cMOF Evidence Base

Synthesis evidence

CO2 Behavior in a Highly Selective Ultramicroporous Framework: Insights from Single-Crystal X-ray Diffraction and Solid-State Nuclear Magnetic Resonance Spectroscopy

Desveaux B.E., Wong Y.T.A., Lucier B.E.G. et al. · Journal of Physical Chemistry C · 2019 · 17798-17807

4 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

PDF p3 / article p17800 · Methods - Sample Activation and Gas Loading

Metal precursorsActivated SIFSIX-3-Zn
AdditivesIsotopically labelled 13CO2 gas
AtmosphereSchlenk line; 13CO2 introduced then frozen into sample with liquid nitrogen
Temperatureliquid nitrogen freezing during loading; activation at 80 +/- 10 C before loading
Time24 h activation before gas loading
Work-upLoaded sample was flame-sealed off from the Schlenk line.
ActivationDynamic vacuum below 1 mbar at 80 +/- 10 C for 24 h before 13CO2 loading.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated SIFSIX-3-ZnNot specifiedPDF p3 / article p17800 · Methods - Sample Activation and Gas Loading
Otherisotopically labelled 13CO2 gas0.25 molar ratio of CO2 to Zn2+PDF p3 / article p17800 · Methods - Sample Activation and Gas Loading
Complete recipeSource: Main

Route 2: Other

PDF p3 / article p17800 · Methods - Sample Activation and Gas Loading

Metal precursorsAs-made SIFSIX-3-Zn
AtmosphereDynamic vacuum below 1 mbar
Temperature80 +/- 10
Time24
Work-upSample placed in an L-shaped glass tube and secured with glass wool before activation.
ActivationDynamic vacuum below 1 mbar at 80 +/- 10 C for 24 h.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otheras-made SIFSIX-3-ZnNot specifiedPDF p3 / article p17800 · Methods - Sample Activation and Gas Loading
Complete recipeSource: Main

Route 3: Solvothermal

PDF p3 / article p17800 · Methods - Sample Preparation

Metal precursorsZnSiF6.xH2O (0.62 g, 3 mmol, Sigma-Aldrich, 99%)
Linker precursorsPyrazine (pyr; 0.48 g, 6 mmol, Alfa Aesar, 98%)
SolventsMethanol; 10 mL for pyrazine solution and 10 mL for ZnSiF6.xH2O solution
AtmosphereAir during drying; synthesis atmosphere otherwise not specified
Temperatureroom temperature for crystallisation; 90 C drying
Time72 h crystallisation; 3 h drying
Work-upYellow crystals were collected, dried at 90 C in air for 3 h, then solvent-exchanged in MeOH for 3 days before activation/loading with daily MeOH replacement.
ActivationActivation not part of as-made sample; subsequent activation route recorded separately.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerpyr (pyrazine), Alfa Aesar, 98%0.48 g, 6 mmol · in 10 mL MeOHPDF p3 / article p17800 · Methods - Sample Preparation
Metal SourceZnSiF6.xH2O, Sigma-Aldrich, 99%0.62 g, 3 mmol · in 10 mL MeOHPDF p3 / article p17800 · Methods - Sample Preparation
Solventmethanol (MeOH)20 mL total reaction solution; MeOH solution for 3 day solvent exchangePDF p3 / article p17800 · Methods - Sample Preparation
Complete recipeSource: Main

Route 4: Other

PDF p3 / article p17800 · Methods - SCXRD Experiments

Metal precursorsSIFSIX-3-Zn single crystals
AdditivesCO2 gas
AtmosphereSchlenk line CO2 loading
Temperatureactivation at 80 +/- 10 C before loading; single-crystal measurement at 110 K
Time24 h activation before loading
Work-upGlass tube broken immediately before SCXRD; crystals coated with Paratone oil to prevent CO2 loss.
ActivationActivated using the same procedure as the bulk sample, then loaded to CO2 saturation.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherSIFSIX-3-Zn single crystalssmall amountPDF p3 / article p17800 · Methods - SCXRD Experiments
OtherCO2 gasloaded to saturationPDF p3 / article p17800 · Methods - SCXRD Experiments