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

8 measurement groups · 35 results

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

13C{1H} REDOR SSNMR

Nuclear magnetic resonance

13CO2-loaded SIFSIX-3-Zn · Powder

REDOR experiments at 293 and 223 K, 10 kHz spinning, used to probe interaction between adsorbed 13CO2 and framework protons.

Temperature: 223 and 293
Atmosphere: 13CO2-loaded
Geometry: MAS REDOR
Context: guest-loaded target sample
Measurement source: PDF p6-p7 / article p17803-p17804 · Studying CO2-Loaded SIFSIX-3-Zn by SSNMR Spectroscopy · Figure 6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
REDOR effect temperature trend	REDOR effect at 223 K is larger than at 293 K	—	—	Text Qualitative	PDF p6 / article p17803 · Studying CO2-Loaded SIFSIX-3-Zn by SSNMR Spectroscopy · Figure 6b

19F to 13C CP/MAS SSNMR

Nuclear magnetic resonance

13CO2-loaded SIFSIX-3-Zn · Powder

CO2-loaded SIFSIX-3-Zn measured at 9.4 T, 15 kHz MAS, contact times of 1, 4, and 9 ms.

Atmosphere: 13CO2-loaded
Geometry: 4 mm MAS HXY probe
Context: guest-loaded target sample
Measurement source: PDF p6 / article p17803 · Studying CO2-Loaded SIFSIX-3-Zn by SSNMR Spectroscopy · Figure 5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Adsorbed 13CO2 signal at longer contact times	124 ppm	—	—	Text Rounded Reported	PDF p6 / article p17803 · Studying CO2-Loaded SIFSIX-3-Zn by SSNMR Spectroscopy · Figure 5
Pyrazine framework 13C signal at 1 ms contact time	146 ppm	—	—	Text Rounded Reported	PDF p6 / article p17803 · Studying CO2-Loaded SIFSIX-3-Zn by SSNMR Spectroscopy · Figure 5

19F MAS and 1H to 29Si CP/MAS SSNMR

Nuclear magnetic resonance

13CO2-loaded SIFSIX-3-Zn · Powder

19F MAS and 1H to 29Si CP/MAS spectra collected at 9.4 T for as-made, activated, and CO2-loaded SIFSIX-3-Zn; table includes all three samples.

Geometry: MAS SSNMR
Context: comparison of pristine controls with guest-loaded target sample
Measurement source: SI p16-p18 / S16-S18 · 19F and 29Si SSNMR Results and Discussion · Figure S5; Table S9

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
19F delta_iso Fax	-151.0(1) ppm	—	(1)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9
19F delta_iso Fax	-150.3(1) ppm	—	(1)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9
19F delta_iso FaxMarked as a best value within this paper	-150.8(1) ppm	—	(1)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9
19F delta_iso Feq	-131.6(1) ppm	—	(1)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9
19F delta_iso Feq	-130.3(1) ppm	—	(1)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9
19F delta_iso FeqMarked as a best value within this paper	-131.8(1) ppm	—	(1)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9
29Si delta_iso	-184.4(2) ppm	—	(2)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9
29Si delta_iso	-185.5(2) ppm	—	(2)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9
29Si delta_isoMarked as a best value within this paper	-184.4(2) ppm	—	(2)	SI Table Exact Reported	SI p18 / S18 · Table S9 · Table S9

Static 67Zn SSNMR with spectral simulation

Nuclear magnetic resonance

Activated SIFSIX-3-Zn · Powder

67Zn experiments at 21.1 T, nu0(67Zn) = 56.3 MHz, modified quadrupolar echo pulse sequence.

Geometry: home-built 7 mm HX probe
Context: activated pristine control
Measurement source: PDF p6 / article p17803 · Studying CO2-Loaded SIFSIX-3-Zn by SSNMR Spectroscopy · Figure 4; Table 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
67Zn quadrupolar coupling constant CQ	13.5(1) MHz	—	(1)	Table Exact Reported	PDF p6 / article p17803 · Table 2 · Table 2
67Zn EFG asymmetry parameter eta_Q	0.03(1)	—	(1)	Table Exact Reported	PDF p6 / article p17803 · Table 2 · Table 2

Static 67Zn SSNMR with spectral simulation

Nuclear magnetic resonance

As-made SIFSIX-3-Zn · Powder

67Zn experiments at 21.1 T, nu0(67Zn) = 56.3 MHz, modified quadrupolar echo pulse sequence, referenced to 1.0 M aqueous Zn(NO3)2.

Geometry: home-built 7 mm HX probe
Context: as-made pristine control
Measurement source: PDF p3-p6 / article p17800-p17803 · SSNMR Experiments; Studying CO2-Loaded SIFSIX-3-Zn by SSNMR Spectroscopy · Figure 4; Table 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
67Zn quadrupolar coupling constant CQ	16.0(1) MHz	—	(1)	Table Exact Reported	PDF p6 / article p17803 · Table 2 · Table 2
67Zn EFG asymmetry parameter eta_Q	0.04(2)	—	(2)	Table Exact Reported	PDF p6 / article p17803 · Table 2 · Table 2

Static 67Zn SSNMR with spectral simulation

Nuclear magnetic resonance

13CO2-loaded SIFSIX-3-Zn · Powder

67Zn wideline spectrum of CO2-loaded SIFSIX-3-Zn recorded under static conditions at 21.1 T; EFG tensor parameters extracted by simulation.

Atmosphere: CO2-loaded
Geometry: home-built 7 mm HX probe
Context: guest-loaded target sample
Measurement source: PDF p5-p6 / article p17802-p17803 · Studying CO2-Loaded SIFSIX-3-Zn by SSNMR Spectroscopy · Figure 4; Table 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
67Zn quadrupolar coupling constant CQMarked as a best value within this paper	13.6(1) MHz	—	(1)	Table Exact Reported	PDF p6 / article p17803 · Table 2 · Table 2
67Zn EFG asymmetry parameter eta_QMarked as a best value within this paper	0.03(1)	—	(1)	Table Exact Reported	PDF p6 / article p17803 · Table 2 · Table 2

Motional simulation of static 13C SSNMR spectra

Nuclear magnetic resonance

13CO2-loaded SIFSIX-3-Zn · Powder

Simulated static 13C spectra for CO2 in SIFSIX-3-Zn using a C3 wobbling rotation with motional angle of 10 deg and rates from 10^1 to 10^7 Hz.

Temperature: 153
Atmosphere: 13CO2-loaded
Geometry: spectral simulation
Context: guest-loaded target sample
Measurement source: SI p19-p20 / S19-S20 · The Influence of Temperature on CO2 Motional Rates in SIFSIX-3-Zn · Figure S6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
CO2 wobbling motional rate lower bound at 153 KMarked as a best value within this paper	>= ca. 10^6 Hz	—	—	Text Approximate	SI p19 / S19 · The Influence of Temperature on CO2 Motional Rates in SIFSIX-3-Zn · Figure S6

Variable-temperature static 13C SSNMR with analytical and motional simulations

Nuclear magnetic resonance

13CO2-loaded SIFSIX-3-Zn · Powder

Static VT 13C SSNMR from 153 to 393 K at 9.4 T; DEPTH-echo pulse sequence; temperature calibration by 207Pb chemical shift of Pb(NO3)2 with +/-2 K error.

Temperature: 153-393
Atmosphere: 13CO2-loaded
Geometry: stationary sample, 5 mm HFXY probe for static experiments
Context: guest-loaded target sample
Measurement source: PDF p6-p7 / article p17803-p17804 · CO2 Dynamics in SIFSIX-3-Zn · Figure 7; Table 3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
13CO2 delta_iso at 153 K	123(2) ppm	—	(2)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 delta_iso at 293 K	125(1) ppm	—	(1)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 delta_iso at 393 K	123(1) ppm	—	(1)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 delta_iso range across 153-393 K	123-125 ppm across Table 3 temperatures	—	individual values have uncertainties of 1-2 ppm	Table Range	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 skew kappa at 153 K	1.00(4)	—	(4)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 skew kappa at 293 K	0.98(2)	—	(2)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 skew kappa at 393 K	0.98(2)	—	(2)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 kappa range across 153-393 KMarked as a best value within this paper	0.98-1.00	—	individual values have uncertainties of 0.02-0.04	Table Range	PDF p7 / article p17804 · CO2 Dynamics in SIFSIX-3-Zn · Table 3
13CO2 chemical shift span Omega at 153 K	315(5) ppm	—	(5)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 chemical shift span Omega at 293 K	303(2) ppm	—	(2)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 chemical shift span Omega at 393 K	288(2) ppm	—	(2)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
13CO2 Omega range across 153-393 KMarked as a best value within this paper	288-315 ppm	—	individual values have uncertainties of 2-5 ppm	Table Range	PDF p7 / article p17804 · Table 3; CO2 Dynamics in SIFSIX-3-Zn · Table 3
CO2 wobbling angle alpha at 153 KMarked as a best value within this paper	10(1) deg	—	(1)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
CO2 wobbling angle alpha at 293 KMarked as a best value within this paper	14(1) deg	—	(1)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
CO2 wobbling angle alpha at 393 KMarked as a best value within this paper	17(1) deg	—	(1)	Table Exact Reported	PDF p7 / article p17804 · Table 3 · Table 3
CO2 wobbling angle alpha range across 153-393 KMarked as a best value within this paper	10-17 deg	—	individual values have uncertainties of 1 deg	Table Range	PDF p7 / article p17804 · CO2 Dynamics in SIFSIX-3-Zn · Table 3