Synthesis evidence

Multifunctional coordination polymers based on copper with modified nucleobases, easily modulated in size and conductivity

Vegas V.G., Maldonado N., Castillo O. et al. · Journal of Inorganic Biochemistry · 2019 · 110805

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

3 · Materials and methods

Metal precursorspreformed CP1
Linker precursorspreformed CP1
Solventsnone reported for vapour exposure
Additivesiodine vapour
Atmosphereambient temperature and pressure
Temperatureambient
Time0-24
Oxidant / reductantIodine vapour used as p-type oxidative dopant
Work-upNo post-doping workup reported.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Oxidantiodine vapornot reported3 · Materials and methods
OtherCP1not reported3 · Materials and methods
Complete recipeSource: Main

Route 2: Other

3 · 2.2. Nanoprocessing of CP1 via top-down approach

Metal precursorspreformed CP1 crystals
Linker precursorspreformed CP1 crystals
Solvents3 mL acetone
Additivesultrasound bath processing
Atmosphereambient; not otherwise specified
Time1
Substrate orientationSiO2 substrate used only for SEM deposition
Work-upSuspension after 1 h sonication sampled before centrifugation; aliquot deposited on SiO2 for SEM.
Scalability contextPart of the top-down nanoprocessing route; final supernatant route gives 55% nanoprocessed material.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCP1 crystals1.5 mg, ca. 2 mm3 · 2.2. Nanoprocessing of CP1 via top-down approach
Solventacetone3 mL3 · 2.2. Nanoprocessing of CP1 via top-down approach
Complete recipeSource: Main

Route 3: Other

3 · 2.2. Nanoprocessing of CP1 via top-down approach

Metal precursorspreformed CP1 crystals
Linker precursorspreformed CP1 crystals
Solvents3 mL acetone
Atmosphereambient; not otherwise specified
Time1
Substrate orientationSiO2 substrate used only for SEM deposition
Work-upSonicated suspension centrifuged at 3000 rpm for 2 min; suspension and supernatant aliquots deposited on SiO2.
Scalability context55% of the initial material was nanoprocessed according to the main text.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCP1 crystals1.5 mg, ca. 2 mm3 · 2.2. Nanoprocessing of CP1 via top-down approach
Solventacetone3 mL3 · 2.2. Nanoprocessing of CP1 via top-down approach
Complete recipeSource: Main

Route 4: Solvothermal

3 · 2.1. Synthesis of CP1

Metal precursorsCu(NO3)2.3H2O (0.1 g, 0.41 mmol)
Linker precursorsthymine-1-acetic acid (0.152 g, 0.82 mmol); 4,4'-bpy (0.065 g, 0.41 mmol); oxalate forms in situ
Solvents18 mL MilliQ water
Atmospheresealed glass reactor; atmosphere not specified
Temperature140
Time72
Oxidant / reductantCu(II) nitrate; oxalate generated in situ from carboxyl groups under acidic solvothermal conditions
Work-upSupernatant removed under vacuum; turquoise crystals separated manually from dark-blue co-crystals.
ActivationDried/worked up under vacuum; no activation protocol reported.
Scalability context60% yield reported for manually separated turquoise CP1 crystals.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O0.1 g, 0.41 mmol3 · 2.1. Synthesis of CP1
Linkerthymine-1-acetic acid (TAcOH)0.152 g, 0.82 mmol3 · 2.1. Synthesis of CP1
Linker4,4'-bpy0.065 g, 0.41 mmol3 · 2.1. Synthesis of CP1
Solventwater MilliQ18 mL3 · 2.1. Synthesis of CP1
Complete recipeSource: Main

Route 5: Solvothermal

3 · 2.3. Synthesis of CP2

Metal precursorsCu(NO3)2.3H2O (100 mg, 0.41 mmol)
Linker precursorsUracil-1-acetic acid (141 mg, 0.82 mmol); 4,4'-bpy (65 mg, 0.41 mmol); oxalate forms in situ
Solvents18 mL water
Atmospheresolvothermal reactor; atmosphere not specified
Temperature120
Time72
Oxidant / reductantCu(II) nitrate; oxalate generated in situ under acidic solvothermal conditions
Work-upLight-blue crystals dried under vacuum after cooling.
ActivationDried under vacuum; no separate activation protocol reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O100 mg, 0.41 mmol3 · 2.3. Synthesis of CP2
LinkerUracil-1-acetic acid (UAcOH)141 mg, 0.82 mmol3 · 2.3. Synthesis of CP2
Linker4,4'-bpy65 mg, 0.41 mmol3 · 2.3. Synthesis of CP2
Solventwater18 mL3 · 2.3. Synthesis of CP2
Complete recipeSource: Main

Route 6: Solvothermal

3 · 2.4. Synthesis of CP3

Metal precursorsaqueous solution (1 mL) of Cu(NO3)2.H2O (100 mg, 0.41 mmol)
Linker precursorsthymine-1-acetic acid (76 mg, 0.41 mmol); 4,4'-bpy (64 mg, 0.41 mmol)
Solvents12 mL ethanol plus 1 mL aqueous copper nitrate solution
Atmospheresolvothermal glass reactor; atmosphere not specified
Temperature140
Time72
Oxidant / reductantEthanol solvent implicated as reducing agent for Cu(II) to Cu(I).
Work-upYellow crystals filtered off and dried in vacuum.
ActivationDried in vacuum; no separate activation protocol reported.
Scalability context41% yield reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.H2O100 mg, 0.41 mmol in 1 mL aqueous solution3 · 2.4. Synthesis of CP3
Linkerthymine-1-acetic acid (TAcOH)76 mg, 0.41 mmol3 · 2.4. Synthesis of CP3
Linker4,4'-bpy64 mg, 0.41 mmol3 · 2.4. Synthesis of CP3
Solventethanol12 mL3 · 2.4. Synthesis of CP3