Synthesis evidence

One‐Pot hydrothermal synthesis of 1D copper (II) coordination polymers involving in-situ decarboxylation

Ay B., Sahin O., Yildiz E. · Solid State Sciences · 2019 · 105958

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: Hydrothermal

main p.2 · 2.2. Synthesis of coordination polymers

Metal precursorsCuSO4.5H2O (0.2497 g, 1.00 mmol) and ZnSO4.H2O (0.1794 g, 1.00 mmol); Zn sulfate reported to influence decarboxylation but not coordinate in the product.
Linker precursors2,6-pydc acid (0.0836 g, 0.50 mmol) as in situ 2-pyc precursor; 1,10-phenanthroline monohydrate (0.0901 g, 0.50 mmol) present in one-pot mixture.
SolventsH2O (5.00 mL, 277.80 mmol).
AdditivesH3BO3 (0.0309 g, 0.50 mmol); ZnSO4.H2O acts as a sulfate salt additive/catalyst for decarboxylation.
AtmosphereAutogenous pressure in a 23 mL PTFE-lined stainless steel/Parr acid reactor.
Temperature180
Time120
Work-upStirred 30 min at room temperature before heating; cooled to room temperature; mixed crystals washed with pure water and dried at room temperature.
ActivationNo activation reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O0.2497 g, 1.00 mmolmain p.2 · 2.2. Synthesis of coordination polymers
AdditiveZnSO4.H2O0.1794 g, 1.00 mmolmain p.2 · 2.2. Synthesis of coordination polymers
Linker2,6-pydc acid0.0836 g, 0.50 mmolmain p.2 · 2.2. Synthesis of coordination polymers
Linker1,10-phenanthroline monohydrate0.0901 g, 0.50 mmolmain p.2 · 2.2. Synthesis of coordination polymers
AdditiveH3BO30.0309 g, 0.50 mmolmain p.2 · 2.2. Synthesis of coordination polymers
SolventH2O5.00 mL, 277.80 mmolmain p.2 · 2.2. Synthesis of coordination polymers
Complete recipeSource: Main

Route 2: Hydrothermal

main p.2 · 2.2. Synthesis of coordination polymers

Metal precursorsCuSO4.5H2O (0.2497 g, 1.00 mmol) and ZnSO4.H2O (0.1794 g, 1.00 mmol); sulfate from the metal salts is incorporated in CP 2.
Linker precursors1,10-phenanthroline monohydrate (0.0901 g, 0.50 mmol); 2,6-pydc acid (0.0836 g, 0.50 mmol) present in one-pot mixture.
SolventsH2O (5.00 mL, 277.80 mmol).
AdditivesH3BO3 (0.0309 g, 0.50 mmol); ZnSO4.H2O.
AtmosphereAutogenous pressure in a 23 mL PTFE-lined stainless steel/Parr acid reactor.
Temperature180
Time120
Work-upStirred 30 min at room temperature before heating; cooled to room temperature; mixed crystals washed with pure water and dried at room temperature.
ActivationNo activation reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O0.2497 g, 1.00 mmolmain p.2 · 2.2. Synthesis of coordination polymers
Metal SourceZnSO4.H2O0.1794 g, 1.00 mmolmain p.2 · 2.2. Synthesis of coordination polymers
Linker1,10-phenanthroline monohydrate0.0901 g, 0.50 mmolmain p.2 · 2.2. Synthesis of coordination polymers
Linker2,6-pydc acid0.0836 g, 0.50 mmolmain p.2 · 2.2. Synthesis of coordination polymers
AdditiveH3BO30.0309 g, 0.50 mmolmain p.2 · 2.2. Synthesis of coordination polymers
SolventH2O5.00 mL, 277.80 mmolmain p.2 · 2.2. Synthesis of coordination polymers