Synthesis evidence

Synthesis of a Cd(ii) based 1D coordination polymer by: In situ ligand generation and fabrication of a photosensitive electronic device

Dutta B., Jana R., Sinha C. et al. · Inorganic Chemistry Frontiers · 2018 · 1998-2005

2 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

1999 · Device fabrication and characterization

Metal precursorsThermally evaporated Al top electrode
SolventsDMF dispersion medium; propanol, ethanol, and distilled water for ITO cleaning
AtmosphereVacuum oven drying; vacuum coating for Al deposition
Temperature50
Substrate orientationITO-coated glass substrate
Work-upITO cleaned ultrasonically; compound 1 dispersion spin-coated at 1200 rpm for 2 min; dried in vacuum oven at 50 deg C; Al electrode deposited by thermal evaporation; diode area 7.065 x 10^-2 cm2.
ActivationNo framework activation reported; film dried at 50 deg C.
Scalability contextSpin-coated small-area device; no scale-up discussion.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1appropriate weight ratio1999 · Device fabrication and characterization
SolventDMFNot specified1999 · Device fabrication and characterization
Solventpropanolused repeatedly for ITO cleaning1999 · Device fabrication and characterization
Solventethanolused repeatedly for ITO cleaning1999 · Device fabrication and characterization
Solventdistilled waterused repeatedly for ITO cleaning1999 · Device fabrication and characterization
OtherAltop electrode; deposited by thermal evaporation1999 · Device fabrication and characterization
Partial recipeSource: Main

Route 2: Liquid Liquid Interface

1999 · Synthesis of compound

Metal precursorsCd(NO3)2.4H2O (0.062 g, 0.2 mmol)
Linker precursors4-nvp (0.046 g, 0.2 mmol); 2-mba (0.031 g, 0.2 mmol), neutralised with Et3N
SolventsMeOH (2 mL), H2O (2 mL), 1:1 DMF/H2O buffer (2 mL), EtOH (2 mL)
AdditivesEt3N (0.010 g, 0.1 mmol)
AtmosphereOxidative medium favoured; no controlled atmosphere reported
Time72
Oxidant / reductantNo separate oxidant stated; in situ oxidation of 2-mba mercapto groups forms the S-S bond.
Work-upYellow needle crystals obtained after three days; no washing or drying workup reported in the main text.
ActivationNo activation reported
Scalability contextSlow layered diffusion on millilitre scale; no scalability discussion.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.4H2O0.062 g, 0.2 mmol1999 · Synthesis of compound
Linker4-nvp0.046 g, 0.2 mmol1999 · Synthesis of compound
Linker2-mba0.031 g, 0.2 mmol1999 · Synthesis of compound
BaseEt3N0.010 g, 0.1 mmol1999 · Synthesis of compound
SolventMeOH2 mL1999 · Synthesis of compound
SolventH2O2 mL plus 1 mL in 1:1 DMF/H2O buffer1999 · Synthesis of compound
SolventDMF1 mL in 2 mL 1:1 DMF/H2O buffer1999 · Synthesis of compound
SolventEtOH2 mL1999 · Synthesis of compound