Spectroscopy — Mechanistic Evidence for Ligand-Centered Electrocatalytic Oxygen Reduction with the Conductive MOF Ni3(hexaiminotriphenylene)2

Measurement evidence

Spectroscopy

Mechanistic Evidence for Ligand-Centered Electrocatalytic Oxygen Reduction with the Conductive MOF Ni3(hexaiminotriphenylene)2 · Miner E.M., Gul S., Ricke N.D. et al. · ACS Catalysis · 2017 · 7726-7731

1 measurement group · 11 results

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

Ni K-edge XANES/EXAFS

X-ray absorption spectroscopy

Ni3(HITP)2 film on ITO-coated PET electrode · Electrode

in situ ORR experiment in 0.1 M aqueous KOH with O2 bubbled; SSRL beamline 9-3; fluorescence mode for in situ ORR

Atmosphere: O2
Geometry: Ni3(HITP)2-coated ITO/PET substrate in two-compartment glass cell
Context: pristine conductive MOF film
Measurement source: S8-S10 · In-situ X-ray absorption spectroscopy · Figure 5, Table S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
EXAFS as-prepared Ni-C distance	2.71 +/- 0.01 Angstrom; N = 4	—	+/-0.01	SI Table Exact Reported	S24 · Additional Figures · Table S3
EXAFS as-prepared Ni-N distance	1.84 +/- 0.01 Angstrom; N = 4	—	+/-0.01	SI Table Exact Reported	S24 · Additional Figures · Table S3
EXAFS as-prepared R-factor	0.81%	—	—	SI Table Exact Reported	S24 · Additional Figures · Table S3
Interlayer distance used in slipped-parallel EXAFS model	3.33 Angstrom	—	—	Text Exact Reported	S10-S11 · XAS methods
EXAFS ORR Ni-C distance	2.71 +/- 0.01 Angstrom; N = 4	—	+/-0.01	SI Table Exact Reported	S24 · Additional Figures · Table S3
EXAFS ORR Ni-N distance	1.84 +/- 0.01 Angstrom; N = 4	—	+/-0.01	SI Table Exact Reported	S24 · Additional Figures · Table S3
EXAFS ORR R-factor	1.15%	—	—	SI Table Exact Reported	S24 · Additional Figures · Table S3
Ni(OH)2 path contribution in EXAFS fit	only ~5% of Ni sites	—	~	Text Approximate	S10-S11 · XAS methods
Ni oxidation state during catalysis	Ni remains in the +2 oxidation state throughout catalysis	—	—	Text Exact Reported	7728 · Results and Discussion · Figure 5a
Ni3(HITP)2 rising edge energy	8343.7 eV at half-height	—	—	Text Exact Reported	7728 · Results and Discussion · Figure 5a
Ni(II) phthalocyanine rising edge energy	8344.1 eV	—	—	Text Exact Reported	7728 · Results and Discussion · Figure 5a