cMOF Evidence Base

Synthesis evidence

Coordination environments and π-conjugation in dense lithium coordination polymers

Tominaka S., Yeung H.H.-M., Henke S. et al. · CrystEngComm · 2016 · 398-406

8 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

p003 · 2.1 Synthesis

Metal precursorsLiOH
Linker precursors23dcaqH2
Solventswater, 8 mL
AtmosphereNot specified; loosely sealed glass vial
Temperature60 °C for 1 h, then 90 °C overnight
Time1 h plus overnight
Work-upGradual drying; composition by elemental analysis; crystals recovered as pale yellow plates
ActivationDried after synthesis; no activation reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLiOH2 mol L-1p003 · 2.1 Synthesis
Linker23dcaqH21 mol L-1p003 · 2.1 Synthesis
Solventwater8 mLp003 · 2.1 Synthesis
Complete recipeSource: Both

Route 2: Solvothermal

p003 · 2.1 Synthesis

Metal precursorsLiOAc
Linker precursors23dcaqH2
Solventsacetonitrile, 20 mL
AtmosphereNot specified; loosely sealed glass vial for product, well-sealed vial for larger crystals
Temperature100 °C
Time48 h for product; overnight well-sealed for structure-determination crystals
Work-upRinsed with ethanol, dried; larger crystals recovered by reduced-pressure filtration, rinsed with ethanol, dried in air
ActivationDried after ethanol rinse; no activation reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLiOAc20 mmol L-1p003 · 2.1 Synthesis
Linker23dcaqH210 mmol L-1p003 · 2.1 Synthesis
Solventacetonitrile20 mLp003 · 2.1 Synthesis
Complete recipeSource: Both

Route 3: Solvothermal

p003 · 2.1 Synthesis

Metal precursorsLiOH
Linker precursors15dhaqH2
Solventsethanol and water, mixed 1:1 volume ratio, total 8 mL
AtmosphereNot specified; well-sealed borosilicate glass vial
Temperature90 °C
Time72 h plus a few days at room temperature
Work-upVacuum filtration, ethanol rinse, dried in air
ActivationDried in air; no activation reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLiOH1.53 mol L-1p003 · 2.1 Synthesis
Linker15dhaqH275 mmol L-1p003 · 2.1 Synthesis
Solventethanol solution and aqueous solution8 mL total, 1:1 volume ratiop003 · 2.1 Synthesis
Complete recipeSource: Both

Route 4: Solvothermal

p003 · 2.1 Synthesis

Metal precursorsLiOH
Linker precursors14dhaqH2
Solventsethanol and water, mixed 1:1 volume ratio, total 8 mL
AtmosphereNot specified; well-sealed borosilicate glass vial
Temperature90 °C
Time48 h plus a few days at room temperature
Work-upFiltration under reduced pressure, ethanol rinse, dried in air
ActivationDried in air; no activation reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLiOH60 mmol L-1p003 · 2.1 Synthesis
Linker14dhaqH223 mmol L-1p003 · 2.1 Synthesis
Solventethanol solution and aqueous solution8 mL total, 1:1 volume ratiop003 · 2.1 Synthesis
Complete recipeSource: Both

Route 5: Hydrothermal

p003 · 2.1 Synthesis

Metal precursorsLiOH
Linker precursors14dhaqH2
Solventswater, 8 mL
AtmosphereNot specified; well-sealed borosilicate glass vial
Temperature90 °C
Time48 h plus a few days at room temperature
Work-upVacuum filtration, ethanol rinse, dried in air
ActivationDried in air; no activation reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLiOH210 mmol L-1p003 · 2.1 Synthesis
Linker14dhaqH2200 mmol L-1p003 · 2.1 Synthesis
Solventwater8 mLp003 · 2.1 Synthesis
Complete recipeSource: Both

Route 6: Hydrothermal

p003 · 2.1 Synthesis

Metal precursorsLiOH
Linker precursors14hnaqH
Solventswater, 8 mL
AtmosphereNot specified; well-sealed borosilicate glass vial
Temperature90 °C, then cooled to room temperature
Time72 h plus gradual cooling
Work-upVacuum filtration, ethanol rinse, dried in air
ActivationDried in air; no activation reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLiOH60 mmol L-1p003 · 2.1 Synthesis
Linker14hnaqH12 mmol L-1p003 · 2.1 Synthesis
Solventwater8 mLp003 · 2.1 Synthesis
Complete recipeSource: SI

Route 7: Hydrothermal

p017 · 9. Additional compound

Metal precursorsLiOH
Linker precursors15dhaqH2
Solventsaqueous solution, 3 mL
Additivespyrazine
AtmosphereNot specified; well-sealed borosilicate glass vial
Temperature90 °C for 6 d, then 100 °C for 3 h, then cooled to room temperature over about 7 h
Time144 h plus 3 h and about 7 h cooling
Work-upReduced-pressure filtration, ethanol rinse, dried in air
ActivationDried in air; no activation reported
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLiOH1.44 mmolp017 · 9. Additional compound
Linker15dhaqH2 aqueous solution0.1 mmol/3 mLp017 · 9. Additional compound
Additivepyrazine0.12 mmolp017 · 9. Additional compound
Solventwater3 mLp017 · 9. Additional compound
Partial recipeSource: Both

Route 8: Solvothermal

p004 · 2.1 Synthesis

Metal precursorsLiOH
Linker precursorsformate generated/represented by formate framework; imidazole present
SolventsN,N-dimethylformamide, 8 mL
Additivesimidazole
AtmosphereNot specified
Temperature90 °C
Time48 h after sonication steps
Work-upRod-like crystals obtained; elemental analysis reported
ActivationNo activation reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceLiOH4 mol L-1p004 · 2.1 Synthesis
SolventN,N-dimethylformamide (DMF)8 mLp004 · 2.1 Synthesis
Additiveimidazole3.9 mol L-1p004 · 2.1 Synthesis