cMOF Evidence Base

Synthesis evidence

Coordination environment dependent selectivity of single-site-Cu enriched crystalline porous catalysts in CO2 reduction to CH4

Zhang Y., Dong L.-Z., Li S. et al. · Nature Communications · 2021 · 6390

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

p004 text layer · Synthesis methods - Synthesis of Cu-DBC

Metal precursorsCu(OAc)2.H2O, 6 mg
Linker precursors8OH-DBC, 8.6 mg
Solvents500 uL degassed DMF and 2 mL degassed deionized water
Atmospheredegassed solvents; vial heated in oven
Temperature85
Time72
Work-upwashed with water and acetone several times
Activationdried overnight in vacuum at room temperature; for gas adsorption solvent-exchanged in methanol for 3 days
Scalability contextMilligram-scale vial synthesis reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker8OH-DBC8.6 mgp004 text layer · Synthesis methods - Synthesis of Cu-DBC
Metal SourceCu(OAc)2.H2O6 mgp004 text layer · Synthesis methods - Synthesis of Cu-DBC
Solventdegassed dimethyformamide (DMF)500 uLp004 text layer · Synthesis methods - Synthesis of Cu-DBC
Solventdegassed deionized water2 mLp004 text layer · Synthesis methods - Synthesis of Cu-DBC
Complete recipeSource: Both

Route 2: Hydrothermal

p004-p005 text layer · Synthesis methods - Synthesis of Cu-HHTP

Metal precursorsCu(C5H4F3O2)2, 10.5 mg
Linker precursorsHHTP, 7.5 mg
Solvents1 mL deionized water plus 0.10 mL NMP
AdditivesNMP added dropwise
Atmospheresealed/closed glass vial not otherwise specified
Temperature85
Time12
Work-upcooled naturally; crystals washed with deionized water and acetone
Activationdried in air
Scalability context4 mL glass-vial synthesis.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP7.5 mgp004-p005 text layer · Synthesis methods - Synthesis of Cu-HHTP
Metal SourceCu(C5H4F3O2)210.5 mgp004-p005 text layer · Synthesis methods - Synthesis of Cu-HHTP
Solventdeionized water1 mLp004-p005 text layer · Synthesis methods - Synthesis of Cu-HHTP
AdditiveNMP0.10 mLp004-p005 text layer · Synthesis methods - Synthesis of Cu-HHTP
Partial recipeSource: Both

Route 3: Other

p006 text layer · Synthesis methods - Synthesis of Cu-PPCOF

Metal precursors[NH2]8CuPc, 17.5 mg
Linker precursorsPDQ, 15.0 mg
Solventsdimethylacetamide (DMAc) and ethylene glycol; volumes not specified
Additivesacetic acid catalyst; amount not specified
Atmospherenot specified
Temperature200
Time168
Work-upgrey-green powder collected; wet sample transferred to Soxhlet extractor and washed with THF 24 h and acetone 24 h
Activationevacuated at 80 deg C under dynamic vacuum overnight
Scalability contextYield reported as 70%; solvent and acid quantities are not given in available SI text.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Source[NH2]8CuPc17.5 mgp006 text layer · Synthesis methods - Synthesis of Cu-PPCOF
LinkerPDQ15.0 mgp006 text layer · Synthesis methods - Synthesis of Cu-PPCOF
Solventdimethylacetamide (DMAc)Not specifiedp006 text layer · Synthesis methods - Synthesis of Cu-PPCOF
Solventethylene glycolNot specifiedp006 text layer · Synthesis methods - Synthesis of Cu-PPCOF
Acidacetic acid catalystNot specifiedp006 text layer · Synthesis methods - Synthesis of Cu-PPCOF
Complete recipeSource: Both

Route 4: Solvothermal

p005 text layer · Synthesis methods - Synthesis of Cu-TTCOF

Metal precursorsCu-TAPP, 14.8 mg, 0.02 mmol
Linker precursorsTTF-4CHO, 12.4 mg, 0.02 mmol
Solvents1,4-dioxane 0.5 mL and 1,3,5-trimethylbenzene 0.5 mL
Additives6 M aqueous acetic acid, 0.2 mL
Atmospherefreeze-pump-thaw degassed, evacuated to about 100 mTorr, sealed Pyrex tube
Temperature120
Time72
Work-upprecipitate isolated by Buchner filtration; washed with THF and acetone until filtrate was colourless; Soxhlet washed with THF 24 h and acetone 24 h
Activationevacuated at 150 deg C under dynamic vacuum overnight
Scalability contextSealed Pyrex tube, 0.02 mmol monomer scale.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu-TAPP14.8 mg · 0.02 mmolp005 text layer · Synthesis methods - Synthesis of Cu-TTCOF
LinkerTTF-4CHO12.4 mg · 0.02 mmolp005 text layer · Synthesis methods - Synthesis of Cu-TTCOF
Solvent1,4-dioxane0.5 mLp005 text layer · Synthesis methods - Synthesis of Cu-TTCOF
Solvent1,3,5-trimethylbenzene0.5 mLp005 text layer · Synthesis methods - Synthesis of Cu-TTCOF
Acidaqueous acetic acid0.2 mL · 6 Mp005 text layer · Synthesis methods - Synthesis of Cu-TTCOF