Synthesis evidence

Air-Stability and Carrier Type in Conductive M3(Hexaaminobenzene)2,(M = Co, Ni, Cu)

Hinckley A.C., Park J., Gomes J. et al. · Journal of the American Chemical Society · 2020 · 11123-11130

3 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

S2 · Materials

Metal precursors21.0 mg (0.072 mmol) [Co(NO3)2.6H2O]; SI text calls it nickel nitrate hexahydrate but bracketed formula is cobalt nitrate
Linker precursors10 mg HAB.3HCl (0.036 mmol)
Solventswater: 6 mL for metal salt plus 5 mL for HAB.3HCl
Additives60 microL of 6 M aqueous ammonium hydroxide (0.36 mmol, 10 equiv to HAB)
Atmosphereair
TemperatureRT synthesis; dried under vacuum at 80 degC
Time1 h stirring; 3 h vacuum drying
Work-upfiltered and washed with copious amounts of water and acetone
Activationdried under vacuum at 80 degC for 3 h prior to characterisation
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Source[Co(NO3)2.6H2O]21.0 mg (0.072 mmol)S2 · Materials
LinkerHAB.3HCl10 mg (0.036 mmol)S2 · Materials
SolventH2O6 mL + 5 mLS2 · Materials
Baseaqueous ammonium hydroxide (NH4OH)60 microL (0.36 mmol, 10 equiv to HAB) · 6 MS2 · Materials
Complete recipeSource: SI

Route 2: Other

S2 · Materials

Metal precursors16.8 mg (0.072 mmol) [Cu(NO3)2.2.5H2O]
Linker precursors10 mg HAB.3HCl (0.036 mmol)
Solventswater: 10 mL for metal salt plus 5 mL for HAB.3HCl
Additives60 microL of 6 M aqueous ammonium hydroxide (0.36 mmol, 10 equiv to HAB)
Atmosphereair
TemperatureRT synthesis; dried under vacuum at 80 degC
Time1 h stirring; 3 h vacuum drying
Work-upfiltered and washed with copious amounts of water and acetone
Activationdried under vacuum at 80 degC for 3 h prior to characterisation
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Source[Cu(NO3)2.2.5H2O]16.8 mg (0.072 mmol)S2 · Materials
LinkerHAB.3HCl10 mg (0.036 mmol)S2 · Materials
SolventH2O10 mL + 5 mLS2 · Materials
Baseaqueous ammonium hydroxide (NH4OH)60 microL (0.36 mmol, 10 equiv to HAB) · 6 MS2 · Materials
Complete recipeSource: SI

Route 3: Other

S2 · Materials

Metal precursors21.0 mg (0.072 mmol) nickel nitrate hexahydrate [Ni(NO3)2.6H2O]
Linker precursors10 mg HAB.3HCl (0.036 mmol)
Solventswater: 10 mL for metal salt plus 5 mL for HAB.3HCl
Additives60 microL of 6 M aqueous ammonium hydroxide (0.36 mmol, 10 equiv to HAB)
Atmosphereair
TemperatureRT synthesis; dried under vacuum at 80 degC
Time1 h stirring; 3 h vacuum drying
Work-upfiltered and washed with copious amounts of water and acetone
Activationdried under vacuum at 80 degC for 3 h prior to characterisation
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Source[Ni(NO3)2.6H2O]21.0 mg (0.072 mmol)S2 · Materials
LinkerHAB.3HCl10 mg (0.036 mmol)S2 · Materials
SolventH2O10 mL + 5 mLS2 · Materials
Baseaqueous ammonium hydroxide (NH4OH)60 microL (0.36 mmol, 10 equiv to HAB) · 6 MS2 · Materials