Spectroscopy — Oxidatively Doped Tetrathiafulvalene-Based Metal-Organic Frameworks for High Specific Energy of Supercapatteries

4 measurement groups · 21 results

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

Solid-state electron spin resonance

Electron paramagnetic resonance

1-ox · Single Crystal

Measured at 110 K for 1 and 1-ox with same parameters; 2/2-ox in missing Figure S14a.

Temperature: 110
Atmosphere: solid state
Context: doped versus pristine
Measurement source: p004-p005 / 6624-6625 · 2.3 · Figure 3b

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
radical ESR g value	g = 2.005	—	—	Text Exact Reported	p005 / 6625 · 2.3 · Figure 3b and Figure S14a

Ex situ PXRD, FTIR and XPS after charge/discharge

Infrared spectroscopy X-ray photoelectron spectroscopy X-ray diffraction and scattering

1-ox electrode · Electrode

Fully discharged and fully charged 1-ox positrode states after cycling; includes C 1s, N 1s, S 2p and Ni 2p XPS.

Geometry: positrode after electrochemical cycling
Context: doped target electrode mechanism
Measurement source: p007-p008 / 6627-6628 · 2.5 Performance of Supercapattery Devices · Figure 6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
new C 1s C-N/C-O discharge peak	286.6 eV after discharge	—	—	Text Exact Reported	p007 / 6627 · 2.5 · Figure 6c
FTIR bands shifting reversibly during discharge/charge	1683, 1552 and 1525 cm^-1 bands negatively shifted during discharge and moved back during charge	—	—	Text Qualitative	p007 / 6627 · 2.5 · Figure 6b
N 1s binding-energy shift during discharge/charge	399.6 eV original; 398.6 eV after discharge; 398.9 eV after charge	398.9 eV after charge	—	Text Exact Reported	p007 / 6627 · 2.5 · Figure 6d
framework integrity after KOH immersion and cycling	Most PXRD peaks remained after 6 M KOH immersion for 24 h and after cycling	—	—	Text Qualitative	p007 / 6627 · 2.5 · Figure 6a and Figure S26a
positive charged sulfur species after discharge	168.9 eV	—	—	Text Exact Reported	p008 / 6628 · 2.5 · Figure 6e

Optical diffuse-reflection spectroscopy converted to UV-vis absorption

UV-visible and optical absorption spectroscopy

1-ox · Single Crystal

Solid-state room-temperature DRS for py-TTF-py, 1, 1-ox, 2 and 2-ox.

Temperature: room temperature
Atmosphere: solid state
Context: doped versus pristine
Measurement source: p004 / 6624 · 2.3 Optical and Electronic Properties · Figure 3a

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
band gap narrowing after iodine treatment	approximately 0.5 eV narrower than pristine crystals	—	~	Text Approximate	p004 / 6624 · 2.3 Optical and Electronic Properties · Figure S13; Table S3
1 direct band gap	1.89 eV	—	—	SI Table Exact Reported	p030 · 4. Table · Table S3
1 indirect band gap	1.74 eV	—	—	SI Table Exact Reported	p030 · 4. Table · Table S3
1-ox direct band gap	1.48 eV	—	—	SI Table Exact Reported	p030 · 4. Table · Table S3
1-ox indirect band gapMarked as a best value within this paper	1.21 eV	—	—	SI Table Exact Reported	p030 · 4. Table · Table S3
2 direct band gap	1.98 eV	—	—	SI Table Exact Reported	p030 · 4. Table · Table S3
2 indirect band gap	1.82 eV	—	—	SI Table Exact Reported	p030 · 4. Table · Table S3
2-ox direct band gap	1.56 eV	—	—	SI Table Exact Reported	p030 · 4. Table · Table S3
2-ox indirect band gapMarked as a best value within this paper	1.28 eV	—	—	SI Table Exact Reported	p030 · 4. Table · Table S3
1 absorption peak after coordinationMarked as a best value within this paper	541 nm	—	—	Text Exact Reported	p004 / 6624 · 2.3 · Figure 3a
1-ox broad absorption bandMarked as a best value within this paper	374 to 650 nm; tail to 1100 nm	—	—	Text Range	p004 / 6624 · 2.3 · Figure 3a
2 absorption peak after coordination	533 nm	—	—	Text Exact Reported	p004 / 6624 · 2.3 · Figure 3a
2-ox broad absorption band	374 to 612 nm; tail to 1100 nm	—	—	Text Range	p004 / 6624 · 2.3 · Figure 3a
py-TTF-py longest-wavelength absorption peak	475 nm	—	—	Text Exact Reported	p004 / 6624 · 2.3 · Figure 3a

X-ray photoelectron spectroscopy, C 1s deconvolution

X-ray photoelectron spectroscopy

1-ox' · Powder

XPS performed on washed 1-ox' because physisorbed-iodine samples were prohibited.

Context: washed doped control
Measurement source: p004 / 6624 · 2.2 Characterization · Figure 2d

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
C 1s evidence for TTF oxidation	C=C at 284.5 eV decreased; C-C at 285.0 eV increased in 1-ox' and 2-ox'	—	—	Text Qualitative	p004 / 6624 · 2.2 · Figure 2d and Figure S11