Spectroscopy — Electrically Conductive 3D Metal-Organic Framework Featuring π-Acidic Hexaazatriphenylene Hexacarbonitrile Ligands with Anion-πInteraction and Efficient Charge-Transport Capabilities

5 measurement groups · 13 results

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

solid-state EPR with quantitative spin integration

Electron paramagnetic resonance

Evacuated [Ag2(HATHCN)(CF3SO3)2]n bulk material · Powder

Bruker EMX EPR X-band at room temperature; 70 mg evacuated MOF powder in 4 mm quartz tube; calibrated using DPPH.

Temperature: 293
Atmosphere: not reported
Geometry: powder in quartz tube
Context: pristine framework
Measurement source: S-3 · EPR Analysis and Spin Quantification · Figure 2a

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
EPR g value	g = 1.997	—	—	Caption Exact Reported	p014 · Figure 2 caption · Figure 2a
Unpaired electron per partially reduced HATHCN ligand	ca. 0.1 spin per HATHCN ligand	—	—	Text Approximate	p006 · Redox and Optical Properties · Figure 2a
Spin concentration per mass	8.4 × 10^16 spins/mg	—	—	Text Exact Reported	p006 · Redox and Optical Properties · Figure 2a
Spin concentration per mole	3.8 × 10^22 spins/mol	—	—	Text Exact Reported	p006 · Redox and Optical Properties · Figure 2a

13C NMR, MALDI-TOF MS, FTIR

Infrared spectroscopy Nuclear magnetic resonance

Free HATHCN ligand powder/crystals · Powder

Ligand identity checks reported in SI after literature synthesis.

Context: molecular control
Measurement source: S-2 · Ligand and MOF Synthesis · Figure S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Free HATHCN C≡N stretch	2241 cm-1	—	—	Text Exact Reported	S-2 · Ligand and MOF Synthesis · Figure S4
HATHCN MALDI-TOF found m/z	384.13	—	—	Text Exact Reported	S-2 · Ligand and MOF Synthesis
HATHCN 13C NMR resonance	114.61 ppm	—	—	Text Exact Reported	S-2 · Ligand and MOF Synthesis · Figure S1

FTIR and XPS

Infrared spectroscopy X-ray photoelectron spectroscopy

Evacuated [Ag2(HATHCN)(CF3SO3)2]n bulk material · Powder

FTIR shows Ag-HATHCN coordination by C≡N red-shift; XPS survey shows expected Ag, C, N, O, F, S elements.

Atmosphere: ambient
Geometry: powder
Context: pristine framework
Measurement source: p004-p005 · Syntheses and Crystal Structures · Figures S4-S5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
MOF C≡N stretch	2161 cm-1 in main text; 2162 cm-1 in SI synthesis characterisation	—	—	Text Exact Reported	p004-p005 · Syntheses and Crystal Structures · Figure S4
MOF XPS survey elements	Ag+, C, N, O, F, and S peaks	—	—	Text Qualitative	p005 · Syntheses and Crystal Structures · Figure S5

UV-vis-NIR diffuse-reflectance spectroscopy and Tauc analysis

UV-visible and optical absorption spectroscopy

Evacuated [Ag2(HATHCN)(CF3SO3)2]n bulk material · Powder

MOF UV-vis-NIR diffuse-reflectance spectrum; sample mixed with BaSO4 (30% by weight) per SI, with Figure 2b red trace described as MOF film; direct-transition optical band gap from Tauc plot.

Atmosphere: ambient
Geometry: powder/film diffuse reflectance
Context: pristine framework
Measurement source: S-2 · General Materials and Methods · Figure 2b

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
MOF NIR radical-anion absorption	additional NIR peak corresponding to HATHCN radical-anion absorption	—	—	Text Qualitative	p006 · Redox and Optical Properties · Figure 2b
MOF optical band gap	Eg ~ 1.3 eV	—	—	Text Approximate	p006 · Redox and Optical Properties · Figure 2b inset

UV-vis-NIR diffuse-reflectance spectroscopy and Tauc analysis

UV-visible and optical absorption spectroscopy

Free HATHCN ligand powder/crystals · Powder

Free HATHCN control diffuse-reflectance spectrum; sample mixed with BaSO4 (30% by weight); direct-transition optical band gap from Tauc plot.

Atmosphere: ambient
Geometry: powder diffuse reflectance
Context: molecular ligand control
Measurement source: S-2 · General Materials and Methods · Figure 2b

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Free HATHCN optical band gap	Eg ~ 2.1 eV	—	—	Text Approximate	p006 · Redox and Optical Properties · Figure 2b inset
Free HATHCN characteristic absorption peak	ca. 420 nm	—	—	Text Approximate	p006 · Redox and Optical Properties · Figure 2b