Synthesis evidence

Synthesis, characterization, and solid state electrical conductivity of coordination polymers with copper and zinc

Prasad R.L., Kushwaha A. · Journal of Coordination Chemistry · 2012 · 4230-4244

6 structured synthesis routes

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

Vague recipeSource: Main

Route 1: Unknown

p003 / 4231 · 2.2.1

Metal precursorsNot reported in this paper; stated to follow earlier reference [11].
Linker precursorsdadb, implied by formula; detailed recipe not reported here.
Vague recipeSource: Main

Route 2: Unknown

p003 / 4231 · 2.2.1

Metal precursorsNot reported in this paper; stated to follow earlier reference [11].
Linker precursorsdadb, implied by formula; detailed recipe not reported here.
Vague recipeSource: Main

Route 3: Unknown

p003 / 4231 · 2.2.1

Metal precursorsNot reported in this paper; stated to follow earlier reference [11].
Linker precursorsdadb, implied by formula; detailed recipe not reported here.
Complete recipeSource: Main

Route 4: Other

p004 / 4232 · 2.2.2

Metal precursorsZnSO4.7H2O (0.431 g, 1.5 mmol); CuSO4.5H2O (0.125 g, 0.5 mmol)
Linker precursorsdadb (0.414 g, 2 mmol)
Solvents40 mL pink 50% ethanolic solution; purification mixture 25% ethanol, 25% acetone, 5% DMF, 45% distilled water
AdditivesKOH (0.224 g, 4 mmol)
Atmospherenot stated
Temperatureroom temperature after water-bath digestion; exact water-bath temperature not stated
Time0.5 h dropwise addition; 5 h stirring; 0.5 h water-bath digestion; 1 h purification stirring
Work-upFiltered using suction, washed with distilled water; purified by stirring in solvent mixture, filtered, washed with distilled water thrice followed by ethanol.
ActivationDried under vacuum over anhydrous CaCl2.
Scalability contextBatch used 2 mmol dadb and stoichiometric Cu/Zn sulfate salts.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZnSO4.7H2O0.431 g, 1.5 mmolp004 / 4232 · 2.2.2
Metal SourceCuSO4.5H2O0.125 g, 0.5 mmolp004 / 4232 · 2.2.2
Linkerdadb0.414 g, 2 mmolp004 / 4232 · 2.2.2
BaseKOH0.224 g, 4 mmolp004 / 4232 · 2.2.2
Solvent50% ethanolic solution40 mL · 50%p004 / 4232 · 2.2.2
Complete recipeSource: Main

Route 5: Other

p004 / 4232 · 2.2.3

Metal precursorsZnSO4.7H2O (0.503 g, 1.75 mmol); CuSO4.5H2O (0.062 g, 0.25 mmol)
Linker precursorsdadb (0.414 g, 2 mmol)
Solvents40 mL pink 50% ethanolic solution; same purification procedure as complex 5
AdditivesKOH (0.224 g, 4 mmol)
Atmospherenot stated
Temperaturesame as route 5; exact water-bath temperature not stated
Time0.5 h dropwise addition; otherwise same as route 5
Work-upSame as synthesis of 5.
ActivationSame as synthesis of 5; dried under vacuum over anhydrous CaCl2.
Scalability contextBatch used 2 mmol dadb with Zn:Cu salt ratio 1.75:0.25 mmol.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZnSO4.7H2O0.503 g, 1.75 mmolp004 / 4232 · 2.2.3
Metal SourceCuSO4.5H2O0.062 g, 0.25 mmolp004 / 4232 · 2.2.3
Linkerdadb0.414 g, 2 mmolp004 / 4232 · 2.2.3
BaseKOH0.224 g, 4 mmolp004 / 4232 · 2.2.3
Solvent50% ethanolic solution40 mL · 50%p004 / 4232 · 2.2.3
Vague recipeSource: Main

Route 6: Unknown

p004 / 4232 · 2.2.1

Metal precursorsNot reported in this paper; stated to follow earlier reference [11].
Linker precursorsdadb, implied by formula; detailed recipe not reported here.