cMOF Evidence Base

Synthesis evidence

Mixed Anionic and Cationic Redox Chemistry in a Tetrathiomolybdate Amorphous Coordination Framework

Zhu Q., Wang J., Liu X. et al. · Angewandte Chemie - International Edition · 2020 · 16579-16586

5 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

2 · Experimental Section, (NH4)2MoS4 synthesis

Metal precursors(NH4)6Mo7O12
SolventsH2O; anhydrous ethanol wash
Additives(NH4)2S solution; NH4Cl
Atmosphereconstant evacuation with water vacuum pump during 80 C step; vacuum drying at RT
Temperature80
Time5 plus overnight stirring after NH4Cl addition
Oxidant / reductant(NH4)2S sulfurising reagent
Work-upcool to RT, add NH4Cl, stir overnight, filter, wash with anhydrous ethanol three times
Activationvacuum dry at room temperature
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Source(NH4)6Mo7O12 (99+%, FisherScientific)10 g2 · Experimental Section, (NH4)2MoS4 synthesis
SolventH2O50 ml2 · Experimental Section, (NH4)2MoS4 synthesis
Additive(NH4)2S (Strem Chemicals) solution50 ml · 40%-44%2 · Experimental Section, (NH4)2MoS4 synthesis
AdditiveNH4Cl (99.6%, FisherScientific)25 g2 · Experimental Section, (NH4)2MoS4 synthesis
Solventanhydrous ethanolwashed 3 times2 · Experimental Section, (NH4)2MoS4 synthesis
Complete recipeSource: Both

Route 2: Other

6 · Figure S2 caption · Figure S2

Metal precursorsNa2MoS4.3.5H2O
Atmospherevacuum
Temperature140
Time3
Work-upannealing removes crystalline water; red compound turns into dark powder
Activationvacuum annealing/dehydration
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Metal SourceNa2MoS4.3.5H2ONot specified6 · Figure S2 caption · Figure S2
Partial recipeSource: SI

Route 3: Other

3 · Electrochemical measurements

Metal precursorsNa2MoS4
Solvents1 M LiPF6 in EC/DMC or 1 M NaPF6 in EC/DEC electrolyte
AdditivesSuper P conducting carbon; glass fibre separator
AtmosphereAr-filled glovebox, less than 0.1 ppm water and oxygen
Temperatureroom temperature
Work-uphand grind with Super P, press composite powder onto CR2032 stainless-steel case, assemble half-cell with Li or Na counter electrode
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherNa2MoS4typical active material mass loading about 2 mg3 · Electrochemical measurements
AdditiveSuper P conducting carbon additive (TOB New Energy)0, 10, 20, or 30 wt % in reported tests3 · Electrochemical measurements
ElectrolyteLiPF6 in EC/DMC1 M; 1:1 v:v EC:DMC3 · Electrochemical measurements
ElectrolyteNaPF6 in EC/DEC1 M; 1:1 v:v EC:DEC3 · Electrochemical measurements
Complete recipeSource: SI

Route 4: Other

4 · MIEC testing and analysis

Metal precursorsNa2MoS4 powder
Additivescarbon-coated aluminium foils
Atmosphereprotective Ar atmosphere; Ar-filled glovebox
Temperatureroom temperature
Time30 s pressing
Work-upcold-press powder between carbon-coated aluminium foils and encapsulate in home-made Swagelok cells
Activationstabilise 30 min at each measurement temperature
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNa2MoS4 or Na2MoS4.3.5H2O powderNot specified4 · MIEC testing and analysis
Additivecarbon coated Aluminum foilsNot specified4 · MIEC testing and analysis
Complete recipeSource: Both

Route 5: Other

2 · Experimental Section, Na2MoS4.3.5H2O synthesis

Metal precursors(NH4)2MoS4
Solventsice-cold aqueous NaOH; acetone; diethyl ether
AdditivesNaOH
Atmospherevacuum oven for drying
Temperature40
Time2 h stirring plus about 4 h rotary evaporation
Work-uprotary evaporation, acetone extraction, precipitate with excess diethyl ether, filter, wash several times with ether
Activationvacuum oven at room temperature
Scalability context55% yield reported for the hydrated sodium salt.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Source(NH4)2MoS40.5 g2 · Experimental Section, Na2MoS4.3.5H2O synthesis
BaseNaOH0.17 g in 2 ml water2 · Experimental Section, Na2MoS4.3.5H2O synthesis
Solventwater2 ml2 · Experimental Section, Na2MoS4.3.5H2O synthesis
Solventacetone6 ml2 · Experimental Section, Na2MoS4.3.5H2O synthesis
Solventdiethyl etherexcess, then several washes2 · Experimental Section, Na2MoS4.3.5H2O synthesis