Synthesis · Fabrication of Cu(II) based halobenzoate appended ladder polymers with efficient charge transport properties

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

6721 · Device fabrication and characterization

SolventsDMSO dispersion medium; FTO/glass cleaned in isopropyl alcohol, acetone and distilled water

AtmosphereN2 gas treatment before vacuum drying; Al deposition at 10^-6 Torr

Temperatureroom temperature

Time0.0083

Substrate orientationFTO coated glass

Work-upspin coated at 400 rpm for 30 s; aluminium top electrode deposited

Activationvacuum chamber drying after N2 gas treatment

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Solvent	N,N-dimethyl sulfoxide (DMSO)	not specified	6721 · Device fabrication and characterization
Other	compound 1	not specified	6721 · Device fabrication and characterization
Other	FTO/glass substrate	not specified	6721 · Device fabrication and characterization
Other	aluminium electrode	not specified	6721 · Device fabrication and characterization

Complete recipeSource: Main

Route 2: Liquid Liquid Interface

6721 · Syntheses of compounds 1 and 2

Metal precursorsCu(NO3)2.3H2O (0.031 g, 0.2 mmol)

Linker precursorsbpe (0.036 g, 0.2 mmol); H2p-clba (0.031 g, 0.2 mmol)

SolventsMeOH (2 mL for bpe; 2 mL 1:1 MeOH/H2O buffer layer), H2O (2 mL for Cu salt), EtOH (2 mL for H2p-clba)

AdditivesEt3N (0.021 g, 0.2 mmol) to neutralise H2p-clba

Atmospherenot specified

Temperaturenot specified; apparently ambient slow diffusion

Time72

Work-upviolet block crystals obtained after three days; yield 0.241 g, 70%

Activationnot specified

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.3H2O	0.031 g, 0.2 mmol	6721 · Syntheses of compounds 1 and 2
Linker	bpe	0.036 g, 0.2 mmol	6721 · Syntheses of compounds 1 and 2
Linker	H2p-clba	0.031 g, 0.2 mmol	6721 · Syntheses of compounds 1 and 2
Base	Et3N	0.021 g, 0.2 mmol	6721 · Syntheses of compounds 1 and 2
Solvent	MeOH	2 mL plus 1 mL in 2 mL 1:1 buffer	6721 · Syntheses of compounds 1 and 2
Solvent	H2O	2 mL plus 1 mL in 2 mL 1:1 buffer	6721 · Syntheses of compounds 1 and 2
Solvent	EtOH	2 mL	6721 · Syntheses of compounds 1 and 2

Complete recipeSource: Main

Route 3: Other

6721 · Device fabrication and characterization

SolventsDMSO dispersion medium; FTO/glass cleaned in isopropyl alcohol, acetone and distilled water

AtmosphereN2 gas treatment before vacuum drying; Al deposition at 10^-6 Torr

Temperatureroom temperature

Time0.0083

Substrate orientationFTO coated glass

Work-upspin coated at 400 rpm for 30 s; aluminium top electrode deposited

Activationvacuum chamber drying after N2 gas treatment

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Solvent	N,N-dimethyl sulfoxide (DMSO)	not specified	6721 · Device fabrication and characterization
Other	compound 2	not specified	6721 · Device fabrication and characterization
Other	FTO/glass substrate	not specified	6721 · Device fabrication and characterization
Other	aluminium electrode	not specified	6721 · Device fabrication and characterization

Complete recipeSource: Main

Route 4: Liquid Liquid Interface

6721 · Syntheses of compounds 1 and 2

Metal precursorsCu(NO3)2.3H2O (0.031 g, 0.2 mmol, inferred from similar procedure to compound 1)

Linker precursorsbpe (0.036 g, 0.2 mmol, inferred from similar procedure to compound 1); H2p-brba (0.040 g, 0.2 mmol)

SolventsMeOH, H2O and EtOH as in compound 1 synthesis

AdditivesEt3N (0.021 g, 0.2 mmol, inferred from similar procedure to compound 1)

Atmospherenot specified

Temperaturenot specified; apparently ambient slow diffusion

Time72

Work-upcolourless block crystals obtained after three days; yield 0.279 g, 70%

Activationnot specified

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.3H2O	0.031 g, 0.2 mmol (from similar procedure)	6721 · Syntheses of compounds 1 and 2
Linker	bpe	0.036 g, 0.2 mmol (from similar procedure)	6721 · Syntheses of compounds 1 and 2
Linker	H2p-brba	0.040 g, 0.2 mmol	6721 · Syntheses of compounds 1 and 2
Base	Et3N	0.021 g, 0.2 mmol (from similar procedure)	6721 · Syntheses of compounds 1 and 2
Solvent	MeOH/H2O/EtOH	as in compound 1 synthesis	6721 · Syntheses of compounds 1 and 2