Synthesis · A Novel Electrocatalyst Pd(II)@Ni3(HITP)2 for Ultrasensitive Detection of Chloramphenicol: Experimental and Computational Investigation

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2

Metal precursorsNiCl2·xH2O, 10.8 mg

Linker precursorsHATP·6HCl, 30 mg

SolventsH2O: 15 mL for Ni salt + 15 mL for HATP·6HCl

Additives0.9 mL concentrated NH3·H2O (28 wt.%) added slowly

Atmospherenot specified during reaction; vacuum during drying

Temperature65 reaction; 80 drying

Time2 reaction; overnight drying

Work-upProduct collected by centrifugation and washed twice each with deionized water and ethanol.

ActivationDried at 80 degC in vacuum overnight.

Scalability contextSmall-batch powder synthesis; no scalability discussion.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	NiCl2·xH2O	10.8 mg	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2
Linker	HATP·6HCl	30 mg	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2
Solvent	H2O	30 mL total	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2
Base	concentrated NH3·H2O	0.9 mL · 28 wt.%	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2

Partial recipeSource: Both

Route 2: Other

4 · Figures · Figure S2

Metal precursorsPdCl2/H2PdCl4 and Ni3(HITP)2 powder

Linker precursorsNi3(HITP)2 contains HITP framework

SolventsHCl(aq), deionized water, hexane

Additivesaqueous HCl to form H2PdCl4

Atmospherenot specified; vacuum drying

Temperatureroom temperature reaction; 80 drying

Time0.5 sonication; 3 reaction; overnight drying

Work-upAqueous phase collected, washed with deionized water and ethanol.

ActivationDried at 80 degC in vacuum overnight.

Scalability contextVariant loading mass only; exact support mass and droplet volume not stated.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	PdCl2	35 mg stock preparation · 0.197 mol/L H2PdCl4 stock	4 · Figures · Figure S2
Other	Ni3(HITP)2 powder	certain amount	4 · Figures · Figure S2
Solvent	hexane	5 mL	4 · Figures · Figure S2
Acid	HCl(aq)	1 mL stock preparation	4 · Figures · Figure S2

Partial recipeSource: Both

Route 3: Other

1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2

Metal precursorsPdCl2 converted to H2PdCl4 solution; Ni3(HITP)2 powder support

Linker precursorsNi3(HITP)2 contains HITP framework

SolventsHCl(aq) (50 μL concentrated HCl + 950 μL deionized water) for PdCl2; 5 mL hexane suspension of Ni3(HITP)2

Additivesaqueous HCl to form H2PdCl4

Atmospherenot specified during reaction; vacuum during drying

Temperatureroom temperature reaction; 80 drying

Time0.5 sonication; 3 reaction; overnight drying

Work-upAqueous phase collected, washed by deionized water and ethanol.

ActivationDried at 80 degC in vacuum overnight.

Scalability contextVariable H2PdCl4 amount expressed as loading mass; actual Ni3(HITP)2 mass and H2PdCl4 volume for the 0.05 mL/mg sample are not explicitly tabulated.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	PdCl2	35 mg · 99.999 %	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2
Acid	HCl(aq)	1 mL (50 μL concentrated hydrochloric acid + 950 μL deionized water) · 36 wt.% concentrated HCl stock	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2
Other	H2PdCl4 solution	0.05 mL/mg loading mass used for optimal sample · 0.197 mol/L	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2
Other	Ni3(HITP)2 powder	certain amount	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2
Solvent	hexane	5 mL · AR	1 · Synthesis of Ni3(HITP)2 and Pd(II)@Ni3(HITP)2

Partial recipeSource: Both

Route 4: Other

5 · Figures · Figure S3

Metal precursorsPdCl2/H2PdCl4 and Ni3(HITP)2 powder

Linker precursorsNi3(HITP)2 contains HITP framework

SolventsHCl(aq), deionized water, hexane

Additivesaqueous HCl to form H2PdCl4

Atmospherenot specified; vacuum drying

Temperatureroom temperature reaction; 80 drying

Time0.5 sonication; 3 reaction; overnight drying

Work-upAqueous phase collected, washed with deionized water and ethanol.

ActivationDried at 80 degC in vacuum overnight.

Scalability contextVariant loading mass only; exact support mass and droplet volume not stated.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	PdCl2	35 mg stock preparation · 0.197 mol/L H2PdCl4 stock	5 · Figures · Figure S3
Other	Ni3(HITP)2 powder	certain amount	5 · Figures · Figure S3
Solvent	hexane	5 mL	5 · Figures · Figure S3
Acid	HCl(aq)	1 mL stock preparation	5 · Figures · Figure S3