Synthesis evidence

Three-Dimensional-Coordination Polymer of Zn(II)-Carboxylate: Structural Elucidation, Photoelectrical Conductivity, and Biological Activity

Chandra A., Das M., Pal K. et al. · ACS Omega · 2019 · 17649-17661

3 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

17658 · Experimental Section, Schottky Device and I-V Measurements

SolventsN,N-dimethylformamide (DMF)
Atmosphereambient for I-V; vacuum drying and Al evaporation
Temperaturenormal temperature for measurement; deposition temperature not stated
Timesubstrate ultrasonication 20 min; spin coating 1 min per cycle, four cycles
Substrate orientationITO-coated glass
Work-upITO cleaned with 2-propanol, acetone and water; film dried under vacuum; Al electrode thermally evaporated at 10^-6 Torr through shadow mask
Activationvacuum drying after spin coating
Scalability contextSpin-coated device film thickness reported as 1 um.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized compound 1not stated17658 · Experimental Section, Schottky Device and I-V Measurements
SolventN,N-dimethylformamide (DMF)not stated17658 · Experimental Section, Schottky Device and I-V Measurements
OtherITO-coated glass substrateNot specified17658 · Experimental Section, Schottky Device and I-V Measurements
OtherAl electrodethermally evaporated at 10^-6 Torr17658 · Experimental Section, Schottky Device and I-V Measurements
Complete recipeSource: Main

Route 2: Liquid Liquid Interface

17657 · Experimental Section, Synthesis of Compound

Metal precursorsZn(NO3)2.6H2O
Linker precursorsppmh; H2bdc
SolventsMeOH, water, MeOH/H2O buffer, EtOH
AdditivesEt3N base to neutralise H2bdc
Atmospherenot stated
Temperatureroom temperature implied; exact temperature not stated
Time3 weeks
Work-upbrown crystals collected; no activation or solvent exchange reported
Activationnone reported
Scalability context163.4 mg isolated, 60% yield.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Linkerppmh39.6 mg, 0.2 mmol17657 · Experimental Section, Synthesis of Compound
Metal SourceZn(NO3)2.6H2O60 mg, 0.2 mmol17657 · Experimental Section, Synthesis of Compound
LinkerH2bdc33.2 mg, 0.2 mmol17657 · Experimental Section, Synthesis of Compound
BaseEt3N0.021 g, 0.2 mmol17657 · Experimental Section, Synthesis of Compound
SolventMeOH2 mL for ppmh plus MeOH/H2O buffer 1:1 v/v, 2 mL17657 · Experimental Section, Synthesis of Compound
Solventwater2 mL for Zn(NO3)2.6H2O plus MeOH/H2O buffer 1:1 v/v, 2 mL17657 · Experimental Section, Synthesis of Compound
SolventEtOH2 mL for H2bdc/Et3N solution17657 · Experimental Section, Synthesis of Compound
Complete recipeSource: Main

Route 3: Other

17657 · Experimental Section, Synthesis of Compound

Linker precursors4-pyridine carboxaldehyde; 2-hydrazinopyridine
SolventsMeOH; hot MeOH for recrystallisation; Et2O wash
Additivesfew drops of AcOH
Atmospherenot stated
Temperaturereflux; exact temperature not stated
Time0.5 h aldehyde stirring + 1 h after hydrazinopyridine addition + 24 h reflux
Work-upcooled; yellow crystals filtered, washed with Et2O, dissolved in hot minimum MeOH and recrystallised by slow evaporation
Activationnone reported
Scalability context356 mg isolated, 90% yield.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker4-Pyridine carboxaldehyde214 mg, 2 mmol17657 · Experimental Section, Synthesis of Compound
Linker2-hydrazinopyridine218 mg, 2 mmol17657 · Experimental Section, Synthesis of Compound
SolventMeOH5 mL plus hot minimum volume for recrystallisation17657 · Experimental Section, Synthesis of Compound
AcidAcOHa few drops17657 · Experimental Section, Synthesis of Compound
SolventEt2Owash17657 · Experimental Section, Synthesis of Compound