Spectroscopy — Paramagnetic Conducting Metal–Organic Frameworks with Three-Dimensional Structure

10 measurement groups · 14 results

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

57Fe Mossbauer spectroscopy

Mossbauer spectroscopy

Fe-THBQ black powder · Powder

Topologic 500A spectrometer and proportional counter; 57Co(Rh) gamma-ray source; samples about 10 mg cm^-2 Fe; velocity calibrated with alpha-iron foil; analysed using MossWinn.

Temperature: 77 and 300
Geometry: powder absorber
Context: pristine Fe-THBQ
Measurement source: 3,8 · Mossbauer spectroscopic characterization · Figure S2; Table S4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
electron hopping rate at 300 K	138(5) Mrad s^-1	—	5 Mrad s^-1	SI Table Exact Reported	8 · Table S4 · Table S4
FeIII/FeII ratio at 300 K	FeIII/FeII ratio 83.8:16.2%	—	—	Text Exact Reported	3 · Mossbauer discussion · Figure S2; Table S4
FeIII/FeII ratio at 77 K	FeIII/FeII ratio 71.7:28.3%	—	—	Text Exact Reported	3 · Mossbauer discussion · Figure S2; Table S4

Raman spectroscopy

Co-THBQ well-crystallised powder · Powder

532 nm excitation, room temperature; powder mixed with KBr and compressed into a flake.

Temperature: room temperature
Geometry: KBr flake
Context: pristine Co-THBQ
Measurement source: 3 · Raman discussion · Figure S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
THBQ4- C-O stretching Raman band	1521 cm^-1	—	—	Text Exact Reported	3 · Raman discussion · Figure S3

Raman spectroscopy

Fe-THBQ black powder · Powder

LabRAM HR Evolution Raman spectrometer, 532 nm excitation, room temperature; powder mixed with KBr and compressed into a flake.

Temperature: room temperature
Geometry: KBr flake
Context: pristine Fe-THBQ
Measurement source: 3 · Raman spectroscopic characterization · Figures S3 and S5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
THBQ4- C-O stretching Raman band	1519 cm^-1	—	—	Text Exact Reported	3 · Raman discussion · Figure S3
semiquinone C-O stretching Raman band	1478 cm^-1	—	—	Text Exact Reported	3 · Raman discussion · Figure S3

Raman spectroscopy

Mn-THBQ powder · Powder

532 nm excitation, room temperature; powder mixed with KBr and compressed into a flake.

Temperature: room temperature
Geometry: KBr flake
Context: pristine Mn-THBQ
Measurement source: 3 · Raman discussion · Figure S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
THBQ4- C-O stretching Raman band	1533 cm^-1	—	—	Text Exact Reported	3 · Raman discussion · Figure S3

UV-visible-NIR diffuse reflectance / absorbance and Tauc analysis

UV-visible and optical absorption spectroscopy

Co-THBQ well-crystallised powder · Powder

UV-2000 SHIMADZU spectrophotometer at room temperature; sample powder on BaSO4.

Temperature: room temperature
Geometry: powder on BaSO4 matrix
Context: pristine Co-THBQ
Measurement source: 3-4 · UV/Vis-NIR discussion · Figure 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
optical band gap from Tauc plot	1.44 eV	—	—	Text Exact Reported	4 · UV/Vis-NIR discussion · Figure 4b

UV-visible-NIR diffuse reflectance / absorbance and Tauc analysis

UV-visible and optical absorption spectroscopy

Fe-THBQ black powder · Powder

UV-2000 SHIMADZU spectrophotometer at room temperature; sample powder spread on barium sulfate non-absorbing matrix.

Temperature: room temperature
Geometry: powder on BaSO4 matrix
Context: pristine Fe-THBQ
Measurement source: 3 · UV-Visible-NIR spectroscopic characterization · Figure 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
optical band gap from Tauc plotMarked as a best value within this paper	0.63 eV	—	—	Text Exact Reported	4 · UV/Vis-NIR discussion · Figure 4b
absorption range	strong absorption bands in the range of 220-1000 nm; Fe absorption started from 520 nm and extended to 1400 nm	—	—	Text Range	3 · UV/Vis-NIR discussion · Figure 4a

UV-visible-NIR diffuse reflectance / absorbance and Tauc analysis

UV-visible and optical absorption spectroscopy

Mn-THBQ powder · Powder

UV-2000 SHIMADZU spectrophotometer at room temperature; sample powder on BaSO4.

Temperature: room temperature
Geometry: powder on BaSO4 matrix
Context: pristine Mn-THBQ
Measurement source: 3-4 · UV/Vis-NIR discussion · Figure 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
optical band gap from Tauc plot	1.69 eV	—	—	Text Exact Reported	4 · UV/Vis-NIR discussion · Figure 4b

X-ray photoelectron spectroscopy

Co-THBQ well-crystallised powder · Powder

AXIS Ultra-DLD XPS with monochromatic Al K alpha source; room temperature.

Temperature: room temperature
Atmosphere: ultrahigh vacuum
Geometry: powder
Context: pristine framework powder
Measurement source: 3 · XPS discussion · Figure S1b

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Co XPS oxidation-state assignment	main peaks at 796.1 and 780.5 eV with satellite peaks at 801.1 and 784.8 eV, confirming CoII	—	—	Text Exact Reported	3 · XPS discussion · Figure S1b

X-ray photoelectron spectroscopy

Fe-THBQ black powder · Powder

AXIS Ultra-DLD ultrahigh vacuum photoemission spectroscopy with monochromatic Al K alpha source (1486.6 eV); calibrated to C-C C 1s at 284.8 eV.

Temperature: room temperature
Atmosphere: ultrahigh vacuum
Geometry: powder
Context: pristine framework powder
Measurement source: 2-3,8 · Component characterization and analysis · Figure S1; Table S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Fe XPS oxidation-state assignment	FeII peaks at 708.5, 709.5, 710.6 eV; FeIII peaks at 710.7, 711.6, 712.9, 714.1 eV; mixed-valence Fe	—	—	Text Exact Reported	3 · XPS discussion · Figure S1a; Table S3

X-ray photoelectron spectroscopy

Mn-THBQ powder · Powder

AXIS Ultra-DLD XPS with monochromatic Al K alpha source; room temperature.

Temperature: room temperature
Atmosphere: ultrahigh vacuum
Geometry: powder
Context: pristine framework powder
Measurement source: 3 · XPS discussion · Figure S1c

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Mn XPS oxidation-state assignment	Mn 2p3/2 peak at 641.5 eV and satellite at 646.2 eV; Mn 3s splitting 6.2 eV; consistent with MnII	—	—	Text Exact Reported	3 · XPS discussion · Figure S1c