cMOF Evidence Base

Synthesis evidence

Mithrene is a self-assembling robustly blue luminescent metal-organic chalcogenolate assembly for 2d optoelectronic applications

Schriber E.A., Popple D.C., Yeung M. et al. · ACS Applied Nano Materials · 2018 · 3498-3508

4 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 p.8, article p.3505 · Crystal Harvesting · Figure S9

Metal precursorsSilver nitrate aqueous solution, standard 3 mM/3 mM reaction conditions for the bulk powder comparison.
Linker precursorsDiphenyl diselenide in toluene, standard 3 mM/3 mM reaction conditions for the bulk powder comparison.
SolventsWater, toluene and isopropanol.
AdditivesNone reported.
AtmosphereBenchtop/laboratory atmosphere.
Temperatureroom temperature, not numerically specified
Timenot specified for bulking beyond standard crystallisation experiments
Substrate orientationBulk product deposited on silicon wafer for GIWAXS.
Work-upMany reactions prepared in parallel; aqueous layer pipetted out; vial swirled to adhere precipitate; toluene decanted; 5 mL isopropanol added with brief sonication; suspension serially transferred; product isolated by ultracentrifugation and decanting.
ActivationNone reported.
Scalability contextAbout 50 individual reactions were combined to obtain enough material for powder-like diffraction.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcesilver nitratemany parallel reactions · 3 mM/3 mM standard stated for Figure 8a bulk comparisonmain p.8, article p.3505 · Crystal Harvesting · Figure S9
Linkerdiphenyl diselenidemany parallel reactions · 3 mM/3 mM standard stated for Figure 8a bulk comparisonmain p.8, article p.3505 · Crystal Harvesting · Figure S9
Solventisopropanol5 mL added to a reaction during bulk collectionmain p.8, article p.3505 · Crystal Harvesting · Figure S9
Complete recipeSource: Main

Route 2: Liquid Liquid Interface

main p.7, article p.3504 · Methods · Figure 4

Metal precursorsAqueous silver nitrate in the range 0.5-10 mM; one reagent varied while the other was held at 3 mM.
Linker precursorsDiphenyl diselenide in toluene in the range 0.5-10 mM; one reagent varied while the other was held at 3 mM.
SolventsWater and toluene.
AdditivesNone for concentration screening.
AtmosphereBenchtop/laboratory atmosphere; direct sunlight excluded, laboratory light uncontrolled.
Temperatureroom temperature, not numerically specified
Time72, 120 and 240 h
Substrate orientationHarvested onto silicon substrates by the standard interface-passing method.
Work-upSilicon harvest, forced-air drying and isopropanol rinse.
ActivationNone reported.
Scalability contextThree identical samples of each reagent combination were allowed to crystallise undisturbed and harvested at 3, 5 and 10 days.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcesilver nitrate3 mL aqueous layer · 0.5-10 mM, varied in the screenmain p.7, article p.3504 · Methods · Figure 4
Linkerdiphenyl diselenide3 mL toluene layer · 0.5-10 mM, varied in the screenmain p.7, article p.3504 · Methods · Figure 4
Solventwater/toluene3 mL + 3 mLmain p.7, article p.3504 · Methods · Figure 4
Partial recipeSource: Main

Route 3: Liquid Liquid Interface

main pp.4 and 7, article pp.3501 and 3504 · Role of Metal Ion Concentration; Methods · Figure 6

Metal precursorsAqueous silver nitrate, described as 3 mM in the text for CTAB experiments.
Linker precursorsDiphenyl diselenide in toluene at standard concentration.
SolventsWater and toluene; isopropanol used for suspension/drop casting after harvest.
AdditivesCetyltrimethylammonium bromide (CTAB), reported as 5 uM in the Results text and 5.0e-4 mM in Methods after dilution from 0.5 mM stock.
AtmosphereBenchtop/laboratory atmosphere; direct sunlight excluded.
Temperatureroom temperature, not numerically specified
Timenot separately specified; standard interface synthesis conditions
Substrate orientationCTAB harvest differed from standard: aqueous layer pipetted out, organic layer decanted, crystals suspended in isopropanol and drop-cast.
Work-upAqueous layer pipetted out; crystals adsorbed on glass; organic layer decanted; isopropanol added and sonicated to yield a suspension for drop-casting.
ActivationNone reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcesilver nitrateaqueous layer · 3 mM described for CTAB testmain pp.4 and 7, article pp.3501 and 3504 · Role of Metal Ion Concentration; Methods · Figure 6
Linkerdiphenyl diselenidetoluene layer · standard concentrationmain pp.4 and 7, article pp.3501 and 3504 · Role of Metal Ion Concentration; Methods · Figure 6
AdditiveCTAB5 uM in Results text; 5.0e-4 mM in Methodsmain pp.4 and 7, article pp.3501 and 3504 · Role of Metal Ion Concentration; Methods · Figure 6
Solventisopropyl alcoholnot quantified for CTAB suspensionmain pp.4 and 7, article pp.3501 and 3504 · Role of Metal Ion Concentration; Methods · Figure 6
Complete recipeSource: Main

Route 4: Liquid Liquid Interface

main pp.7-8, article pp.3504-3505 · Materials and Methods

Metal precursorsSilver nitrate (>99%) in 18.2 Mohm water; representative concentration 3 mM.
Linker precursorsDiphenyl diselenide (98%) in toluene; representative concentration 3 mM.
SolventsWater and toluene, 3 mL each, forming an immiscible liquid-liquid interface.
AdditivesNone for the standard route.
AtmosphereBenchtop/laboratory atmosphere; protected from direct sunlight but laboratory light not controlled.
Temperatureroom temperature, not numerically specified
Timenot fixed; samples in the study were typically grown for 3, 5 or 10 days
Substrate orientationPolished silicon substrate passed vertically through organic layer into aqueous layer, tilted to about 45 degrees, then raised through the interface.
Work-upFilm harvested on silicon, dried by forced air, then gently rinsed with isopropanol to remove dried solvent and precursors.
ActivationNone reported.
Scalability contextInterfacial reactions have low yield, about 0.1-1 mg, and bulk powder required combining about 50 reactions.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcesilver nitrate (>99%)3 mL aqueous solution · 3 mM representative standard; 0.5-10 mM in screensmain pp.7-8, article pp.3504-3505 · Materials and Methods
Linkerdiphenyl diselenide (98%)3 mL toluene solution · 3 mM representative standard; 0.5-10 mM in screensmain pp.7-8, article pp.3504-3505 · Materials and Methods
Solvent18.2 Mohm water3 mL aqueous layermain pp.7-8, article pp.3504-3505 · Materials and Methods
Solventtoluene3 mL organic layermain pp.7-8, article pp.3504-3505 · Materials and Methods