cMOF Evidence Base

Synthesis evidence

Hybrid metal-organic chalcogenide nanowires with electrically conductive inorganic core through diamondoid-directed assembly

Yan H., Hohman J.N., Li F.H. et al. · Nature Materials · 2017 · 349-355

8 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Liquid Liquid Interface

main Methods page · Synthesis

Metal precursorsAnhydrous CuSO4, 20 mM in ethylene glycol.
Linker precursorsAdamantane-1-thiol, 20 mM in toluene.
SolventsEthylene glycol and toluene.
AtmosphereAir; anhydrous/dry reagents used when possible.
Temperature80
TimeCuSO4 dissolution 24 h at 80 C; crystal growth >24 h at 80 C.
Substrate orientationBorosilicate scintillation vial; EG phase at bottom, toluene phase above.
Oxidant / reductantCu(II) was reduced to Cu(I), probably during CuSO4 dissolution in EG or reaction with thiol.
Work-upVacuum filtration over P4 filter paper, ethanol rinse, vacuum dry at room temperature.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous CuSO420 mMmain Methods page · Synthesis
Linkeradamantane-1-thiol20 mMmain Methods page · Synthesis
Solventethylene glycolNot specifiedmain Methods page · Synthesis
SolventtolueneNot specifiedmain Methods page · Synthesis
Complete recipeSource: Both

Route 2: Other

main Methods page · Synthesis · Fig. S9; Fig. S10

Metal precursorsAs-synthesised 1ADCu powder.
SolventsIsopropanol.
AdditivesHydrogen peroxide.
AtmosphereRoom-temperature ambient atmosphere not further specified.
Temperatureroom temperature
Time0.5
Oxidant / reductantH2O2 oxidative dopant diluted in IPA to 10, 100, 1000 and 10000 ppm; SI also shows 100000 ppm.
Work-upVacuum filtration, rinsing and vacuum drying.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Other1ADCu powdersNot specifiedmain Methods page · Synthesis · Fig. S9; Fig. S10
OxidantH2O210, 100, 1000, 10000 ppm; SI also 100000 ppmmain Methods page · Synthesis · Fig. S9; Fig. S10
SolventIPANot specifiedmain Methods page · Synthesis · Fig. S9; Fig. S10
Complete recipeSource: Main

Route 3: Liquid Liquid Interface

main Methods page · Synthesis · Fig. 5f

Metal precursorsCuSO4 solution as in copper-based MOC route.
Linker precursorsAdamantane-1-thiol solution as in copper-based MOC route.
SolventsEthylene glycol and toluene.
AdditivesAAO membrane template.
AtmosphereAir.
Temperature80
TimeSame growth conditions as bulk copper-based MOCs; >24 h implied.
Substrate orientationAAO membrane with 200 nm pores and 60 um thickness placed at toluene/EG interface.
Work-upRinsed with toluene and IPA; dried in CO2 critical point dryer; Ti/Au electrodes evaporated for measurements.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO420 mMmain Methods page · Synthesis · Fig. 5f
Linkeradamantane-1-thiol20 mMmain Methods page · Synthesis · Fig. 5f
OtherAAO membrane, 200 nm pore size, 60 um thicknessNot specifiedmain Methods page · Synthesis · Fig. 5f
OtherTi/Au electrodes5 nm Ti and 200 nm Aumain Methods page · Synthesis · Fig. 5f
Complete recipeSource: Main

Route 4: Liquid Liquid Interface

main Methods page · Synthesis

Metal precursorsAnhydrous CuSO4, 20 mM in ethylene glycol.
Linker precursorsDiamantane-4-thiol, 20 mM in toluene.
SolventsEthylene glycol and toluene.
AtmosphereAir; anhydrous/dry reagents used when possible.
Temperature80
TimeCuSO4 dissolution 24 h at 80 C; crystal growth >24 h at 80 C.
Substrate orientationBorosilicate scintillation vial; EG phase at bottom, toluene phase above.
Oxidant / reductantCu(II) reduction to Cu(I) as in copper-based MOC synthesis.
Work-upVacuum filtration over P4 filter paper, ethanol rinse, vacuum dry at room temperature.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous CuSO420 mMmain Methods page · Synthesis
Linkerdiamantane-4-thiol20 mMmain Methods page · Synthesis
Solventethylene glycolNot specifiedmain Methods page · Synthesis
SolventtolueneNot specifiedmain Methods page · Synthesis
Partial recipeSource: Both

Route 5: Liquid Liquid Interface

main Methods page · Synthesis · Fig. S11-S12

Metal precursorsAgNO3, 20 mM in water.
Linker precursorsAdamantane-1-thiol, diamantane-4-thiol, [121]tetramantane-6-thiol or [1(2)3]tetramantane-3-thiol.
SolventsWater for AgNO3; thiol phase as in copper route, with ethanol/toluene composition varied for [121]tetramantane-6-thiolate.
AtmosphereAir.
Temperature80
TimeSimilar to copper-based route; exact Ag growth time not separately reported.
Substrate orientationLiquid-liquid interface.
Work-upNot separately specified; similar procedure to copper-based MOCs.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceAgNO320 mMmain Methods page · Synthesis · Fig. S11-S12
Linkeradamantane-1-thiol / diamantane-4-thiol / [121]tetramantane-6-thiol / [1(2)3]tetramantane-3-thiolNot specifiedmain Methods page · Synthesis · Fig. S11-S12
SolventwaterNot specifiedmain Methods page · Synthesis · Fig. S11-S12
Solventtoluene and/or ethanolNot specifiedmain Methods page · Synthesis · Fig. S11-S12
Partial recipeSource: Main

Route 6: Liquid Liquid Interface

main Methods page · Synthesis · Fig. 6b

Metal precursorsSaturated CdSO4 solution in EG with some solid at the bottom.
Linker precursorsm-carborane-9-thiol, 20 mM in toluene.
SolventsEthylene glycol and toluene.
AtmosphereAir.
Temperature80
TimeSimilar to copper-based route; exact time not separately reported.
Substrate orientationToluene/EG interface.
Work-upUnreacted CdSO4 solid removed by pipette; crystals harvested from interface.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCdSO4saturated solution with some solid · saturatedmain Methods page · Synthesis · Fig. 6b
Linkerm-carborane-9-thiol20 mMmain Methods page · Synthesis · Fig. 6b
Solventethylene glycolNot specifiedmain Methods page · Synthesis · Fig. 6b
SolventtolueneNot specifiedmain Methods page · Synthesis · Fig. 6b
Complete recipeSource: Main

Route 7: Liquid Liquid Interface

main Methods page · Synthesis · Fig. 6d

Metal precursorsAnhydrous FeCl2, 20 mM in acetonitrile.
Linker precursorsAdamantane-1-selenol, 20 mM in n-octane.
SolventsAcetonitrile and n-octane.
AdditivesTributylphosphine (TBP), 1 mL.
AtmosphereArgon-filled glove box with <0.5 ppm oxygen and water.
Temperature40-50
TimeFeCl2 dissolution 1-2 days; crystal formation 1-2 weeks.
Substrate orientation5 mL of each solution layered with acetonitrile phase at the bottom.
Oxidant / reductantTBP reported to facilitate Fe-Se bond formation without incorporation.
Work-upCollected by filtration through PTFE membrane or centrifugation at 12000 rpm.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous FeCl25 mL solution · 20 mMmain Methods page · Synthesis · Fig. 6d
Linkeradamantane-1-selenol5 mL solution · 20 mMmain Methods page · Synthesis · Fig. 6d
SolventacetonitrileNot specifiedmain Methods page · Synthesis · Fig. 6d
Solventn-octaneNot specifiedmain Methods page · Synthesis · Fig. 6d
Additivetributylphosphine (TBP)1 mLmain Methods page · Synthesis · Fig. 6d
Partial recipeSource: Main

Route 8: Liquid Liquid Interface

main Methods page · Synthesis · Fig. 6c

Metal precursorsZnSO4, 20 mM in ethylene glycol.
Linker precursorsAdamantane-1-thiol in toluene, by analogy with copper route.
SolventsEthylene glycol and toluene.
AtmosphereAir.
Temperature80
TimeAbout one month crystal growth before harvest.
Substrate orientationLiquid-liquid interface.
Work-upHarvest after one month; detailed workup not separately reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZnSO420 mMmain Methods page · Synthesis · Fig. 6c
Linkeradamantane-1-thiolNot specifiedmain Methods page · Synthesis · Fig. 6c
Solventethylene glycolNot specifiedmain Methods page · Synthesis · Fig. 6c
SolventtolueneNot specifiedmain Methods page · Synthesis · Fig. 6c