Synthesis · Porous Molecular Conductor: Electrochemical Fabrication of Through-Space Conduction Pathways among Linear Coordination Polymers

4 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

S2 · Syntheses

Linker precursors1,4,5,8-Naphthalenetetracarboxylic dianhydride (NDA); 4-aminopyridine

SolventsN,N-dimethylfolmamide (DMF); recrystallised from DMF; washed with MeOH

Atmosphereambient atmosphere

TemperatureDMF reflux, temperature not specified

Timeovernight

Work-upCrude product collected by filtration, recrystallised from DMF, filtered, washed with MeOH, dried in a desiccator

ActivationDried in a desiccator

Scalability contextYield 80% reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	1,4,5,8-Naphthalenetetracarboxylic dianhydride (NDA)	1.70 g, 6.34 mmol	S2 · Syntheses
Linker	4-aminopyridine	1.25 g, 13.3 mmol	S2 · Syntheses
Solvent	N,N-dimethylfolmamide (DMF)	55 mL	S2 · Syntheses
Solvent	MeOH	wash	S2 · Syntheses

Complete recipeSource: Both

Route 2: Electrochemical

S2-S3 · Synthesis of PMC-1

Metal precursorsCd(NO3)2.4H2O

Linker precursorsNDI-py

SolventsN,N-dimethylacetamide (DMA)

AtmosphereRoom temperature; dried in N2 atmosphere after washing

Temperatureroom temperature

Time48

Substrate orientationPtIr alloy wire cathode; 0.3 mm diameter Pt:Ir = 80:20 electrodes

Oxidant / reductantConstant direct current of 30 uA; electrochemical reduction during crystallisation

Work-upDark brown rod-like crystals isolated from cathode, washed with DMA and ethanol, dried in N2 atmosphere

ActivationNone for as-synthesised PMC-1

Scalability contextApplied current varied 5-70 uA; 30 uA chosen for reproducibility and yield; 100 and 200 mg Cd(NO3)2.4H2O gave same x values.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	NDI-py	20 mg, 0.0476 mmol	S2-S3 · Synthesis of PMC-1
Metal Source	Cd(NO3)2.4H2O	100 mg, 0.32 mmol	S2-S3 · Synthesis of PMC-1
Solvent	N,N-dimethylacetamide (DMA)	5 mL	S2-S3 · Synthesis of PMC-1
Other	PtIr alloy wire cathode	0.3 mm diameter; Pt:Ir = 80:20	S2-S3 · Synthesis of PMC-1

Complete recipeSource: Both

Route 3: Other

S3 · Preparation of PMC-1h · Figure S3, Table S2

Metal precursorsPMC-1

Linker precursorsPMC-1

AtmosphereNitrogen flow / N2 atmosphere; partial water readsorption from air during handling

Temperature210

Time0.5 in main text; SI says maintained at 210 deg C until weight became constant

Work-upCool to room temperature; handle in air causing partial hydration

ActivationThermal removal of DMA and coordinated water at 210 deg C

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Fresh crystals of PMC-1	Not specified	S3 · Preparation of PMC-1h · Figure S3, Table S2
Other	nitrogen flow	0.1 L/min for TG general method	S3 · Preparation of PMC-1h · Figure S3, Table S2

Partial recipeSource: SI

Route 4: Other

S3 · Preparation of PMC-1s by soaking method · Figures S12-S16

Metal precursorsPMC-1

Linker precursorsPMC-1

SolventsN2-bubbled toluene

AtmosphereN2-bubbled solvent; dried in N2 atmosphere

Temperatureroom temperature implied, not specified

Time168

Work-upProduct collected and dried in N2 atmosphere

ActivationSolvent extraction of DMA into toluene

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Fresh crystals of PMC-1	Not specified	S3 · Preparation of PMC-1s by soaking method · Figures S12-S16
Solvent	N2-bubbled toluene	Not specified	S3 · Preparation of PMC-1s by soaking method · Figures S12-S16