Synthesis evidence

Quantum spin liquid state in a two-dimensional semiconductive metal−organic framework

Misumi Y., Yamaguchi A., Zhang Z. et al. · Journal of the American Chemical Society · 2020 · 16513-16517

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: Solvothermal

SI p.S2 · S1 Experimental details

Metal precursors53 mg M(trifluoroacetylacetonate)2 for M = Cu(II)
Linker precursors37 mg 2,3,6,7,10,11-hexahydroxytriphenylene
Solvents5 mL deionized water; 0.5 mL NMP added after 10 min stirring; water and acetone for activation solvent exchange
AtmosphereSynthesis atmosphere not stated; activated powder placed under argon atmosphere
Temperature85
Time12
Work-upAllowed to cool to room temperature, filtered with a 100 nm PTFE membrane filter, rinsed with a large amount of water and acetone, and collected as as-prepared dark purplish powder.
ActivationAs-prepared sample immersed in deionized water for a day, decanted/exchanged with fresh water and repeated three times; treated with acetone in the same manner; vacuumed for 3 h; stored under argon.
Scalability contextBatch preparation in a 30 mL vial; no scale-up discussion.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceM(trifluoroacetylacetonate)2 (for M = CuII)53 mgSI p.S2 · S1 Experimental details
Linker2,3,6,7,10,11-hexahydroxytriphenlyene37 mgSI p.S2 · S1 Experimental details
Solventdeionized water5 mLSI p.S2 · S1 Experimental details
SolventNMP (N-methyl-2-pyrrolidone)0.5 mLSI p.S2 · S1 Experimental details
Solventacetonelarge amount for rinse; used for solvent exchangeSI p.S2 · S1 Experimental details
Complete recipeSource: SI

Route 2: Solvothermal

SI p.S2 · S1 Experimental details

Metal precursors35 mg M(acetylacetonate)2 for M = Zn(II)
Linker precursors37 mg 2,3,6,7,10,11-hexahydroxytriphenylene
Solvents5 mL deionized water; 0.5 mL NMP added after 10 min stirring; water and acetone for activation solvent exchange
AtmosphereSynthesis atmosphere not stated; activated powder placed under argon atmosphere
Temperature85
Time12
Work-upAllowed to cool to room temperature, filtered with a 100 nm PTFE membrane filter, rinsed with a large amount of water and acetone, and collected as as-prepared sample.
ActivationAs-prepared sample immersed in deionized water for a day, decanted/exchanged with fresh water and repeated three times; treated with acetone in the same manner; vacuumed for 3 h; stored under argon.
Scalability contextBatch preparation in a 30 mL vial; no scale-up discussion.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceM(acetylacetonate)2 (for M = ZnII)35 mgSI p.S2 · S1 Experimental details
Linker2,3,6,7,10,11-hexahydroxytriphenlyene37 mgSI p.S2 · S1 Experimental details
Solventdeionized water5 mLSI p.S2 · S1 Experimental details
SolventNMP (N-methyl-2-pyrrolidone)0.5 mLSI p.S2 · S1 Experimental details
Solventacetonelarge amount for rinse; used for solvent exchangeSI p.S2 · S1 Experimental details