cMOF Evidence Base

Synthesis evidence

Soluble semi-conductive chelate polymers containing Cr(III) in the backbone: Synthesis, characterization, optical, electrochemical, and electrical properties

Yildirim M., Kaya I. · Polymer · 2009 · 5653-5660

7 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

5655 (p003) · 2.5 Electrical properties · Figures 6-8

Additivesiodine vapour
Atmosphereatmospheric pressure in a desiccator
Temperature20 for time-dependent P-2/P-3 measurements; 20-80 for temperature-dependent measurements
Timeup to 24 h; P-1 also measured after 3 h and 5 h
Substrate orientationdip-coated polymer films on ITO glass
Oxidant / reductantiodine dopant
Work-upexposure to iodine vapour
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Oxidantiodine vaporNot specified5655 (p003) · 2.5 Electrical properties · Figures 6-8
Otherdip-coated polymer film on ITONot specified5655 (p003) · 2.5 Electrical properties · Figures 6-8
Complete recipeSource: Main

Route 2: Other

5655 (p003) · 2.5 Electrical properties

Solventsmethanol
Atmosphereambient, not otherwise stated
Time50 cycles with 1 min drying after each dip
Substrate orientationITO glass plate
Work-upsuccessive dipping and withdrawal; dried 1 min after each dip
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherP-1 polymer50 mg/mL in methanol5655 (p003) · 2.5 Electrical properties
SolventmethanolNot specified5655 (p003) · 2.5 Electrical properties
OtherITO glass plateNot specified5655 (p003) · 2.5 Electrical properties
Complete recipeSource: Main

Route 3: Other

5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2

Metal precursorsCrCl3.6H2O (1.86 g, 0.7 x 10-2 mol)
Linker precursors3,4-dihydroxybenzaldehyde (1.38 g, 1 x 10-2 mol); o-phenylenediamine (0.54 g, 0.5 x 10-2 mol)
Solventsmethanol (50 mL initial + 30 mL Cr solution + 30 mL diamine solution); toluene precipitation/wash; water wash
Atmospherenot stated
Temperature60 for Cr coordination step; reflux for polymerisation
Time1 h Cr coordination, then 3 h reflux after diamine addition
Work-upprecipitated by dropping into 250 mL toluene; washed with toluene (2 x 100 mL) and water (2 x 100 mL)
Activationdried in vacuum oven for 24 h
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Linker3,4-dihydroxybenzaldehyde (3,4-HBA)1.38 g, 1 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Metal SourceCrCl3.6H2O1.86 g, 0.7 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Linkero-phenylenediamine (OPDA)0.54 g, 0.5 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventmethanol50 mL + 30 mL + 30 mL5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventtoluene250 mL precipitation; 2 x 100 mL wash5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventwater2 x 100 mL wash5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Complete recipeSource: Main

Route 4: Other

5655 (p003) · 2.5 Electrical properties

Solventsmethanol
Atmosphereambient, not otherwise stated
Time50 cycles with 1 min drying after each dip
Substrate orientationITO glass plate
Work-upsuccessive dipping and withdrawal; dried 1 min after each dip
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherP-2 polymer50 mg/mL in methanol5655 (p003) · 2.5 Electrical properties
SolventmethanolNot specified5655 (p003) · 2.5 Electrical properties
OtherITO glass plateNot specified5655 (p003) · 2.5 Electrical properties
Complete recipeSource: Main

Route 5: Other

5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2

Metal precursorsCrCl3.6H2O (1.86 g, 0.7 x 10-2 mol)
Linker precursors3,4-dihydroxybenzaldehyde (1.38 g, 1 x 10-2 mol); p-phenylenediamine (0.54 g, 0.5 x 10-2 mol)
Solventsmethanol (50 mL initial + 30 mL Cr solution + 30 mL diamine solution); toluene precipitation/wash; water wash
Atmospherenot stated
Temperature60 for Cr coordination step; reflux for polymerisation
Time1 h Cr coordination, then 3 h reflux after diamine addition
Work-upprecipitated by dropping into 250 mL toluene; washed with toluene (2 x 100 mL) and water (2 x 100 mL)
Activationdried in vacuum oven for 24 h
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Linker3,4-dihydroxybenzaldehyde (3,4-HBA)1.38 g, 1 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Metal SourceCrCl3.6H2O1.86 g, 0.7 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Linkerp-phenylenediamine (PPDA)0.54 g, 0.5 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventmethanol50 mL + 30 mL + 30 mL5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventtoluene250 mL precipitation; 2 x 100 mL wash5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventwater2 x 100 mL wash5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Complete recipeSource: Main

Route 6: Other

5655 (p003) · 2.5 Electrical properties

Solventsmethanol
Atmosphereambient, not otherwise stated
Time50 cycles with 1 min drying after each dip
Substrate orientationITO glass plate
Work-upsuccessive dipping and withdrawal; dried 1 min after each dip
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherP-3 polymer50 mg/mL in methanol5655 (p003) · 2.5 Electrical properties
SolventmethanolNot specified5655 (p003) · 2.5 Electrical properties
OtherITO glass plateNot specified5655 (p003) · 2.5 Electrical properties
Complete recipeSource: Main

Route 7: Other

5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2

Metal precursorsCrCl3.6H2O (1.86 g, 0.7 x 10-2 mol)
Linker precursors3,4-dihydroxybenzaldehyde (1.38 g, 1 x 10-2 mol); naphthalene-1,5-diamine (0.79 g, 0.5 x 10-2 mol)
Solventsmethanol (50 mL initial + 30 mL Cr solution + 30 mL diamine solution); toluene precipitation/wash; water wash
Atmospherenot stated
Temperature60 for Cr coordination step; reflux for polymerisation
Time1 h Cr coordination, then 3 h reflux after diamine addition
Work-upprecipitated by dropping into 250 mL toluene; washed with toluene (2 x 100 mL) and water (2 x 100 mL)
Activationdried in vacuum oven for 24 h
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Linker3,4-dihydroxybenzaldehyde (3,4-HBA)1.38 g, 1 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Metal SourceCrCl3.6H2O1.86 g, 0.7 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Linkernaphthalene-1,5-diamine (NDA)0.79 g, 0.5 x 10-2 mol5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventmethanol50 mL + 30 mL + 30 mL5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventtoluene250 mL precipitation; 2 x 100 mL wash5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2
Solventwater2 x 100 mL wash5654 (p002) · 2.2 Syntheses of the polymers · Scheme 2