Spectroscopy — Uninterrupted π-d Conjugated Three-Dimensional Conductive Metal-Organic Framework

5 measurement groups · 13 results

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

As-synthesised Ni3HBC greenish-black nanocrystalline powder · Powder

Shimadzu UV-3600, 400-2600 nm; Ni3HBC blended with BaSO4 and pelletized; BaSO4 background subtraction; UVProbe conversion.

Geometry: Flattened powder/BaSO4 pellet on sample holder.
Context: pristine Ni3HBC
Measurement source: S5 · Diffuse-reflectance ultraviolet-visible absorption spectroscopy (DRUV-vis) · Figure 3d

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
DRUV-vis intense band	intense band at 1000-1400 nm	—	—	Text Range	2059 · Photophysical properties · Figure 3d
Optical bandgap from Tauc plotMarked as a best value within this paper	0.64 eV	—	—	Text Rounded Reported	2059 · Photophysical and transport properties · Figure 3d inset

As-synthesised Ni3HBC greenish-black nanocrystalline powder · Powder

Bruker BioSpin spectrometer at 110 K; X-band 9.4 GHz, microwave power 2.14 mW, modulation frequency 100 kHz, amplitude 4 G.

Temperature: 110
Context: pristine Ni3HBC compared with HBC and Ni(OAc)2 references.
Measurement source: S5 · Electron Paramagnetic Resonance (EPR) · Figure 3e; Figure S11

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
EPR g valueMarked as a best value within this paper	g = 2.002 at 110 K	—	—	Text Exact Reported	2059 · EPR spectroscopy · Figure 3e

As-synthesised Ni3HBC greenish-black nanocrystalline powder · Powder

FT-IR in Ar glovebox on ATR pellet, 400-4000 cm-1, 2 cm-1 resolution; Raman compared Ni acetate, HBC and Ni3HBC.

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
FT-IR OH stretching reduction	Reduced OH stretching vibration near 3300 cm-1 in Ni3HBC compared with HBC	—	near	Text Approximate	2057 · Synthesis and characterisation · Figure S1
Raman Ni-O stretching bandMarked as a best value within this paper	Ni-O stretching band at 522 cm-1	—	—	Text Rounded Reported	2057 · Synthesis and characterisation · Figure S2

As-synthesised Ni3HBC greenish-black nanocrystalline powder · Powder

PAL 8C beamline at Ni K-edge (8.333 keV); 4.0-22.0 keV; transmittance mode; Ni foil calibration; Athena/Artemis Demeter 0.9.26.

Geometry: Powder packed and sealed with Kapton tape.
Context: pristine Ni3HBC framework compared with Ni foil, NiO, NiPc and Ni9(HHTP)4 references.
Measurement source: S4 · X-ray absorption fine structure (XAFS) · Figure 3b-c; Table S2; Figure S7

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
EXAFS Ni-O1 coordination number	C.N. = 2.43428 +/- 0.24152	—	+/-0.24152	SI Table Exact Reported	S11 · Table S2 · Table S2
EXAFS Ni-O1 distanceMarked as a best value within this paper	R = 1.96967 +/- 0.01166 Angstrom	—	+/-0.01166 Angstrom	SI Table Exact Reported	S11 · Table S2 · Table S2
EXAFS Ni-O2 coordination number	C.N. = 5.46861 +/- 0.24179	—	+/-0.24179	SI Table Exact Reported	S11 · Table S2 · Table S2
EXAFS Ni-O2 distanceMarked as a best value within this paper	R = 2.09755 +/- 0.00811 Angstrom	—	+/-0.00811 Angstrom	SI Table Exact Reported	S11 · Table S2 · Table S2
Ni oxidation-state assignment by XANES	White line peak similar to NiO, indicating Ni2+; similar to Ni9(HHTP)4	—	—	Text Qualitative	2058 · Spectroscopic analyses · Figure 3b

As-synthesised Ni3HBC greenish-black nanocrystalline powder · Powder

PAL 10A2 beamline; Au 4f calibration; aromatic carbon aligned to 284.8 eV; CasaXPS fitting with Shirley background and Gaussian-Lorentzian functions.

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni 2p1/2 XPS main peak	874.3 eV	—	—	Text Rounded Reported	2058 · Spectroscopic analyses · Figure 3a
Ni 2p3/2 XPS main peak	856.7 eV	—	—	Text Rounded Reported	2058 · Spectroscopic analyses · Figure 3a
Ni 2p XPS shakeup satellite	862.2 eV	—	—	Text Rounded Reported	2058 · Spectroscopic analyses · Figure 3a