Synthesis evidence

Multi-stimulus semiconductor Cu(i)-I-pyrimidine coordination polymer with thermo- and mechanochromic sensing

Lopez J., Murillo M., Lifante-Pedrola G. et al. · CrystEngComm · 2022 · 341-349

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: Other

main p.3 / article p.343 · Synthetic procedure

Metal precursorsCuI (190 mg, 1.00 mmol)
Linker precursors2-amino-4-chloropyrimidine (aClpym) (130 mg, 1.00 mmol)
SolventsEthanol (23 mL) for ligand solution; acetonitrile (12 mL) for CuI solution.
AtmosphereNot specified for synthesis.
Temperature25
Time24
Oxidant / reductantNone reported.
Work-upFiltered; washed with acetonitrile (2 x 3 mL) and ethanol (2 x 3 mL); dried under vacuum.
ActivationDried under vacuum; no porosity activation reported.
Scalability contextSingle-step room-temperature precipitation; yield 242 mg, 76% based on Cu.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(I) iodide (CuI)190 mg, 1.00 mmolmain p.3 / article p.343 · Synthetic procedure
Linker2-amino-4-chloropyrimidine (aClpym)130 mg, 1.00 mmolmain p.3 / article p.343 · Synthetic procedure
Solventethanol (EtOH)23 mLmain p.3 / article p.343 · Synthetic procedure
Solventacetonitrile (CH3CN)12 mLmain p.3 / article p.343 · Synthetic procedure
Complete recipeSource: Main

Route 2: Other

main p.3 / article p.343 · Synthetic procedure

Metal precursorsMother liquor from CuI/aClpym synthesis.
Linker precursorsMother liquor from CuI/aClpym synthesis.
SolventsAcetonitrile/ethanol mother solution.
AtmosphereNot specified.
Temperatureroom temperature
Time48
Oxidant / reductantNone reported.
Work-upSlow evaporation of mother solution to give colourless needle-shaped crystals.
ActivationNone reported.
Scalability contextCrystallisation route for X-ray-quality crystals rather than bulk scale-up.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othermother solution from CP1 synthesisNot specifiedmain p.3 / article p.343 · Synthetic procedure
Solventacetonitrile/ethanolNot specifiedmain p.3 / article p.343 · Synthetic procedure