Synthesis evidence

Electrical bistability around room temperature in an unprecedented one-dimensional coordination magnetic polymer

Amo-Ochoa P., Delgado E., Gomez-Garcia C.J. et al. · Inorganic Chemistry · 2013 · 5943-5950

1 structured synthesis route

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

Complete recipeSource: Main

Route 1: Other

2 · Experimental Section - Synthesis of Compound 1 · Scheme 1

Metal precursors[Fe2(S2C6H2Cl2)(CO)6] (300 mg, 0.61 mmol); K2CO3 (120 mg, 0.86 mmol)
Linker precursorsH2S2C6H2Cl2 (386 mg, 1.83 mmol)
SolventsPreviously degassed DMF (15 mL) for reaction; THF with a few drops of DMF, followed by H2O and n-hexane for crystallisation
AdditivesK2CO3 base; H2O and n-hexane added during crystallisation
AtmosphereArgon; DMF previously degassed
Temperatureroom temperature
Time8
Work-upSolvent removed to dryness; residue washed several times with dichloromethane; recrystallised from THF/DMF/H2O/n-hexane.
Scalability contextSmall-molecule Schlenk/solution synthesis; isolated yield 246 mg, 30%.
Show 9 structured reagent records
RoleReagentAmount / concentrationSource
BaseK2CO3120 mg, 0.86 mmol2 · Experimental Section - Synthesis of Compound 1 · Scheme 1
Solventdimethylformamide (DMF), previously degassed15 mL2 · Experimental Section - Synthesis of Compound 1 · Scheme 1
Metal Source[Fe2(S2C6H2Cl2)(CO)6]300 mg, 0.61 mmol2 · Experimental Section - Synthesis of Compound 1 · Scheme 1
LinkerH2S2C6H2Cl2386 mg, 1.83 mmol2 · Experimental Section - Synthesis of Compound 1 · Scheme 1
Solventtetrahydrofuran (THF)Not specified2 · Experimental Section - Synthesis of Compound 1 · Scheme 1
SolventDMFa few drops2 · Experimental Section - Synthesis of Compound 1 · Scheme 1
AdditiveH2ONot specified2 · Experimental Section - Synthesis of Compound 1 · Scheme 1
Solventn-hexaneNot specified2 · Experimental Section - Synthesis of Compound 1 · Scheme 1
Solventdichloromethaneseveral washes2 · Experimental Section - Synthesis of Compound 1 · Scheme 1