Synthesis evidence

Pyridyl-Isonicotinoyl Hydrazone-Bridged Zn(II) Coordination Framework with Thiophenedicarboxylato Link: Structure, Biological Activity, and Electrical Conductivity

Shit M., Halder S., Dey A. et al. · Inorganic Chemistry · 2023 · 19937-19947

2 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

rendered page 2 / article p.19938 · Experimental Section - Synthesis · Scheme 1

Metal precursorsZn(NO3)2.6H2O (0.060 g, 0.2 mmol) in water (2 mL)
Linker precursorspcih (0.045 g, 0.2 mmol) in methanol (2 mL); H2tdc (0.035 g, 0.2 mmol) neutralized with Et3N (0.042 g, 0.4 mmol) in EtOH (2 mL)
Solventsmethanol, water, DMF/MeOH buffer (2 mL, 1:1 v/v), ethanol
AdditivesEt3N used to neutralize H2tdc; DMF/MeOH buffer
Atmospherenot reported in main text
Temperatureroom temperature implied for layered crystallisation but not explicitly reported
Time168
Work-upBlock-shaped yellow crystals isolated after 7 days; further washing/drying not reported in main text or SI.
Activationnot reported
Scalability contextSmall-batch layered crystallisation; reported isolated amount 0.201 g and 70% yield.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Linkerpyridine-4-carboxaldehyde isonicotinoyl hydrazine (pcih)0.045 g, 0.2 mmol · in methanol (2 mL)rendered page 2 / article p.19938 · Experimental Section - Synthesis · Scheme 1
Metal SourceZn(NO3)2.6H2O0.060 g, 0.2 mmol · in water (2 mL)rendered page 2 / article p.19938 · Experimental Section - Synthesis · Scheme 1
SolventDMF and MeOH buffer2 mL, 1:1 v/vrendered page 2 / article p.19938 · Experimental Section - Synthesis · Scheme 1
LinkerH2tdc / 2,5-thiophene dicarboxylic acid0.035 g, 0.2 mmol · in EtOH (2 mL) after neutralisationrendered page 2 / article p.19938 · Experimental Section - Synthesis · Scheme 1
BaseEt3N0.042 g, 0.4 mmol · used to neutralize H2tdcrendered page 2 / article p.19938 · Experimental Section - Synthesis · Scheme 1
SolventEtOH2 mLrendered page 2 / article p.19938 · Experimental Section - Synthesis · Scheme 1
Partial recipeSource: SI

Route 2: Other

rendered page 18 / SI p.S18 · Device Fabrication

Metal precursorspre-synthesised compound 1
Linker precursorspre-synthesised compound 1
SolventsN,N-dimethylformamide (DMF)
Atmosphereambient conditions for fabrication/measurement; vacuum oven drying
Temperature80 for vacuum drying; room temperature for device measurement
Time0.083 h at 600 rpm plus 0.083 h at 900 rpm spin coating; drying for several minutes
Substrate orientationITO-coated glass substrate; sandwich MS junction
Work-upFresh 18 mg/mL DMF dispersion spin-coated, vacuum dried at 80 deg C, and metal electrode deposited through shadow mask with effective area 7.065 x 10^-2 cm^2.
Activationvacuum drying at 80 deg C to remove solvent
Scalability contextSpin-coated thin-film device recipe; not a bulk framework synthesis.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othersynthesized compound 118 mg/ml · dispersion in DMFrendered page 18 / SI p.S18 · Device Fabrication
SolventN,N-dimethylformamide (DMF)Not specifiedrendered page 18 / SI p.S18 · Device Fabrication
OtherITO-coated glass substrateNot specifiedrendered page 18 / SI p.S18 · Device Fabrication
OtherAl top electrode / gold metal electrode (inconsistent SI wording)effective area 7.065 x 10^-2 cm^-2 as printed in SIrendered page 18 / SI p.S18 · Device Fabrication