cMOF Evidence Base

Synthesis evidence

A highly crystalline anthracene-based MOF-74 series featuring electrical conductivity and luminescence

Scheurle P.I., Mahringer A., Jakowetz A.C. et al. · Nanoscale · 2019 · 20949-20955

10 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

S11 · Anthracene-based MOF-74 (ANMOF-74) synthesis

Metal precursorsCo(NO3)2 · 6H2O (24.30 mg, 0.084 mmol)
Linker precursors4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid) (10.00 mg, 0.022 mmol)
SolventsDMF (1.1 mL), EtOH (0.3 mL) and H2O (1 mL)
Additivesbenzoic acid (2.7 mg, 0.022 mmol)
Atmospherenot specified; culture tube
Temperature120
Time48
Work-upprecipitate washed with DMF (2 x 10 mL) and MeOH (1 x 10 mL)
Activationactivated at 120 deg C to remove less volatile solvent; elemental analysis after vacuum treatment
Scalability contextSmall culture-tube synthesis using 10 mg linker scale.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid)10.00 mg, 0.022 mmolS11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Metal SourceCo(NO3)2 · 6H2O24.30 mg, 0.084 mmolS11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
SolventDMF (1.1 mL), EtOH (0.3 mL) and H2O (1 mL)Not specifiedS11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Additivebenzoic acid2.7 mg, 0.022 mmolS11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Complete recipeSource: Both

Route 2: Solvothermal

S10 · Anthracene-based MOF-74 (ANMOF-74) synthesis

Metal precursorsMg(NO3)2 ·6H2O (21.60 mg, 0.084 mmol)
Linker precursors4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid) (10.00 mg, 0.022 mmol)
SolventsDMF (1.3 mL) and MeOH (0.2 mL)
Additivesnone reported
Atmospherenot specified; culture tube
Temperature120
Time48
Work-upprecipitate washed with DMF (2 x 10 mL) and MeOH (1 x 10 mL)
Activationactivated at 120 deg C to remove less volatile solvent; elemental analysis after vacuum treatment
Scalability contextSmall culture-tube synthesis using 10 mg linker scale.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid)10.00 mg, 0.022 mmolS10 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Metal SourceMg(NO3)2 ·6H2O21.60 mg, 0.084 mmolS10 · Anthracene-based MOF-74 (ANMOF-74) synthesis
SolventDMF (1.3 mL) and MeOH (0.2 mL)Not specifiedS10 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Complete recipeSource: Both

Route 3: Solvothermal

S11 · Anthracene-based MOF-74 (ANMOF-74) synthesis

Metal precursorsMnCl2 · 4H2O (22.60 mg, 0.084 mmol)
Linker precursors4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid) (10.00 mg, 0.022 mmol)
SolventsDMF (1.5 mL)
Additivesnone reported
Atmospherenot specified; culture tube
Temperature120
Time48
Work-upprecipitate washed with DMF (2 x 10 mL) and MeOH (1 x 10 mL)
Activationactivated at 120 deg C to remove less volatile solvent; elemental analysis after vacuum treatment
Scalability contextSmall culture-tube synthesis using 10 mg linker scale.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid)10.00 mg, 0.022 mmolS11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Metal SourceMnCl2 · 4H2O22.60 mg, 0.084 mmolS11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
SolventDMF (1.5 mL)Not specifiedS11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Complete recipeSource: Both

Route 4: Solvothermal

S10-S11 · Anthracene-based MOF-74 (ANMOF-74) synthesis

Metal precursorsNiCl2 (10.80 mg, 0.084 mmol)
Linker precursors4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid) (10.00 mg, 0.022 mmol)
Solventsbenzyl alcohol (0.7 mL) and EtOH (0.7 mL)
Additivesbenzoic acid (2.7 mg, 0.022 mmol)
Atmospherenot specified; culture tube
Temperature120
Time48
Work-upprecipitate washed with DMF (2 x 10 mL) and MeOH (1 x 10 mL)
Activationactivated at 120 deg C to remove less volatile solvent; elemental analysis after vacuum treatment
Scalability contextSmall culture-tube synthesis using 10 mg linker scale.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid)10.00 mg, 0.022 mmolS10-S11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Metal SourceNiCl210.80 mg, 0.084 mmolS10-S11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Solventbenzyl alcohol (0.7 mL) and EtOH (0.7 mL)Not specifiedS10-S11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Additivebenzoic acid2.7 mg, 0.022 mmolS10-S11 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Complete recipeSource: Both

Route 5: Solvothermal

S10 · Anthracene-based MOF-74 (ANMOF-74) synthesis

Metal precursorsZn(NO3)2 ·4H2O (22.07 mg, 0.084 mmol)
Linker precursors4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid) (10.00 mg, 0.022 mmol)
SolventsDMF (1.5 mL)
Additivesbenzoic acid (2.7 mg, 0.022 mmol)
Atmospherenot specified; culture tube
Temperature120
Time48
Work-upprecipitate washed with DMF (2 x 10 mL) and MeOH (1 x 10 mL)
Activationactivated at 120 deg C to remove less volatile solvent; elemental analysis after vacuum treatment
Scalability contextSmall culture-tube synthesis using 10 mg linker scale.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker4,4'-(anthracene-9,10-diyl)bis(2-hydroxybenzoic acid)10.00 mg, 0.022 mmolS10 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Metal SourceZn(NO3)2 ·4H2O22.07 mg, 0.084 mmolS10 · Anthracene-based MOF-74 (ANMOF-74) synthesis
SolventDMF (1.5 mL)Not specifiedS10 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Additivebenzoic acid2.7 mg, 0.022 mmolS10 · Anthracene-based MOF-74 (ANMOF-74) synthesis
Complete recipeSource: Both

Route 6: Solvothermal

S13 · MOF-74 synthesis

Metal precursorscobalt nitrate hexahydrate, Co(NO3)2·6H2O (2.377 g, 8.67 mmol)
Linker precursors2,5-dihydroxy-1,4-benzenedicarboxylic acid (0.482 g, 2.43 mmol)
Solvents1:1:1 mixture of DMF-ethanol-water (200 mL)
Additivesnone reported
Atmospherenot specified
Temperature100
Time24
Work-upprecipitate washed with DMF (2 x 10 mL) and ethanol or methanol (1 x 10 mL); dried under reduced pressure
Activationmain text states crystalline MOF-74 powders were activated (vacuum dried) before pellet conductivity evaluation
Scalability contextRegular MOF-74 control synthesis; some batches use 200 mL total solvent and three 100 mL bottles.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,5-dihydroxy-1,4-benzenedicarboxylic acid0.482 g, 2.43 mmolS13 · MOF-74 synthesis
Metal Sourcecobalt nitrate hexahydrate, Co(NO3)2·6H2O2.377 g, 8.67 mmolS13 · MOF-74 synthesis
Solvent1:1:1 mixture of DMF-ethanol-water (200 mL)Not specifiedS13 · MOF-74 synthesis
Complete recipeSource: Both

Route 7: Solvothermal

S12 · MOF-74 synthesis

Metal precursorsmagnesia nitrate hexahydrate, Mg(NO3)2·6H2O (0.475 mg, 1.85 mmol (as printed))
Linker precursors2,5-dihydroxy-1,4-benzenedicarboxylic acid (0.111 g, 0.559 mmol)
Solvents15:1:1 mixture of DMF-ethanol-water (50 mL)
Additivesnone reported
Atmospherenot specified
Temperature125
Time24
Work-upprecipitate washed with DMF (2 x 10 mL) and ethanol or methanol (1 x 10 mL); dried under reduced pressure
Activationmain text states crystalline MOF-74 powders were activated (vacuum dried) before pellet conductivity evaluation
Scalability contextRegular MOF-74 control synthesis; some batches use 200 mL total solvent and three 100 mL bottles.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,5-dihydroxy-1,4-benzenedicarboxylic acid0.111 g, 0.559 mmolS12 · MOF-74 synthesis
Metal Sourcemagnesia nitrate hexahydrate, Mg(NO3)2·6H2O0.475 mg, 1.85 mmol (as printed)S12 · MOF-74 synthesis
Solvent15:1:1 mixture of DMF-ethanol-water (50 mL)Not specifiedS12 · MOF-74 synthesis
Complete recipeSource: Both

Route 8: Solvothermal

S13 · MOF-74 synthesis

Metal precursorsMnCl2·4H2O (1.07 g, 5.41 mmol)
Linker precursors2,5-dihydroxy-1,4-benzenedicarboxylic acid (0.27 g, 1.3 mmol)
Solvents15:1 mixture of DMF-ethanol (32 mL)
Additivesnone reported
Atmosphereargon
Temperature135
Time72
Work-upprecipitate washed with DMF (2 x 10 mL) and ethanol or methanol (1 x 10 mL); dried under reduced pressure
Activationmain text states crystalline MOF-74 powders were activated (vacuum dried) before pellet conductivity evaluation
Scalability contextRegular MOF-74 control synthesis; some batches use 200 mL total solvent and three 100 mL bottles.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,5-dihydroxy-1,4-benzenedicarboxylic acid0.27 g, 1.3 mmolS13 · MOF-74 synthesis
Metal SourceMnCl2·4H2O1.07 g, 5.41 mmolS13 · MOF-74 synthesis
Solvent15:1 mixture of DMF-ethanol (32 mL)Not specifiedS13 · MOF-74 synthesis
Complete recipeSource: Both

Route 9: Solvothermal

S12 · MOF-74 synthesis

Metal precursorsnickel nitrate hexahydrate, Ni(NO3)2·6H2O (2.378 mg, 8.178 mmol (as printed))
Linker precursors2,5-dihydroxy-1,4-benzenedicarboxylic acid (0.478 g, 2.41 mmol)
Solvents1:1:1 mixture of DMF-ethanol-water (200 mL)
Additivesnone reported
Atmospherenot specified
Temperature100
Time24
Work-upprecipitate washed with DMF (2 x 10 mL) and ethanol or methanol (1 x 10 mL); dried under reduced pressure
Activationmain text states crystalline MOF-74 powders were activated (vacuum dried) before pellet conductivity evaluation
Scalability contextRegular MOF-74 control synthesis; some batches use 200 mL total solvent and three 100 mL bottles.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,5-dihydroxy-1,4-benzenedicarboxylic acid0.478 g, 2.41 mmolS12 · MOF-74 synthesis
Metal Sourcenickel nitrate hexahydrate, Ni(NO3)2·6H2O2.378 mg, 8.178 mmol (as printed)S12 · MOF-74 synthesis
Solvent1:1:1 mixture of DMF-ethanol-water (200 mL)Not specifiedS12 · MOF-74 synthesis
Complete recipeSource: Both

Route 10: Solvothermal

S11-S12 · MOF-74 synthesis

Metal precursorszinc nitrate tetrahydrate, Zn(NO3)2·4H2O (0.053 mg, 0.203 mmol (as printed))
Linker precursors2,5-dihydroxy-1,4-benzenedicarboxylic acid (0.019 g, 0.096 mmol)
SolventsDMF (2 mL), 2-propanol (0.1 mL) and water (0.1 mL)
Additivesnone reported
Atmospherenot specified
Temperature105
Time24
Work-upprecipitate washed with DMF (2 x 10 mL) and ethanol or methanol (1 x 10 mL); dried under reduced pressure
Activationmain text states crystalline MOF-74 powders were activated (vacuum dried) before pellet conductivity evaluation
Scalability contextRegular MOF-74 control synthesis; some batches use 200 mL total solvent and three 100 mL bottles.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,5-dihydroxy-1,4-benzenedicarboxylic acid0.019 g, 0.096 mmolS11-S12 · MOF-74 synthesis
Metal Sourcezinc nitrate tetrahydrate, Zn(NO3)2·4H2O0.053 mg, 0.203 mmol (as printed)S11-S12 · MOF-74 synthesis
SolventDMF (2 mL), 2-propanol (0.1 mL) and water (0.1 mL)Not specifiedS11-S12 · MOF-74 synthesis