Synthesis · Dense Conductive Metal-Organic Frameworks as Robust Electrocatalysts for Biosensing

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: Hydrothermal

main p.3, article p.17179 · Synthesis of Cu3(HHTP)2

Metal precursorsCu(OAc)2.H2O (78 mg)

Linker precursorsHHTP (70 mg)

SolventsH2O (15 mL); dimethyl formamide (1.5 mL)

AtmosphereNot specified.

Temperature85

Time24

Work-upCentrifuged at 8000 rpm for 5 min; washed with deionized H2O twice and acetone twice.

ActivationDried in a vacuum oven at 80 C for 24 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	70 mg	main p.3, article p.17179 · Synthesis of Cu3(HHTP)2
Metal Source	Cu(OAc)2.H2O	78 mg	main p.3, article p.17179 · Synthesis of Cu3(HHTP)2
Solvent	H2O	15 mL	main p.3, article p.17179 · Synthesis of Cu3(HHTP)2
Solvent	dimethyl formamide	1.5 mL	main p.3, article p.17179 · Synthesis of Cu3(HHTP)2

Complete recipeSource: Main

Route 2: Hydrothermal

main p.3, article p.17179 · Synthesis of Cu3(THQ)2

Metal precursorsCu(NO3)2.2.5H2O (53 mg)

Linker precursorsTHQ (30 mg)

SolventsDegassed H2O (10 mL for THQ; 10 mL for Cu/ethylenediamine mixture)

AdditivesEthylenediamine (23 uL) as competing coordination reagent.

AtmosphereN2 atmosphere; degassed H2O.

Temperature85

Time24

Work-upCentrifuged at 8000 rpm for 5 min; washed with deionized H2O three times.

ActivationDried in a vacuum oven at 80 C for 24 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	THQ	30 mg	main p.3, article p.17179 · Synthesis of Cu3(THQ)2
Metal Source	Cu(NO3)2.2.5H2O	53 mg	main p.3, article p.17179 · Synthesis of Cu3(THQ)2
Additive	ethylene diamine	23 uL	main p.3, article p.17179 · Synthesis of Cu3(THQ)2
Solvent	degassed H2O	20 mL total	main p.3, article p.17179 · Synthesis of Cu3(THQ)2

Complete recipeSource: Main

Route 3: Drop Cast

main p.3, article p.17179 · Preparation of Biosensors · Figure S3

SolventsDeionized water for cMOF suspension; deionized water and ethanol for electrode cleaning.

AdditivesGlutaraldehyde (0.25 wt%); AChE solution prepared in 2.5 wt% BSA.

AtmosphereRoom atmosphere for drying; oven drying at 35 C after AChE coating.

Temperature35

Time0.5

Substrate orientationPolished glassy carbon working electrode, 3 mm diameter.

Work-upGC polished with 1, 0.3, and 0.05 um alumina slurry; sonicated in water and ethanol. cMOFs (1 mg) suspended in 1 mL water and sonicated 30 min; 5 uL suspension pipetted onto GC and dried; 2 uL glutaraldehyde added; 2 uL AChE coated.

ActivationDried at 35 C in an oven for 30 min after AChE coating.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu3(THQ)2 cMOF	1 mg in 1 mL; 5 uL deposited · 1 mg mL-1	main p.3, article p.17179 · Preparation of Biosensors · Figure S3
Additive	glutaraldehyde	2 uL · 0.25 wt%	main p.3, article p.17179 · Preparation of Biosensors · Figure S3
Other	AChE solution in BSA	2 uL · AChE prepared in 2.5 wt% BSA; 20 mU uL-1 selected for paraoxon assays	main p.3, article p.17179 · Preparation of Biosensors · Figure S3
Solvent	deionized water	1 mL for suspension	main p.3, article p.17179 · Preparation of Biosensors · Figure S3

Complete recipeSource: Main

Route 4: Hydrothermal

main p.3, article p.17179 · Synthesis of Ni3(HHTP)2

Metal precursorsNi(OAc)2.4H2O (100 mg)

Linker precursorsHHTP (70 mg)

SolventsH2O (15 mL)

AtmosphereNot specified.

Temperature85

Time24

Work-upCentrifuged at 8000 rpm for 5 min; washed with deionized H2O twice and acetone twice.

ActivationDried in a vacuum oven at 80 C for 24 h.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	70 mg	main p.3, article p.17179 · Synthesis of Ni3(HHTP)2
Metal Source	Ni(OAc)2.4H2O	100 mg	main p.3, article p.17179 · Synthesis of Ni3(HHTP)2
Solvent	H2O	15 mL	main p.3, article p.17179 · Synthesis of Ni3(HHTP)2