Synthesis evidence

Photodimerization of a 1D Ladder Polymer through Single-Crystal to Single-Crystal Transformation Has an Effect on Electrical Conductivity

Islam S., Datta J., Maity S. et al. · Crystal Growth and Design · 2019 · 4057-4062

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

p002 / article p.4058 · Experimental Section - Device Fabrication and Characterization

Metal precursorssynthesised compound 1
SolventsDMF dispersion medium
Atmosphereambient fabrication followed by vacuum drying and vacuum Al deposition
Time0.033 h spin coating
Substrate orientationFTO-coated glass
Work-upFTO glass cleaned sequentially with 2-isopropanol, acetone, and distilled water; dispersion spin coated at 800 rpm for 2 min; film dried in vacuum chamber; Al deposited by vacuum coating through shadow mask.
Activationvacuum drying before Al deposition
Scalability contextEffective device area controlled with a shadow mask, but area value was not reported in the main text.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1dispersed as per the concentration of 4 mg/uL · 4 mg/uLp002 / article p.4058 · Experimental Section - Device Fabrication and Characterization
SolventDMFnot reportedp002 / article p.4058 · Experimental Section - Device Fabrication and Characterization
OtherFTO coated glass substratenot reportedp002 / article p.4058 · Experimental Section - Device Fabrication and Characterization
OtherAl metal top electrodenot reportedp002 / article p.4058 · Experimental Section - Device Fabrication and Characterization
Complete recipeSource: Main

Route 2: Liquid Liquid Interface

p002 / article p.4058 · Experimental Section - Syntheses of Compounds

Metal precursorsCd(NO3)2.4H2O (0.062 g, 0.2 mmol); abstract lists Cd(NO3)2.6H2O
Linker precursorsbpe (0.036 g, 0.2 mmol); H2p-brba (0.040 g, 0.2 mmol) neutralised with Et3N
SolventsMeOH (2 mL), H2O (2 mL), DMF buffer solution (2 mL), EtOH (2 mL)
AdditivesEt3N (0.021 g, 0.2 mmol); DMF buffer solution
Atmospherekept in a dark cabinet; gas atmosphere not reported
Temperatureroom temperature not otherwise specified
Time168
Work-upColourless block crystals collected after one week; no washing/drying workup reported in main text.
Activationnone reported
Scalability context0.097 g product, 70% yield.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.4H2O0.062 g, 0.2 mmolp002 / article p.4058 · Experimental Section - Syntheses of Compounds
Linker1,2-bis(4-pyridyl)ethylene (bpe)0.036 g, 0.2 mmolp002 / article p.4058 · Experimental Section - Syntheses of Compounds
LinkerH2p-brba / para-bromobenzoic acid0.040 g, 0.2 mmolp002 / article p.4058 · Experimental Section - Syntheses of Compounds
BaseEt3N0.021 g, 0.2 mmolp002 / article p.4058 · Experimental Section - Syntheses of Compounds
SolventMeOH2 mLp002 / article p.4058 · Experimental Section - Syntheses of Compounds
SolventH2O2 mLp002 / article p.4058 · Experimental Section - Syntheses of Compounds
SolventDMF buffer solution2 mLp002 / article p.4058 · Experimental Section - Syntheses of Compounds
SolventEtOH2 mLp002 / article p.4058 · Experimental Section - Syntheses of Compounds
Partial recipeSource: Main

Route 3: Other

p002 / article p.4058 · Experimental Section - Device Fabrication and Characterization

Metal precursorssynthesised compound 2
SolventsDMF dispersion medium
Atmosphereambient fabrication followed by vacuum drying and vacuum Al deposition
Time0.033 h spin coating
Substrate orientationFTO-coated glass
Work-upFTO glass cleaned sequentially with 2-isopropanol, acetone, and distilled water; dispersion spin coated at 800 rpm for 2 min; film dried in vacuum chamber; Al deposited by vacuum coating through shadow mask.
Activationvacuum drying before Al deposition
Scalability contextEffective device area controlled with a shadow mask, but area value was not reported in the main text.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 2dispersed as per the concentration of 4 mg/uL · 4 mg/uLp002 / article p.4058 · Experimental Section - Device Fabrication and Characterization
SolventDMFnot reportedp002 / article p.4058 · Experimental Section - Device Fabrication and Characterization
OtherFTO coated glass substratenot reportedp002 / article p.4058 · Experimental Section - Device Fabrication and Characterization
OtherAl metal top electrodenot reportedp002 / article p.4058 · Experimental Section - Device Fabrication and Characterization
Complete recipeSource: Main

Route 4: Other

p002-p003 / article pp.4058-4059 · Experimental Section - Materials and Methods; Syntheses of Compounds; Results and Discussion · Figure 1

Metal precursorssingle crystals of compound 1
Linker precursorsbpe ligands in compound 1 undergo [2 + 2] photodimerisation to rctt-tpcb
Solventssolvent-free solid-state irradiation
Atmosphereroom-temperature irradiation; gas atmosphere not reported
Temperatureroom temperature
Time0.5
Oxidant / reductantUV light, approximately 350 nm, 8 W UVA lamps
Work-upLight yellow block crystals obtained; no further workup reported.
Activationnone reported
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercrystals of compound 1not reportedp002-p003 / article pp.4058-4059 · Experimental Section - Materials and Methods; Syntheses of Compounds; Results and Discussion · Figure 1
OtherUV irradiation8 W UVA lamps, approximately 350 nm, 30 minp002-p003 / article pp.4058-4059 · Experimental Section - Materials and Methods; Syntheses of Compounds; Results and Discussion · Figure 1