Synthesis evidence

Diamagnetic Carrier-Doping-Induced Continuous Electronic and Magnetic Crossover in One-Dimensional Coordination Polymers

Shen Y., Cui M., Li G. et al. · Journal of the American Chemical Society · 2024 · 35367-35376

8 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

7 · Experimental Section

Metal precursorscobalt acetate and copper acetate mixed at nominal Cu:Co = 5:95
Linker precursorsH4L, 0.05 mmol by doped-compound method
Solventsdistilled water for premixing; NEt3, 20 mL for reaction
Additivestriethylamine/NEt3
Atmospherenot specified
Temperatureroom temperature reaction; dried at 60 C
Timeseveral days
Work-upSimilar to Cu0.5Co0.5 doped-compound method; filtration, washing, drying.
ActivationWater removed under vacuum during salt premix; final drying at 60 C.
Scalability contextQuantitative yield implied for doped compounds.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt acetatenot individually stated7 · Experimental Section
Metal Sourcecopper acetatenot individually stated7 · Experimental Section
LinkerH4L0.05 mmol by common doped route7 · Experimental Section
SolventNEt320 mL by common doped route7 · Experimental Section
Complete recipeSource: Main

Route 2: Other

7 · Experimental Section

Metal precursorscobalt acetate, 0.05 mmol
Linker precursorsH4L, 0.05 mmol
SolventsNEt3, 20 mL
Additivestriethylamine/NEt3 used in large excess
Atmospherenot specified
Temperatureroom temperature reaction; dried at 60 C
Time72-120
Work-upCollected by filtration; washed with large amounts of ethyl acetate, acetone, and water; dried at 60 C under vacuum.
ActivationDried at 60 C under vacuum.
Scalability contextQuantitative yield reported; no scale-up discussion.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt acetate0.05 mmol7 · Experimental Section
LinkerH4L0.05 mmol7 · Experimental Section
SolventNEt320 mL7 · Experimental Section
Solventethyl acetatelarge amounts for washing7 · Experimental Section
Solventacetonelarge amounts for washing7 · Experimental Section
Solventwaterlarge amounts for washing7 · Experimental Section
Partial recipeSource: Main

Route 3: Other

7 · Experimental Section

Metal precursorscobalt acetate and copper acetate mixed at nominal Cu:Co = 30:70
Linker precursorsH4L, 0.05 mmol by doped-compound method
Solventsdistilled water for premixing; NEt3, 20 mL for reaction
Additivestriethylamine/NEt3
Atmospherenot specified
Temperatureroom temperature reaction; dried at 60 C
Timeseveral days
Work-upSimilar to Cu0.5Co0.5 doped-compound method.
ActivationWater removed under vacuum during salt premix; final drying at 60 C.
Scalability contextQuantitative yield implied for doped compounds.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt acetatenot individually stated7 · Experimental Section
Metal Sourcecopper acetatenot individually stated7 · Experimental Section
LinkerH4L0.05 mmol by common doped route7 · Experimental Section
SolventNEt320 mL by common doped route7 · Experimental Section
Complete recipeSource: Main

Route 4: Other

7 · Experimental Section

Metal precursorscobalt acetate, 0.025 mmol; copper acetate, 0.025 mmol
Linker precursorsH4L, 0.05 mmol
Solventsdistilled water, 3 mL for salt premix; NEt3, 20 mL for reaction
Additivestriethylamine/NEt3
Atmospherenot specified
Temperatureroom temperature reaction; dried at 60 C
Timeseveral days
Work-upSalt solution sonicated and stirred 30 min; water removed under vacuum; black solids filtered, washed with ethyl acetate, acetone, and water; dried at 60 C.
ActivationWater removed under vacuum before reaction; final dried at 60 C.
Scalability contextQuantitative yield reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt acetate0.025 mmol7 · Experimental Section
Metal Sourcecopper acetate0.025 mmol7 · Experimental Section
Solventdistilled water3 mL7 · Experimental Section
LinkerH4L0.05 mmol7 · Experimental Section
SolventNEt320 mL7 · Experimental Section
Partial recipeSource: Main

Route 5: Other

7 · Experimental Section

Metal precursorscobalt acetate and copper acetate mixed at nominal Cu:Co = 75:25
Linker precursorsH4L, 0.05 mmol by doped-compound method
Solventsdistilled water for premixing; NEt3, 20 mL for reaction
Additivestriethylamine/NEt3
Atmospherenot specified
Temperatureroom temperature reaction; dried at 60 C
Timeseveral days
Work-upSimilar to Cu0.5Co0.5 doped-compound method.
ActivationWater removed under vacuum during salt premix; final drying at 60 C.
Scalability contextQuantitative yield implied for doped compounds.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt acetatenot individually stated7 · Experimental Section
Metal Sourcecopper acetatenot individually stated7 · Experimental Section
LinkerH4L0.05 mmol by common doped route7 · Experimental Section
SolventNEt320 mL by common doped route7 · Experimental Section
Partial recipeSource: Main

Route 6: Other

7 · Experimental Section

Metal precursorscobalt acetate and copper acetate mixed at nominal Cu:Co = 90:10
Linker precursorsH4L, 0.05 mmol by doped-compound method
Solventsdistilled water for premixing; NEt3, 20 mL for reaction
Additivestriethylamine/NEt3
Atmospherenot specified
Temperatureroom temperature reaction; dried at 60 C
Timeseveral days
Work-upSimilar to Cu0.5Co0.5 doped-compound method.
ActivationWater removed under vacuum during salt premix; final drying at 60 C.
Scalability contextQuantitative yield implied for doped compounds.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt acetatenot individually stated7 · Experimental Section
Metal Sourcecopper acetatenot individually stated7 · Experimental Section
LinkerH4L0.05 mmol by common doped route7 · Experimental Section
SolventNEt320 mL by common doped route7 · Experimental Section
Partial recipeSource: Main

Route 7: Other

7 · Experimental Section

Metal precursorscobalt acetate and copper acetate mixed at nominal Cu:Co = 95:5
Linker precursorsH4L, 0.05 mmol by doped-compound method
Solventsdistilled water for premixing; NEt3, 20 mL for reaction
Additivestriethylamine/NEt3
Atmospherenot specified
Temperatureroom temperature reaction; dried at 60 C
Timeseveral days
Work-upSimilar to Cu0.5Co0.5 doped-compound method.
ActivationWater removed under vacuum during salt premix; final drying at 60 C.
Scalability contextQuantitative yield implied for doped compounds.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt acetatenot individually stated7 · Experimental Section
Metal Sourcecopper acetatenot individually stated7 · Experimental Section
LinkerH4L0.05 mmol by common doped route7 · Experimental Section
SolventNEt320 mL by common doped route7 · Experimental Section
Complete recipeSource: Main

Route 8: Other

7 · Experimental Section

Metal precursorscopper acetate replacing cobalt acetate
Linker precursorsH4L, as in Cu0.0Co1.0 synthesis
SolventsNEt3, as in Cu0.0Co1.0 synthesis
Additivestriethylamine/NEt3 used in large excess
Atmospherenot specified
Temperatureroom temperature reaction; drying temperature not separately restated
Time72-120 (by similarity to Cu0.0Co1.0 route)
Work-upSynthetic procedure similar to Cu0.0Co1.0; final product black; quantitative yield.
Activationnot separately specified; similar to Cu0.0Co1.0 route
Scalability contextQuantitative yield reported; no scale-up discussion.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetatenot separately stated; cobalt acetate replaced7 · Experimental Section
LinkerH4Las in Cu0.0Co1.0 synthesis7 · Experimental Section
SolventNEt3as in Cu0.0Co1.0 synthesis7 · Experimental Section