Synthesis · Synthesis, Characterization, and Catalytic Performance of a New Heterobimetallic Y/Tb Metal-Organic Framework with High Catalytic Activity

3 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Solvothermal

p005 / S5 · General procedures

Metal precursorsTb(NO3)3.5H2O (0.019 g, 0.0434 mmol).

Linker precursors3-amino-4-hydroxybenzoic acid (0.010 g, 0.0625 mmol).

SolventsDistilled water and DMF: metal solution initially in 0.8 mL water then plus 0.2 mL DMF; ligand solution initially in 0.2 mL DMF then plus 0.8 mL water.

AdditivesEt3N, 10 uL (0.072 mmol).

AtmosphereNot specified for MOF synthesis; screw-capped vial.

Temperature100

Time2

Work-upStir resulting MOF for 1 h in 2 mL distilled water to remove excess ligand, then filter.

ActivationNo separate activation reported.

Scalability contextNo scaled-up Tb-MOF synthesis was reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Tb(NO3)3.5H2O	0.019 g, 0.0434 mmol	p005 / S5 · General procedures
Linker	3-amino-4-hydroxybenzoic acid	0.010 g, 0.0625 mmol	p005 / S5 · General procedures
Solvent	distilled water	0.8 mL for metal solution; 0.8 mL added to ligand solution; 2 mL workup	p005 / S5 · General procedures
Solvent	DMF	0.2 mL containing linker; 0.2 mL added to metal solution	p005 / S5 · General procedures
Base	Et3N	10 uL, 0.072 mmol	p005 / S5 · General procedures

Complete recipeSource: Both

Route 2: Solvothermal

p005-p006 / S5-S6 · General procedures

Metal precursorsY(NO3)3.6H2O (0.132 g, 0.3468 mmol) and Tb(NO3)3.5H2O (0.072 g, 0.174 mmol), dissolved in 1 mL water.

Linker precursors3-amino-4-hydroxybenzoic acid (0.2 g, 1.2 mmol).

SolventsDMF/H2O mixture 3 mL/2 mL for ligand solution; 1 mL water for metal salts.

AdditivesEt3N, 200 uL (1.44 mmol).

AtmosphereNot specified for MOF synthesis; 25 mL screw-capped vial.

Temperature100

Time2

Work-upStir resulting MOF for 1 h in 10 mL distilled water, then filter; purity confirmed by PXRD.

ActivationNo separate activation reported.

Scalability contextScaled-up procedure produced 75-85 mg, higher than the no-more-than-4 mg small-scale isolated amounts reported in the main text.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Y(NO3)3.6H2O	0.132 g, 0.3468 mmol	p005-p006 / S5-S6 · General procedures
Metal Source	Tb(NO3)3.5H2O	0.072 g, 0.174 mmol	p005-p006 / S5-S6 · General procedures
Linker	3-amino-4-hydroxybenzoic acid	0.2 g, 1.2 mmol	p005-p006 / S5-S6 · General procedures
Solvent	DMF/H2O	3 mL/2 mL for ligand solution	p005-p006 / S5-S6 · General procedures
Solvent	water	1 mL for metal solution; 10 mL workup	p005-p006 / S5-S6 · General procedures
Base	Et3N	200 uL, 1.44 mmol	p005-p006 / S5-S6 · General procedures

Complete recipeSource: Both

Route 3: Solvothermal

p005 / S5 · General procedures

Metal precursorsY(NO3)3.6H2O (0.011 g, 0.0289 mmol) and Tb(NO3)3.5H2O (0.006 g, 0.0145 mmol); SI states ratio 1:2 respectively but the listed mmol correspond to about 2:1 Y:Tb.

Linker precursors3-amino-4-hydroxybenzoic acid (0.010 g, 0.0625 mmol).

SolventsDistilled water and DMF: metal solution initially in 0.8 mL water then plus 0.2 mL DMF; ligand solution initially in 0.2 mL DMF then plus 0.8 mL water.

AdditivesEt3N, 10 uL (0.072 mmol).

AtmosphereNot specified for MOF synthesis; screw-capped vial.

Temperature100

Time2

Work-upStir resulting MOF for 1 h in 2 mL distilled water to remove excess ligand, then filter.

ActivationNo separate evacuation/thermal activation reported for the as-synthesised MOF.

Scalability contextMain text reports 1:2, 1:1 and 2:1 precursor ratios all gave no more than 4 mg; SI states 1:2 gave the highest isolated yield of 20%.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Y(NO3)3.6H2O	0.011 g, 0.0289 mmol	p005 / S5 · General procedures
Metal Source	Tb(NO3)3.5H2O	0.006 g, 0.0145 mmol	p005 / S5 · General procedures
Linker	3-amino-4-hydroxybenzoic acid	0.010 g, 0.0625 mmol	p005 / S5 · General procedures
Solvent	distilled water	0.8 mL for metal solution; 0.8 mL added to ligand solution; 2 mL wash/stirring workup	p005 / S5 · General procedures
Solvent	DMF	0.2 mL containing linker; 0.2 mL added to metal solution	p005 / S5 · General procedures
Base	Et3N	10 uL, 0.072 mmol	p005 / S5 · General procedures