Vague recipeSource: Main
Route 1: Unknown
2 · Experimental Section
Synthesis evidence
2D Conductive Iron-Quinoid Magnets Ordering up to Tc = 105 K via Heterogenous Redox Chemistry
DeGayner J.A., Jeon I.-R., Sun L. et al. · Journal of the American Chemical Society · 2017 · 4175-4184
4 structured synthesis routes
Completeness describes how fully the route could be reconstructed from the main article and supporting information.
Complete recipeSource: Main
Route 2: Other
2 · Experimental Section
Metal precursorscompound 1, (Me2NH2)2[Fe2L3].2H2O.6DMF
Linker precursorschloranilate linkers already present in compound 1
SolventsTHF; benzene
Atmospheredinitrogen glovebox for manipulations; reduced pressure for sublimation/activation
Temperature-78 C sublimation; 120 C activation
Time72 h THF soak + 72 h benzene soak + 36 h sublimation + 24 h heating
Work-upfinal benzene wash removed by sublimation at reduced pressure at -78 C for 36 h
Activationheated for 24 h at 120 C under reduced pressure
Scalability context180 mg starting 1 gave 95.5 mg 1a, 83% yield.
Show 3 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | compound 1 | 180 mg, 0.139 mmol | 2 · Experimental Section |
| Solvent | THF | 10 x 10 mL | 2 · Experimental Section |
| Solvent | benzene | 10 x 10 mL | 2 · Experimental Section |
Complete recipeSource: Main
Route 3: Other
2 · Experimental Section
Metal precursorscompound 1, (Me2NH2)2[Fe2L3].2H2O.6DMF
Linker precursorschloranilate linkers already present in compound 1
SolventsDMF
Atmospheredinitrogen glovebox general conditions
Temperatureambient temperature
Time48 h reaction; 72 h DMF washing
Oxidant / reductantcobaltocene (Cp2Co), reductant
Work-upsupernatant decanted; solid washed with DMF (10 x 10 mL) over 3 days; collected by filtration
Activationnot desolvated; attempts to desolvate 2 led to loss of crystallinity and porosity
Scalability context203 mg compound 1 and 118 mg cobaltocene gave 0.198 g compound 2, 88% yield.
Show 3 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Other | crystals of 1 | 203 mg, 0.156 mmol | 2 · Experimental Section |
| Reductant | cobaltocene | 118 mg, 0.624 mmol | 2 · Experimental Section |
| Solvent | DMF | 6 mL reaction solvent; 10 x 10 mL wash | 2 · Experimental Section |
Vague recipeSource: Main
Route 4: Unknown
2 · Experimental Section