Synthesis · Supramolecular Host-Guest Assembly Based on Phosphotungstate Nanostructures for Pseudocapacitive and Electrochemical Sensing Applications

9 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

S5 · Preparation of the Electrodes

Metal precursorscompound 1

Solvents200 uL ethyl alcohol and DI water (3:1)

Additivesactivated carbon; 10 uL Nafion solution

Atmospherevacuum drying oven for final drying

Temperature60

Time2

Substrate orientation1 x 1 cm2 carbon paper

Work-upgrind compound and activated carbon 1:3 for about 30 min; disperse 8 mg; drop-cast 100 uL slurry; vacuum dry at 60 C for 2 h

Activationvacuum drying at 60 C for 2 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 1	compound and activated carbon mixed at weight ratio 1:3; 8 mg dispersed	S5 · Preparation of the Electrodes
Additive	activated carbon	1:3 active:carbon mass ratio	S5 · Preparation of the Electrodes
Solvent	ethyl alcohol and DI water (3:1)	200 uL	S5 · Preparation of the Electrodes
Additive	Nafion solution	10 uL · 5% supplier solution	S5 · Preparation of the Electrodes

Complete recipeSource: SI

Route 2: Drop Cast

S4-S5 · Preparation of the Electrodes

Metal precursorscompound 1

Solvents180 uL ethyl alcohol and DI water (3:1)

Additivesactivated carbon; Nafion solution

Atmosphereambient air

Temperatureroom temperature

Time2

Substrate orientation3 mm diameter glassy carbon electrode

Work-updrop-cast 5 uL slurry; dry 2 h; add 5 uL Nafion; dry at room temperature

Activationnone reported beyond room-temperature drying

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 1	5 mg active material in mixture with 25 mg activated carbon	S4-S5 · Preparation of the Electrodes
Additive	activated carbon	25 mg	S4-S5 · Preparation of the Electrodes
Solvent	ethyl alcohol and DI water (3:1)	180 uL	S4-S5 · Preparation of the Electrodes
Additive	Nafion solution	5 uL · 5% supplier solution	S4-S5 · Preparation of the Electrodes

Complete recipeSource: SI

Route 3: Drop Cast

S5 · Preparation of the Electrodes

Metal precursorscompound 2

Solvents200 uL ethyl alcohol and DI water (3:1)

Additivesactivated carbon; 10 uL Nafion solution

Atmospherevacuum drying oven for final drying

Temperature60

Time2

Substrate orientation1 x 1 cm2 carbon paper

Work-upgrind compound and activated carbon 1:3 for about 30 min; disperse 8 mg; drop-cast 100 uL slurry; vacuum dry at 60 C for 2 h

Activationvacuum drying at 60 C for 2 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 2	compound and activated carbon mixed at weight ratio 1:3; 8 mg dispersed	S5 · Preparation of the Electrodes
Additive	activated carbon	1:3 active:carbon mass ratio	S5 · Preparation of the Electrodes
Solvent	ethyl alcohol and DI water (3:1)	200 uL	S5 · Preparation of the Electrodes
Additive	Nafion solution	10 uL · 5% supplier solution	S5 · Preparation of the Electrodes

Complete recipeSource: SI

Route 4: Drop Cast

S4-S5 · Preparation of the Electrodes

Metal precursorscompound 2

Solvents180 uL ethyl alcohol and DI water (3:1)

Additivesactivated carbon; Nafion solution

Atmosphereambient air

Temperatureroom temperature

Time2

Substrate orientation3 mm diameter glassy carbon electrode

Work-updrop-cast 5 uL slurry; dry 2 h; add 5 uL Nafion; dry at room temperature

Activationnone reported beyond room-temperature drying

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 2	5 mg active material in mixture with 25 mg activated carbon	S4-S5 · Preparation of the Electrodes
Additive	activated carbon	25 mg	S4-S5 · Preparation of the Electrodes
Solvent	ethyl alcohol and DI water (3:1)	180 uL	S4-S5 · Preparation of the Electrodes
Additive	Nafion solution	5 uL · 5% supplier solution	S4-S5 · Preparation of the Electrodes

Complete recipeSource: SI

Route 5: Hydrothermal

S3-S4 · Experimental Section; Synthesis of compound 1

Metal precursorsK6P2W18O62.14H2O (1.051 g, 0.20 mmol)

Linker precursorsbip (0.114 g, 0.56 mmol)

SolventsH2O (18 mL, 1 mol)

AdditivespH adjusted to about 2-4 with 2 M H3PO4

Atmospherenot reported

Temperature160

Time120

Work-upBlue crystals isolated by filtration, washed thoroughly with distilled water, dried at room temperature; waste liquid collected and treated separately.

Activationdried at room temperature

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	K6P2W18O62.14H2O	1.051 g, 0.20 mmol	S3-S4 · Experimental Section; Synthesis of compound 1
Linker	bip	0.114 g, 0.56 mmol	S3-S4 · Experimental Section; Synthesis of compound 1
Solvent	H2O	18 mL, 1 mol	S3-S4 · Experimental Section; Synthesis of compound 1
Acid	H3PO4	pH adjusted to about 2-4 · 2 M	S3-S4 · Experimental Section; Synthesis of compound 1

Complete recipeSource: SI

Route 6: Hydrothermal

S4 · Experimental Section; Synthesis of compound 2

Metal precursorsK6P2W18O62.14H2O (1.053 g, 0.20 mmol); AgNO3.2H2O (0.1401 g, 0.68 mmol)

Linker precursorsbipy (0.1220 g, 0.78 mmol)

SolventsH2O (18 mL, 1 mol)

AdditivespH adjusted to about 4 with 2 M H3PO4

Atmospherenot reported

Temperature160

Time120

Work-upYellow crystals isolated by filtration, washed thoroughly with distilled water, dried at room temperature; waste liquid collected and treated separately.

Activationdried at room temperature

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	K6P2W18O62.14H2O	1.053 g, 0.20 mmol	S4 · Experimental Section; Synthesis of compound 2
Metal Source	AgNO3.2H2O	0.1401 g, 0.68 mmol	S4 · Experimental Section; Synthesis of compound 2
Linker	bipy	0.1220 g, 0.78 mmol	S4 · Experimental Section; Synthesis of compound 2
Solvent	H2O	18 mL, 1 mol	S4 · Experimental Section; Synthesis of compound 2
Acid	H3PO4	pH adjusted to about 4 · 2 M	S4 · Experimental Section; Synthesis of compound 2

Complete recipeSource: SI

Route 7: Drop Cast

S5 · Preparation of the Electrodes

Metal precursors{P2W18O62}

Solvents200 uL ethyl alcohol and DI water (3:1)

Additivesactivated carbon; 10 uL Nafion solution

Atmospherevacuum drying oven for final drying

Temperature60

Time2

Substrate orientation1 x 1 cm2 carbon paper

Work-upgrind compound and activated carbon 1:3 for about 30 min; disperse 8 mg; drop-cast 100 uL slurry; vacuum dry at 60 C for 2 h

Activationvacuum drying at 60 C for 2 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	{P2W18O62}	compound and activated carbon mixed at weight ratio 1:3; 8 mg dispersed	S5 · Preparation of the Electrodes
Additive	activated carbon	1:3 active:carbon mass ratio	S5 · Preparation of the Electrodes
Solvent	ethyl alcohol and DI water (3:1)	200 uL	S5 · Preparation of the Electrodes
Additive	Nafion solution	10 uL · 5% supplier solution	S5 · Preparation of the Electrodes

Complete recipeSource: SI

Route 8: Drop Cast

S4-S5 · Preparation of the Electrodes

Metal precursors{P2W18O62}

Solvents180 uL ethyl alcohol and DI water (3:1)

Additivesactivated carbon; Nafion solution

Atmosphereambient air

Temperatureroom temperature

Time2

Substrate orientation3 mm diameter glassy carbon electrode

Work-updrop-cast 5 uL slurry; dry 2 h; add 5 uL Nafion; dry at room temperature

Activationnone reported beyond room-temperature drying

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	{P2W18O62}	5 mg active material in mixture with 25 mg activated carbon	S4-S5 · Preparation of the Electrodes
Additive	activated carbon	25 mg	S4-S5 · Preparation of the Electrodes
Solvent	ethyl alcohol and DI water (3:1)	180 uL	S4-S5 · Preparation of the Electrodes
Additive	Nafion solution	5 uL · 5% supplier solution	S4-S5 · Preparation of the Electrodes

Vague recipeSource: SI

Route 9: Other

S2 · Experimental Section; General Methods and Materials

Metal precursorsalpha-K6[P2W18O62].14H2O prepared by literature method; details not reproduced

Work-upverified by IR spectrum

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Metal Source	alpha-K6[P2W18O62].14H2O	not reported; literature method	S2 · Experimental Section; General Methods and Materials