cMOF Evidence Base

Synthesis evidence

Highly Conducting Neutral Coordination Polymer with Infinite Two-Dimensional Silver-Sulfur Networks

Huang X., Li H., Tu Z. et al. · Journal of the American Chemical Society · 2018 · 15153-15156

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: Drop Cast

S7 · Electrochemical characterization · Figure S22

Metal precursorsAg-BHT powder
Solventsethanol; dichloromethane electrolyte solution used for CV
AdditivesNafion solution, 0.5 wt%
Time24
Substrate orientation3 uL suspension loaded onto polished 3 mm glassy carbon disk electrode
Work-upSonication for 24 h to form uniform dispersed suspension before drop loading.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherAg-BHT2 mgS7 · Electrochemical characterization · Figure S22
AdditiveNafion solution100 uL · 0.5 wt%S7 · Electrochemical characterization · Figure S22
Solventethanol900 uLS7 · Electrochemical characterization · Figure S22
ElectrolyteBu4NClO4 in dichloromethane0.1 MS7 · Electrochemical characterization · Figure S22
Complete recipeSource: Both

Route 2: Liquid Liquid Interface

S4-S5 · Synthesis of Ag-BHT film; Transfer method · Figure 1a

Metal precursorsAgNO3, 339.7 mg in 20 mL aqueous solution
Linker precursorsbenzenehexathiol (BHT), 1 mM in 400 mL toluene
Solvents400 mL degassed water; 400 mL toluene; workup solvents water, dimethylformamide, ethanol, diethyl ether
Atmosphereargon; water and toluene degassed by freeze-thaw before use
Temperature60
Time48
Substrate orientationself-standing film grown at the toluene-water interface
Oxidant / reductantexcess Ag(I) nitrate; dilute nitric acid side product proposed to create an oxidising environment
Work-upAqueous and organic reaction solutions gently removed by syringe; insoluble films rinsed sequentially with water, dimethylformamide, ethanol and diethyl ether.
ActivationFor deposited films, dried overnight in glove box until H2O concentration below 0.1 ppm.
Scalability contextLarge-volume 1000 mL flask recipe gave 310 mg Ag-BHT film at 95% yield.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceAgNO3339.7 mg in 20 mL aqueous solutionS4-S5 · Synthesis of Ag-BHT film; Transfer method · Figure 1a
Linkerbenzenehexathiol (BHT)400 mL toluene solution · 1 mMS4-S5 · Synthesis of Ag-BHT film; Transfer method · Figure 1a
Solventwater400 mL · degassedS4-S5 · Synthesis of Ag-BHT film; Transfer method · Figure 1a
Solventtoluene400 mL · degassedS4-S5 · Synthesis of Ag-BHT film; Transfer method · Figure 1a
Solventdimethylformamiderinse solventS4-S5 · Synthesis of Ag-BHT film; Transfer method · Figure 1a
Solventethanolrinse solventS4-S5 · Synthesis of Ag-BHT film; Transfer method · Figure 1a
Solventdiethyl etherrinse solventS4-S5 · Synthesis of Ag-BHT film; Transfer method · Figure 1a
Vague recipeSource: Main

Route 3: Other

p003 / 15155 · Results and discussion · Figure 5; Figures S12-S15

Metal precursorsAg-BHT
Linker precursorsAg-BHT framework
Oxidant / reductantLiBHEt3 reductant
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
ReductantLiBHEt3Not specifiedp003 / 15155 · Results and discussion · Figure 5; Figures S12-S15
OtherAg-BHTNot specifiedp003 / 15155 · Results and discussion · Figure 5; Figures S12-S15