Synthesis · Wells-Dawson Arsenotungstate Porous Derivatives for Electrochemical Supercapacitor Electrodes and Electrocatalytically Active Materials

6 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

p005 · Preparation of the Electrodes

Solventsethyl alcohol (1 mL) and DI water (3 mL)

Additivesacetylene black; Nafion solution

Atmosphereambient

Temperatureroom temperature

Time2

Substrate orientationpolished 3 mm glassy carbon electrode

Work-up5 uL well-dispersed slurry dropped onto GCE and dried 2 h; 5 uL Nafion solution dropped and electrode dried at room temperature.

ActivationRoom-temperature drying only.

Scalability contextElectrode mass loading about 0.052 mg.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 1	compound:acetylene black weight ratio 1:5	p005 · Preparation of the Electrodes
Additive	acetylene black	compound:acetylene black weight ratio 1:5	p005 · Preparation of the Electrodes
Solvent	ethyl alcohol	1 mL	p005 · Preparation of the Electrodes
Solvent	DI water	3 mL	p005 · Preparation of the Electrodes
Additive	Nafion solution (Aldrich)	5 uL	p005 · Preparation of the Electrodes

Complete recipeSource: Both

Route 2: Hydrothermal

p003 · Synthesis of compound 1

Metal precursorsNa2WO4.2H2O; NaAsO2; Cu(CH3COO)2.H2O

Linker precursorsbim (2,2'-biimidazole)

SolventsH2O (18 mL, 1 mol)

Additives6 M HCl to adjust pH to about 2.5

Temperature160

Time120

Work-upDark-blue crystals collected by filtration, washed thoroughly with distilled water, dried at room temperature; waste liquid collected and treated separately for sodium arsenite toxicity.

ActivationDried at room temperature; no separate solvent exchange or evacuation activation reported.

Scalability context25 mL Teflon-lined stainless-steel reactor; 43% yield based on W.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Na2WO4.2H2O	0.66 g, 2.0 mmol	p003 · Synthesis of compound 1
Metal Source	NaAsO2	0.0324 g, 0.25 mmol	p003 · Synthesis of compound 1
Linker	bim	0.0335 g, 0.25 mmol	p003 · Synthesis of compound 1
Metal Source	Cu(CH3COO)2.H2O	0.0599 g, 0.3 mmol	p003 · Synthesis of compound 1
Solvent	H2O	18 mL, 1 mol	p003 · Synthesis of compound 1
Acid	HCl	to pH about 2.5 · 6 M	p003 · Synthesis of compound 1

Complete recipeSource: SI

Route 3: Drop Cast

p005 · Preparation of the Electrodes

Solventsethyl alcohol (1 mL) and DI water (3 mL)

Additivesacetylene black; Nafion solution

Atmosphereambient

Temperatureroom temperature

Time2

Substrate orientationpolished 3 mm glassy carbon electrode

Work-up5 uL well-dispersed slurry dropped onto GCE and dried 2 h; 5 uL Nafion solution dropped and electrode dried at room temperature.

ActivationRoom-temperature drying only.

Scalability contextElectrode mass loading about 0.052 mg.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	compound 2	compound:acetylene black weight ratio 1:5	p005 · Preparation of the Electrodes
Additive	acetylene black	compound:acetylene black weight ratio 1:5	p005 · Preparation of the Electrodes
Solvent	ethyl alcohol	1 mL	p005 · Preparation of the Electrodes
Solvent	DI water	3 mL	p005 · Preparation of the Electrodes
Additive	Nafion solution (Aldrich)	5 uL	p005 · Preparation of the Electrodes

Complete recipeSource: Both

Route 4: Hydrothermal

p003 · Synthesis of compound 2

Metal precursorsNa2WO4.2H2O; NaAsO2; CuCl2.2H2O

Linker precursorspyrazine (pz)

SolventsH2O (18 mL, 1 mol)

Additives6 M HCl to adjust pH to about 3.0; chloride supplied by CuCl2.2H2O

Temperature160

Time120

Work-upDark-blue crystals collected by filtration, washed thoroughly with distilled water, dried at room temperature; waste liquid collected and treated separately for sodium arsenite toxicity.

ActivationDried at room temperature; no separate solvent exchange or evacuation activation reported.

Scalability context25 mL Teflon-lined stainless-steel reactor; 47% yield based on W.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Na2WO4.2H2O	0.66 g, 2.0 mmol	p003 · Synthesis of compound 2
Metal Source	NaAsO2	0.032 g, 0.25 mmol	p003 · Synthesis of compound 2
Linker	pz	0.016 g, 0.2 mmol	p003 · Synthesis of compound 2
Metal Source	CuCl2.2H2O	0.043 g, 0.25 mmol	p003 · Synthesis of compound 2
Solvent	H2O	18 mL, 1 mol	p003 · Synthesis of compound 2
Acid	HCl	to pH about 3.0 · 6 M	p003 · Synthesis of compound 2

Partial recipeSource: SI

Route 5: Drop Cast

p002 · General Methods and Materials

Solventsethyl alcohol and DI water inferred from shared electrode preparation

Additivesacetylene black; Nafion solution

Atmosphereambient

Temperatureroom temperature

Time2

Substrate orientationglassy carbon electrode

Work-upControl modified GCE was used in electrochemical tests; exact slurry paragraph explicitly describes 1 or 2, so control electrode preparation is inferred from shared method.

ActivationRoom-temperature drying only.

Scalability contextMass loading likely about 0.052 mg from shared statement.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	{As2W18O62} control compound	not separately stated	p002 · General Methods and Materials
Additive	acetylene black	inferred compound:acetylene black weight ratio 1:5	p002 · General Methods and Materials
Additive	Nafion solution	inferred 5 uL	p002 · General Methods and Materials

Partial recipeSource: SI

Route 6: Hydrothermal

p003 · Synthesis of control compound

Metal precursorsNa2WO4.2H2O; NaAsO2; copper source not used/replaced conditions not fully restated

Linker precursorsbih (1,6-bis(imidazole)hexane)

SolventsH2O, inferred from similar method

AdditivesHCl/pH conditions inferred from similar method but not explicitly restated for the control

Temperature160

Time120

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

ActivationDried at room temperature; no separate activation reported.

Scalability context38% yield based on W.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	bih	0.0441 g, 0.20 mmol	p003 · Synthesis of control compound
Metal Source	Na2WO4.2H2O	inferred from similar method	p003 · Synthesis of control compound
Metal Source	NaAsO2	inferred from similar method	p003 · Synthesis of control compound
Solvent	H2O	inferred from similar method	p003 · Synthesis of control compound