Synthesis evidence

Exploration of Variable Temperature Magnetism and Electrical Properties of a Pyridyl-isonicotinoyl Hydrazone Bridged Three-Dimensional Mn-Metal-Organic Framework with a Thiophene Dicarboxylato Link

Shit M., Sahoo D., Dutta B. et al. · Crystal Growth and Design · 2022 · 7143-7152

3 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

3 · Electrochemical Measurement

SolventsN-methyl-2-pyrrolidone (NMP)
Additivesgraphite powder and PVDF binder
Atmospherevacuum drying after drop casting
Temperature325 K (51.85 C) drying
Time4
Substrate orientationtop surface of a glassy carbon rod working electrode
Work-upslurry drop-cast on glassy carbon rod and dried in vacuum
Activationvacuum dried at 325 K for 4 h
Scalability contextElectrode recipe only; no active mass loading or geometric area reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Othersynthesized material / compound 185 wt %3 · Electrochemical Measurement
Additivegraphite powder10 wt %3 · Electrochemical Measurement
AdditivePVDF5 wt %3 · Electrochemical Measurement
SolventN-methyl-2-pyrrolidone (NMP)not reported3 · Electrochemical Measurement
Otherglassy carbon rodNot specified3 · Electrochemical Measurement
Partial recipeSource: Main

Route 2: Other

2 · Device Fabrication and Optical Measurements

SolventsDMF dispersion; Extran MA 02, distilled water, ethanol, acetone and IPA used for ITO cleaning
Atmosphereambient processing; not otherwise reported
Temperature90 C substrate drying for 1 h; 95 C hot plate for 15 min after spin coating
Timespin coating 60 s per coat, repeated once; ITO drying 1 h; hot plate drying 0.25 h
Substrate orientationITO-coated glass substrate; Al top electrodes through mask
Work-upcrushed crystals dispersed in DMF, spin coated at 1000 rpm, dried; aluminium electrodes deposited with 3 x 3 mm2 effective area
Activationsolvent evaporated on hot plate at 95 C for 15 min
Scalability contextSmall-area device, 3 x 3 mm2 active area.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1 crushed crystals15 mg · 15 mg in 1 mL DMF2 · Device Fabrication and Optical Measurements
SolventDMF1 mL2 · Device Fabrication and Optical Measurements
OtherITO-coated glass substrateNot specified2 · Device Fabrication and Optical Measurements
OtherAl electrodes3 x 3 mm2 effective area2 · Device Fabrication and Optical Measurements
Partial recipeSource: Main

Route 3: Liquid Liquid Interface

2 · Synthesis of Compound 1 · Scheme 1

Metal precursorsMnCl2.4H2O (0.039 g, 0.2 mmol)
Linker precursorspcih (0.045 g, 0.2 mmol); tdc2- (0.035 g, 0.2 mmol), neutralised with Et3N
SolventsMeOH, water, DMF/MeOH buffer (1:1 v/v), EtOH
AdditivesEt3N (0.042 g, 0.4 mmol)
Atmospherenot reported
Temperaturenot reported; apparently ambient layered crystallisation
Time168
Work-upyellow needle-shaped crystals collected; yield 0.201 g, 70%; no washing details reported
Activationnot reported
Scalability contextLayered crystallisation over 7 days; no scale-up information.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMnCl2.4H2O0.039 g, 0.2 mmol2 · Synthesis of Compound 1 · Scheme 1
Linkerpcih0.045 g, 0.2 mmol2 · Synthesis of Compound 1 · Scheme 1
Linkertdc2-0.035 g, 0.2 mmol2 · Synthesis of Compound 1 · Scheme 1
BaseEt3N0.042 g, 0.4 mmol2 · Synthesis of Compound 1 · Scheme 1
SolventMeOH2 mL for pcih layer; also in 2 mL DMF/MeOH buffer · DMF/MeOH 1:1 v/v buffer2 · Synthesis of Compound 1 · Scheme 1
Solventwater2 mL for MnCl2.4H2O solution2 · Synthesis of Compound 1 · Scheme 1
SolventDMFpart of 2 mL DMF/MeOH buffer · DMF/MeOH 1:1 v/v2 · Synthesis of Compound 1 · Scheme 1
SolventEtOH2 mL for neutralised tdc2- layer2 · Synthesis of Compound 1 · Scheme 1