Synthesis · Controllable Construction of Two-Dimensional Conductive M3(HHTP)2 Nanorods for Electrochemical Sensing of Malachite Green in Fish

8 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode

Metal precursorsCo3(HHTP)2 nanorod powder

AdditivesGraphite powder; paraffin oil

AtmosphereAmbient electrode fabrication implied

Work-upCarbon paste pressed into the CPE end cavity; surface polished.

Scalability contextHand-mixed agate-mortar carbon paste.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Co3(HHTP)2	2% sample	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode
Other	graphite powder	total mass 1.00 g with MOF	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode
Additive	paraffin oil	200 uL	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode

Complete recipeSource: Main

Route 2: Other

main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode

AdditivesGraphite powder; paraffin oil

AtmosphereAmbient electrode fabrication implied

Work-upProduced by the same carbon paste pressing and polishing method.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	graphite powder	1.00 g	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode
Additive	paraffin oil	200 uL	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode

Complete recipeSource: Main

Route 3: Other

main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode · Scheme 2

Metal precursorsCu3(HHTP)2 nanorod powder

AdditivesGraphite powder; paraffin oil

AtmosphereAmbient electrode fabrication implied

Work-upCarbon paste pressed into the CPE end cavity; surface polished.

Scalability contextHand-mixed agate-mortar carbon paste; no fabrication scale-up reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(HHTP)2	2% sample	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode · Scheme 2
Other	graphite powder	total mass 1.00 g with MOF	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode · Scheme 2
Additive	paraffin oil	200 uL	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode · Scheme 2

Complete recipeSource: Main

Route 4: Other

main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode

Metal precursorsNi3(HHTP)2 nanorod powder

AdditivesGraphite powder; paraffin oil

AtmosphereAmbient electrode fabrication implied

Work-upCarbon paste pressed into the CPE end cavity; surface polished.

Scalability contextHand-mixed agate-mortar carbon paste.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni3(HHTP)2	2% sample	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode
Other	graphite powder	total mass 1.00 g with MOF	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode
Additive	paraffin oil	200 uL	main p.3, article p.22918 · Preparation of the M3(HHTP)2 Nanorod Modified Electrode

Partial recipeSource: Main

Route 5: Solvothermal

main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1

Metal precursorsCo(OAc)2.4H2O replacing Cu2(OAc)4.H2O; exact mass not separately stated

Linker precursorsHHTP; amount inferred from Cu recipe but not separately restated

SolventsH2O and DMF as in Cu recipe

AdditivesDMF limiting reagent/modulator

AtmosphereCapped glass vial; atmosphere not otherwise specified

Temperature80

Time12

Work-upSimilar to Cu3(HHTP)2 route; centrifugation, washing, vacuum drying implied.

ActivationVacuum drying at 49 C for 12 h implied from Cu route.

Scalability contextNo scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(OAc)2.4H2O	not explicitly stated	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Linker	HHTP	not explicitly restated	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Solvent	H2O	as Cu route	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Additive	DMF	as Cu route	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1

Complete recipeSource: Main

Route 6: Solvothermal

main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1

Metal precursors8.98 mg (0.045 mmol) Cu2(OAc)4.H2O

Linker precursors7.13 mg (0.022 mmol) HHTP

Solvents4 mL ultrapure H2O; 0.5 mL DMF added dropwise

AdditivesDMF limiting reagent/modulator

AtmosphereCapped glass vial; atmosphere not otherwise specified

Temperature80

Time12

Work-upCentrifuged; washed three times each with H2O, ethanol, and acetone.

ActivationDried in a vacuum oven at 49 C for 12 h.

Scalability context10 mL glass-vial batch; no scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu2(OAc)4.H2O	8.98 mg · 0.045 mmol	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Linker	HHTP	7.13 mg · 0.022 mmol	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Solvent	ultrapure H2O	4 mL	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Additive	DMF	0.5 mL	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1

Partial recipeSource: Both

Route 7: Solvothermal

main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Figure S1

Metal precursorsCu2(OAc)4.H2O, Ni(OAc)2.4H2O, or Co(OAc)2.4H2O

Linker precursorsHHTP

SolventsH2O; DMF omitted

AdditivesNo DMF limiting reagent

AtmosphereNot specified

Temperature80

Time12

Work-upSame method as DMF-limited controls, but exact workup not restated.

ActivationSame as DMF-limited controls, but not restated.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	acetate metal salts	same method	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Figure S1
Linker	HHTP	same method	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Figure S1
Solvent	H2O	same method	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Figure S1

Partial recipeSource: Main

Route 8: Solvothermal

main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1

Metal precursorsNi(OAc)2.4H2O replacing Cu2(OAc)4.H2O; exact mass not separately stated

Linker precursorsHHTP; amount inferred from Cu recipe but not separately restated

SolventsH2O and DMF as in Cu recipe

AdditivesDMF limiting reagent/modulator

AtmosphereCapped glass vial; atmosphere not otherwise specified

Temperature80

Time12

Work-upSimilar to Cu3(HHTP)2 route; centrifugation, washing, vacuum drying implied.

ActivationVacuum drying at 49 C for 12 h implied from Cu route.

Scalability contextNo scale-up data reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	not explicitly stated	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Linker	HHTP	not explicitly restated	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Solvent	H2O	as Cu route	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1
Additive	DMF	as Cu route	main p.3, article p.22918 · Preparation of M3(HHTP)2 Nanorod Materials · Scheme 1