cMOF Evidence Base

Synthesis evidence

Structural, Thermodynamic, and Transport Properties of the Small-Gap Two-Dimensional Metal-Organic Kagomé Materials Cu3(hexaiminobenzene)2and Ni3(hexaiminobenzene)2

Berry T., Morey J.R., Arpino K.E. et al. · Inorganic Chemistry · 2022 · 6480-6487

2 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

p002 / 6481 · Experimental Section

Metal precursorsCuSO4.5H2O
Linker precursorsHAB.3HCl prepared through TNA and TATB intermediates
SolventsDMSO; deionised water; acetone; precursor steps used H2SO4, aqueous HCl, HNO3, ethyl acetate
Additives14 M NH4OH in DMSO; 10% Pd/C and HCl used in HAB precursor synthesis
AtmosphereDegassed DMSO for MOF formation; H2 at 4.2 bar used in HAB precursor hydrogenation; final product dried under vacuum on a Schlenk line
Temperature65
Time2
Oxidant / reductantH2/Pd-C reduction in HAB precursor synthesis
Work-upBlack suspended mixture centrifuged, decanted, washed with deionised water and acetone.
ActivationSolid product dried under vacuum on a Schlenk line for 10 min.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O0.11 mmolp002 / 6481 · Experimental Section
LinkerHAB.3HCl0.072 mmolp002 / 6481 · Experimental Section
BaseNH4OH14 M in DMSOp002 / 6481 · Experimental Section
Solventdegassed DMSONot specifiedp002 / 6481 · Experimental Section
OtherKNO30.70 mol · precursor TNA synthesisp002 / 6481 · Experimental Section
Other4-nitroaniline0.14 mol · precursor TNA synthesisp002 / 6481 · Experimental Section
OtherTATB0.012 mol · precursor HAB synthesisp002 / 6481 · Experimental Section
ReductantH2 with 10% Pd/C4.2 bar H2 for 3 daysp002 / 6481 · Experimental Section
Partial recipeSource: Main

Route 2: Other

p002 / 6481 · Experimental Section

Metal precursorsNi(NO3)2.6H2O
Linker precursorsHAB.3HCl prepared through TNA and TATB intermediates
SolventsDMSO; deionised water; acetone; precursor steps used H2SO4, aqueous HCl, HNO3, ethyl acetate
Additives14 M NH4OH in DMSO; 10% Pd/C and HCl used in HAB precursor synthesis
AtmosphereDegassed DMSO for MOF formation; H2 at 4.2 bar used in HAB precursor hydrogenation; final product dried under vacuum on a Schlenk line
Temperature65
Time2
Oxidant / reductantH2/Pd-C reduction in HAB precursor synthesis
Work-upBlack suspended mixture centrifuged, decanted, washed with deionised water and acetone.
ActivationSolid product dried under vacuum on a Schlenk line for 10 min.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(NO3)2.6H2O0.11 mmolp002 / 6481 · Experimental Section
LinkerHAB.3HCl0.072 mmolp002 / 6481 · Experimental Section
BaseNH4OH14 M in DMSOp002 / 6481 · Experimental Section
Solventdegassed DMSONot specifiedp002 / 6481 · Experimental Section
OtherKNO30.70 mol · precursor TNA synthesisp002 / 6481 · Experimental Section
Other4-nitroaniline0.14 mol · precursor TNA synthesisp002 / 6481 · Experimental Section
OtherTATB0.012 mol · precursor HAB synthesisp002 / 6481 · Experimental Section
ReductantH2 with 10% Pd/C4.2 bar H2 for 3 daysp002 / 6481 · Experimental Section