Synthesis evidence

Intercatenated Coordination Polymers (ICPs) of Carboxylato Bridged Zn(II)-Isoniazid and Their Electrical Conductivity

Naskar K., Dey A., Dutta B. et al. · Crystal Growth and Design · 2017 · 3267-3276

6 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Liquid Liquid Interface

main p.3 · Synthesis of [Zn2(INH)2(succ)2]n (1)

Metal precursorsZn(NO3)2.6H2O (0.297 g, 1 mmol)
Linker precursorsSuccinic acid (H2succ) (0.118 g, 1 mmol); isoniazid (0.137 g, 1 mmol)
SolventsWater (10 mL for Zn source); ethanol (10 mL for H2succ/Et3N solution; 10 mL for isoniazid solution); methanol/water 1:1 wash
AdditivesTriethylamine, Et3N (0.212 g, 2 mmol), used to neutralise succinic acid
AtmosphereAmbient; no inert atmosphere reported
Temperatureroom temperature (not explicitly stated)
Timeabout 168 h diffusion (one week)
Work-upCrystals separated mechanically under a microscope, washed with methanol/water (1:1), and dried.
ActivationNo activation reported.
Scalability contextLayer-diffusion single-crystal synthesis; small isolated yield of 0.026 g reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O0.297 g, 1 mmolmain p.3 · Synthesis of [Zn2(INH)2(succ)2]n (1)
Linkersuccinic acid (H2succ)0.118 g, 1 mmolmain p.3 · Synthesis of [Zn2(INH)2(succ)2]n (1)
Linkerisoniazid0.137 g, 1 mmolmain p.3 · Synthesis of [Zn2(INH)2(succ)2]n (1)
BaseEt3N0.212 g, 2 mmolmain p.3 · Synthesis of [Zn2(INH)2(succ)2]n (1)
Solventwater10 mLmain p.3 · Synthesis of [Zn2(INH)2(succ)2]n (1)
Solventethanol20 mL total in two 10 mL portionsmain p.3 · Synthesis of [Zn2(INH)2(succ)2]n (1)
Partial recipeSource: Main

Route 2: Liquid Liquid Interface

main p.3 · Synthesis

Metal precursorsZn(NO3)2.6H2O; identical procedure to 1
Linker precursorsFumaric acid (H2fum) substituted for succinic acid; isoniazid
SolventsWater and ethanol; methanol/water 1:1 wash inferred from identical procedure to 1
AdditivesTriethylamine (Et3N) inferred from identical procedure to 1
AtmosphereAmbient; no inert atmosphere reported
Temperatureroom temperature (not explicitly stated)
Timeabout 168 h diffusion (one week, from identical procedure)
Work-upSame mechanical separation, methanol/water washing, and drying as 1 inferred from identical procedure.
ActivationNo activation reported.
Scalability contextLayer-diffusion single-crystal synthesis; yield 79% reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2Oidentical procedure to 1; explicit mass not repeatedmain p.3 · Synthesis
Linkerfumaric acid (H2fum)identical procedure to 1; explicit mass not repeatedmain p.3 · Synthesis
Linkerisoniazididentical procedure to 1; explicit mass not repeatedmain p.3 · Synthesis
BaseEt3Nidentical procedure to 1; explicit mass not repeatedmain p.3 · Synthesis
Partial recipeSource: Main

Route 3: Liquid Liquid Interface

main p.3 · Synthesis

Metal precursorsZn(NO3)2.6H2O; identical procedure to 1
Linker precursorsTerephthalic acid (H2bdc) substituted for succinic acid; isoniazid
SolventsWater and ethanol; methanol/water 1:1 wash inferred from identical procedure to 1
AdditivesTriethylamine (Et3N) inferred from identical procedure to 1
AtmosphereAmbient; no inert atmosphere reported
Temperatureroom temperature (not explicitly stated)
Timeabout 168 h diffusion (one week, from identical procedure)
Work-upSame mechanical separation, methanol/water washing, and drying as 1 inferred from identical procedure.
ActivationNo activation reported.
Scalability contextLayer-diffusion single-crystal synthesis; yield 82% reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2Oidentical procedure to 1; explicit mass not repeatedmain p.3 · Synthesis
Linkerterephthalic acid (H2bdc)identical procedure to 1; explicit mass not repeatedmain p.3 · Synthesis
Linkerisoniazididentical procedure to 1; explicit mass not repeatedmain p.3 · Synthesis
BaseEt3Nidentical procedure to 1; explicit mass not repeatedmain p.3 · Synthesis
Complete recipeSource: Main

Route 4: Drop Cast

main p.6 · Fabrication of Schottky Device

SolventsDMSO dispersion of compound 1
AtmosphereNot reported
TimeSpin coating for 2 min
Substrate orientationITO-coated glass substrate; Al top contact
Work-upITO cleaned sequentially with soap solution, acetone, ethanol, and distilled water in an ultrasonic bath; film dried; Al thermally evaporated.
Scalability contextThin-film device fabrication, not bulk framework synthesis.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
SolventDMSONot specifiedmain p.6 · Fabrication of Schottky Device
OtherITO-coated glassNot specifiedmain p.6 · Fabrication of Schottky Device
OtherAl rectifier metal contactNot specifiedmain p.6 · Fabrication of Schottky Device
Complete recipeSource: Main

Route 5: Drop Cast

main p.6 · Fabrication of Schottky Device

SolventsDMSO dispersion of compound 2
AtmosphereNot reported
TimeSpin coating for 2 min
Substrate orientationITO-coated glass substrate; Al top contact
Work-upITO cleaned sequentially with soap solution, acetone, ethanol, and distilled water in an ultrasonic bath; film dried; Al thermally evaporated.
Scalability contextThin-film device fabrication, not bulk framework synthesis.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
SolventDMSONot specifiedmain p.6 · Fabrication of Schottky Device
OtherITO-coated glassNot specifiedmain p.6 · Fabrication of Schottky Device
OtherAl rectifier metal contactNot specifiedmain p.6 · Fabrication of Schottky Device
Complete recipeSource: Main

Route 6: Drop Cast

main p.6 · Fabrication of Schottky Device

SolventsDMSO dispersion of compound 3
AtmosphereNot reported
TimeSpin coating for 2 min
Substrate orientationITO-coated glass substrate; Al top contact
Work-upITO cleaned sequentially with soap solution, acetone, ethanol, and distilled water in an ultrasonic bath; film dried; Al thermally evaporated.
Scalability contextThin-film device fabrication, not bulk framework synthesis.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
SolventDMSONot specifiedmain p.6 · Fabrication of Schottky Device
OtherITO-coated glassNot specifiedmain p.6 · Fabrication of Schottky Device
OtherAl rectifier metal contactNot specifiedmain p.6 · Fabrication of Schottky Device