Synthesis evidence

Biporous Cd(II) Coordination Polymer via in Situ Disulfide Bond Formation: Self-Healing and Application to Photosensitive Optoelectronic Device

Naskar K., Dey A., Maity S. et al. · Inorganic Chemistry · 2020 · 5518-5528

2 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

2 · Experimental Section - Synthesis

Metal precursorsCdI2 (0.074 g, 0.2 mmol)
Linker precursorsisoniazid/INH (0.028 g, 0.2 mmol); neutralised 2-mercaptobenzoic acid/2-MBA (0.031 g, 0.2 mmol)
Solventswater (2 mL); 1:1 v/v DMF-H2O buffer solution (2 mL); methanol (10 mL); ethanol (2 mL)
AdditivesEt3N used to neutralise 2-MBA
Atmosphereair; authors state the oxidative in situ disulfide-bond generation occurs in the presence of air
Temperatureroom temperature not explicitly stated
Time168
Oxidant / reductantAir/O2 acts as oxidant for in situ oxidation of thiol groups to disulfide.
Work-upPrism-shaped yellow crystals isolated after 1 week; no washing protocol reported for crystals.
Activationnone reported
Scalability contextSmall solution-layering crystallisation; 43 mg product, 75% yield.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCdI20.074 g, 0.2 mmol2 · Experimental Section - Synthesis
Linkerisoniazid (INH)0.028 g, 0.2 mmol2 · Experimental Section - Synthesis
Linker2-MBA (2-mercaptobenzoic acid), neutralized by Et3N0.031 g, 0.2 mmol2 · Experimental Section - Synthesis
Solventwater2 mL2 · Experimental Section - Synthesis
Solvent1:1 (v/v) DMF-H2O buffer solution2 mL2 · Experimental Section - Synthesis
Solventmethanol10 mL2 · Experimental Section - Synthesis
Solventethanol2 mL2 · Experimental Section - Synthesis
BaseEt3Nnot reported2 · Experimental Section - Synthesis
Complete recipeSource: Both

Route 2: Other

S8-S9 · Device Fabrication and Measurements · Scheme S1

SolventsN,N-dimethylformamide (DMF)
Atmosphereambient conditions for measurements; vacuum oven drying; Al deposition at 10^-6 Torr
Temperature80 for drying
Timespin coating 5 min at 600 rpm plus 5 min at 1000 rpm; drying for several minutes
Substrate orientationITO-coated glass substrate; Al top electrode deposited through shadow mask
Work-upDMF dispersion of compound 1 (30 mg/mL) sonicated, spin-coated on ITO glass, vacuum dried at 80 deg C, then aluminium electrode deposited with effective area 7.065 x 10^-6 m2.
Activationvacuum oven drying at 80 deg C to remove solvent
Scalability contextDevice-scale spin coating; film thickness measured as approximately 1 um.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized compound 130 mg/ml dispersion · 30 mg/ml in DMFS8-S9 · Device Fabrication and Measurements · Scheme S1
SolventN,N-dimethylformamide (DMF)not reportedS8-S9 · Device Fabrication and Measurements · Scheme S1
OtherITO coated glass substrateNot specifiedS8-S9 · Device Fabrication and Measurements · Scheme S1
Otheraluminium electrodesdeposited at 10^-6 Torr; effective area 7.065 x 10^-6 m2S8-S9 · Device Fabrication and Measurements · Scheme S1