Synthesis evidence

Influence of Axial Linkers on Polymerization in Paddle-Wheel Cu(II) Coordination Polymers for the Application of Optoelectronics Devices

Jana S., Jana R., Sil S. et al. · Crystal Growth and Design · 2019 · 6283-6290

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: Liquid Liquid Interface

6-7 · Synthesis of Compounds 1 and 2 · Figure 14

Metal precursorsCu(NO3)2.3H2O (24.16 mg, 0.1 mmol) in water (1 mL)
Linker precursors4,4'-BPY (15.619 mg, 0.1 mmol) in methanol (1 mL); HDABA (21.726 mg, 0.1 mmol) in ethanol (1 mL)
Solventswater, methanol, ethanol, water-methanol mixed solvent
AdditivesEt3N (10.119 mg, 0.1 mmol) to neutralise HDABA
Atmospherenot specified
Temperatureroom temperature
Time168
Substrate orientationlayered diffusion in glass vessel; crystals deposited on glass wall
Work-upCrystals separated mechanically under a microscope, washed with methanol/water (1:1), and dried.
Activationdried; no separate activation reported
Scalability contextLayered diffusion single-crystal route; no scale-up route reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O24.16 mg, 0.1 mmol · in 1 mL aqueous solution6-7 · Synthesis of Compounds 1 and 2 · Figure 14
Linker4,4-BPY15.619 mg, 0.1 mmol · in 1 mL methanol6-7 · Synthesis of Compounds 1 and 2 · Figure 14
LinkerHDABA21.726 mg, 0.1 mmol · in 1 mL ethanol6-7 · Synthesis of Compounds 1 and 2 · Figure 14
BaseEt3N10.119 mg, 0.1 mmol6-7 · Synthesis of Compounds 1 and 2 · Figure 14
Solventwater-methanol mixed solventNot specified6-7 · Synthesis of Compounds 1 and 2 · Figure 14
Complete recipeSource: SI

Route 2: Other

7 · Fabrication of Schottky device

Metal precursorspre-synthesised compound 1
SolventsN,N-dimethylformamide (DMF); substrate cleaning with 2-propanol, distilled water and acetone
Atmospherevacuum drying; Al evaporation under 10-6 Torr
Temperatureroom temperature not explicitly stated for coating/evaporation
Time0.033 for spin coating step (2 min)
Substrate orientationITO-coated glass; Al/compound/ITO sandwich junction with shadow mask
Work-upITO cleaned sequentially by 2-propanol, distilled water and acetone with repeated ultrasonication, dried in vacuum; compound dispersion spin coated at 800 rpm for 2 min; film dried under vacuum; Al thermally evaporated.
Activationdried under vacuum condition
Scalability contextSpin-coating route for thin-film device; no large-area scale-up reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1not specified · dispersed in DMF7 · Fabrication of Schottky device
SolventN,N-dimethylformamide (DMF)not specified7 · Fabrication of Schottky device
Solvent2-propanol, distilled water and acetonenot specified · substrate cleaning solvents7 · Fabrication of Schottky device
OtherAlnot specified · thermally evaporated top contact7 · Fabrication of Schottky device
OtherITO-coated glassnot specified · substrate7 · Fabrication of Schottky device
Complete recipeSource: Main

Route 3: Liquid Liquid Interface

7 · Synthesis of Compounds 1 and 2

Metal precursorsCu(NO3)2.3H2O (24.16 mg, 0.1 mmol) in water (1 mL)
Linker precursorsPYZ (8.009 mg, 0.1 mmol); HDABA (21.726 mg, 0.1 mmol) in ethanol (1 mL)
Solventswater, methanol, ethanol, water-methanol mixed solvent
AdditivesEt3N (10.119 mg, 0.1 mmol) to neutralise HDABA
Atmospherenot specified
Temperatureroom temperature
Time168
Substrate orientationlayered diffusion in glass vessel; crystals deposited on glass wall
Work-upBlue block-shaped crystals deposited on the glass wall; same separation/washing/drying procedure as compound 1 unless otherwise specified.
Activationdried; no separate activation reported
Scalability contextLayered diffusion single-crystal route; no scale-up route reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O24.16 mg, 0.1 mmol · in 1 mL aqueous solution7 · Synthesis of Compounds 1 and 2
LinkerPYZ8.009 mg, 0.1 mmol7 · Synthesis of Compounds 1 and 2
LinkerHDABA21.726 mg, 0.1 mmol · in 1 mL ethanol7 · Synthesis of Compounds 1 and 2
BaseEt3N10.119 mg, 0.1 mmol7 · Synthesis of Compounds 1 and 2
Solventwater-methanol mixed solventNot specified7 · Synthesis of Compounds 1 and 2
Complete recipeSource: SI

Route 4: Other

7 · Fabrication of Schottky device

Metal precursorspre-synthesised compound 2
SolventsN,N-dimethylformamide (DMF); substrate cleaning with 2-propanol, distilled water and acetone
Atmospherevacuum drying; Al evaporation under 10-6 Torr
Temperatureroom temperature not explicitly stated for coating/evaporation
Time0.033 for spin coating step (2 min)
Substrate orientationITO-coated glass; Al/compound/ITO sandwich junction with shadow mask
Work-upITO cleaned sequentially by 2-propanol, distilled water and acetone with repeated ultrasonication, dried in vacuum; compound dispersion spin coated at 800 rpm for 2 min; film dried under vacuum; Al thermally evaporated.
Activationdried under vacuum condition
Scalability contextSpin-coating route for thin-film device; no large-area scale-up reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 2not specified · dispersed in DMF7 · Fabrication of Schottky device
SolventN,N-dimethylformamide (DMF)not specified7 · Fabrication of Schottky device
Solvent2-propanol, distilled water and acetonenot specified · substrate cleaning solvents7 · Fabrication of Schottky device
OtherAlnot specified · thermally evaporated top contact7 · Fabrication of Schottky device
OtherITO-coated glassnot specified · substrate7 · Fabrication of Schottky device