Synthesis evidence

A europium(III) based metal-organic framework: Bifunctional properties related to sensing and electronic conductivity

Hao Z., Yang G., Song X. et al. · Journal of Materials Chemistry A · 2014 · 237-244

3 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

238 · Synthesis of EuL

Metal precursorsEu(NO3)3.6H2O (0.112 mmol, 50 mg)
Linker precursorsBiphenyl-3,4',5-tricarboxylate / H3BPT (0.07 mmol, 20 mg)
SolventsDMF (1.0 mL) and H2O (1.0 mL)
Additivesnone reported
Atmospheresealed 10 mL glass vial; atmosphere otherwise not specified
Temperature80
Time24
Oxidant / reductantnone reported
Work-upcooled to room temperature; colourless crystals collected and air-dried
Activationnone for as-synthesised crystals
Scalability context87% yield based on H3BPT; authors state a moderate ligand:metal ratio gave higher purity and yield than a prior excess-reagent method.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceEu(NO3)3.6H2O0.112 mmol, 50 mg238 · Synthesis of EuL
LinkerBiphenyl-3,4',5-tricarboxylate (H3BPT)0.07 mmol, 20 mg238 · Synthesis of EuL
SolventDMF1.0 mL238 · Synthesis of EuL
SolventH2O1.0 mL238 · Synthesis of EuL
Complete recipeSource: SI

Route 2: Other

2 · Impedance test

Metal precursorsI2-incorporated EuL powder
Linker precursorsBPT framework in I2-incorporated EuL
Solventsnone reported during pressing
Additivesnone reported
Atmospherenot specified; subsequent EIS under anhydrous conditions
Time0.083 h pressing (5 min)
Work-upground to homogeneous powder with mortar and pestle; pressed in standard 8 mm die between two stainless steel electrodes at 5000 kg for 5 min
ActivationI2-loaded sample had been outgassed before iodine loading; no additional pellet activation reported
Scalability contextPellet pressing described for impedance measurement only.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherI2-incorporated EuL powderNot specified2 · Impedance test
Complete recipeSource: Main

Route 3: Other

238 · Synthesis of I2-incorporated EuL

Metal precursorspreformed EuL crystals (200 mg)
Linker precursorspreformed EuL framework containing BPT linker
Solventsdry methanol; dry hexane; hexane wash
AdditivesI2 in dry hexane solution (2 x 10^-2 mol L-1)
Atmospheredry media; no inert gas specified
Temperature120 for outgassing; soaking temperature not explicitly stated
Time72 h methanol exchange; 12 h outgassing; 48 h I2/hexane immersion
Oxidant / reductantI2 guest/charge-carrier precursor
Work-updry methanol renewed three times a day for 3 days; washed by hexane 4-6 times after I2 loading
Activationoutgassed at 120 degC for 12 h before iodine loading
Scalability contextUses 200 mg EuL crystals for loading; no scale-up discussion.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherEuL crystals200 mg238 · Synthesis of I2-incorporated EuL
Solventdry methanol25 mL glass bottle; renewed three times a day for 3 days238 · Synthesis of I2-incorporated EuL
AdditiveI22 x 10^-2 mol L-1 in dry hexane238 · Synthesis of I2-incorporated EuL
Solventdry hexaneNot specified238 · Synthesis of I2-incorporated EuL