Synthesis · Control of crystalline proton-conducting pathways by water-induced transformations of hydrogen-bonding networks in a metal-organic framework

3 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

7703 · Structural Analysis

Metal precursors1·3H2O crystals

Solventsdistilled water wash

Atmosphereambient air

Temperatureambient

Work-upwashed samples dried under air

Activationambient drying converts 1·3H2O to hydrated 1·2H2O

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	1·3H2O	Not specified	7703 · Structural Analysis

Complete recipeSource: Main

Route 2: Hydrothermal

7702 · Preparation of 1·3H2O

Metal precursorsZnO (10 mmol, 814 mg)

Linker precursorsoxalic acid dihydrate (20 mmol, 2521 mg); adipamide (10 mmol, 1442 mg)

Solventsdistilled water (550 mmol, 10 mL)

Atmospherenot specified; sealed 50 mL Teflon-lined bottle

Temperature130

Time24 h at 130 °C, then slow cooling to room temperature over 168 h

Work-upprecipitate collected by filtration; several crystals stored in mother liquid; washed with distilled water; dried under air for air-dried sample

Scalability contextReported yield 2891 mg, 92%.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	ZnO	10 mmol, 814 mg	7702 · Preparation of 1·3H2O
Linker	oxalic acid dihydrate (H2(ox)·2H2O)	20 mmol, 2521 mg	7702 · Preparation of 1·3H2O
Linker	adipamide	10 mmol, 1442 mg	7702 · Preparation of 1·3H2O
Solvent	distilled water	550 mmol, 10 mL	7702 · Preparation of 1·3H2O

Complete recipeSource: Main

Route 3: Other

7702 · Crystal Structure Determination; Physical Measurements

Metal precursors1·2H2O single crystal

AtmosphereN2 flow for SCXRD sample; vacuum for pellet; vacuum/heat for adsorption sample

Temperature50 for SCXRD single crystal; 80 for adsorption activation

Timeovernight

Activationdrying 1·2H2O at 50 °C overnight under N2 flow; pellet prepared by heating under vacuum; sorption sample dehydrated at 80 °C overnight

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	1·2H2O	Not specified	7702 · Crystal Structure Determination; Physical Measurements