Synthesis evidence

Dominant Role of Hole Transport Pathway in Achieving Record High Photoconductivity in Two-Dimensional Metal–Organic Frameworks

Wang D., Ostresh S., Streater D. et al. · Angewandte Chemie - International Edition · 2023 · e202309505

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: Solvothermal

p003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs

Metal precursorsCu(Ac)2.H2O
Linker precursors2,3,6,7,10,11-Hexahydroxytriphenylene (HHTP), 65 mg, 0.2 mmol
Solvents1 mL NMP + 9 mL DI H2O for HHTP; metal source dissolved in 5 mL DI H2O
Additivesnone reported
Atmospherenot reported
Temperature60
Time12
Substrate orientationnot applicable
Oxidant / reductantno external oxidant/reductant reported; FTIR suggests ligands were partially oxidised during reaction
Work-upSequential washing with deionised water (3 times, 3 mL each) and acetone (6 times, 3 mL each); collected by centrifugation at 6000 rpm.
ActivationDried overnight in an oven at 50 deg C for further characterisation.
Scalability contextSmall-batch solution/oven synthesis; no scale-up discussion.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(Ac)2.H2O60 mg, 0.3 mmolp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
Linker2,3,6,7,10,11-Hexahydroxytriphenylene (HHTP)65 mg, 0.2 mmolp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
SolventNMP1 mLp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
SolventDI H2O9 mL for HHTP solution plus 5 mL for metal-source solutionp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
Complete recipeSource: SI

Route 2: Solvothermal

p003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs

Metal precursorsCu(Ac)2.H2O; Zn(acac)2
Linker precursors2,3,6,7,10,11-Hexahydroxytriphenylene (HHTP), 65 mg, 0.2 mmol
Solvents1 mL NMP + 9 mL DI H2O for HHTP; metal source dissolved in 5 mL DI H2O
Additivesnone reported
Atmospherenot reported
Temperature60
Time12
Substrate orientationnot applicable
Oxidant / reductantno external oxidant/reductant reported; FTIR suggests ligands were partially oxidised during reaction
Work-upSequential washing with deionised water (3 times, 3 mL each) and acetone (6 times, 3 mL each); collected by centrifugation at 6000 rpm.
ActivationDried overnight in an oven at 50 deg C for further characterisation.
Scalability contextSmall-batch solution/oven synthesis; no scale-up discussion.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(Ac)2.H2O; Zn(acac)230 mg, 0.15 mmol; 39 mg, 0.15 mmolp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
Linker2,3,6,7,10,11-Hexahydroxytriphenylene (HHTP)65 mg, 0.2 mmolp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
SolventNMP1 mLp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
SolventDI H2O9 mL for HHTP solution plus 5 mL for metal-source solutionp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
Complete recipeSource: SI

Route 3: Solvothermal

p003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs

Metal precursorsZn(acac)2
Linker precursors2,3,6,7,10,11-Hexahydroxytriphenylene (HHTP), 65 mg, 0.2 mmol
Solvents1 mL NMP + 9 mL DI H2O for HHTP; metal source dissolved in 5 mL DI H2O
Additivesnone reported
Atmospherenot reported
Temperature60
Time12
Substrate orientationnot applicable
Oxidant / reductantno external oxidant/reductant reported; FTIR suggests ligands were partially oxidised during reaction
Work-upSequential washing with deionised water (3 times, 3 mL each) and acetone (6 times, 3 mL each); collected by centrifugation at 6000 rpm.
ActivationDried overnight in an oven at 50 deg C for further characterisation.
Scalability contextSmall-batch solution/oven synthesis; no scale-up discussion.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(acac)278 mg, 0.3 mmolp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
Linker2,3,6,7,10,11-Hexahydroxytriphenylene (HHTP)65 mg, 0.2 mmolp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
SolventNMP1 mLp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs
SolventDI H2O9 mL for HHTP solution plus 5 mL for metal-source solutionp003 / SI p.S2 · S1. Synthesis of M-HHTP MOFs