Synthesis · Lanthanide-Hypophosphite Frameworks with Guanidinium Guest Showing High Proton Conductivity

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

1 · Experimental Section - Synthesis

Metal precursorsGdCl3.6H2O

Linker precursorsaqueous hypophosphorous acid solution (50% w/w)

Solventswater; aqueous hypophosphorous acid solution

Additivesguanidine carbonate

Atmosphereambient air not explicitly specified

Temperatureroom temperature

Time0.17-0.33 h crystallisation after guest addition

Work-upcolourless crystals collected by filtering the solution

Activationnone reported

Scalability context20 mL glass bottle batch; yield 60% based on GdCl3.6H2O

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	GdCl3.6H2O	90 mg, 0.24 mmol	1 · Experimental Section - Synthesis
Linker	aqueous hypophosphorous acid solution	400 mg, 3.0 mmol · 50% w/w	1 · Experimental Section - Synthesis
Solvent	water	extra 0.5 mL	1 · Experimental Section - Synthesis
Base	guanidine carbonate	270 mg, 1.5 mmol	1 · Experimental Section - Synthesis

Complete recipeSource: Both

Route 2: Other

1 · Experimental Section - Synthesis

Metal precursorsGdCl3.6H2O

Linker precursorsaqueous hypophosphorous acid solution (50% w/w)

Solventswater; aqueous hypophosphorous acid solution

Additivesimidazolium

Atmosphereambient air not explicitly specified

Temperatureroom temperature

Time0.17-0.33 h crystallisation inferred from complex 1 procedure

Work-upcrystals collected by filtering the solution, as in complex 1 procedure

Activationnone reported

Scalability context20 mL glass bottle batch; yield 55% based on GdCl3.6H2O

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	GdCl3.6H2O	90 mg, 0.24 mmol	1 · Experimental Section - Synthesis
Linker	aqueous hypophosphorous acid solution	400 mg, 3.0 mmol · 50% w/w	1 · Experimental Section - Synthesis
Solvent	water	extra 0.5 mL	1 · Experimental Section - Synthesis
Additive	imidazolium	204 mg, 3.0 mmol	1 · Experimental Section - Synthesis

Complete recipeSource: Both

Route 3: Other

1 · Experimental Section - Synthesis

Metal precursorsGdCl3.6H2O

Linker precursorsaqueous hypophosphorous acid solution (50% w/w)

Solventswater; aqueous hypophosphorous acid solution

Additivespyrazole

Atmosphereambient air not explicitly specified

Temperatureroom temperature

Time0.17-0.33 h crystallisation inferred from complex 1 procedure

Work-upcrystals collected by filtering the solution, as in complex 1 procedure

Activationnone reported

Scalability context20 mL glass bottle batch; yield 69% based on GdCl3.6H2O

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	GdCl3.6H2O	90 mg, 0.24 mmol	1 · Experimental Section - Synthesis
Linker	aqueous hypophosphorous acid solution	400 mg, 3.0 mmol · 50% w/w	1 · Experimental Section - Synthesis
Solvent	water	extra 0.5 mL	1 · Experimental Section - Synthesis
Additive	pyrazole	204 mg, 3.0 mmol	1 · Experimental Section - Synthesis

Complete recipeSource: Both

Route 4: Other

1 · Experimental Section - Synthesis

Metal precursorsGdCl3.6H2O

Linker precursorsaqueous hypophosphorous acid solution (50% w/w)

Solventswater; aqueous hypophosphorous acid solution

Additivestriazolium

Atmosphereambient air not explicitly specified

Temperatureroom temperature

Time0.17-0.33 h crystallisation inferred from complex 1 procedure

Work-upcrystals collected by filtering the solution, as in complex 1 procedure

Activationnone reported

Scalability context20 mL glass bottle batch; yield 54% based on GdCl3.6H2O

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	GdCl3.6H2O	90 mg, 0.24 mmol	1 · Experimental Section - Synthesis
Linker	aqueous hypophosphorous acid solution	400 mg, 3.0 mmol · 50% w/w	1 · Experimental Section - Synthesis
Solvent	water	extra 0.5 mL	1 · Experimental Section - Synthesis
Additive	triazolium	207 mg, 3.0 mmol	1 · Experimental Section - Synthesis