cMOF Evidence Base

Synthesis evidence

Triphenylene-Bridged Trinuclear Complexes of Cu: Models for Spin Interactions in Two-Dimensional Electrically Conductive Metal-Organic Frameworks

Yang L., He X., Dinca M. · Journal of the American Chemical Society · 2019 · 10475-10480

2 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

p001 / S1 · Synthesis of 1

Metal precursorsCu(BF4)2.6H2O, 35 mg; Me3tacn, 20 uL
Linker precursors2,3,6,7,10,11-hexahydroxytriphenylene (HHTP), 11 mg
SolventsAcetonitrile during reaction; acetonitrile/diethyl ether recrystallisation; 4:1 1,2-dichloroethane:methanol with t-butyl-methyl ether for final recrystallisation
AdditivesTriethylamine, 32 uL
AtmosphereStandard Schlenk techniques; under N2/inert atmosphere; transferred into nitrogen-filled glovebox for recrystallisation
Temperatureroom temperature reaction; -30 C final recrystallisation
Time5 min after Me3tacn addition; 15 min after base addition; 1 h after oxidant addition
Oxidant / reductantFerrocenium tetrafluoroborate, 28 mg; main text describes 3 equiv FcBF4 oxidation
Work-upDried under vacuum to black solid; recrystallised by layering diethyl ether; two additional recrystallisations by t-butyl-methyl ether layering; 32 mg crude product, 73% yield
ActivationNo MOF activation; drying under vacuum before recrystallisation and later extensive drying before magnetic/PXRD measurements
Scalability contextMolecular model synthesis only; no scale-up described.
Show 9 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(BF4)2.6H2O35 mgp001 / S1 · Synthesis of 1
OtherMe3tacn20 uL · 95+%p001 / S1 · Synthesis of 1
LinkerHHTP11 mg · 95%p001 / S1 · Synthesis of 1
Basetriethylamine32 uL · >=99.0%p001 / S1 · Synthesis of 1
Oxidantferrocenium tetrafluoroborate28 mg · technical grade; 3 equiv in main textp001 / S1 · Synthesis of 1
Solventacetonitrile3 mL + 2 mL + 6 mL + 2 mL + 3 mL portions · HPLC Plus >99.9%p001 / S1 · Synthesis of 1
Solventdiethyl etherlayering solvent · anhydrous ACS >=99%p001 / S1 · Synthesis of 1
Solventt-butyl-methyl-etherlayering solvent · ACS >99%p001 / S1 · Synthesis of 1
Solvent1,2-dichloroethane:methanol4:1 mixture · 1,2-dichloroethane 99.9%; methanol ACS >99.8%p001 / S1 · Synthesis of 1
Complete recipeSource: Both

Route 2: Other

p002 / S2 · Synthesis of 2

Metal precursorsCu(BF4)2.6H2O, 35 mg; Me3tacn, 20 uL
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6HCl), 18.4 mg
SolventsAcetonitrile during reaction; acetonitrile/diethyl ether recrystallisation; 4:1 1,2-dichloroethane:methanol with t-butyl-methyl ether vapour diffusion for final recrystallisation
AdditivesTriethylamine, 64 uL
AtmosphereStandard Schlenk techniques; under N2/inert atmosphere; transferred into nitrogen-filled glovebox for recrystallisation
Temperatureroom temperature reaction; -30 C final recrystallisation
Time5 min after Me3tacn addition; 15 min after base addition; 1 h after oxidant addition
Oxidant / reductantFerrocenium tetrafluoroborate, 37.4 mg; main text describes oxidation by 3 equiv FcBF4 but Scheme S1 shows 4 Cp2FeBF4 for isolated 2
Work-upDried under vacuum to black solid; recrystallised by layering diethyl ether; two additional recrystallisations by t-butyl-methyl ether vapour diffusion; 26 mg crude product, 56% yield
ActivationNo MOF activation; drying under vacuum before recrystallisation and later extensive drying before magnetic/PXRD measurements
Scalability contextMolecular model synthesis only; no scale-up described.
Show 9 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(BF4)2.6H2O35 mgp002 / S2 · Synthesis of 2
OtherMe3tacn20 uL · 95+%p002 / S2 · Synthesis of 2
LinkerHATP.6HCl18.4 mg · synthesised by reported procedurep002 / S2 · Synthesis of 2
Basetriethylamine64 uL · >=99.0%p002 / S2 · Synthesis of 2
Oxidantferrocenium tetrafluoroborate37.4 mg · technical gradep002 / S2 · Synthesis of 2
Solventacetonitrile3 mL + 2 mL + 20 mL + 2 mL + 3 mL portions · HPLC Plus >99.9%p002 / S2 · Synthesis of 2
Solventdiethyl etherlayering solvent · anhydrous ACS >=99%p002 / S2 · Synthesis of 2
Solventt-butyl-methyl-ethervapour diffusion solvent · ACS >99%p002 / S2 · Synthesis of 2
Solvent1,2-dichloroethane:methanol4:1 mixture · 1,2-dichloroethane 99.9%; methanol ACS >99.8%p002 / S2 · Synthesis of 2