Synthesis · Particle size dependence of proton conduction in a cationic lanthanum phosphonate MOF

3 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 / journal page 4023 · Particle sieving and collection · Figure 3

Metal precursorspre-synthesised PCMOF21-AcO powder

Linker precursorspre-synthesised PCMOF21-AcO powder

Solventswater used only to sonicate/clean sieves before drying; isopropanol used for separate laser particle-size dispersion

Additivesnone

Atmosphereambient

Temperatureroom temperature

Time0.25 h per sieving run; repeated twice more

Work-upSieves separated to prevent cross-contamination; each particle-size collection placed into a different vial; total 300 mg powder separated.

ActivationConductivity samples loaded as is and compressed at 0.4 N m.

Scalability contextApproximately 100 mg portions loaded onto top sieve; repeated to process 300 mg total.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	PCMOF21-AcO bulk powder	~100 mg portions; 300 mg total	p002 / journal page 4023 · Particle sieving and collection · Figure 3
Solvent	H2O	used to sonicate sieves, then dried	p002 / journal page 4023 · Particle sieving and collection · Figure 3

Complete recipeSource: Main

Route 2: Other

p002 / journal page 4023 · Synthesis of PCMOF21-AcO

Metal precursorslanthanum(III) acetate sesquihydrate, 187 mg, 0.545 mmol

Linker precursorsH4L ligand [N,N'-4,4'-bipiperidinebis(methylenephosphonic acid)], 174 mg, 0.406 mmol; ligand itself prepared according to literature procedure

SolventsH2O, 7.2 mL

Additivesacetate supplied by lanthanum(III) acetate sesquihydrate

Atmospherenot specified; aqueous reflux under ambient laboratory conditions inferred but not stated

Temperaturereflux, nominally about 100 deg C

Time96

Work-upFiltered hot; residual powder scraped from flask; washed with liberal amounts of H2O; white solid collected, 216 mg, 0.197 mmol, 72.8%.

ActivationStored in a vacuum desiccator prior to use; CO2 uptake sample separately activated at 100 deg C overnight.

Scalability contextSmall-batch aqueous reflux; 216 mg product reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H4L ligand [N,N'-4,4'-Bipiperidinebis(methylenephosphonic acid)]	174 mg, 0.406 mmol	p002 / journal page 4023 · Synthesis of PCMOF21-AcO
Metal Source	lanthanum(III) acetate sesquihydrate	187 mg, 0.545 mmol	p002 / journal page 4023 · Synthesis of PCMOF21-AcO
Solvent	H2O	7.2 mL	p002 / journal page 4023 · Synthesis of PCMOF21-AcO

Partial recipeSource: Main

Route 3: Hydrothermal

p002 / journal page 4023 · Single crystal synthesis of PCMOF21-AcO

Metal precursorslanthanum(III) acetate sesquihydrate; 4:3 metal salt to ligand ratio

Linker precursorsH4L ligand, approximately 170 mg

SolventsH2O, 7 mL

Additivesacetate supplied by lanthanum(III) acetate sesquihydrate

Atmospheresealed Teflon-lined autoclave; atmosphere not otherwise specified

Temperature120

Time72 h hold after 2 h ramp; 12 h cooling

Work-upCrystals kept in mother liquor prior to use and mechanically separated from crystalline powder surrounding them.

ActivationNone specified for single-crystal structure; measured/collected at 100 K in SI/CIF.

Scalability context23 mL Teflon-lined autoclave crystal growth; yield not reported.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	H4L ligand	~170 mg	p002 / journal page 4023 · Single crystal synthesis of PCMOF21-AcO
Metal Source	lanthanum(III) acetate sesquihydrate	4:3 ratio to ligand	p002 / journal page 4023 · Single crystal synthesis of PCMOF21-AcO
Solvent	H2O	7 mL	p002 / journal page 4023 · Single crystal synthesis of PCMOF21-AcO