cMOF Evidence Base

Synthesis evidence

Synthesis, characterization and solid state electrical properties of 1-D coordination polymer of the type [CuxNi1-x(dadb) ·yH2O]n

Prasad R.L., Kushwaha A., Shrivastava O.N. · Journal of Solid State Chemistry · 2012 · 471-481

6 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

p002 · 2.2.1 Monometallic complexes

Metal precursorsmetal salt, 2 mmol; assigned to Cu source by product identity but the text does not name the salt in the monometallic general recipe
Linker precursorsdadb, 0.414 g, 2 mmol
Solvents40 ml 50% ethanolic solution; metal salt dissolved in 15 ml distilled water; purification solvent 25% ethanol/25% acetone/5% DMF/45% water
AdditivesKOH, 0.224 g, 4 mmol
Atmospherenot specified; handled in air-stable solid state
Temperaturewater bath, then room temperature; pellet curing 110 deg C is measurement preparation, not synthesis
Time0.5 h metal addition; 5 h stirring; 0.5 h water-bath heating; 2 h standing; 1 h purification stirring
Oxidant / reductantnone intentionally added
Work-upStir 5 h; heat/digest on water bath 30 min; stand/cool to room temperature 2 h where specified; filter precipitate; wash distilled water three times; purify by stirring 1 h in 25% ethanol/25% acetone/5% DMF/45% water; filter; wash water three times then ethanol; dry under vacuo over anhydrous CaCl2.
Activationdried under vacuo over anhydrous CaCl2
Scalability contextBatch precipitation from solution; no scale-up discussion.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linkerdadb0.414 g, 2 mmolp002 · 2.2.1 Monometallic complexes
BaseKOH0.224 g, 4 mmolp002 · 2.2.1 Monometallic complexes
Metal Sourcemetal salt for Cu complex, not named2 mmolp002 · 2.2.1 Monometallic complexes
Solvent50% ethanolic solution40 ml · 50%p002 · 2.2.1 Monometallic complexes
Solventdistilled water15 ml for metal salt solutionp002 · 2.2.1 Monometallic complexes
Partial recipeSource: Main

Route 2: Other

p002 · 2.2.1 Monometallic complexes

Metal precursorsmetal salt, 2 mmol; assigned to Ni source by product identity but the text does not name the salt in the monometallic general recipe
Linker precursorsdadb, 0.414 g, 2 mmol
Solvents40 ml 50% ethanolic solution; metal salt dissolved in 15 ml distilled water; purification solvent 25% ethanol/25% acetone/5% DMF/45% water
AdditivesKOH, 0.224 g, 4 mmol
Atmospherenot specified; handled in air-stable solid state
Temperaturewater bath, then room temperature; pellet curing 110 deg C is measurement preparation, not synthesis
Time0.5 h metal addition; 5 h stirring; 0.5 h water-bath heating; 2 h standing; 1 h purification stirring
Oxidant / reductantnone intentionally added
Work-upStir 5 h; heat/digest on water bath 30 min; stand/cool to room temperature 2 h where specified; filter precipitate; wash distilled water three times; purify by stirring 1 h in 25% ethanol/25% acetone/5% DMF/45% water; filter; wash water three times then ethanol; dry under vacuo over anhydrous CaCl2.
Activationdried under vacuo over anhydrous CaCl2
Scalability contextBatch precipitation from solution; no scale-up discussion.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linkerdadb0.414 g, 2 mmolp002 · 2.2.1 Monometallic complexes
BaseKOH0.224 g, 4 mmolp002 · 2.2.1 Monometallic complexes
Metal Sourcemetal salt for Ni complex, not named2 mmolp002 · 2.2.1 Monometallic complexes
Solvent50% ethanolic solution40 ml · 50%p002 · 2.2.1 Monometallic complexes
Solventdistilled water15 ml for metal salt solutionp002 · 2.2.1 Monometallic complexes
Complete recipeSource: Main

Route 3: Other

p002 · 2.2.2 Synthesis of heterobimetallic complexes

Metal precursorsNiCl2.6H2O (0.238 g, 1 mmol); CuCl2.2H2O (0.171 g, 1 mmol)
Linker precursorsdadb, 0.414 g, 2 mmol
Solventspink coloured 50% ethanolic solution (40 ml) containing dadb and KOH; metal chlorides in 10 ml homogeneous aqueous solution
AdditivesKOH, 0.224 g, 4 mmol
Atmospherenot specified; handled in air-stable solid state
Temperaturewater bath digestion; room-temperature cooling
Time0.5 h dropwise metal addition; 5 h further stirring; 0.5 h water-bath digestion; cool to room temperature; workup as for complex 2
Oxidant / reductantnone intentionally added
Work-upStir 5 h; heat/digest on water bath 30 min; stand/cool to room temperature 2 h where specified; filter precipitate; wash distilled water three times; purify by stirring 1 h in 25% ethanol/25% acetone/5% DMF/45% water; filter; wash water three times then ethanol; dry under vacuo over anhydrous CaCl2.
Activationdried under vacuo over anhydrous CaCl2
Scalability contextBatch precipitation from solution; no scale-up discussion.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O(0.238 g, 1 mmol)p002 · 2.2.2 Synthesis of heterobimetallic complexes
Metal SourceCuCl2.2H2O(0.171 g, 1 mmol)p002 · 2.2.2 Synthesis of heterobimetallic complexes
Linkerdadb0.414 g, 2 mmolp002 · 2.2.2 Synthesis of heterobimetallic complexes
BaseKOH0.224 g, 4 mmolp002 · 2.2.2 Synthesis of heterobimetallic complexes
Solvent50% ethanolic solution40 ml · 50%p002 · 2.2.2 Synthesis of heterobimetallic complexes
Solventwater10 ml for complex 4; aqueous solution amount not fully specified for complexes 5-7p002 · 2.2.2 Synthesis of heterobimetallic complexes
Complete recipeSource: Main

Route 4: Other

p002 · 2.2.2 Synthesis of heterobimetallic complexes

Metal precursorsNiCl2.6H2O (0.357 g, 1.5 mmol); CuCl2.2H2O (0.086 g, 0.5 mmol)
Linker precursorsdadb, 0.414 g, 2 mmol
Solventspink coloured 50% ethanolic solution (40 ml) containing dadb and KOH; metal chlorides in aqueous solution
AdditivesKOH, 0.224 g, 4 mmol
Atmospherenot specified; handled in air-stable solid state
Temperaturewater bath digestion; room-temperature cooling
Time0.5 h dropwise metal addition; 5 h further stirring; 0.5 h water-bath digestion; cool to room temperature; workup as for complex 2
Oxidant / reductantnone intentionally added
Work-upStir 5 h; heat/digest on water bath 30 min; stand/cool to room temperature 2 h where specified; filter precipitate; wash distilled water three times; purify by stirring 1 h in 25% ethanol/25% acetone/5% DMF/45% water; filter; wash water three times then ethanol; dry under vacuo over anhydrous CaCl2.
Activationdried under vacuo over anhydrous CaCl2
Scalability contextBatch precipitation from solution; no scale-up discussion.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O(0.357 g, 1.5 mmol)p002 · 2.2.2 Synthesis of heterobimetallic complexes
Metal SourceCuCl2.2H2O(0.086 g, 0.5 mmol)p002 · 2.2.2 Synthesis of heterobimetallic complexes
Linkerdadb0.414 g, 2 mmolp002 · 2.2.2 Synthesis of heterobimetallic complexes
BaseKOH0.224 g, 4 mmolp002 · 2.2.2 Synthesis of heterobimetallic complexes
Solvent50% ethanolic solution40 ml · 50%p002 · 2.2.2 Synthesis of heterobimetallic complexes
Solventwater10 ml for complex 4; aqueous solution amount not fully specified for complexes 5-7p002 · 2.2.2 Synthesis of heterobimetallic complexes
Complete recipeSource: Main

Route 5: Other

p002 · 2.2.2 Synthesis of heterobimetallic complexes

Metal precursorsNiCl2.6H2O (0.417 g, 1.75 mmol); CuCl2.2H2O (0.043 g, 0.25 mmol)
Linker precursorsdadb, 0.414 g, 2 mmol
Solventspink coloured 50% ethanolic solution (40 ml) containing dadb and KOH; metal chlorides in aqueous solution
AdditivesKOH, 0.224 g, 4 mmol
Atmospherenot specified; handled in air-stable solid state
Temperaturewater bath digestion; room-temperature cooling
Time0.5 h dropwise metal addition; 5 h further stirring; 0.5 h water-bath digestion; cool to room temperature; workup as for complex 2
Oxidant / reductantnone intentionally added
Work-upStir 5 h; heat/digest on water bath 30 min; stand/cool to room temperature 2 h where specified; filter precipitate; wash distilled water three times; purify by stirring 1 h in 25% ethanol/25% acetone/5% DMF/45% water; filter; wash water three times then ethanol; dry under vacuo over anhydrous CaCl2.
Activationdried under vacuo over anhydrous CaCl2
Scalability contextBatch precipitation from solution; no scale-up discussion.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O(0.417 g, 1.75 mmol)p002 · 2.2.2 Synthesis of heterobimetallic complexes
Metal SourceCuCl2.2H2O(0.043 g, 0.25 mmol)p002 · 2.2.2 Synthesis of heterobimetallic complexes
Linkerdadb0.414 g, 2 mmolp002 · 2.2.2 Synthesis of heterobimetallic complexes
BaseKOH0.224 g, 4 mmolp002 · 2.2.2 Synthesis of heterobimetallic complexes
Solvent50% ethanolic solution40 ml · 50%p002 · 2.2.2 Synthesis of heterobimetallic complexes
Solventwater10 ml for complex 4; aqueous solution amount not fully specified for complexes 5-7p002 · 2.2.2 Synthesis of heterobimetallic complexes
Complete recipeSource: Main

Route 6: Other

p002 · 2.2.2 Synthesis of heterobimetallic complexes

Metal precursorsNiCl2.6H2O (0.446 g, 1.88 mmol); CuCl2.2H2O (0.021 g, 0.12 mmol)
Linker precursorsdadb, 0.414 g, 2 mmol
Solventspink coloured 50% ethanolic solution (40 ml) containing dadb and KOH; metal chlorides in aqueous solution
AdditivesKOH, 0.224 g, 4 mmol
Atmospherenot specified; handled in air-stable solid state
Temperaturewater bath digestion; room-temperature cooling
Time0.5 h dropwise metal addition; 5 h further stirring; 0.5 h water-bath digestion; cool to room temperature; workup as for complex 2
Oxidant / reductantnone intentionally added
Work-upStir 5 h; heat/digest on water bath 30 min; stand/cool to room temperature 2 h where specified; filter precipitate; wash distilled water three times; purify by stirring 1 h in 25% ethanol/25% acetone/5% DMF/45% water; filter; wash water three times then ethanol; dry under vacuo over anhydrous CaCl2.
Activationdried under vacuo over anhydrous CaCl2
Scalability contextBatch precipitation from solution; no scale-up discussion.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O(0.446 g, 1.88 mmol)p002 · 2.2.2 Synthesis of heterobimetallic complexes
Metal SourceCuCl2.2H2O(0.021 g, 0.12 mmol)p002 · 2.2.2 Synthesis of heterobimetallic complexes
Linkerdadb0.414 g, 2 mmolp002 · 2.2.2 Synthesis of heterobimetallic complexes
BaseKOH0.224 g, 4 mmolp002 · 2.2.2 Synthesis of heterobimetallic complexes
Solvent50% ethanolic solution40 ml · 50%p002 · 2.2.2 Synthesis of heterobimetallic complexes
Solventwater10 ml for complex 4; aqueous solution amount not fully specified for complexes 5-7p002 · 2.2.2 Synthesis of heterobimetallic complexes