Spectroscopy — An Electrically Conducting Three-Dimensional Iron–Catecholate Porous Framework

7 measurement groups · 30 results

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

Energy-dispersive X-ray spectroscopy (EDX)

Elemental microanalysis and mapping

Pressed Fe-HHTP-MOF pellet · Pellet

EDX analysis of Fe-HHTP pressed pellet at four spots; average composition reported with Si excluded.

Geometry: Pressed pellet
Context: pristine Fe-HHTP-MOF pellet
Measurement source: SI p.6 · Energy-dispersive X-ray analysis of Fe-HHTP pressed pellet · Figure S2; Table S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Elemental analysis carbon found	Found in analysis (%): C, 42.27	42.27 wt %	—	Text Exact Reported	SI p.6 · Elemental Analysis CHNSCl
Elemental analysis hydrogen found	Found in analysis (%): H, 3.25	3.25 wt %	—	Text Exact Reported	SI p.6 · Elemental Analysis CHNSCl
Elemental analysis nitrogen found	Found in analysis (%): N, 1.46	1.46 wt %	—	Text Exact Reported	SI p.6 · Elemental Analysis CHNSCl
EDX average carbon content	C Ave. / exp. Atom % = 62.88	62.88 atom %	—	SI Table Exact Reported	SI p.6 · Energy-dispersive X-ray analysis · Table S2
Average EDX composition without SiMarked as a best value within this paper	C63.1O29.0Fe7.9	—	—	SI Table Exact Reported	SI p.6 · Energy-dispersive X-ray analysis · Table S2
EDX average iron content	Fe Ave. / exp. Atom % = 7.91	7.91 atom %	—	SI Table Exact Reported	SI p.6 · Energy-dispersive X-ray analysis · Table S2
EDX average oxygen content	O Ave. / exp. Atom % = 28.91	28.91 atom %	—	SI Table Exact Reported	SI p.6 · Energy-dispersive X-ray analysis · Table S2

Continuous-wave X-band EPR spectroscopy

Electron paramagnetic resonance

Fe-HHTP-MOF black microcrystalline powder · Powder

JEOL JES-FA200; X-band 8.959 GHz; solid under nitrogen in quartz glass EPR tubes at 293, 95, and 7 K.

Temperature: 7, 95, 293
Atmosphere: nitrogen
Geometry: Powder in quartz EPR tubes
Context: pristine Fe-HHTP-MOF powder
Measurement source: SI p.10-11 · EPR-spectroscopy · Figure S9

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
EPR isotropic g value at 293 KMarked as a best value within this paper	giso = 2.02	2.02	—	Text Exact Reported	SI p.10 · EPR-spectroscopy · Figure S9A
EPR linewidth at 293 K	Wiso = 120 mT	120 mT	—	Text Exact Reported	SI p.10 · EPR-spectroscopy · Figure S9A
EPR linewidth at 7 KMarked as a best value within this paper	Wiso = 315 mT at 7 K	315 mT	—	Text Exact Reported	SI p.10 · EPR-spectroscopy · Figure S9B-C
EPR linewidth at 95 K	Wiso = 155 mT at 95 K	155 mT	—	Text Exact Reported	SI p.10 · EPR-spectroscopy · Figure S9B

Zero-field 57Fe Mossbauer spectroscopy

Mossbauer spectroscopy

Fe-HHTP-MOF black microcrystalline powder · Powder

WissEl MRG-500, 57Co/Rh source, 77 K, constant acceleration mode; isomer shifts versus alpha-iron at 300 K.

Temperature: 77
Geometry: Solid sample
Context: pristine Fe-HHTP-MOF powder
Measurement source: 18069 · Iron Valency · Figure 5A

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Iron valence assignmentMarked as a best value within this paper	single high-spin FeIII coordination site; absence of residual FeII precursor	—	—	Text Qualitative	SI p.10 · Further Information Regarding the Electronic Structure · Figure 5A
57Fe Mossbauer isomer shiftMarked as a best value within this paper	delta = 0.54 mm s^-1	0.54 mm/s	—	Text Exact Reported	18069 · Iron Valency · Figure 5A
57Fe Mossbauer quadrupole splittingMarked as a best value within this paper	DeltaEQ = 0.97 mm s^-1	0.97 mm/s	—	Text Exact Reported	18069 · Iron Valency · Figure 5A

VT-VF SQUID magnetometry

Magnetometry and magnetic susceptibility

Fe-HHTP-MOF black microcrystalline powder · Powder

Quantum Design MPMS-3, 2-300 K, applied DC fields 0.01-7 T; susceptibility corrected for core diamagnetism.

Temperature: 2-300
Geometry: Microcrystalline and powdered samples in polycarbonate gel capsules
Context: pristine Fe-HHTP-MOF powder
Measurement source: SI p.11-12 · Variable temperature - variable field SQUID magnetization studies · Figures S10-S12

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Low-temperature mueff kink	kink at approx. 7 K with magnetic moment 3.23 muB	3.23 muB	approx. 7 K	Text Exact Reported	SI p.12 · VT-VF SQUID magnetization studies · Figure S10
Effective magnetic moment at 2 K and 7 T	1.25 muB (7 T) at 2 K	1.25 muB	—	Text Exact Reported	SI p.11 · VT-VF SQUID magnetization studies · Figures S10-S11
Effective magnetic moment at 2 K low field	1.8 muB (0.01 T) at 2 K	1.8 muB	—	Text Rounded Reported	SI p.11 · VT-VF SQUID magnetization studies · Figures S10-S11
Effective magnetic moment at 300 K	approx. 7.0 muB at 300 K	7 muB	approx.	Text Approximate	SI p.11 · VT-VF SQUID magnetization studies · Figures S10-S11

Total hemispherical reflectance in 8 deg/di geometry

Pressed Fe-HHTP-MOF pellet · Pellet

Agilent Cary 5000 with external diffuse reflectance accessory eDRA; 150 mm integrating sphere; gloss component included; two-step measurement relative to PTFE and grey standards.

Geometry: Pelletised sample, mechanically pressed 3 mm thickness and manually prepared doubled-thickness sample.
Context: pristine Fe-HHTP-MOF pellet
Measurement source: SI p.2-3 · Total Hemispherical reflectance in geometry 8 deg/di · Figure 4C

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Total absorption over UV/Vis/NIR regionMarked as a best value within this paper	98.5%	98.5 %	—	Text Exact Reported	18069 · Photophysical Properties · Figure 4C
Low spectral reflectance to 800 nmMarked as a best value within this paper	not more than 0.015 over the whole visible spectrum up to 800 nm	1.5 %	upper bound	Caption Exact Reported	18068 · Photophysical Properties · Figure 4C
Maximum visible reflectance	less than 3% in the visible spectrum	3 %	upper bound	Text Rounded Reported	18069 · Photophysical Properties · Figure 4C

UV-Vis-NIR diffuse reflectance / Kubelka-Munk absorption and Tauc analysis

UV-visible and optical absorption spectroscopy

Fe-HHTP-MOF black microcrystalline powder · Powder

PerkinElmer Lambda 1050 with 150 mm InGaAs integrating sphere; Praying Mantis diffuse-reflectance accessory; BaSO4 white standard.

Geometry: Powder diffuse reflectance
Context: pristine Fe-HHTP-MOF powder
Measurement source: 18068-18069 · Photophysical Properties · Figure 4A-B

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Broad-band absorption upper wavelengthMarked as a best value within this paper	475 up to 1900 nm	1900 nm	range upper bound	Caption Range	18068 · Photophysical Properties · Figure 4
Broad-band absorption lower wavelength	475 up to 1900 nm	475 nm	range lower bound	Caption Range	18068 · Photophysical Properties · Figure 4
Direct optical band gap from Tauc plotMarked as a best value within this paper	1.09 eV	1.09 eV	—	Caption Exact Reported	18068 · Photophysical Properties · Figure 4B
Absorption onset	onset at 1400 nm	1400 nm	—	Text Rounded Reported	18068-18069 · Photophysical Properties · Figure 4
UV-Vis-NIR local maximum 1	local maxima at 380 nm	380 nm	—	Text Exact Reported	18068 · Photophysical Properties · Figure 4A
UV-Vis-NIR local maximum 2	local maxima at 950 nm	950 nm	—	Text Exact Reported	18068 · Photophysical Properties · Figure 4A

X-ray photoelectron spectroscopy (XPS)

X-ray photoelectron spectroscopy

Pressed Fe-HHTP-MOF pellet · Pellet

ESCALAB 250 Xi, monochromated Al Kalpha 1486.6 eV, 500 um spot, survey pass energy 200 eV, high-resolution pass energy 10 eV.

Geometry: Compressed Fe-HHTP-MOF pellet surface
Context: pristine Fe-HHTP-MOF pellet
Measurement source: SI p.3 and p.8 · X-ray photoelectron spectroscopy · Figure S6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Boron impurity check	No boron impurities detected	—	—	Caption Qualitative	SI p.8 · X-ray photoelectron spectroscopy · Figure S6A
XPS O 1s component hydroxyl	O 1s at 530.04 eV	530.04 eV	—	Caption Exact Reported	SI p.8 · X-ray photoelectron spectroscopy · Figure S6C
XPS O 1s component water/powder oxygen	O 1s at 531.28 eV	531.28 eV	—	Caption Exact Reported	SI p.8 · X-ray photoelectron spectroscopy · Figure S6C