Synthesis · Cu/Fe-MOFs based on mixed ligands: Synthesis, crystal structure and electrocatalytic hydrogen evolution performance

3 structured synthesis routes

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

Complete recipeSource: Main

2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF

Metal precursorsCu(NO3)2.3H2O, 0.1 mmol

Linker precursorsDPA, 0.0167 g, 0.1 mmol; Py2TTz, 0.0296 g, 0.1 mmol

Solventsdeionised water, 6 mL

Atmospherenot reported

Temperature100

Time72

Work-upultrasonicated for 20 min before reaction; cooled to room temperature; crystals collected by filtration, washed, and dried

Activationdried in a vacuum oven at 80 deg C

Scalability context6 mL reaction mixture in a 25 mL Teflon-lined stainless steel container.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Cu(NO3)2.3H2O	0.1 mmol	2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF
Linker	DPA	0.0167 g, 0.1 mmol	2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF
Linker	Py2TTz	0.0296 g, 0.1 mmol	2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF
Solvent	deionized water	6 mL	2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF

Complete recipeSource: Main

2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF

Metal precursorsFe(NO3)3.9H2O, 0.1 mmol

Linker precursorsDPA, 0.0167 g, 0.1 mmol; Py2TTz, 0.0296 g, 0.1 mmol

Solventsdeionised water, 6 mL

Atmospherenot reported

Temperature100

Time72

Work-upultrasonicated for 20 min before reaction; cooled to room temperature; crystals collected by filtration, washed, and dried

Activationdried in a vacuum oven at 80 deg C

Scalability context6 mL reaction mixture in a 25 mL Teflon-lined stainless steel container.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Fe(NO3)3.9H2O	0.1 mmol	2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF
Linker	DPA	0.0167 g, 0.1 mmol	2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF
Linker	Py2TTz	0.0296 g, 0.1 mmol	2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF
Solvent	deionized water	6 mL	2 · 2.2 Synthesis of Cu-MOF, and Fe-MOF

Complete recipeSource: Main

2 · 2.1 Synthesis of ligand Py2TTz · Fig. 1

Linker precursorsdithioacetamide; pyridine-4-carboxaldehyde

SolventsDMF, 40 mL

Atmospherenot reported

Temperature153

Time8

Work-upcooling, filtration, and washing

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	Dithioacetamide	1 g, 8.34 mmol	2 · 2.1 Synthesis of ligand Py2TTz · Fig. 1
Linker	pyridine-4-carboxaldehyde	2 mL, 21.6 mmol	2 · 2.1 Synthesis of ligand Py2TTz · Fig. 1
Solvent	DMF	40 mL	2 · 2.1 Synthesis of ligand Py2TTz · Fig. 1