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

Measurement evidence

Diffraction Structure

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

2 measurement groups · 21 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

Powder X-ray diffraction (PXRD)

X-ray diffraction and scattering

As-made SIFSIX-3-Zn · Powder

Experimental PXRD pattern of as-made SIFSIX-3-Zn compared with simulated pattern from reported as-made crystal structure; Cu Kalpha source, lambda = 1.5418 A, 2theta from 5 to 120 deg.

Geometry
powder diffraction
Context
pristine control
Measurement source
SI p3 / S3 · Figure S2 caption · Figure S2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
PXRD identity and purity agreementExperimental PXRD pattern agrees with simulated pattern——Text
Qualitative		PDF p3 / article p17800 · Methods - Sample Preparation · Figure S2

Single-crystal X-ray diffraction (SCXRD)

X-ray diffraction and scattering

CO2-saturated SIFSIX-3-Zn single crystals · Single Crystal

CO2-loaded single crystals measured on a Bruker-Nonius KappaCCD Apex2 diffractometer at 110 K using Cu Kalpha radiation; structure solved with SHELXT and refined with SHELXL-2014.

Temperature
110
Atmosphere
CO2-loaded crystal coated with Paratone oil after sealed tube opening
Geometry
single crystal on Mitegen polyimide micromount
Context
guest-loaded target sample
Measurement source
PDF p3-p4 / article p17800-p17801 · Methods - SCXRD Experiments; Results and Discussion · Figure 1c,d; Tables S1-S7
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
checkCIF alert summary0 level A, 3 level B, 5 level C, 8 level G alerts——Table
Exact Reported		SI2 p2 · checkCIF/PLATON report · Alerts summary
Unit-cell a parameterMarked as a best value within this papera = 9.9917(14) A—(14)SI Table
Exact Reported		SI p4 / S4 · Table S1 · Table S1
Unit-cell c parameterMarked as a best value within this paperc = 15.088(2) A—(2)SI Table
Exact Reported		SI p4 / S4 · Table S1 · Table S1
CIF refined CO2 atom occupancy0.466(7)—(7)Table
Exact Reported		CIF text · atom_site loop
CO2 occupancy at each adsorption positionMarked as a best value within this paperca. 0.47 at each position——Text
Approximate		PDF p4 / article p17801 · SCXRD of CO2-Loaded SIFSIX-3-Zn · Figure 3a
Equivalent CO2 adsorption-site separation1.10 A——Text
Rounded Reported		PDF p4 / article p17801 · SCXRD of CO2-Loaded SIFSIX-3-Zn · Figure 3a
Calculated crystal densityrho = 1.802 g/cm3——SI Table
Exact Reported		SI p4 / S4 · Table S1 · Table S1
CO2-loaded crystal formulaC17.86H16F12N8O3.73Si2Zn2——SI Table
Exact Reported		SI p4 / S4 · Table S1 · Table S1
Potential hydrogen bond H...F1 distanceC1-H1...F1 H...A = 2.51 A——SI Table
Exact Reported		SI p12 / S12 · Table S7 · Table S7
Potential hydrogen bond H...F2 distanceC1-H1...F2 H...A = 2.37 A——SI Table
Exact Reported		SI p12 / S12 · Table S7 · Table S7
CO2-loaded pore size with van der Waals radii subtractedMarked as a best value within this paper3.72 A——Text
Rounded Reported		PDF p4 / article p17801 · SCXRD of CO2-Loaded SIFSIX-3-Zn · Figure 1d
Pyr ring angle to Fax-Zn-N planeMarked as a best value within this paper22.9 deg——Table
Rounded Reported		PDF p5 / article p17802 · Table 1 · Table 1
SCXRD R1 for observed reflectionsR1 = 0.0209——SI Table
Exact Reported		SI p5 / S5 · Table S1 · Table S1
Si-F axial bond distance1.7260(17), 1.7261(17) A—(17)SI Table
Exact Reported		SI p8 / S8 · Table S4 · Table S4
Si-F equatorial bond distance1.6687(13) A—(13)SI Table
Exact Reported		SI p8 / S8 · Table S4 · Table S4
CO2-loaded space groupMarked as a best value within this paperI 4/m c m——SI Table
Exact Reported		CIF text · data_n17104
Unit-cell volumeMarked as a best value within this paperV = 1506.3(5) A3—(5)SI Table
Exact Reported		SI p4 / S4 · Table S1 · Table S1
SCXRD wR2 all datawR2 (all data) = 0.0605——SI Table
Exact Reported		SI p5 / S5 · Table S1 · Table S1
Zn-F bond distance2.0460(17) A—(17)SI Table
Exact Reported		SI p8 / S8 · Table S4 · Table S4
Zn-N bond distance2.144(2) A—(2)SI Table
Exact Reported		SI p8 / S8 · Table S4 · Table S4