cMOF Evidence Base

Synthesis evidence

Million-fold electrical conductivity enhancement in Fe2(DEBDC) versus Mn2(DEBDC) (E = S, O)

Sun L., Hendon C.H., Minier M.A. et al. · Journal of the American Chemical Society · 2015 · 6164-6167

8 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Other

S8-S9 · Fe2(DOBDC)(DMF)2

Metal precursorsFe2(DOBDC)(DMF)2.x(DMF)
Solventsdegassed and dry DCM (15 mL)
Atmosphereair-free conditions
Temperature100
Time2
Work-upDCM soak ca. 12 h with solvent refreshed three times; dried under vacuum.
ActivationVacuum drying at 100 degC for 2 h.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherFe2(DOBDC)(DMF)2.x(DMF)Not specifiedS8-S9 · Fe2(DOBDC)(DMF)2
Solventdegassed and dry DCM15 mLS8-S9 · Fe2(DOBDC)(DMF)2
Partial recipeSource: SI

Route 2: Other

S8 · Fe2(DOBDC)(DMF)2

Metal precursorsas-synthesized Fe2(DOBDC), prepared according to reported procedure
Solventsdegassed and dry DMF (10 mL)
AtmosphereN2-filled glovebox
Temperature24
Time12
Work-upDMF solvent refreshed three times; dried under vacuum at 24 degC for 0.5 h.
ActivationVacuum drying at 24 degC for 0.5 h; guest-loaded state retained.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized Fe2(DOBDC)Not specifiedS8 · Fe2(DOBDC)(DMF)2
Solventdegassed and dry DMF10 mLS8 · Fe2(DOBDC)(DMF)2
Complete recipeSource: SI

Route 3: Other

S8 · Fe2(DSBDC)(DMF)2

Metal precursorsFe2(DSBDC)(DMF)2.x(DMF)
Solventsdry and degassed DCM (15 mL)
Atmosphereair-free conditions
Temperature100
Time2
Work-upSoaked in DCM with solvent refreshed twice; dried under vacuum.
ActivationVacuum drying at 100 degC for 2 h removed guest solvent; coordinated DMF remains.
Scalability context83 mg, 31% reported for Fe2(DSBDC)(DMF)2.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherFe2(DSBDC)(DMF)2.x(DMF)Not specifiedS8 · Fe2(DSBDC)(DMF)2
Solventdry and degassed DCM15 mLS8 · Fe2(DSBDC)(DMF)2
Complete recipeSource: Both

Route 4: Solvothermal

S7 · Fe2(DSBDC)(DMF)2.x(DMF)

Metal precursorsanhydrous FeCl2 (330 mg, 2.60 mmol)
Linker precursorsH4DSBDC (120 mg, 0.52 mmol)
Solventsdry and degassed DMF (20 mL); DMF wash/extraction (10 mL)
Atmospherenitrogen; air-free handling; N2-filled glovebox workup
Temperature140
Time18
Work-upReaction mixture transferred in N2 glovebox; extracted with dry/degassed DMF ca. 12 h, solvent refreshed twice; dried under vacuum at 24 degC for 0.5 h.
ActivationVacuum drying at 24 degC for 0.5 h; product retains guest DMF.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous FeCl2330 mg, 2.60 mmolS7 · Fe2(DSBDC)(DMF)2.x(DMF)
LinkerH4DSBDC120 mg, 0.52 mmolS7 · Fe2(DSBDC)(DMF)2.x(DMF)
Solventdry and degassed DMF20 mL reaction solvent; 10 mL extraction solventS7 · Fe2(DSBDC)(DMF)2.x(DMF)
Partial recipeSource: SI

Route 5: Other

S9 · Mn2(DOBDC)(DMF)2

Metal precursorsMn2(DOBDC)(DMF)2.x(DMF)
Solventsdegassed and dry DCM (15 mL)
Atmosphereair-free conditions
Temperature100
Time2
Work-upDCM soak ca. 12 h with solvent refreshed three times; dried under vacuum.
ActivationVacuum drying at 100 degC for 2 h.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMn2(DOBDC)(DMF)2.x(DMF)Not specifiedS9 · Mn2(DOBDC)(DMF)2
Solventdegassed and dry DCM15 mLS9 · Mn2(DOBDC)(DMF)2
Partial recipeSource: SI

Route 6: Other

S9 · Mn2(DOBDC)(DMF)2

Metal precursorsas-synthesized Mn2(DOBDC), prepared according to reported procedure
Solventsdegassed and dry DMF (10 mL)
AtmosphereN2-filled glovebox
Temperature24
Time12
Work-upDMF solvent refreshed three times; dried under vacuum at 24 degC for 0.5 h.
ActivationVacuum drying at 24 degC for 0.5 h; guest-loaded state retained.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized Mn2(DOBDC)Not specifiedS9 · Mn2(DOBDC)(DMF)2
Solventdegassed and dry DMF10 mLS9 · Mn2(DOBDC)(DMF)2
Partial recipeSource: SI

Route 7: Other

S8 · Mn2(DSBDC)(DMF)2

Metal precursorsMn2(DSBDC)(DMF)2.x(DMF)
Solventsdegassed and dry DCM (15 mL)
Atmosphereair-free conditions
Temperature100
Time2
Work-upDCM soak ca. 12 h with solvent refreshed three times; dried under vacuum.
ActivationVacuum drying at 100 degC for 2 h.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMn2(DSBDC)(DMF)2.x(DMF)Not specifiedS8 · Mn2(DSBDC)(DMF)2
Solventdegassed and dry DCM15 mLS8 · Mn2(DSBDC)(DMF)2
Partial recipeSource: SI

Route 8: Other

S8 · Mn2(DSBDC)(DMF)2

Metal precursorsas-synthesized Mn2(DSBDC), prepared according to reported procedure
Solventsdegassed and dry DMF (10 mL)
AtmosphereN2-filled glovebox
Temperature24
Time12
Work-upDMF solvent refreshed three times; dried under vacuum at 24 degC for 0.5 h.
ActivationVacuum drying at 24 degC for 0.5 h; guest-loaded state retained.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-synthesized Mn2(DSBDC)Not specifiedS8 · Mn2(DSBDC)(DMF)2
Solventdegassed and dry DMF10 mLS8 · Mn2(DSBDC)(DMF)2