Synthesis evidence

CH⋯Cl relevant discrepancy on structure, magnetic and electronic conductivity of two mixed-valence CuICuII coordination polymers

Shi L., Yang P., Huang G. et al. · Journal of Solid State Chemistry · 2011 · 1699-1706

2 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Solvothermal

2 · 2.2 Synthesis

Metal precursorsCuCl2.2H2O (0.4 mmol, 0.0682 g)
Linker precursorsH2qdiol (0.6 mmol, 0.0973 g); bpy (0.3 mmol, 0.0469 g)
Solventsethanol (10 mL)
Additivesethanolic NaOH to adjust pH to 8
Atmospheresealed Teflon-lined stainless steel reactor; gas atmosphere not specified
Temperature140
Time72
Oxidant / reductantCu(II) partially reduced to Cu(I) under solvothermal conditions; no separate reductant specified
Work-upcooled at 3 C/h to 100 C and then 5 C/h to room temperature; crystals collected and washed with distilled water
Activationnone reported for isolated crystals
Scalability context23 mL Teflon-lined stainless steel reactor; isolated yield 0.0679 g.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuCl2.2H2O0.4 mmol, 0.0682 g2 · 2.2 Synthesis
LinkerH2qdiol0.6 mmol, 0.0973 g2 · 2.2 Synthesis
Linkerbpy0.3 mmol, 0.0469 g2 · 2.2 Synthesis
Solventethanol10 ml2 · 2.2 Synthesis
Baseethanolic NaOHto pH 82 · 2.2 Synthesis
Complete recipeSource: Main

Route 2: Solvothermal

2 · 2.2 Synthesis

Metal precursorsCuCl2.2H2O (0.4 mmol, 0.0682 g)
Linker precursorsH2qdiol (0.6 mmol, 0.0973 g); phen (0.3 mmol, 0.0541 g)
Solventsethanol (10 mL)
Additivesethanolic NaOH to adjust pH to 8
Atmospheresealed Teflon-lined stainless steel reactor; gas atmosphere not specified
Temperature140
Time72
Oxidant / reductantCu(II) partially reduced to Cu(I) under solvothermal conditions; no separate reductant specified
Work-upanalogous cooling and washing procedure to compound 1
Activationnone reported for isolated crystals
Scalability context23 mL Teflon-lined stainless steel reactor inferred from analogous procedure; isolated yield 0.0553 g.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuCl2.2H2O0.4 mmol, 0.0682 g2 · 2.2 Synthesis
LinkerH2qdiol0.6 mmol, 0.0973 g2 · 2.2 Synthesis
Linkerphen0.3 mmol, 0.0541 g2 · 2.2 Synthesis
Solventethanol10 ml2 · 2.2 Synthesis
Baseethanolic NaOHto pH 82 · 2.2 Synthesis