Spectroscopy — Controlling the Thermoelectric Properties of Organometallic Coordination Polymers via Ligand Design

13 measurement groups · 40 results

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

EPR spectroscopy

Electron paramagnetic resonance

purified Ni-btt powder · Powder

77 K EMX X-band (~10 GHz) spectrometer; spin concentration estimated against CuSO4 x 5 H2O standard.

Temperature: 77
Context: pristine purified powder
Measurement source: 20 · General Experimental / Table S4 · Table S4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-btt EPR g1	2.015	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-btt EPR g2	2.050	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-btt EPR g3	2.178	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-btt moment per repeat unit	0.09 muB	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-btt EPR spin concentration	1.3 x 10^21 /mol	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4

EPR spectroscopy

Electron paramagnetic resonance

purified Ni-diett powder · Powder

77 K EMX X-band (~10 GHz) spectrometer; spin concentration estimated against CuSO4 x 5 H2O standard.

Temperature: 77
Context: pristine purified powder
Measurement source: 20 · General Experimental / Table S4 · Table S4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-diett EPR g1	2.003	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-diett EPR g2	2.025	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-diett EPR g3	2.047	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-diett moment per repeat unit	0.06 muB	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-diett EPR spin concentration	7.0 x 10^20 /mol	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4

EPR spectroscopy

Electron paramagnetic resonance

purified Ni-ett powder · Powder

77 K EMX X-band (~10 GHz) spectrometer; spin concentration estimated against CuSO4 x 5 H2O standard.

Temperature: 77
Context: pristine purified powder
Measurement source: 20 · General Experimental / Table S4 · Table S4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-ett EPR zero-field splitting parameter	b02 approximately 0.314 cm-1	—	—	Text Approximate	20 · Table S4 · Table S4
Ni-ett moment per repeat unit	0.50 muB	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-ett EPR spin concentration	4.0 x 10^22 /mol	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
Ni-ett EPR spin state	S = 1	—	—	SI Table Exact Reported	S20 · Table S4 · Table S4
OMCP spin concentration range	10^20 to 10^22 spin per mole; around one per hundredth repeat unit	—	—	Text Range	6 · 2.3 Electronic Structure Characterization · Table S4 referenced

EPR spectroscopy and SQUID magnetometry

Electron paramagnetic resonance Magnetometry and magnetic susceptibility

purified Ni-ett powder · Powder

First-derivative EPR spectra at 77 K; SQUID M-T curves and M-H hysteresis at 2 K.

Temperature: 77 K EPR; 2 K M-H inset; M-T variable temperature
Context: purified pristine OMCP powders
Measurement source: 6 · 2.3 Electronic Structure Characterization · Figure 3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source

ATR-FTIR and resonance Raman spectroscopy

Infrared spectroscopy Raman spectroscopy

purified Ni-ett powder · Powder

FTIR and Raman spectra of all three purified OMCPs after purification.

Context: purified pristine OMCP powders
Measurement source: 4 · 2.2 Compositional and Structural Characterization · Figure 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-diett FTIR C=S radical modes	split peak at 1173-1142 cm-1 and weaker peak at 1038 cm-1	—	—	Text Range	4 · 2.2 · Figure 2
Ni-ett FTIR C=S radical modes	1163 and 1074 cm-1	—	—	Text Exact Reported	4 · 2.2 · Figure 2
Raman thiocarbonyl radical split peaks	Ni-ett and Ni-diett split peaks at 1158 and 1186 cm-1	—	—	Text Exact Reported	5 · 2.2 · Figure 2

Ultraviolet photoelectron spectroscopy (UPS)

Ultraviolet photoelectron spectroscopy

purified Ni-btt powder · Powder

Work functions and densities of valence electronic states measured for purified OMCPs.

Context: purified pristine OMCP powders
Measurement source: 5 · 2.3 Electronic Structure Characterization · Figure S15 referenced

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source

Ultraviolet photoelectron spectroscopy (UPS)

Ultraviolet photoelectron spectroscopy

purified Ni-btt powder · Powder

Thermo Scientific Theta-Probe spectrometer, He I = 21.22 eV; work functions/densities of valence states.

Context: pristine purified powder
Measurement source: 20 · General Experimental / Figure S15 · Figure S15

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-btt work function	4.9 eV	—	—	Text Exact Reported	5 · 2.3 Electronic Structure Characterization · Figure S15

Ultraviolet photoelectron spectroscopy (UPS)

Ultraviolet photoelectron spectroscopy

purified Ni-diett powder · Powder

Thermo Scientific Theta-Probe spectrometer, He I = 21.22 eV; work functions/densities of valence states.

Context: pristine purified powder
Measurement source: 20 · General Experimental / Figure S15 · Figure S15

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-diett work function	4.6 eV	—	—	Text Exact Reported	5 · 2.3 Electronic Structure Characterization · Figure S15

Ultraviolet photoelectron spectroscopy (UPS)

Ultraviolet photoelectron spectroscopy

purified Ni-ett powder · Powder

Thermo Scientific Theta-Probe spectrometer, He I = 21.22 eV; work functions/densities of valence states.

Context: pristine purified powder
Measurement source: 20 · General Experimental / Figure S15 · Figure S15

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-ett work function	4.7 eV	—	—	Text Exact Reported	5 · 2.3 Electronic Structure Characterization · Figure S15

X-ray photoelectron spectroscopy (XPS)

X-ray photoelectron spectroscopy

purified Ni-ett powder · Powder

Comparison of pristine/nonpurified and Soxhlet-purified OMCPs; main text gives peak assignments and impurity removal.

Context: purified framework compared with nonpurified polymer
Measurement source: 3 · 2.2 Compositional and Structural Characterization

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Na 1s impurity removal	Na 1s peak at 1071 eV completely disappeared after purification; XRF confirmed absence of Na in all three OMCPs	—	—	Text Rounded Reported	3 · 2.2
Ni 2p peak assignment	Ni 2p3/2 at 853 eV and Ni 2p1/2 at 873 eV assigned to Ni2+ species	—	—	Text Rounded Reported	3 · 2.2
S 2p Ni-S complexation peaks	Main S 2p peaks at 161.9 and 163.3 eV from complexation between Ni and S	—	—	Text Exact Reported	3 · 2.2
Sulfur oxidation peak	Weak S 2p peak at 168.3 eV before purification; aged Ni-ett showed intense peak around 168.5 eV after air exposure	—	—	Text Exact Reported	3 · 2.2

Energy-dispersive X-ray fluorescence (ED-XRF)

Elemental microanalysis and mapping Bulk elemental and compositional analysis

purified Ni-btt powder · Powder

Inert helium atmosphere using Malvern Panalytical Epsilon 4; quantified element wt% and at%.

Atmosphere: inert helium
Context: pristine purified powder
Measurement source: 15 · General Experimental / Table S2 · Table S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-btt XRF Ni at%	20.5	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-btt XRF Ni wt%	34.5	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-btt XRF S at%	67.9	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-btt XRF S/Ni	3.31	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-btt XRF S wt%	62.5	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2

Energy-dispersive X-ray fluorescence (ED-XRF)

Elemental microanalysis and mapping Bulk elemental and compositional analysis

purified Ni-diett powder · Powder

Inert helium atmosphere using Malvern Panalytical Epsilon 4; quantified element wt% and at%.

Atmosphere: inert helium
Context: pristine purified powder
Measurement source: 15 · General Experimental / Table S2 · Table S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-diett XRF Ni at%	10.7	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-diett XRF Ni wt%	19.7	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-diett XRF S at%	78.4	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-diett XRF S/Ni	7.33	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-diett XRF S wt%	79.1	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2

Energy-dispersive X-ray fluorescence (ED-XRF)

Elemental microanalysis and mapping Bulk elemental and compositional analysis

purified Ni-ett powder · Powder

Inert helium atmosphere using Malvern Panalytical Epsilon 4; quantified element wt% and at%.

Atmosphere: inert helium
Context: pristine purified powder
Measurement source: 15 · General Experimental / Table S2 · Table S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-ett XRF Ni at%	22.7	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-ett XRF Ni wt%	37.5	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-ett XRF S at%	68.3	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-ett XRF S/Ni	3.01	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2
Ni-ett XRF S wt%	61.6	—	—	SI Table Exact Reported	S15 · Table S2 · Table S2