Synthesis evidence

Cation dependent charge transport in linear dicarboxylate based isotypical 1D coordination polymers

Ahmed F., Datta J., Dutta B. et al. · RSC Advances · 2017 · 10369-10375

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

2 · Device fabrication and characterization · Fig. S1

SolventsDMSO dispersion medium; substrate cleaning with isopropanol, acetone and deionised water
Atmospherevacuum drying; Al deposition at 1 x 10^-6 Torr
Temperatureroom temperature for I-V measurement; drying temperature not specified
Substrate orientationITO-coated glass
Work-upITO ultrasonicated in isopropanol for 15 min, cleaned with acetone and deionised water, dried in vacuum; film vacuum-dried after spin coating.
Activationnone reported
Scalability contextSpin coating repeated four times; electrode area controlled by shadow mask at 7.065 x 10^-6 m2.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Solventdimethyl sulfoxide (DMSO)not specified2 · Device fabrication and characterization · Fig. S1
Othercompound 1not specified2 · Device fabrication and characterization · Fig. S1
Otheraluminum electrodesarea 7.065 x 10^-6 m22 · Device fabrication and characterization · Fig. S1
Partial recipeSource: Main

Route 2: Other

2 · Synthesis of compounds 1 and 2

Metal precursorsCd(NO3)2.4H2O (62 mg, 0.2 mmol) in H2O (2 mL)
Linker precursors4-phpy (31 mg, 0.2 mmol) in MeOH (2 mL); H2adc (23 mg, 0.2 mmol) neutralised with Et3N (0.027 mL, 0.2 mmol) in EtOH (2 mL)
SolventsMeOH, H2O, 1:1 MeOH/H2O buffer solution, EtOH
AdditivesEt3N; 1:1 (v/v) MeOH/H2O buffer solution
Atmospherenot specified
Temperaturenot specified
Time72
Work-upColourless block crystals isolated; no washing or drying workup reported.
Activationnone reported
Scalability contextSmall-batch slow solution layering; 69 mg product, 60% yield.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.4H2O62 mg, 0.2 mmol2 · Synthesis of compounds 1 and 2
Linker4-phpy31 mg, 0.2 mmol2 · Synthesis of compounds 1 and 2
LinkerH2adc23 mg, 0.2 mmol2 · Synthesis of compounds 1 and 2
BaseEt3N0.027 mL, 0.2 mmol2 · Synthesis of compounds 1 and 2
SolventMeOH2 mL plus 1:1 buffer component2 · Synthesis of compounds 1 and 2
SolventH2O2 mL plus 1:1 buffer component2 · Synthesis of compounds 1 and 2
SolventEtOH2 mL2 · Synthesis of compounds 1 and 2
Complete recipeSource: Both

Route 3: Other

2 · Device fabrication and characterization · Fig. S1

SolventsDMSO dispersion medium; substrate cleaning with isopropanol, acetone and deionised water
Atmospherevacuum drying; Al deposition at 1 x 10^-6 Torr
Temperatureroom temperature for I-V measurement; drying temperature not specified
Substrate orientationITO-coated glass
Work-upITO ultrasonicated in isopropanol for 15 min, cleaned with acetone and deionised water, dried in vacuum; film vacuum-dried after spin coating.
Activationnone reported
Scalability contextSpin coating repeated four times; electrode area controlled by shadow mask at 7.065 x 10^-6 m2.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Solventdimethyl sulfoxide (DMSO)not specified2 · Device fabrication and characterization · Fig. S1
Othercompound 2not specified2 · Device fabrication and characterization · Fig. S1
Otheraluminum electrodesarea 7.065 x 10^-6 m22 · Device fabrication and characterization · Fig. S1
Partial recipeSource: Main

Route 4: Other

2 · Synthesis of compounds 1 and 2

Metal precursorsZn(NO3)2.6H2O reported as Zn(NO)3.6H2O in extracted text (60 mg, 0.2 mmol)
Linker precursorsSame as compound 1: 4-phpy, H2adc neutralised with Et3N
SolventsMeOH, H2O, 1:1 MeOH/H2O buffer solution, EtOH
AdditivesEt3N; 1:1 (v/v) MeOH/H2O buffer solution
Atmospherenot specified
Temperaturenot specified
Timefew days
Work-upColourless block-shaped crystals isolated; no washing or drying workup reported.
Activationnone reported
Scalability contextSmall-batch slow solution layering; 68 mg product, 65% yield.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO)3.6H2O60 mg, 0.2 mmol2 · Synthesis of compounds 1 and 2
Linker4-phpy31 mg, 0.2 mmol (same as compound 1)2 · Synthesis of compounds 1 and 2
LinkerH2adc23 mg, 0.2 mmol (same as compound 1)2 · Synthesis of compounds 1 and 2
BaseEt3N0.027 mL, 0.2 mmol (same as compound 1)2 · Synthesis of compounds 1 and 2