cMOF Evidence Base

Synthesis evidence

2D conjugated metal-organic framework as a proton-electron dual conductor

Choi J.Y., Stodolka M., Kim N. et al. · Chem · 2023 · 143-153

4 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

main p.7 / article p.148 · Results and discussion - Urea functionalization of Zn-HHTP-H2O · Figure S15

Metal precursorsPreformed Zn-HHTP-H2O.
Linker precursorsPreformed HHTP-based framework.
SolventsEthylene glycol.
AdditivesNo urea in control treatment.
AtmosphereNot fully specified.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherZn-HHTP-H2ONot specifiedmain p.7 / article p.148 · Results and discussion - Urea functionalization of Zn-HHTP-H2O · Figure S15
SolventEthylene glycolNot specifiedmain p.7 / article p.148 · Results and discussion - Urea functionalization of Zn-HHTP-H2O · Figure S15
Complete recipeSource: Both

Route 2: Hydrothermal

main p.10 / article p.151 · Experimental procedures - Synthesis of Zn-HHTP-H2O · Figures S1-S4

Metal precursorsZn(NO3)2.6H2O (0.011 g, 0.037 mmol).
Linker precursorsHHTP (0.013 g, 0.024 mmol) dispersed in 4 mL H2O.
SolventsH2O, 4 mL for Zn salt plus 4 mL for HHTP dispersion; 1 mL aqueous NaOAc solution.
AdditivesNaOAc aqueous solution, 1 mL of 0.25 M, rate-modulating reagent.
AtmosphereNot reported; stirred reaction.
Temperature85
Time2
Work-upWashed and centrifuged with H2O, methanol and acetone (2 x 5 mL each).
ActivationDried in a vacuum oven for 1 h at 60 deg C; BET activation separately used evacuation to 50 mmHg then 80 deg C for 2 h.
Scalability contextSmall powder batch; yield and scale-up not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2.6H2O0.011 g, 0.037 mmolmain p.10 / article p.151 · Experimental procedures - Synthesis of Zn-HHTP-H2O · Figures S1-S4
LinkerHHTP0.013 g, 0.024 mmolmain p.10 / article p.151 · Experimental procedures - Synthesis of Zn-HHTP-H2O · Figures S1-S4
SolventH2O4 mL for metal solution; 4 mL for linker dispersionmain p.10 / article p.151 · Experimental procedures - Synthesis of Zn-HHTP-H2O · Figures S1-S4
AdditiveNaOAc aqueous solution1 mL · 0.25 Mmain p.10 / article p.151 · Experimental procedures - Synthesis of Zn-HHTP-H2O · Figures S1-S4
Complete recipeSource: SI

Route 3: Hydrothermal

SI p.3-p.6 · Synthesis optimization of Zn-HHTP-H2O · Figures S1-S4

Metal precursorsZn(NO3)2.6H2O (0.011 g, 0.037 mmol).
Linker precursorsHHTP (0.013 g, 0.024 mmol).
SolventsH2O; 50% H2O + 50% DMF; or 100% DMF in solvent-effect series.
AdditivesNaOAc varied as 5, 10 or 100 equivalents relative to ligand in base-amount series.
AtmosphereNot reported.
Temperature25, 60, or 85
Time2, 4, or 6
Work-upWashed and centrifuged with H2O, methanol and acetone (2 x 5 mL each); dried in a vacuum oven for 1 h at 60 deg C.
ActivationDrying at 60 deg C for 1 h after washing.
Scalability contextOptimisation screens only; no yield or scale-up reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(NO3)2x6H2O0.011 g, 0.037 mmolSI p.3-p.6 · Synthesis optimization of Zn-HHTP-H2O · Figures S1-S4
LinkerHHTP0.013 g, 0.024 mmolSI p.3-p.6 · Synthesis optimization of Zn-HHTP-H2O · Figures S1-S4
SolventH2O, H2O/DMF, or DMFtargeted solvent; 4 mL for metal/linker portions where specifiedSI p.3-p.6 · Synthesis optimization of Zn-HHTP-H2O · Figures S1-S4
AdditiveNaOAc aqueous solution1 mL; 5, 10, or 100 equivalents according to ligand · 0.25 M in temperature, solvent and time screensSI p.3-p.6 · Synthesis optimization of Zn-HHTP-H2O · Figures S1-S4
Complete recipeSource: Main

Route 4: Other

main p.10-p.11 / article p.151-p.152 · Experimental procedures - Synthesis of Zn-HHTP-urea · Figure 4A

Metal precursorsPreformed Zn-HHTP-H2O.
Linker precursorsPreformed HHTP-based framework.
SolventsEthylene glycol, 5 mL.
AdditivesUrea, 100 equivalents relative to activated MOF; raw mass not reported.
AtmosphereVacuum activation before ligand substitution; reaction atmosphere not otherwise reported.
Temperature85
Time2
Work-upCentrifuged and washed with methanol and acetone twice each.
ActivationZn-HHTP-H2O activated in a vacuum oven for 1 h at 100 deg C; final product vacuum dried for 1 h at 60 deg C.
Scalability context10 mg activated MOF batch; no yield or scale-up reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherActivated Zn-HHTP-H2O10 mgmain p.10-p.11 / article p.151-p.152 · Experimental procedures - Synthesis of Zn-HHTP-urea · Figure 4A
AdditiveUrea100 equivalentsmain p.10-p.11 / article p.151-p.152 · Experimental procedures - Synthesis of Zn-HHTP-urea · Figure 4A
SolventEthylene glycol5 mLmain p.10-p.11 / article p.151-p.152 · Experimental procedures - Synthesis of Zn-HHTP-urea · Figure 4A