Synthesis evidence

Construction of a Succinate-Bridged Cd(II)-Based Two-Dimensional Coordination Polymer for Efficient Optoelectronic Device Fabrication and Explosive Sensing Application

Dutta B., Hazra A., Dey A. et al. · Crystal Growth and Design · 2020 · 765-776

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

S6-S7 · Sensing Application · Figure S6

Metal precursorsAs-synthesised compound 1
Linker precursorsNot applicable after compound synthesis
Solventsacetonitrile (ACN)
AdditivesepNAC analytes added during sensing; TNP stock solution 1 x 10^-4 M for detection limit
Atmosphereambient/not specified
Temperatureroom temperature/not specified
Substrate orientationsolution/dispersion fluorescence cuvette not otherwise specified
Oxidant / reductantnone reported
Work-upDisperse 1 mg compound 1 in 5 mL ACN; add analyte solutions incrementally.
Activationnone reported
Scalability contextAnalytical sensing preparation only.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 11 mg · 1 mg in 5 mL ACNS6-S7 · Sensing Application · Figure S6
Solventacetonitrile (ACN)5 mLS6-S7 · Sensing Application · Figure S6
AdditiveTNPincremental additions · 1 x 10^-4 M stock solutionS6-S7 · Sensing Application · Figure S6
Complete recipeSource: Main

Route 2: Other

766 · Synthesis of Compound 1

Metal precursorsCd(NO3)2.4H2O (0.062 g, 0.2 mmol)
Linker precursors4-nvp (0.046 g, 0.2 mmol); H2suc/succinic acid (0.023 g, 0.2 mmol)
SolventsMeOH (2 mL), H2O (2 mL), 1:1 v/v DMF/H2O buffer solution (2 mL), EtOH (2 mL)
AdditivesEt3N (0.042 g, 0.4 mmol) to neutralise H2suc
Atmosphereambient/not specified
Temperatureroom temperature/not specified
Time72
Substrate orientationlayered solution growth; no substrate
Oxidant / reductantnone reported
Work-upYellow needle-shaped crystals collected after 3 days; no washing/drying details reported.
Activationnone reported
Scalability contextSmall-batch layered crystallisation; 0.201 g product, 70% yield.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecadmium(II) nitrate tetrahydrate, Cd(NO3)2.4H2O0.062 g, 0.2 mmol766 · Synthesis of Compound 1
Linker4-(1-naphthylvinyl)pyridine (4-nvp)0.046 g, 0.2 mmol766 · Synthesis of Compound 1
Linkersuccinic acid (H2suc)0.023 g, 0.2 mmol766 · Synthesis of Compound 1
BaseEt3N0.042 g, 0.4 mmol766 · Synthesis of Compound 1
SolventMeOH2 mL766 · Synthesis of Compound 1
SolventH2O2 mL plus part of 2 mL 1:1 DMF/H2O buffer766 · Synthesis of Compound 1
SolventDMFpart of 2 mL 1:1 DMF/H2O buffer766 · Synthesis of Compound 1
SolventEtOH2 mL766 · Synthesis of Compound 1
Complete recipeSource: Main

Route 3: Other

766-767 · Device Fabrication

Metal precursorsAs-synthesised compound 1; Al electrode source not specified
Linker precursorsNot applicable after compound synthesis
SolventsN,N-dimethylformamide (DMF)
Additivesnone reported
Atmosphereambient for preparation/measurement; vacuum oven at 5 x 10^-3 Torr; Al deposition at 10^-6 Torr
Temperature75 for vacuum drying
Timespin coating 5 min at 700 rpm plus 6 min at 1000 rpm; drying several minutes
Substrate orientationITO-coated glass substrate; Al top electrodes deposited through shadow mask
Oxidant / reductantnone reported
Work-upDMF dispersion sonicated, spin-coated, vacuum-dried to remove solvent, Al evaporated.
ActivationVacuum drying at 75 deg C for several minutes.
Scalability contextDevice-scale spin coating; effective area 7.065 x 10^-2 cm2 (reported also as 7.065 x 10^-6 m2).
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 135 mg/mL dispersion · 35 mg/mL766-767 · Device Fabrication
SolventN,N-dimethylformamide (DMF)not specified766-767 · Device Fabrication
OtherITO-coated glass substratenot specified766-767 · Device Fabrication
OtherAl electrodenot specified766-767 · Device Fabrication
Partial recipeSource: Main

Route 4: Other

767 · Optical Characterization · Figure 2

Metal precursorsAs-synthesised compound 1
Linker precursorsNot applicable after compound synthesis
SolventsDMF
Additivesnone reported
Atmospherenot specified
Substrate orientationnormal glass substrate
Oxidant / reductantnone reported
Work-upA stable DMF dispersion was used to prepare a film; deposition details not reported.
Activationnot specified
Scalability contextPreparation described only to support UV-vis band-gap measurement.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1not specified767 · Optical Characterization · Figure 2
SolventDMFnot specified767 · Optical Characterization · Figure 2
Othernormal glass substratenot specified767 · Optical Characterization · Figure 2