cMOF Evidence Base

Synthesis evidence

Effect on Schottky behaviour of 1D coordination polymers by altering para-substituents on benzoate ligands

Islam S., Datta J., Ahmed F. et al. · New Journal of Chemistry · 2018 · 13971-13977

4 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

13972 · Fabrication and characterisation of the device

SolventsDMSO dispersion at 4 mg mL^-1
Atmospherevacuum during Al deposition, 10^-6 Torr
Temperatureroom temperature
Time0.033 for spin coating step
Substrate orientationITO-coated glass
Work-upITO cleaned sequentially with acetone, ethanol and distilled water by sonication and dried; Al deposited through shadow mask.
Activationsonication to form stable dispersion
Scalability contextSpin-coated laboratory diode with effective area 7.065 x 10^-6 m^2.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 14 mg mL^-1 in DMSO13972 · Fabrication and characterisation of the device
SolventDMSONot specified13972 · Fabrication and characterisation of the device
OtherITO-coated glass substrateNot specified13972 · Fabrication and characterisation of the device
Otheraluminium top electrodeNot specified13972 · Fabrication and characterisation of the device
Partial recipeSource: Main

Route 2: Liquid Liquid Interface

13972 · Synthesis of compound 1

Metal precursorsZn(NO3)2.6H2O (0.06 g, 0.2 mmol)
Linker precursorsbpd (0.042 g, 0.2 mmol); H2p-clba (0.031 g, 0.2 mmol)
SolventsMeOH, H2O and EtOH; 2 mL 1:1 v/v MeOH/H2O buffer layer
AdditivesEt3N (0.021 g, 0.2 mmol) to neutralise H2p-clba
Atmospherenot reported
Temperaturenot reported; crystallisation appears ambient
Time72
Work-upYellow block crystals obtained after 3 days; no washing or activation reported.
Activationnot reported
Scalability contextSmall-volume layered slow-diffusion crystallisation; no scale-up discussed.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O0.06 g, 0.2 mmol13972 · Synthesis of compound 1
Linkerbpd0.042 g, 0.2 mmol13972 · Synthesis of compound 1
LinkerH2p-clba0.031 g, 0.2 mmol13972 · Synthesis of compound 1
BaseEt3N0.021 g, 0.2 mmol13972 · Synthesis of compound 1
SolventMeOH2 mL for bpd plus 1 mL equivalent in buffer13972 · Synthesis of compound 1
SolventH2O2 mL for Zn salt plus 1 mL equivalent in buffer13972 · Synthesis of compound 1
SolventEtOH2 mL13972 · Synthesis of compound 1
Partial recipeSource: Main

Route 3: Other

13972 · Fabrication and characterisation of the device

SolventsDMSO dispersion at 4 mg mL^-1
Atmospherevacuum during Al deposition, 10^-6 Torr
Temperatureroom temperature
Time0.033 for spin coating step
Substrate orientationITO-coated glass
Work-upITO cleaned sequentially with acetone, ethanol and distilled water by sonication and dried; Al deposited through shadow mask.
Activationsonication to form stable dispersion
Scalability contextSpin-coated laboratory diode with effective area 7.065 x 10^-6 m^2.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 24 mg mL^-1 in DMSO13972 · Fabrication and characterisation of the device
SolventDMSONot specified13972 · Fabrication and characterisation of the device
OtherITO-coated glass substrateNot specified13972 · Fabrication and characterisation of the device
Otheraluminium top electrodeNot specified13972 · Fabrication and characterisation of the device
Partial recipeSource: Main

Route 4: Liquid Liquid Interface

13972 · Synthesis of compound 2

Metal precursorsZn(NO3)2.6H2O (same as compound 1 procedure)
Linker precursorsbpd (same as compound 1 procedure); H2p-brba (0.040 g, 0.2 mmol)
SolventsMeOH, H2O and EtOH using the compound 1 procedure
AdditivesEt3N using the compound 1 procedure
Atmospherenot reported
Temperaturenot reported; crystallisation appears ambient
Time72
Work-upYellow block crystals obtained after 3 days; no washing or activation reported.
Activationnot reported
Scalability contextSmall-volume layered slow-diffusion crystallisation; no scale-up discussed.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O0.06 g, 0.2 mmol inferred from compound 1 procedure13972 · Synthesis of compound 2
Linkerbpd0.042 g, 0.2 mmol inferred from compound 1 procedure13972 · Synthesis of compound 2
LinkerH2p-brba0.040 g, 0.2 mmol13972 · Synthesis of compound 2
BaseEt3N0.021 g, 0.2 mmol inferred from compound 1 procedure13972 · Synthesis of compound 2
SolventMeOH/H2O/EtOHsame volumes as compound 1 procedure13972 · Synthesis of compound 2