Spectroscopy — A Rationally Designed Iron–Dihydroxybenzoquinone Metal–Organic Framework as Practical Cathode Material for Rechargeable Batteries

6 measurement groups · 46 results

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

Energy-dispersive spectroscopy

air-stabilised Fe2(DHBQ)3 powder · Powder

EDS elemental composition of Fe2(DHBQ)3 powder.

Context: pristine powder
Measurement source: 428 · 2.1. Synthesis and characterization · Fig. S8

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
C atomic percent by EDS	C 59.0%	—	—	Text Exact Reported	428 · 2.1 · Fig. S8
Fe atomic percent by EDS	Fe 6.7%	—	—	Text Exact Reported	428 · 2.1 · Fig. S8
Fe/O/C atomic ratio	Fe/O/C = 1:5.1:8.8 (Fe 6.7%, O 34.3%, C 59.0%)	—	—	Text Exact Reported	428 · 2.1 · Fig. S8
O atomic percent by EDS	O 34.3%	—	—	Text Exact Reported	428 · 2.1 · Fig. S8

Ex-situ FTIR and O 1s XPS of electrodes in pristine/discharged/recharged states

Infrared spectroscopy X-ray photoelectron spectroscopy

Fe2(DHBQ)3 electrode A/default (AM/KB/PTFE = 6:3:1, low loading) · Electrode

Li cells discharged to 1.5 V or charged to 3.8 V at specified cycle; electrodes rinsed/dried. FTIR KBr pellet; XPS sealed under Ar before characterisation.

Atmosphere: post-mortem glovebox handling
Geometry: composite electrode film
Context: cycled composite electrode
Measurement source: 431 · 2.4. Redox reaction mechanism · Fig. 4a,b

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
C=O FTIR peak after discharge	1500 cm-1 red-shifted to 1480 cm-1 after discharge to 1.5 V	—	—	Text Exact Reported	431 · 2.4 · Fig. 4a
New FTIR peak in recharged electrode	1202 cm-1	—	—	Text Exact Reported	431 · 2.4 · Fig. 4a
Second new FTIR peak in recharged electrode	1141 cm-1	—	—	Text Exact Reported	431 · 2.4 · Fig. 4a
O 1s C-O binding energy	532.4 eV	—	—	Text Exact Reported	431 · 2.4 · Fig. 4b
O 1s C=O binding energy	531.0 eV	—	—	Text Exact Reported	431 · 2.4 · Fig. 4b
Pristine C=O/C-O areal ratio	3.1	—	—	Text Exact Reported	431 · 2.4 · Fig. 4b
C=O/C-O areal ratio after recharging	2.2 after recharging; pristine ratio 3.1	—	—	Text Exact Reported	431 · 2.4 · Fig. 4b

Ex-situ 57Fe Mossbauer spectroscopy of electrodes

Mossbauer spectroscopy

Fe2(DHBQ)3 electrode A/default (AM/KB/PTFE = 6:3:1, low loading) · Electrode

Discharged and recharged electrodes compared with pristine powder; 77 K.

Temperature: 77
Atmosphere: post-mortem
Geometry: composite electrode
Context: cycled composite electrode
Measurement source: 28 · Supporting Information · Table S4, Fig. 4c

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Fe3+ fraction after discharge	Ferric percentage = 56.3% after discharging	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Fe3+ fraction after recharge	Ferric percentage = 66.0% after recharging	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Subsequent discharge product at 2.5-1.5 V	(Li+)6.9(Fe2+)0.9(Fe3+)1.1(DHBQ4-)3	—	—	Text Qualitative	431 · 2.4 · Fig. 4f
First-discharge intermediate above 2.5 V	(Li+)1.8(Fe2+)0.9(Fe3+)1.1(DHBQ2.3-)3	—	—	Text Qualitative	431 · 2.4 · Fig. 4f
Irreversible electron number per formula unit	1.3 electrons	—	—	Text Exact Reported	431 · 2.4 · Fig. 4f
Recharge stable phase	(Li+)1.3(Fe2+)0.7(Fe3+)1.3(DHBQ2.2-)3	—	—	Text Qualitative	431 · 2.4 · Fig. 4f
Reversible electron number per formula unit	5.6 electrons	—	—	Text Exact Reported	431 · 2.4 · Fig. 4f
Theoretical irreversible capacity from mechanism	62 mAh g-1	—	—	Calculated From Reported Rounded Reported	431 · 2.4 · Fig. 4f
Theoretical reversible capacity from mechanism	267 mAh g-1	—	—	Calculated From Reported Rounded Reported	431 · 2.4 · Fig. 4f
Mossbauer Isomer shift: Discharged electrode Ferric	Discharged electrode Ferric Isomer shift = 0.556 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Linewidth: Discharged electrode Ferric	Discharged electrode Ferric Linewidth = 0.484 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Percentage: Discharged electrode Ferric	Discharged electrode Ferric Percentage = 56.3 %	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Quadrupole splitting: Discharged electrode Ferric	Discharged electrode Ferric Quadrupole splitting = 0.823 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Isomer shift: Discharged electrode Ferrous	Discharged electrode Ferrous Isomer shift = 1.158 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Linewidth: Discharged electrode Ferrous	Discharged electrode Ferrous Linewidth = 0.484 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Percentage: Discharged electrode Ferrous	Discharged electrode Ferrous Percentage = 43.7 %	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Quadrupole splitting: Discharged electrode Ferrous	Discharged electrode Ferrous Quadrupole splitting = 2.573 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Isomer shift: Recharged electrode Ferric	Recharged electrode Ferric Isomer shift = 0.539 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Linewidth: Recharged electrode Ferric	Recharged electrode Ferric Linewidth = 0.435 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Percentage: Recharged electrode Ferric	Recharged electrode Ferric Percentage = 66 %	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Quadrupole splitting: Recharged electrode Ferric	Recharged electrode Ferric Quadrupole splitting = 0.987 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Isomer shift: Recharged electrode Ferrous	Recharged electrode Ferrous Isomer shift = 1.218 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Linewidth: Recharged electrode Ferrous	Recharged electrode Ferrous Linewidth = 0.435 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Percentage: Recharged electrode Ferrous	Recharged electrode Ferrous Percentage = 34 %	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Quadrupole splitting: Recharged electrode Ferrous	Recharged electrode Ferrous Quadrupole splitting = 2.742 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4

FTIR using KBr pellets

Infrared spectroscopy

air-stabilised Fe2(DHBQ)3 powder · Powder

Comparison of DHBQ ligand and Fe2(DHBQ)3 powder.

Context: pristine powder
Measurement source: 428 · 2.1. Synthesis and characterization · Fig. 1c

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
C=O FTIR red-shift after coordination	1620 cm-1 (DHBQ) red-shifted to 1500 cm-1 (Fe2(DHBQ)3)	—	—	Text Exact Reported	428 · 2.1 · Fig. 1c
DHBQ C-O-H FTIR peak	1125 cm-1 for C-O-H group in DHBQ	—	—	Text Exact Reported	428 · 2.1 · Fig. 1c
DHBQ O-H FTIR peak	3302 cm-1 for O-H group in DHBQ	—	—	Text Exact Reported	428 · 2.1 · Fig. 1c
absorbed water FTIR peak	broad peak at 3450 cm-1	—	—	Text Exact Reported	428 · 2.1 · Fig. 1c

57Fe Mossbauer spectroscopy

Mossbauer spectroscopy

air-stabilised Fe2(DHBQ)3 powder · Powder

Recorded at 77 K; symmetric Lorentzian quadrupole doublets.

Temperature: 77
Context: pristine powder
Measurement source: 428 · 2.1. Synthesis and characterization · Fig. 1e

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Pristine Fe isomer shift at 77 K	IS77K = 0.464 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Isomer shift: Pristine powder Ferric	Pristine powder Ferric Isomer shift = 0.464 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Linewidth: Pristine powder Ferric	Pristine powder Ferric Linewidth = 0.575 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Percentage: Pristine powder Ferric	Pristine powder Ferric Percentage = 100 %	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4
Mossbauer Quadrupole splitting: Pristine powder Ferric	Pristine powder Ferric Quadrupole splitting = 0.801 mm s-1	—	—	SI Table Exact Reported	28 · Supporting Information · Table S4

XPS survey and fitted O 1s/Fe 2p spectra

X-ray photoelectron spectroscopy

air-stabilised Fe2(DHBQ)3 powder · Powder

K-Alpha+ spectrometer, Al Kalpha X-ray source.

Context: pristine powder
Measurement source: 428 · 2.1. Synthesis and characterization · Fig. 1d, Fig. S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
XPS detected elements	Only C, O, and Fe; no Cl signal	—	—	Qualitative Qualitative	428 · 2.1 · Fig. 1d