Synthesis · High-Performance H2S Sensors to Detect SF6 Leakage

7 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 · Preparation of CoxNi3-x(HITP)2

Metal precursors12 mL mixture of Co(NO3)2.6H2O and Ni(OAc)2.4H2O in nominal 1:4 Co:Ni ratio, total metal ion concentration 4.66 mmol L-1

Linker precursorsHATP.6HCl, 20 mg (0.0093 mmol, 1 eq.) in 6 mL water

SolventsDMF 12 mL for metal mixture; water 6 mL for linker

AdditivesNaOAc, 8 mL of 2 mol L-1 solution

Atmosphereopen glass vial; atmosphere not otherwise specified

Temperature65

Time2

Work-upextensive washing with water and filtration

Activationdried in a vacuum oven at 65 C

Scalability contextComposition tuned by changing Co/Ni source ratio.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	2 · Preparation of CoxNi3-x(HITP)2
Metal Source	Ni(OAc)2.4H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	2 · Preparation of CoxNi3-x(HITP)2
Linker	HATP.6HCl	20 mg (0.0093 mmol, 1 eq.)	2 · Preparation of CoxNi3-x(HITP)2
Solvent	DMF	12 mL	2 · Preparation of CoxNi3-x(HITP)2
Solvent	water	6 mL	2 · Preparation of CoxNi3-x(HITP)2
Base	NaOAc solution	8 mL · 2 mol L-1	2 · Preparation of CoxNi3-x(HITP)2

Complete recipeSource: SI

Route 2: Other

2 · Preparation of CoxNi3-x(HITP)2

Metal precursors12 mL mixture of Co(NO3)2.6H2O and Ni(OAc)2.4H2O in nominal 2:3 Co:Ni ratio, total metal ion concentration 4.66 mmol L-1

Linker precursorsHATP.6HCl, 20 mg (0.0093 mmol, 1 eq.) in 6 mL water

SolventsDMF 12 mL for metal mixture; water 6 mL for linker

AdditivesNaOAc, 8 mL of 2 mol L-1 solution

Atmosphereopen glass vial; atmosphere not otherwise specified

Temperature65

Time2

Work-upextensive washing with water and filtration

Activationdried in a vacuum oven at 65 C

Scalability contextComposition tuned by changing Co/Ni source ratio.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	2 · Preparation of CoxNi3-x(HITP)2
Metal Source	Ni(OAc)2.4H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	2 · Preparation of CoxNi3-x(HITP)2
Linker	HATP.6HCl	20 mg (0.0093 mmol, 1 eq.)	2 · Preparation of CoxNi3-x(HITP)2
Solvent	DMF	12 mL	2 · Preparation of CoxNi3-x(HITP)2
Solvent	water	6 mL	2 · Preparation of CoxNi3-x(HITP)2
Base	NaOAc solution	8 mL · 2 mol L-1	2 · Preparation of CoxNi3-x(HITP)2

Complete recipeSource: SI

Route 3: Other

2 · Preparation of CoxNi3-x(HITP)2

Metal precursors12 mL mixture of Co(NO3)2.6H2O and Ni(OAc)2.4H2O in nominal 1:1 Co:Ni ratio, total metal ion concentration 4.66 mmol L-1

Linker precursorsHATP.6HCl, 20 mg (0.0093 mmol, 1 eq.) in 6 mL water

SolventsDMF 12 mL for metal mixture; water 6 mL for linker

AdditivesNaOAc, 8 mL of 2 mol L-1 solution

Atmosphereopen glass vial; atmosphere not otherwise specified

Temperature65

Time2

Work-upextensive washing with water and filtration

Activationdried in a vacuum oven at 65 C

Scalability contextComposition tuned by changing Co/Ni source ratio.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	2 · Preparation of CoxNi3-x(HITP)2
Metal Source	Ni(OAc)2.4H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	2 · Preparation of CoxNi3-x(HITP)2
Linker	HATP.6HCl	20 mg (0.0093 mmol, 1 eq.)	2 · Preparation of CoxNi3-x(HITP)2
Solvent	DMF	12 mL	2 · Preparation of CoxNi3-x(HITP)2
Solvent	water	6 mL	2 · Preparation of CoxNi3-x(HITP)2
Base	NaOAc solution	8 mL · 2 mol L-1	2 · Preparation of CoxNi3-x(HITP)2

Complete recipeSource: SI

Route 4: Other

2-3 · Preparation of CoxNi3-x(HITP)2

Metal precursors12 mL mixture of Co(NO3)2.6H2O and Ni(OAc)2.4H2O in nominal 3:2 Co:Ni ratio, total metal ion concentration 4.66 mmol L-1

Linker precursorsHATP.6HCl, 20 mg (0.0093 mmol, 1 eq.) in 6 mL water

SolventsDMF 12 mL for metal mixture; water 6 mL for linker

AdditivesNaOAc, 8 mL of 2 mol L-1 solution

Atmosphereopen glass vial; atmosphere not otherwise specified

Temperature65

Time2

Work-upextensive washing with water and filtration

Activationdried in a vacuum oven at 65 C

Scalability contextComposition tuned by changing Co/Ni source ratio.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	2-3 · Preparation of CoxNi3-x(HITP)2
Metal Source	Ni(OAc)2.4H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	2-3 · Preparation of CoxNi3-x(HITP)2
Linker	HATP.6HCl	20 mg (0.0093 mmol, 1 eq.)	2-3 · Preparation of CoxNi3-x(HITP)2
Solvent	DMF	12 mL	2-3 · Preparation of CoxNi3-x(HITP)2
Solvent	water	6 mL	2-3 · Preparation of CoxNi3-x(HITP)2
Base	NaOAc solution	8 mL · 2 mol L-1	2-3 · Preparation of CoxNi3-x(HITP)2

Complete recipeSource: SI

Route 5: Other

3 · Preparation of CoxNi3-x(HITP)2

Metal precursors12 mL mixture of Co(NO3)2.6H2O and Ni(OAc)2.4H2O in nominal 4:1 Co:Ni ratio, total metal ion concentration 4.66 mmol L-1

Linker precursorsHATP.6HCl, 20 mg (0.0093 mmol, 1 eq.) in 6 mL water

SolventsDMF 12 mL for metal mixture; water 6 mL for linker

AdditivesNaOAc, 8 mL of 2 mol L-1 solution

Atmosphereopen glass vial; atmosphere not otherwise specified

Temperature65

Time2

Work-upextensive washing with water and filtration

Activationdried in a vacuum oven at 65 C

Scalability contextComposition tuned by changing Co/Ni source ratio.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	3 · Preparation of CoxNi3-x(HITP)2
Metal Source	Ni(OAc)2.4H2O	part of 12 mL mixed-metal DMF solution · total metal 4.66 mmol L-1	3 · Preparation of CoxNi3-x(HITP)2
Linker	HATP.6HCl	20 mg (0.0093 mmol, 1 eq.)	3 · Preparation of CoxNi3-x(HITP)2
Solvent	DMF	12 mL	3 · Preparation of CoxNi3-x(HITP)2
Solvent	water	6 mL	3 · Preparation of CoxNi3-x(HITP)2
Base	NaOAc solution	8 mL · 2 mol L-1	3 · Preparation of CoxNi3-x(HITP)2

Complete recipeSource: SI

Route 6: Other

2 · Preparation of Co3(HITP)2

Metal precursorsCo(NO3)2.6H2O, 81.3 mg

Linker precursorsHATP.6HCl, 15 mg in 4.5 mL water

SolventsDMF 4.5 mL; water 4.5 mL

AdditivesNaOAc, 2 mL of 2 mol L-1 solution

Atmosphereopen glass vial; atmosphere not otherwise specified

Temperature65

Time2

Work-upwashed thoroughly with large volume of water; suction filtration

Activationdried in a vacuum oven at 65 C

Scalability contextMild stirred water-bath/open-vial route.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	81.3 mg	2 · Preparation of Co3(HITP)2
Linker	HATP.6HCl	15 mg	2 · Preparation of Co3(HITP)2
Solvent	DMF	4.5 mL	2 · Preparation of Co3(HITP)2
Solvent	water	4.5 mL	2 · Preparation of Co3(HITP)2
Base	NaOAc solution	2 mL · 2 mol L-1	2 · Preparation of Co3(HITP)2

Complete recipeSource: SI

Route 7: Other

2 · Preparation of Ni3(HITP)2

Metal precursorsNi(OAc)2.4H2O, 14 mg

Linker precursorsHATP.6HCl, 20 mg in 6 mL water

SolventsDMSO 6 mL; water 6 mL

AdditivesNaOAc, 8 mL of 4 mol L-1 solution

Atmosphereopen glass vial; atmosphere not otherwise specified

Temperature65

Time2

Work-upwashed with large amount of water and methanol; suction filtration

Activationdried in a vacuum oven at 65 C

Scalability contextMild stirred water-bath/open-vial route.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	14 mg	2 · Preparation of Ni3(HITP)2
Linker	HATP.6HCl	20 mg	2 · Preparation of Ni3(HITP)2
Solvent	DMSO	6 mL	2 · Preparation of Ni3(HITP)2
Solvent	water	6 mL	2 · Preparation of Ni3(HITP)2
Base	NaOAc solution	8 mL · 4 mol L-1	2 · Preparation of Ni3(HITP)2