Synthesis · Alkali-metal-regulated construction of superhydrophilic ZnII and CdII coordination polymers with perhalogenated terephthalate ligands

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

p002 · Syntheses of complexes 1-6

Metal precursorsCd(NO3)2.4H2O (92.5 mg, 0.3 mmol)

Linker precursorsH2BDC-F4 (71.4 mg, 0.3 mmol)

SolventsMeOH/DMF (v/v 3:1, 8 mL)

AdditivesLi(OAc).2H2O (30.6 mg, 0.3 mmol)

Atmospherenot specified

Temperatureroom temperature

Timeca. 0.5 h stirring plus seven weeks standing

Work-upstir ca. 30 min, filter, leave colourless solution to stand; slow evaporation gave block crystals in 76% yield (105.2 mg)

Activationnone reported

Scalability contextSlow evaporation over weeks; milligram-to-gram quantities reported depending on complex.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2BDC-F4	71.4 mg, 0.3 mmol	p002 · Syntheses of complexes 1-6
Metal Source	Cd(NO3)2.4H2O	92.5 mg, 0.3 mmol	p002 · Syntheses of complexes 1-6
Additive	Li(OAc).2H2O	30.6 mg, 0.3 mmol	p002 · Syntheses of complexes 1-6
Solvent	MeOH/DMF	8 mL, v/v 3:1	p002 · Syntheses of complexes 1-6

Complete recipeSource: Main

Route 2: Other

p003 · Syntheses of complexes 1-6

Metal precursorsCd(NO3)2.4H2O (92.5 mg, 0.3 mmol; inherited from route 1)

Linker precursorsH2BDC-F4 (71.4 mg, 0.3 mmol; inherited from route 1)

SolventsMeOH/DMF (v/v 3:1, 8 mL; inherited from route 1)

AdditivesNa(OAc).3H2O (41.1 mg, 0.3 mmol)

Atmospherenot specified

Temperatureroom temperature

Timeca. 0.5 h stirring plus seven weeks standing by inherited procedure

Work-upsame synthetic procedure as 1 except LiOAc replaced by Na(OAc).3H2O; colourless block crystals in 63% yield (100.3 mg)

Activationnone reported

Scalability contextSlow evaporation over weeks; milligram-to-gram quantities reported depending on complex.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2BDC-F4	71.4 mg, 0.3 mmol (inherited)	p003 · Syntheses of complexes 1-6
Metal Source	Cd(NO3)2.4H2O	92.5 mg, 0.3 mmol (inherited)	p003 · Syntheses of complexes 1-6
Additive	Na(OAc).3H2O	41.1 mg, 0.3 mmol	p003 · Syntheses of complexes 1-6
Solvent	MeOH/DMF	8 mL, v/v 3:1 (inherited)	p003 · Syntheses of complexes 1-6

Complete recipeSource: Main

Route 3: Other

p003 · Syntheses of complexes 1-6

Metal precursorsZn(NO3)2.6H2O (89.2 mg, 0.3 mmol)

Linker precursorsH2BDC-Cl4 (91.2 mg, 0.30 mmol)

SolventsMeOH/DMF (v/v 3:1, 8 mL; inherited from route 1)

AdditivesNa(OAc).3H2O (41.1 mg, 0.3 mmol; inherited from route 2)

Atmospherenot specified

Temperatureroom temperature

Timeca. 0.5 h stirring plus seven weeks standing by inherited procedure

Work-upsame synthetic procedure as 2 except H2BDC-F4 and Cd nitrate replaced by H2BDC-Cl4 and Zn nitrate; colourless block crystals in 42% yield (59.1 mg based on H2BDC-Cl4)

Activationnone reported

Scalability contextSlow evaporation over weeks; milligram-to-gram quantities reported depending on complex.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2BDC-Cl4	91.2 mg, 0.30 mmol	p003 · Syntheses of complexes 1-6
Metal Source	Zn(NO3)2.6H2O	89.2 mg, 0.3 mmol	p003 · Syntheses of complexes 1-6
Additive	Na(OAc).3H2O	41.1 mg, 0.3 mmol (inherited)	p003 · Syntheses of complexes 1-6
Solvent	MeOH/DMF	8 mL, v/v 3:1 (inherited)	p003 · Syntheses of complexes 1-6

Complete recipeSource: Main

Route 4: Other

p003 · Syntheses of complexes 1-6

Metal precursorsZn(NO3)2.6H2O (89.2 mg, 0.3 mmol; inherited from route 3)

Linker precursorsH2BDC-Cl4 (91.2 mg, 0.30 mmol; inherited from route 3)

SolventsMeOH/DMF (v/v 3:1, 8 mL; inherited from route 1)

AdditivesK(OAc) (29.7 mg, 0.30 mmol); text says NaNO3 was replaced

Atmospherenot specified

Temperatureroom temperature

Timeca. 0.5 h stirring plus seven weeks standing by inherited procedure

Work-upsame synthetic procedure as 3 except stated replacement by K(OAc); colourless block crystals in 53% yield (71.6 mg based on H2BDC-Cl4)

Activationnone reported

Scalability contextSlow evaporation over weeks; milligram-to-gram quantities reported depending on complex.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H2BDC-Cl4	91.2 mg, 0.30 mmol (inherited)	p003 · Syntheses of complexes 1-6
Metal Source	Zn(NO3)2.6H2O	89.2 mg, 0.3 mmol (inherited)	p003 · Syntheses of complexes 1-6
Additive	K(OAc)	29.7 mg, 0.30 mmol	p003 · Syntheses of complexes 1-6
Solvent	MeOH/DMF	8 mL, v/v 3:1 (inherited)	p003 · Syntheses of complexes 1-6

Complete recipeSource: Main

Route 5: Other

p003 · Syntheses of complexes 1-6

Metal precursorsComplex 1 precursor

Linker precursorscoordinated BDC-F4 retained from precursor

Solventspure water (8 mL)

Atmospherenot specified

Temperatureroom temperature

Timea few weeks slow evaporation

Work-upComplex 1 dissolved in pure water; slow evaporation over a few weeks gave colourless needlelike crystals of 5 in 60% yield (0.737 g) based on 1

Activationnone reported

Scalability contextSlow evaporation over weeks; milligram-to-gram quantities reported depending on complex.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Complex 1	1.384 g, 1 mmol	p003 · Syntheses of complexes 1-6
Solvent	pure water	8 mL	p003 · Syntheses of complexes 1-6

Complete recipeSource: Main

Route 6: Other

p003 · Syntheses of complexes 1-6

Metal precursorsComplex 2 precursor

Linker precursorscoordinated BDC-F4 retained from precursor

Solventspure water (8 mL)

Atmospherenot specified

Temperatureroom temperature

Timea few weeks slow evaporation

Work-upComplex 2 dissolved in pure water; slow evaporation over a few weeks gave colourless needlelike crystals of 5 in 55% yield (0.450 g) based on 2

Activationnone reported

Scalability contextSlow evaporation over weeks; milligram-to-gram quantities reported depending on complex.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Complex 2	1.062 g, 2 mmol	p003 · Syntheses of complexes 1-6
Solvent	pure water	8 mL	p003 · Syntheses of complexes 1-6

Complete recipeSource: Main

Route 7: Other

p003 · Syntheses of complexes 1-6

Metal precursorsComplex 3 precursor

Linker precursorsBDC-Cl4 retained as counter-anion from precursor

Solventspure water (10 mL)

Atmospherenot specified

Temperatureroom temperature

Timea few weeks slow evaporation

Work-upComplex 3 dissolved in pure water; slow evaporation over a few weeks gave colourless needlelike crystals of 6 in 65% yield (0.712 g) based on 3

Activationnone reported

Scalability contextSlow evaporation over weeks; milligram-to-gram quantities reported depending on complex.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Complex 3	1.407 g, 1 mmol	p003 · Syntheses of complexes 1-6
Solvent	pure water	10 mL	p003 · Syntheses of complexes 1-6

Complete recipeSource: Main

Route 8: Other

p003 · Syntheses of complexes 1-6

Metal precursorsComplex 4 precursor

Linker precursorsBDC-Cl4 retained as counter-anion from precursor

Solventspure water (10 mL)

Atmospherenot specified

Temperatureroom temperature

Timea few weeks slow evaporation

Work-upComplex 4 dissolved in pure water; slow evaporation over a few weeks gave colourless needlelike crystals of 6 in 73% yield (0.799 g) based on 4

Activationnone reported

Scalability contextSlow evaporation over weeks; milligram-to-gram quantities reported depending on complex.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Complex 4	1.351 g, 2 mmol	p003 · Syntheses of complexes 1-6
Solvent	pure water	10 mL	p003 · Syntheses of complexes 1-6