D [CuI(L3)]n CP3

Partial recipeSource: Both

Route 6: Liquid Liquid Interface

5 · Synthesis of 1D [CuI(L3)]n CP3

Metal precursorsCuI in aqueous KI solution

Linker precursorsL3 in ethanol solution

Solventswater, ethanol, CH3CN buffer layer

AdditivesKI

Temperatureroom temperature

Time168-240

Work-upLayering aqueous KI/CuI and ethanol L3 solution with CH3CN buffer; yellow rod-like crystals obtained

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	aqueous solution with KI	5 · Synthesis of 1D [CuI(L3)]n CP3
Additive	KI	aqueous solution with CuI	5 · Synthesis of 1D [CuI(L3)]n CP3
Linker	L3	ethanol solution	5 · Synthesis of 1D [CuI(L3)]n CP3
Solvent	CH3CN	buffer layer	5 · Synthesis of 1D [CuI(L3)]n CP3