Spectroscopy — Solid-State Electrochemical Carbon Dioxide Capture by Conductive Metal-Organic Framework Incorporating Nickel Bis(diimine) Units

5 measurement groups · 23 results

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

Ni3(HITP)2 on carbon fibre paper eCC electrode · Electrode

Custom sealed PTFE electrochemical cell; silicon crystal with drop-cast MOF layer; spectra every 2 min during reduction.

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni3(HITP)2 13C=O stretching band	1706 cm-1	—	—	Text Rounded Reported	33099-33100 · Mechanism of CO2 Capture · Figure 5d; Figure S37
Ni3(HITP)2 N-13CO2 stretching band	1090-1100 cm-1	—	range	Text Range	33099-33100 · Mechanism of CO2 Capture · Figure 5d; Figure S37
Ni(DIB)2 13C=O stretching band	1706 cm-1	—	—	Text Rounded Reported	33099 · Mechanism of CO2 Capture · Figure 5c
Ni(DIB)2 N-13CO2 stretching band	1080-1090 cm-1	—	range	Text Range	33099 · Mechanism of CO2 Capture · Figure 5c

As-synthesised Ni3(HITP)2 dark-blue powder · Powder

Samples dried under room-temperature oil-pump vacuum for 2 h; 128 scans from 4000 to 550 cm-1.

Atmosphere: ambient test after vacuum drying
Geometry: ATR accessory ZnSe crystal/ejector pin contact
Context: pristine framework characterisation
Measurement source: S9-S10 · 4. Attenuated Total Reflectance Infrared Spectroscopy · Figure S7

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni3(HITP)2 triphenylene ring in-plane stretch	1424 cm-1	—	—	Text Rounded Reported	S10 · 4. Attenuated Total Reflectance Infrared Spectroscopy · Figure S7
Ni3(HITP)2 triphenylene ring in-plane stretch	1503 cm-1	—	—	Text Rounded Reported	S10 · 4. Attenuated Total Reflectance Infrared Spectroscopy · Figure S7
Ni3(HITP)2 triphenylene ring in-plane stretch	1624 cm-1	—	—	Text Rounded Reported	S10 · 4. Attenuated Total Reflectance Infrared Spectroscopy · Figure S7

Ni(DIB)2 crystals/powder · Powder

DAB ligand and Ni(DIB)2 comparison; samples dried and measured by ATR-IR.

Atmosphere: ambient test after vacuum drying
Geometry: ATR accessory ZnSe crystal/ejector pin contact
Context: pristine molecular analogue control
Measurement source: S9 · 4. Attenuated Total Reflectance Infrared Spectroscopy · Figure S6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni(DIB)2 N-H stretch label in ATR-IR	3292 cm-1 labelled -NH-	—	—	Figure Axis Rounded Reported	S9 · 4. Attenuated Total Reflectance Infrared Spectroscopy · Figure S6

Ni(DIB)2 solution electrochemical control · Unknown

Reduced Ni(DIB)2 prepared in H-cell; CO2-purged samples diluted in DMSO-d6 for NMR; MOF after 13CO2 capture measured by 13C ssNMR.

Temperature: 298
Atmosphere: N2 reduction then CO2 or 13CO2 exposure
Geometry: Solution NMR/MS and solid-state NMR
Context: molecular analogue and MOF mechanism
Measurement source: S30-S32 · 12.2 NMR Spectrum and Mass Spectrum · Figures S33-S35

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
1H NMR aromatic adduct peak after CO2 exposure	6.30 ppm	—	—	Text Exact Reported	S30-S31 · 12.2. NMR Spectrum and Mass Spectrum · Figure S33
1H NMR aromatic adduct peak after CO2 exposure	6.67 ppm	—	—	Text Exact Reported	S30-S31 · 12.2. NMR Spectrum and Mass Spectrum · Figure S33
1H NMR low-field -COOH peak after CO2 exposure	9.82 ppm	—	—	Text Exact Reported	S30-S31 · 12.2. NMR Spectrum and Mass Spectrum · Figure S33
1H NMR imine-region adduct peak after CO2 exposure	8.75 ppm	—	—	Text Exact Reported	S30-S31 · 12.2. NMR Spectrum and Mass Spectrum · Figure S33
Mass peak for reduced Ni(DIB)2 CO2 adduct	m/z = 316.1091	—	—	Text Exact Reported	S32 · 12.2 NMR Spectrum and Mass Spectrum · Figure S35
13C ssNMR carbamate/carbamic-acid signal after MOF CO2 capture	161.20 ppm	—	—	Text Exact Reported	S31-S32 · 12.2 NMR Spectrum and Mass Spectrum · Figure S34
13C ssNMR free CO2 signal	125.04 ppm	—	—	Text Exact Reported	S32 · 12.2 NMR Spectrum and Mass Spectrum · Figure S34

Ni(DIB)2 solution electrochemical control · Unknown

20 microL aliquots diluted to 3 mL DMF; reduction sampled every 20 min; CO2 exposure sampled every 15 min.

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Oscillator strength for [Ni(DIB)2-CO2]- adduct at 700-1000 nm transition	0.11	—	—	Text Exact Reported	S29 · 12.1. UV-vis-NIR Spectra · Figure S32
Oscillator strength for pristine Ni(DIB)2 at 700-1000 nm transition	0.34	—	—	Text Exact Reported	S29 · 12.1. UV-vis-NIR Spectra · Figure S32
Oscillator strength for reduced [Ni(DIB)2]- at 700-1000 nm transition	0.28	—	—	Text Exact Reported	S29 · 12.1. UV-vis-NIR Spectra · Figure S32
785 nm absorption intensity decrease after CO2 exposure	decreased by 46%	—	—	Text Rounded Reported	33098 · Mechanism of CO2 Capture · Figure 5a; Figure S32
785 nm absorption intensity decrease after reduction	decreased by 10%	—	—	Text Rounded Reported	33098 · Mechanism of CO2 Capture · Figure 5a; Figure S32
Transition electric dipole moment of [Ni(DIB)2-CO2]-	3.24 Debye	—	—	Text Exact Reported	S29 · 12.1 UV-vis-NIR Spectra · Figure S32
Transition electric dipole moment of pristine Ni(DIB)2	11.25 Debye	—	—	Text Exact Reported	S29 · 12.1 UV-vis-NIR Spectra · Figure S32
Transition electric dipole moment of reduced [Ni(DIB)2]-	8.40 Debye	—	—	Text Exact Reported	S29 · 12.1 UV-vis-NIR Spectra · Figure S32