Synthesis evidence

Enhancement of Electrical Conductivity due to Structural Distortion from Linear to Nonlinear Dicarboxylato-Bridged Zn(II) 1D-Coordination Polymers

Naskar K., Sil S., Sahu N. et al. · Crystal Growth and Design · 2019 · 2632-2641

6 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

p010-p011; SI pages S10-S11 · Conductivity measurement · Figure S8

Solventsnot specified for direct-conductivity film; likely dispersion of as-synthesised compound
Atmosphereopen atmosphere during measurement
Temperatureroom temperature
Time0.033 h spin-coating step (2 min)
Substrate orientationITO-coated glass
Work-upThin film spin-coated on ITO at 800 rpm for 2 min; one silver electrode taken from the film and another from the ITO-coated glass substrate.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1not specified · not reportedp010-p011; SI pages S10-S11 · Conductivity measurement · Figure S8
OtherITO-coated glass substrateNot specifiedp010-p011; SI pages S10-S11 · Conductivity measurement · Figure S8
Othersilver electrodesNot specifiedp010-p011; SI pages S10-S11 · Conductivity measurement · Figure S8
Partial recipeSource: Main

Route 2: Other

p002; article page 2633 · Experimental Section - Synthesis

Metal precursorsZn(NO3)2.6H2O (60 mg, 0.2 mmol) in H2O (2 mL)
Linker precursorsPBT (42 mg, 0.2 mmol) in MeOH (2 mL); H2ADC (23 mg, 0.2 mmol) neutralised with Et3N in EtOH (2 mL)
SolventsMeOH, H2O, EtOH; 2 mL 1/1 (v/v) MeOH/H2O buffer layer
AdditivesEt3N (0.027 mL, 0.2 mmol); MeOH/H2O buffer solution
Work-upColourless prismatic crystals isolated after a few days; no washing or activation described in the main text.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O60 mg, 0.2 mmolp002; article page 2633 · Experimental Section - Synthesis
Linker2-pyridin-4-ylbenzothiazole (PBT)42 mg, 0.2 mmolp002; article page 2633 · Experimental Section - Synthesis
LinkerH2ADC23 mg, 0.2 mmolp002; article page 2633 · Experimental Section - Synthesis
BaseEt3N0.027 mL, 0.2 mmolp002; article page 2633 · Experimental Section - Synthesis
SolventMeOH2 mL for PBT plus part of 2 mL 1/1 MeOH/H2O bufferp002; article page 2633 · Experimental Section - Synthesis
SolventH2O2 mL for Zn(NO3)2.6H2O plus part of 2 mL 1/1 MeOH/H2O bufferp002; article page 2633 · Experimental Section - Synthesis
SolventEtOH2 mLp002; article page 2633 · Experimental Section - Synthesis
Partial recipeSource: SI

Route 3: Other

p009; SI page S9 · Fabrication of Schottky device

SolventsN,N-dimethylformamide (DMF)
Atmospherevacuum drying; Al deposited under 10^-6 Torr; electrical measurements under dark ambient room-temperature conditions
Substrate orientationpre-cleaned ITO-coated glass
Work-upITO glass cleaned with 2-propanol, acetone and distilled water by ultrasonication for 20 min; DMF dispersion spin-coated at 600 rpm for 1 min, repeated 4 times; film dried under vacuum; Al evaporated through shadow mask.
Activationdried under vacuum condition
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1not specified · DMF dispersion; concentration not reportedp009; SI page S9 · Fabrication of Schottky device
SolventN,N-dimethylformamide (DMF)not specifiedp009; SI page S9 · Fabrication of Schottky device
OtherITO-coated glass substrateNot specifiedp009; SI page S9 · Fabrication of Schottky device
OtherAluminium top electrodeeffective diode area 7.065e-6 m2p009; SI page S9 · Fabrication of Schottky device
Partial recipeSource: SI

Route 4: Other

p010-p011; SI pages S10-S11 · Conductivity measurement · Figure S8

Solventsnot specified for direct-conductivity film; likely dispersion of as-synthesised compound
Atmosphereopen atmosphere during measurement
Temperatureroom temperature
Time0.033 h spin-coating step (2 min)
Substrate orientationITO-coated glass
Work-upThin film spin-coated on ITO at 800 rpm for 2 min; one silver electrode taken from the film and another from the ITO-coated glass substrate.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 2not specified · not reportedp010-p011; SI pages S10-S11 · Conductivity measurement · Figure S8
OtherITO-coated glass substrateNot specifiedp010-p011; SI pages S10-S11 · Conductivity measurement · Figure S8
Othersilver electrodesNot specifiedp010-p011; SI pages S10-S11 · Conductivity measurement · Figure S8
Partial recipeSource: Main

Route 5: Other

p002; article page 2633 · Experimental Section - Synthesis

Metal precursorsZn(NO3)2.6H2O (60 mg, 0.2 mmol) in water
Linker precursorsPBT in MeOH; H2Succ, amount not specified in main text
SolventsMeOH and water; EtOH likely by identical procedure to 1 but not restated explicitly
AdditivesNot restated for 2; likely Et3N if identical with 1, but not extracted as a firm detail.
Work-upYellowish rectangular crystals isolated after a few days; no washing or activation described in the main text.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O60 mg, 0.2 mmolp002; article page 2633 · Experimental Section - Synthesis
Linker2-pyridin-4-ylbenzothiazole (PBT)not restated for 2; procedure identical with 1p002; article page 2633 · Experimental Section - Synthesis
LinkerH2Succnot specified in main textp002; article page 2633 · Experimental Section - Synthesis
SolventMeOHnot restated; PBT solution in MeOHp002; article page 2633 · Experimental Section - Synthesis
Solventwaternot restated; Zn(NO3)2.6H2O in waterp002; article page 2633 · Experimental Section - Synthesis
Partial recipeSource: SI

Route 6: Other

p009; SI page S9 · Fabrication of Schottky device

SolventsN,N-dimethylformamide (DMF)
Atmospherevacuum drying; Al deposited under 10^-6 Torr; electrical measurements under dark ambient room-temperature conditions
Substrate orientationpre-cleaned ITO-coated glass
Work-upITO glass cleaned with 2-propanol, acetone and distilled water by ultrasonication for 20 min; DMF dispersion spin-coated at 600 rpm for 1 min, repeated 4 times; film dried under vacuum; Al evaporated through shadow mask.
Activationdried under vacuum condition
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 2not specified · DMF dispersion; concentration not reportedp009; SI page S9 · Fabrication of Schottky device
SolventN,N-dimethylformamide (DMF)not specifiedp009; SI page S9 · Fabrication of Schottky device
OtherITO-coated glass substrateNot specifiedp009; SI page S9 · Fabrication of Schottky device
OtherAluminium top electrodeeffective diode area 7.065e-6 m2p009; SI page S9 · Fabrication of Schottky device