Synthesis · Catalytic Metal Nanoparticles Embedded in Conductive Metal–Organic Frameworks for Chemiresistors: Highly Active and Conductive Porous Materials

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: Solvothermal

p008 · Experimental Section

Metal precursors0.320 g copper(II) acetate monohydrate

Linker precursors0.260 g HHTP

Solvents100 mL methanol for copper salt; 125 mL methanol for HHTP

AtmosphereAir during drying; vacuum during final activation

Temperature65 for solvothermal step; 50 air dry; 100 vacuum activation

Time24 h solvothermal; 12 h air dry; 12 h vacuum

Work-upNatural cooling, removal of upper transparent solvent, washing with fresh methanol three times and acetone two times by centrifugation.

ActivationDried at 50 C for 12 h in air and at 100 C for 12 h in vacuum.

Scalability contextAuthors describe the method as facile and general for metal-NP-loaded conductive MOFs; no explicit scale-up demonstration beyond 500 mL capped bottle.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Copper(II) acetate monohydrate (Cu(CO2CH3) . H2O, 99.9%)	0.320 g	p008 · Experimental Section
Linker	2,3,6,7,10,11-hexahydroxytriphenylene hydrate (HHTP, C18H12O6 . H2O, 95.0%)	0.260 g	p008 · Experimental Section
Solvent	methanol	225 mL total	p008 · Experimental Section

Complete recipeSource: Main

Route 2: Other

p008 · Experimental Section

Metal precursors5 mg potassium tetrachloropalladate(II) added to 40 mg Cu3(HHTP)2 suspension

Linker precursorsPreformed Cu3(HHTP)2

Solvents5 mL deionised water

AtmosphereAir during 50 C drying; vacuum during 100 C activation

TemperatureRoom temperature stirring; 50 air dry; 100 vacuum activation

Time0.5 h precursor infiltration; 0.5 h after NaBH4 addition; 6 h air dry; 12 h vacuum

Oxidant / reductantNaBH4 solution, 1 mg mL-1

Work-upPurified by centrifugation and washing with DI water three times and acetone two times.

ActivationDried at 50 C for 6 h in air and at 100 C for 12 h in vacuum.

Scalability contextAuthors state the proposed synthesis can be extended by varying metals and C-MOFs.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(HHTP)2	40 mg	p008 · Experimental Section
Metal Source	potassium tetrachloropalladate(II) (K2PdCl4)	5 mg	p008 · Experimental Section
Solvent	DI water	5 mL	p008 · Experimental Section
Reductant	NaBH4 solution	not reported · 1 mg mL-1	p008 · Experimental Section

Complete recipeSource: Main

Route 3: Other

p008 · Experimental Section

Metal precursors5 mg potassium tetrachloroplatinate(II) added to 40 mg Cu3(HHTP)2 suspension

Linker precursorsPreformed Cu3(HHTP)2

Solvents5 mL deionised water

AtmosphereAir during 50 C drying; vacuum during 100 C activation

TemperatureRoom temperature stirring; 50 air dry; 100 vacuum activation

Time0.5 h precursor infiltration; 0.5 h after NaBH4 addition; 6 h air dry; 12 h vacuum

Oxidant / reductantNaBH4 solution, 1 mg mL-1

Work-upPurified by centrifugation and washing with DI water three times and acetone two times.

ActivationDried at 50 C for 6 h in air and at 100 C for 12 h in vacuum.

Scalability contextAuthors state the proposed synthesis can be extended by varying metals and C-MOFs.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(HHTP)2	40 mg	p008 · Experimental Section
Metal Source	potassium tetrachloroplatinate(II) (K2PtCl4)	5 mg	p008 · Experimental Section
Solvent	DI water	5 mL	p008 · Experimental Section
Reductant	NaBH4 solution	not reported · 1 mg mL-1	p008 · Experimental Section

Complete recipeSource: Main

Route 4: Drop Cast

p008 · Experimental Section

Solventsethanol

AtmosphereDry air during sensing; room-temperature fabrication atmosphere not specified

Temperatureroom temperature

Time0.1667 h sonication; 3 h air stabilisation before sensing

Substrate orientationTop-side parallel Au electrodes on Al2O3 substrate; back-side Pt microheater

Work-up6 mg sensing material dispersed in 300 mL ethanol and sonicated for 10 min; 5 uL drop-coated three times.

ActivationSensors stabilised in air for 3 h before each sensing test.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(HHTP)2, Pd@Cu3(HHTP)2, or Pt@Cu3(HHTP)2	6 mg	p008 · Experimental Section
Solvent	ethanol	300 mL	p008 · Experimental Section
Other	drop-coated suspension	5 uL, three times	p008 · Experimental Section