Synthesis · Tunable Charge Transport Properties Through Precise π-Stacking Modulation in Isostructural Porous Molecular Conductors

3 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Electrochemical

SI p.S2 · Synthesis of PMC-3-Br

Metal precursorsZnBr2 (130 mg, 0.58 mmol)

Linker precursorsNDI-py (20 mg, 0.0476 mmol)

Solvents5 mL N,N-dimethylacetamide (DMA)

Additives30 uL pure water

AtmosphereElectrocrystallisation in ambient atmosphere; product dried in N2 atmosphere.

TemperatureRoom temperature

Time48

Substrate orientation0.3 mm diameter Pt-Ir alloy wire cathode/anode, 80:20 Pt:Ir.

Oxidant / reductantConstant direct current of 30 uA; electrochemical reduction generates NDI.- species.

Work-upCrystals isolated from cathode, washed with DMA and ethanol, then dried in N2 atmosphere.

ActivationNo separate activation reported; compound rapidly loses some solvent during drying.

Scalability contextSmall single-crystal electrocrystallisation; no scale-up demonstrated.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	NDI-py	20 mg, 0.0476 mmol	SI p.S2 · Synthesis of PMC-3-Br
Metal Source	ZnBr2	130 mg, 0.58 mmol	SI p.S2 · Synthesis of PMC-3-Br
Solvent	N,N-dimethylacetamide (DMA)	5 mL	SI p.S2 · Synthesis of PMC-3-Br
Additive	pure water	30 uL	SI p.S2 · Synthesis of PMC-3-Br
Other	Pt-Ir alloy wire electrodes	0.3 mm diameter, Pt:Ir 80:20	SI p.S2 · Synthesis of PMC-3-Br

Complete recipeSource: Both

Route 2: Electrochemical

SI p.S2 · Synthesis of PMC-3-Cl

Metal precursorsZnCl2 (80 mg, 0.59 mmol)

Linker precursorsNDI-py (20 mg, 0.0476 mmol)

Solvents5 mL N,N-dimethylacetamide (DMA)

Additives30 uL pure water

AtmosphereElectrocrystallisation in ambient atmosphere; product dried in N2 atmosphere.

TemperatureRoom temperature

Time48

Substrate orientation0.3 mm diameter Pt-Ir alloy wire cathode/anode, 80:20 Pt:Ir.

Oxidant / reductantConstant direct current of 30 uA; electrochemical reduction generates NDI.- species.

Work-upCrystals isolated from cathode, washed with DMA and ethanol, then dried in N2 atmosphere.

ActivationNo separate activation reported for synthesis; drying under N2 after washing. Lattice solvent begins to leave at RT.

Scalability contextSmall single-crystal electrocrystallisation; no scale-up demonstrated.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	NDI-py	20 mg, 0.0476 mmol	SI p.S2 · Synthesis of PMC-3-Cl
Metal Source	ZnCl2	80 mg, 0.59 mmol	SI p.S2 · Synthesis of PMC-3-Cl
Solvent	N,N-dimethylacetamide (DMA)	5 mL	SI p.S2 · Synthesis of PMC-3-Cl
Additive	pure water	30 uL	SI p.S2 · Synthesis of PMC-3-Cl
Other	Pt-Ir alloy wire electrodes	0.3 mm diameter, Pt:Ir 80:20	SI p.S2 · Synthesis of PMC-3-Cl

Complete recipeSource: Both

Route 3: Electrochemical

SI p.S2-p.S3 · Synthesis of PMC-3-I

Metal precursorsZnI2 (190 mg, 0.60 mmol)

Linker precursorsNDI-py (20 mg, 0.0476 mmol)

Solvents5 mL N,N-dimethylacetamide (DMA)

Additives30 uL pure water

AtmosphereElectrocrystallisation in ambient atmosphere; product dried in N2 atmosphere.

TemperatureRoom temperature

Time48

Substrate orientation0.3 mm diameter Pt-Ir alloy wire cathode/anode, 80:20 Pt:Ir.

Oxidant / reductantConstant direct current of 30 uA; electrochemical reduction generates NDI.- species.

Work-upCrystals isolated from cathode, washed with DMA and ethanol, then dried in N2 atmosphere.

ActivationNo separate activation reported for synthesis; drying under N2 after washing.

Scalability contextSmall single-crystal electrocrystallisation; no scale-up demonstrated.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	NDI-py	20 mg, 0.0476 mmol	SI p.S2-p.S3 · Synthesis of PMC-3-I
Metal Source	ZnI2	190 mg, 0.60 mmol	SI p.S2-p.S3 · Synthesis of PMC-3-I
Solvent	N,N-dimethylacetamide (DMA)	5 mL	SI p.S2-p.S3 · Synthesis of PMC-3-I
Additive	pure water	30 uL	SI p.S2-p.S3 · Synthesis of PMC-3-I
Other	Pt-Ir alloy wire electrodes	0.3 mm diameter, Pt:Ir 80:20	SI p.S2-p.S3 · Synthesis of PMC-3-I