cMOF Evidence Base

Synthesis evidence

High Thermopower in a Zn-Based 3D Semiconductive Metal-Organic Framework

Park J., Hinckley A.C., Huang Z. et al. · Journal of the American Chemical Society · 2020 · 20531-20535

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

S3 · NH4OH as the base · Figure S1

Metal precursors22.0 mg zinc nitrate hexahydrate [Zn(NO3)2.6H2O]
Linker precursors13.8 mg HAB.3HCl
Solvents10 mL H2O for zinc nitrate; additional 5 mL H2O for HAB.3HCl
Additives82.8 uL NH4OH (6 M; 10 equiv. to HAB)
AtmosphereAir
Temperatureroom temperature
Time2
Work-upFiltered; washed with H2O (2 x 80 mL) and acetone (2 x 50 mL).
ActivationDried under vacuum for 1 h at room temperature unless otherwise noted.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezinc nitrate hexahydrate [Zn(NO3)2.6H2O]22.0 mgS3 · NH4OH as the base · Figure S1
LinkerHAB.3HCl13.8 mgS3 · NH4OH as the base · Figure S1
SolventH2O10 mL + 5 mLS3 · NH4OH as the base · Figure S1
BaseNH4OH82.8 uL · 6 M; 10 equiv. to HABS3 · NH4OH as the base · Figure S1
Complete recipeSource: SI

Route 2: Other

S3-S4 · Triethylamine (TEA) as the base · Figure S2

Metal precursors22.0 mg zinc nitrate hexahydrate [Zn(NO3)2.6H2O]
Linker precursors13.8 mg HAB.3HCl
Solvents7.5 mL DMF and 7.5 mL H2O
AdditivesTEA varied to 3 equiv. relative to HAB
AtmosphereAir
Temperatureroom temperature
Time2
Work-upSame as TEA 9 equiv route: filtered and washed with H2O and acetone.
ActivationDried under vacuum for 1 h at room temperature unless otherwise noted.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezinc nitrate hexahydrate [Zn(NO3)2.6H2O]22.0 mgS3-S4 · Triethylamine (TEA) as the base · Figure S2
LinkerHAB.3HCl13.8 mgS3-S4 · Triethylamine (TEA) as the base · Figure S2
BaseTEA3 equiv. to HABS3-S4 · Triethylamine (TEA) as the base · Figure S2
Complete recipeSource: SI

Route 3: Other

S3-S4 · Triethylamine (TEA) as the base · Figure S2

Metal precursors22.0 mg zinc nitrate hexahydrate [Zn(NO3)2.6H2O]
Linker precursors13.8 mg HAB.3HCl
Solvents7.5 mL DMF and 7.5 mL H2O
AdditivesTEA varied to 6 equiv. relative to HAB
AtmosphereAir
Temperatureroom temperature
Time2
Work-upSame as TEA 9 equiv route: filtered and washed with H2O and acetone.
ActivationDried under vacuum for 1 h at room temperature unless otherwise noted.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezinc nitrate hexahydrate [Zn(NO3)2.6H2O]22.0 mgS3-S4 · Triethylamine (TEA) as the base · Figure S2
LinkerHAB.3HCl13.8 mgS3-S4 · Triethylamine (TEA) as the base · Figure S2
BaseTEA6 equiv. to HABS3-S4 · Triethylamine (TEA) as the base · Figure S2
Complete recipeSource: SI

Route 4: Other

S3 · Triethylamine (TEA) as the base

Metal precursors22.0 mg zinc nitrate hexahydrate [Zn(NO3)2.6H2O]
Linker precursors13.8 mg HAB.3HCl
Solvents7.5 mL DMF for zinc nitrate; 7.5 mL H2O for HAB.3HCl
Additives62.5 uL trimethylamine / TEA (reported as 9 equiv. to HAB)
AtmosphereAir
Temperatureroom temperature
Time2
Work-upFiltered; washed with H2O (2 x 80 mL) and acetone (2 x 50 mL).
ActivationDried under vacuum for 1 h at room temperature unless otherwise noted.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezinc nitrate hexahydrate [Zn(NO3)2.6H2O]22.0 mgS3 · Triethylamine (TEA) as the base
LinkerHAB.3HCl13.8 mgS3 · Triethylamine (TEA) as the base
SolventDMF7.5 mLS3 · Triethylamine (TEA) as the base
SolventH2O7.5 mLS3 · Triethylamine (TEA) as the base
Basetrimethylamine (TEA)62.5 uL · 9 equiv. to HABS3 · Triethylamine (TEA) as the base