Synthesis evidence

A chiral SrSi2 (srs) superstructure constructed by a dual interaction system showing isotropic electrical conductivity

Liu J., Lu Z.-X., Wu F.-F. et al. · Chinese Chemical Letters · 2023 · 108100

3 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.3 · Main text · Figs. S3, S5

Metal precursorscompound 1
Solventsmixed MeOH/acetone
Atmospherenot specified
Temperaturenot specified
Timenot specified
Work-upCrystals recovered from solution of compound 1 in mixed MeOH/acetone by recrystallisation.
Activationnot specified
Scalability contextRegeneration described qualitatively; no cycle number, recovery yield, or scale reported in the available text.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1Not specifiedmain p.3 · Main text · Figs. S3, S5
SolventMeOHmixed MeOH/acetonemain p.3 · Main text · Figs. S3, S5
Solventacetonemixed MeOH/acetonemain p.3 · Main text · Figs. S3, S5
Complete recipeSource: Both

Route 2: Other

SI office text · Experimental Section

Metal precursorsAgOTf (silver triflate), 150 mg, 0.58 mmol
Linker precursorsL = tris(2-naphthimidazolylmethyl)amine, 28 mg, 0.05 mmol
SolventsMeOH/DMF/acetone, 6 mL total, v/v/v 8/1/3; equivalent to main-text MeOH/acetone/DMF 8/3/1
Additivestetrabutylammonium bromide, 10 mg, 0.03 mmol
Atmospherenot specified
Temperatureroom temperature
Time2 h stirring plus 3 days undisturbed crystallisation
Work-upTurbid solution stirred at room temperature for 2 h; insoluble matter removed by filtration; filtrate left undisturbed at room temperature for 3 days; crystals obtained.
ActivationNo activation reported; main text states the 3D pi-stacked supramolecular structure collapses upon solvent removal.
Scalability contextCrystallisation recipe at milligram ligand scale; yield 65% based on L; no scale-up demonstrated.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
LinkerL (tris(2-naphthimidazolylmethyl)amine)28 mg, 0.05 mmolSI office text · Experimental Section
Metal SourceAgOTf150 mg, 0.58 mmolSI office text · Experimental Section
Additivetetrabutylammonium bromide10 mg, 0.03 mmolSI office text · Experimental Section
SolventMeOHpart of 6 mL MeOH/DMF/acetone mixture, v/v/v 8/1/3SI office text · Experimental Section
SolventDMFpart of 6 mL MeOH/DMF/acetone mixture, v/v/v 8/1/3SI office text · Experimental Section
Solventacetonepart of 6 mL MeOH/DMF/acetone mixture, v/v/v 8/1/3SI office text · Experimental Section
Partial recipeSource: Both

Route 3: Drop Cast

SI office text · Regeneration of 1 and fabrication of thin film of 1 · Fig. S6

Metal precursorscompound 1
Solventsnot specified
Atmospherenot specified
Temperaturenot specified
Timenot specified
Substrate orientationsubstrate not specified
Work-upThin film prepared by simple cast coating/drop casting.
Activationnot specified
Scalability contextThin-film processability claimed qualitatively; no film area, thickness, substrate, or electrical measurement reported.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Othercompound 1Not specifiedSI office text · Regeneration of 1 and fabrication of thin film of 1 · Fig. S6