Synthesis evidence

Synthesis, characterization and electrical conductivity of mixed-ligand heterobimetallic coordination polymers

Singh N., Kumar Sinha R. · Inorganic Chemistry Communications · 2002 · 255-258

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

2 · Experimental - Synthesis of the complexes

Metal precursorsCoHg(C7H4NS2)4 (0.923 g, 1 mmol); precursor itself prepared from metal salt solutions as in reference [10]
Linker precursorspotassium 2-sulfanylbenzothiazolate used to prepare precursor; 1,10-phenanthroline added as neutral ligand
Solvents50 cm3 ethanol-water (90:10 v/v) for precursor suspension; 5 cm3 ethanolic ligand solution
Atmospherenot specified
Temperatureroom temperature
Timeovernight (exact hours not specified)
Work-upfiltered coloured precipitate; washed with ethanol then Et2O; dried in vacuo over CaCl2
Activationdried in vacuo over CaCl2; no framework activation reported
Scalability contextmillimole-scale precipitation synthesis; no scale-up data
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoHg(C7H4NS2)40.923 g, 1 mmol2 · Experimental - Synthesis of the complexes
Linker1,10-phenanthroline0.198 g, 1 mmol · in 5 cm3 ethanol2 · Experimental - Synthesis of the complexes
SolventC2H5OH-H2O (90:10 v/v)50 cm32 · Experimental - Synthesis of the complexes
Solventethanol5 cm3 · ligand solution2 · Experimental - Synthesis of the complexes
OtherCaCl2not specified · drying agent2 · Experimental - Synthesis of the complexes
Partial recipeSource: Main

Route 2: Other

2 · Experimental - Synthesis of the complexes

Metal precursorsCoHg(C7H4NS2)4 (0.923 g, 1 mmol); precursor itself prepared from metal salt solutions as in reference [10]
Linker precursorspotassium 2-sulfanylbenzothiazolate used to prepare precursor; 1,10-phenanthroline added as neutral ligand
Solvents50 cm3 ethanol-water (90:10 v/v) for precursor suspension; 5 cm3 ethanolic ligand solution
Atmospherenot specified
Temperatureroom temperature
Timeovernight (exact hours not specified)
Work-upfiltered coloured precipitate; washed with ethanol then Et2O; dried in vacuo over CaCl2
Activationdried in vacuo over CaCl2; no framework activation reported
Scalability contextmillimole-scale precipitation synthesis; no scale-up data
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoHg(C7H4NS2)40.923 g, 1 mmol2 · Experimental - Synthesis of the complexes
Linker1,10-phenanthroline0.594 g, 3 mmol · in 5 cm3 ethanol2 · Experimental - Synthesis of the complexes
SolventC2H5OH-H2O (90:10 v/v)50 cm32 · Experimental - Synthesis of the complexes
Solventethanol5 cm3 · ligand solution2 · Experimental - Synthesis of the complexes
OtherCaCl2not specified · drying agent2 · Experimental - Synthesis of the complexes
Partial recipeSource: Main

Route 3: Other

2 · Experimental - Synthesis of the complexes

Metal precursorsNiZn(C7H4NS2)4 (0.788 g, 1 mmol); precursor itself prepared from metal salt solutions as in reference [10]
Linker precursorspotassium 2-sulfanylbenzothiazolate used to prepare precursor; ethylenediamine added as neutral ligand
Solvents50 cm3 ethanol-water (90:10 v/v) for precursor suspension; 5 cm3 ethanolic ligand solution
Atmospherenot specified
Temperatureroom temperature
Timeovernight (exact hours not specified)
Work-upfiltered coloured precipitate; washed with ethanol then Et2O; dried in vacuo over CaCl2
Activationdried in vacuo over CaCl2; no framework activation reported
Scalability contextmillimole-scale precipitation synthesis; no scale-up data
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiZn(C7H4NS2)40.788 g, 1 mmol2 · Experimental - Synthesis of the complexes
Linkerethylenediamine0.060 g, 1 mmol · in 5 cm3 ethanol2 · Experimental - Synthesis of the complexes
SolventC2H5OH-H2O (90:10 v/v)50 cm32 · Experimental - Synthesis of the complexes
Solventethanol5 cm3 · ligand solution2 · Experimental - Synthesis of the complexes
OtherCaCl2not specified · drying agent2 · Experimental - Synthesis of the complexes
Partial recipeSource: Main

Route 4: Other

2 · Experimental - Synthesis of the complexes

Metal precursorsNiZn(C7H4NS2)4 (0.788 g, 1 mmol); precursor itself prepared from metal salt solutions as in reference [10]
Linker precursorspotassium 2-sulfanylbenzothiazolate used to prepare precursor; ethylenediamine added as neutral ligand
Solvents50 cm3 ethanol-water (90:10 v/v) for precursor suspension; 5 cm3 ethanolic ligand solution
Atmospherenot specified
Temperatureroom temperature
Timeovernight (exact hours not specified)
Work-upfiltered coloured precipitate; washed with ethanol then Et2O; dried in vacuo over CaCl2
Activationdried in vacuo over CaCl2; no framework activation reported
Scalability contextmillimole-scale precipitation synthesis; no scale-up data
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiZn(C7H4NS2)40.788 g, 1 mmol2 · Experimental - Synthesis of the complexes
Linkerethylenediamine0.180 g, 3 mmol · in 5 cm3 ethanol2 · Experimental - Synthesis of the complexes
SolventC2H5OH-H2O (90:10 v/v)50 cm32 · Experimental - Synthesis of the complexes
Solventethanol5 cm3 · ligand solution2 · Experimental - Synthesis of the complexes
OtherCaCl2not specified · drying agent2 · Experimental - Synthesis of the complexes
Partial recipeSource: Main

Route 5: Other

2 · Experimental - Synthesis of the complexes

Metal precursorsNiZn(C7H4NS2)4 (0.788 g, 1 mmol); precursor itself prepared from metal salt solutions as in reference [10]
Linker precursorspotassium 2-sulfanylbenzothiazolate used to prepare precursor; 1,10-phenanthroline added as neutral ligand
Solvents50 cm3 ethanol-water (90:10 v/v) for precursor suspension; 5 cm3 ethanolic ligand solution
Atmospherenot specified
Temperatureroom temperature
Timeovernight (exact hours not specified)
Work-upfiltered coloured precipitate; washed with ethanol then Et2O; dried in vacuo over CaCl2
Activationdried in vacuo over CaCl2; no framework activation reported
Scalability contextmillimole-scale precipitation synthesis; no scale-up data
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiZn(C7H4NS2)40.788 g, 1 mmol2 · Experimental - Synthesis of the complexes
Linker1,10-phenanthroline0.198 g, 1 mmol · in 5 cm3 ethanol2 · Experimental - Synthesis of the complexes
SolventC2H5OH-H2O (90:10 v/v)50 cm32 · Experimental - Synthesis of the complexes
Solventethanol5 cm3 · ligand solution2 · Experimental - Synthesis of the complexes
OtherCaCl2not specified · drying agent2 · Experimental - Synthesis of the complexes
Partial recipeSource: Main

Route 6: Other

2 · Experimental - Synthesis of the complexes

Metal precursorsNiZn(C7H4NS2)4 (0.788 g, 1 mmol); precursor itself prepared from metal salt solutions as in reference [10]
Linker precursorspotassium 2-sulfanylbenzothiazolate used to prepare precursor; 1,10-phenanthroline added as neutral ligand
Solvents50 cm3 ethanol-water (90:10 v/v) for precursor suspension; 5 cm3 ethanolic ligand solution
Atmospherenot specified
Temperatureroom temperature
Timeovernight (exact hours not specified)
Work-upfiltered coloured precipitate; washed with ethanol then Et2O; dried in vacuo over CaCl2
Activationdried in vacuo over CaCl2; no framework activation reported
Scalability contextmillimole-scale precipitation synthesis; no scale-up data
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiZn(C7H4NS2)40.788 g, 1 mmol2 · Experimental - Synthesis of the complexes
Linker1,10-phenanthroline0.594 g, 3 mmol · in 5 cm3 ethanol2 · Experimental - Synthesis of the complexes
SolventC2H5OH-H2O (90:10 v/v)50 cm32 · Experimental - Synthesis of the complexes
Solventethanol5 cm3 · ligand solution2 · Experimental - Synthesis of the complexes
OtherCaCl2not specified · drying agent2 · Experimental - Synthesis of the complexes
Partial recipeSource: Main

Route 7: Other

1 · Experimental - Synthesis of the complexes

Metal precursorsNiZn(C7H4NS2)4 (0.788 g, 1 mmol); precursor itself prepared from metal salt solutions as in reference [10]
Linker precursorspotassium 2-sulfanylbenzothiazolate used to prepare precursor; pyridine added as neutral ligand
Solvents50 cm3 ethanol-water (90:10 v/v) for precursor suspension; 5 cm3 ethanolic ligand solution
Atmospherenot specified
Temperatureroom temperature
Timeovernight (exact hours not specified)
Work-upfiltered coloured precipitate; washed with ethanol then Et2O; dried in vacuo over CaCl2
Activationdried in vacuo over CaCl2; no framework activation reported
Scalability contextmillimole-scale precipitation synthesis; no scale-up data
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiZn(C7H4NS2)40.788 g, 1 mmol1 · Experimental - Synthesis of the complexes
Linkerpyridine0.158 g, 2 mmol · in 5 cm3 ethanol1 · Experimental - Synthesis of the complexes
SolventC2H5OH-H2O (90:10 v/v)50 cm31 · Experimental - Synthesis of the complexes
Solventethanol5 cm3 · ligand solution1 · Experimental - Synthesis of the complexes
OtherCaCl2not specified · drying agent1 · Experimental - Synthesis of the complexes