Synthesis evidence

Exploration of semiconducting properties of Zn(ii)- And Cd(ii)-based coordination polymers with dicarboxylate of a chair-type backbone

Akhtaruzzaman, Pal B., Khan S. et al. · CrystEngComm · 2021 · 7525-7533

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

7527 · Device fabrication

SolventsN,N-dimethylformamide (DMF)
AtmosphereAl electrode deposited under 10^-6 Torr
Time2 h ultrasonication; 2 min spin coating
Substrate orientationITO-coated glass substrate
Work-upITO glass cleaned sequentially with 2-propanol, acetone and distilled water; CP 1/DMF dispersion spin-coated at 1000 rpm for 2 min; film vacuum dried; Al electrode vacuum deposited.
Activationvacuum oven drying; temperature and time not reported
Scalability contextSpin-coated thin-film device fabrication; dispersion concentration and drying conditions not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized CP 1Not specified7527 · Device fabrication
SolventN,N-dimethylformamide (DMF)Not specified7527 · Device fabrication
OtherITO-coated glass substrateNot specified7527 · Device fabrication
OtherAl electrodeNot specified7527 · Device fabrication
Complete recipeSource: Main

Route 2: Liquid Liquid Interface

7526 · Synthesis of CP 1 and CP 2

Metal precursorsCd(NO3)2.4H2O (0.062 g, 0.2 mmol)
Linker precursors1,10-phenanthroline (0.036 g, 0.2 mmol); 1,4-H2chdc (0.034 g, 0.2 mmol)
SolventsMeOH, H2O, 1:1 MeOH/H2O buffer solution, EtOH
AdditivesEt3N (0.021 g, 0.2 mmol) used to neutralise 1,4-H2chdc
Atmospherenot specified; room-temperature slow diffusion
Temperatureroom temperature
Timefew days
Work-upColourless block crystals collected after a few days; yield 0.069 g, 68%.
Activationnone reported
Scalability contextSmall-volume layered slow-diffusion crystal growth; no scale-up information reported.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.4H2O0.062 g, 0.2 mmol7526 · Synthesis of CP 1 and CP 2
Linker1,10-phenanthroline (1,10-phen)0.036 g, 0.2 mmol7526 · Synthesis of CP 1 and CP 2
Linker1,4-H2chdc0.034 g, 0.2 mmol7526 · Synthesis of CP 1 and CP 2
BaseEt3N0.021 g, 0.2 mmol7526 · Synthesis of CP 1 and CP 2
SolventMeOH2 mL plus part of 2 mL 1:1 MeOH/H2O buffer7526 · Synthesis of CP 1 and CP 2
SolventH2O2 mL plus part of 2 mL 1:1 MeOH/H2O buffer7526 · Synthesis of CP 1 and CP 2
SolventEtOH2 mL7526 · Synthesis of CP 1 and CP 2
Partial recipeSource: Main

Route 3: Other

7527 · Device fabrication

SolventsN,N-dimethylformamide (DMF)
AtmosphereAl electrode deposited under 10^-6 Torr
Time2 h ultrasonication; 2 min spin coating
Substrate orientationITO-coated glass substrate
Work-upITO glass cleaned sequentially with 2-propanol, acetone and distilled water; CP 2/DMF dispersion spin-coated at 1000 rpm for 2 min; film vacuum dried; Al electrode vacuum deposited.
Activationvacuum oven drying; temperature and time not reported
Scalability contextSpin-coated thin-film device fabrication; dispersion concentration and drying conditions not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized CP 2Not specified7527 · Device fabrication
SolventN,N-dimethylformamide (DMF)Not specified7527 · Device fabrication
OtherITO-coated glass substrateNot specified7527 · Device fabrication
OtherAl electrodeNot specified7527 · Device fabrication
Complete recipeSource: Main

Route 4: Liquid Liquid Interface

7526 · Synthesis of CP 1 and CP 2

Metal precursorsZn(NO3)2.6H2O (0.059 g, 0.2 mmol)
Linker precursors1,10-phenanthroline (0.036 g, 0.2 mmol); 1,4-H2chdc (0.034 g, 0.2 mmol)
SolventsMeOH, H2O, 1:1 MeOH/H2O buffer solution, EtOH
AdditivesEt3N (0.021 g, 0.2 mmol) used to neutralise 1,4-H2chdc
Atmospherenot specified; room-temperature slow diffusion
Temperatureroom temperature
Timefew days
Work-upColourless block crystals collected after a few days; yield 0.061 g, 70%.
Activationnone reported
Scalability contextSmall-volume layered slow-diffusion crystal growth; no scale-up information reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O0.059 g, 0.2 mmol7526 · Synthesis of CP 1 and CP 2
Linker1,10-phenanthroline (1,10-phen)0.036 g, 0.2 mmol7526 · Synthesis of CP 1 and CP 2
Linker1,4-H2chdc0.034 g, 0.2 mmol7526 · Synthesis of CP 1 and CP 2
BaseEt3N0.021 g, 0.2 mmol7526 · Synthesis of CP 1 and CP 2
SolventMeOH/H2O/EtOHsame as CP 1 route7526 · Synthesis of CP 1 and CP 2