Synthesis evidence

Two isostructural linear coordination polymers: The size of the metal ion impacts the electrical conductivity

Dutta B., Dey A., Naskar K. et al. · New Journal of Chemistry · 2018 · 10309-10316

4 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

2 · Device fabrication and characterization

Metal precursorsas-synthesised compound 2
SolventsN,N-dimethylformamide (DMF)
Atmosphereambient for spin coating; vacuum oven drying; Al deposition at 10^-6 Torr
Temperature100 for vacuum oven drying
Timespin coating: 4 min at 800 rpm then 6 min at 1200 rpm; drying several minutes
Substrate orientationprecleaned ITO-coated glass; Al top electrode through shadow mask
Work-upVacuum oven dried to evaporate solvent; aluminium electrode deposited.
Activationvacuum oven at 100 deg C for several minutes
Scalability contextThin-film device fabrication only; effective device area 7.065 x 10^-2 cm2.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 240 mg mL-1 in DMF2 · Device fabrication and characterization
SolventN,N-dimethylformamide (DMF)Not specified2 · Device fabrication and characterization
OtherITO-coated glassNot specified2 · Device fabrication and characterization
OtherAl electrodeNot specified2 · Device fabrication and characterization
Partial recipeSource: Main

Route 2: Liquid Liquid Interface

2 · Synthesis of the compounds

Metal precursorsCd(NO3)2.4H2O (0.062 g, 0.2 mmol)
Linker precursorsSame as compound 1: 4-spy (0.036 g, 0.2 mmol); H2adc (0.023 g, 0.2 mmol)
SolventsSame layered MeOH/H2O/EtOH procedure as compound 1
AdditivesEt3N (0.021 g, 0.2 mmol), as in route for compound 1
Atmosphereambient/not specified
Temperatureroom temperature/not specified
Timea few days
Work-upColourless prism crystals isolated; detailed washing/drying not reported in main text.
Activationnot reported
Scalability contextLayering route gives 0.088 g, 70% yield; no scale-up information.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.4H2O0.062 g, 0.2 mmol2 · Synthesis of the compounds
Linker4-spysame as compound 1: 0.036 g, 0.2 mmol2 · Synthesis of the compounds
LinkerH2adcsame as compound 1: 0.023 g, 0.2 mmol2 · Synthesis of the compounds
BaseEt3Nsame as compound 1: 0.021 g, 0.2 mmol2 · Synthesis of the compounds
SolventMeOH/H2O/EtOHsame as compound 12 · Synthesis of the compounds
Partial recipeSource: Main

Route 3: Other

2 · Device fabrication and characterization

Metal precursorsas-synthesised compound 1
SolventsN,N-dimethylformamide (DMF)
Atmosphereambient for spin coating; vacuum oven drying; Al deposition at 10^-6 Torr
Temperature100 for vacuum oven drying
Timespin coating: 4 min at 800 rpm then 6 min at 1200 rpm; drying several minutes
Substrate orientationprecleaned ITO-coated glass; Al top electrode through shadow mask
Work-upVacuum oven dried to evaporate solvent; aluminium electrode deposited.
Activationvacuum oven at 100 deg C for several minutes
Scalability contextThin-film device fabrication only; effective device area 7.065 x 10^-2 cm2.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 140 mg mL-1 in DMF2 · Device fabrication and characterization
SolventN,N-dimethylformamide (DMF)Not specified2 · Device fabrication and characterization
OtherITO-coated glassNot specified2 · Device fabrication and characterization
OtherAl electrodeNot specified2 · Device fabrication and characterization
Partial recipeSource: Main

Route 4: Liquid Liquid Interface

2 · Synthesis of the compounds

Metal precursorsZn(NO3)2.6H2O (text/OCR gives Zn(NO)3.6H2O), 0.06 g, 0.2 mmol
Linker precursors4-spy (0.036 g, 0.2 mmol); H2adc (0.023 g, 0.2 mmol)
SolventsMeOH 2 mL; H2O 2 mL; 2 mL 1:1 v/v MeOH/H2O buffer solution; EtOH 2 mL
AdditivesEt3N (0.021 g, 0.2 mmol) used to neutralise H2adc
Atmosphereambient/not specified
Temperatureroom temperature/not specified
Time72
Work-upColourless prism crystals isolated; detailed washing/drying not reported in main text.
Activationnot reported
Scalability contextLayering route gives 0.074 g, 65% yield; no scale-up information.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O / OCR: Zn(NO)3.6H2O0.06 g, 0.2 mmol2 · Synthesis of the compounds
Linker4-spy0.036 g, 0.2 mmol2 · Synthesis of the compounds
LinkerH2adc0.023 g, 0.2 mmol2 · Synthesis of the compounds
BaseEt3N0.021 g, 0.2 mmol2 · Synthesis of the compounds
SolventMeOH2 mL plus MeOH/H2O buffer2 · Synthesis of the compounds
SolventH2O2 mL plus MeOH/H2O buffer2 · Synthesis of the compounds
SolventEtOH2 mL2 · Synthesis of the compounds