Synthesis · Semiconducting neutral microstructures fabricated by coordinative self-assembly of intramolecular charge-transfer tetrathiafulvalene derivatives

3 structured synthesis routes

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

Complete recipeSource: Main

5128 · Experimental Section

Metal precursorsnone in ligand synthesis; Pb2+ used later for binding/morphology control

Linker precursors4,4'(5')-Bisiodotetrathiafulvalene and 4-ethynylpyridine

Solventsanhydrous THF; Et3N; ethyl acetate/dichloromethane for chromatography

Additives[Pd(PPh3)4], CuI

Atmospherenot stated

Temperatureroom temperature

Time5

Work-upFiltered, solvent evaporated, residue purified by silica-gel column chromatography to afford red solid.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	4,4'(5')-Bisiodotetrathiafulvalene	68 mg, 0.15 mmol	5128 · Experimental Section
Linker	4-ethynylpyridine	26 mg, 0.3 mmol	5128 · Experimental Section
Additive	[Pd(PPh3)4]	17 mg	5128 · Experimental Section
Additive	CuI	6.0 mg	5128 · Experimental Section
Base	Et3N	0.2 mL	5128 · Experimental Section
Solvent	anhydrous THF	20 mL	5128 · Experimental Section

Partial recipeSource: Both

5128-5129 · Experimental Section

Metal precursorsPb(ClO4)2

Linker precursorscompound 1, 4,4'(5')-[bis-(4-pyridineethenyl)]tetrathiafulvalene

Solventsacetonitrile for Pb(ClO4)2; dichloromethane for compound 1

Atmospherenot stated

Temperatureroom temperature

Time672

Work-upPurple precipitate found in tube after four weeks; isolation/drying details not stated.

Scalability contextConclusion claims construction of microstructures in large quantities, but no batch-size scale-up data are given.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Pb(ClO4)2	0.02 mmol	5128-5129 · Experimental Section
Linker	precursor 1	0.02 mmol	5128-5129 · Experimental Section
Solvent	acetonitrile	5 mL	5128-5129 · Experimental Section
Solvent	dichloromethane	5 mL	5128-5129 · Experimental Section

Partial recipeSource: Both

5129 · Experimental Section

Metal precursorsZn(ClO4)2

Linker precursorscompound 1, 4,4'(5')-[bis-(4-pyridineethenyl)]tetrathiafulvalene

Solventsacetone for Zn(ClO4)2; dichloromethane for compound 1

Atmospherenot stated

Temperatureroom temperature

Time336

Work-upPurple precipitate found in tube after two weeks; isolation/drying details not stated.

Scalability contextNo scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(ClO4)2	0.02 mmol	5129 · Experimental Section
Linker	precursor 1	0.02 mmol	5129 · Experimental Section
Solvent	acetone	5 mL	5129 · Experimental Section
Solvent	dichloromethane	5 mL	5129 · Experimental Section