Spectroscopy — Semiconducting neutral microstructures fabricated by coordinative self-assembly of intramolecular charge-transfer tetrathiafulvalene derivatives

4 measurement groups · 19 results

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

Solution UV/Vis and 1H NMR binding analysis of compound 1 with Pb(ClO4)2 and Zn(ClO4)2

UV-visible and optical absorption spectroscopy Nuclear magnetic resonance

compound 1 plus Pb2+ or Zn2+ solution binding samples · Model

Solution UV/Vis Job plots and spectra plus 1H NMR titrations of compound 1 with Pb(ClO4)2 or Zn(ClO4)2; addition of metal salt changed colour from yellow to deep purple.

Context: model binding data supporting target coordination-polymer formation
Measurement source: S3-S7 · Supporting Information · Figures S1-S5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
compound 1 to metal ion binding ratio	1:1	—	—	Text Exact Reported	S3-S4 · Supporting Information · Figures S1-S2
binding constant log Ks for compound 1 with Pb2+	log Ks up to 5.57 for Pb2+	—	—	Text Exact Reported	5125 · Results and Discussion · Figure S1 referenced
binding constant log Ks for compound 1 with Zn2+	log Ks = 4.44 for Zn2+	—	—	Text Exact Reported	S5 · Supporting Information · Figure S3
total concentration for Pb2+ Job plot of compound 1	[Pb2+] + [1] = 1.2 x 10-4 mol dm-3	0.00012 mol L-1	—	Caption Exact Reported	S3 · Supporting Information · Figure S1
total concentration for Zn2+ Job plot of compound 1	[Zn2+] + [1] = 8.6 x 10-5 mol dm-3	0.000086 mol L-1	—	Caption Exact Reported	S4 · Supporting Information · Figure S2
Zn2+-induced absorption growth wavelength for compound 1	growth at 525 nm at the expense of absorption at 432 nm	—	—	Text Exact Reported	S5 · Supporting Information · Figure S3
Zn2+ UV/Vis titration isosbestic points for compound 1	475, 383, and 324 nm	—	—	Text Exact Reported	S5 · Supporting Information · Figure S3
compound 1 concentration in Zn2+ UV/Vis titration	1 (4.3 x 10-5 mol dm-3) in CH3CN	0.000043 mol L-1	—	Caption Exact Reported	S5 · Supporting Information · Figure S3
Zn2+ concentration range in compound 1 UV/Vis titration	[Zn2+]: 0 -> 4.3 x 10-5 mol dm-3	—	—	Caption Range	S5 · Supporting Information · Figure S3
new absorption growth range after Pb2+ or Zn2+ addition	500-600 nm	—	—	Text Range	5125 · Results and Discussion

UV/Vis and NMR spectra plus morphology comparison

UV-visible and optical absorption spectroscopy Nuclear magnetic resonance

compound 3 plus Pb2+ micro-nest-like structures · Powder

Pb2+ binding to triple-bond compound 3 was compared with compound 1; micro-nest-like structures were observed instead of microwires.

Context: model-system control
Measurement source: 5126-5127 · Results and Discussion · Figures S10-S12 referenced

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
binding constant log Ks for compound 3 with Pb2+	log Ks = 3.44 for 3	—	—	Text Exact Reported	5127 · Results and Discussion · Figures S11-S12 referenced
Pb2+ to compound 3 ratio	1:1 ratio of Pb2+ to 3	—	—	Text Exact Reported	5127 · Results and Discussion
compound 3 synthesis yield	yield 62%	—	—	Text Exact Reported	5128 · Experimental Section

Solid-state X-band ESR spectroscopy

Electron paramagnetic resonance

TTF-Pb coordination-polymer microwires · Powder

Solid-state ESR spectra recorded at 298 K; g value calibrated by DPPH. Figure 4 compares microwires and spherical particles.

Temperature: 298
Context: target coordination-polymer samples and controls
Measurement source: 5127-5128 · Results and Discussion / Experimental Section · Figure 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
ESR g value for coordination-polymer stacks	g value of 2.008 at 298 K	—	—	Text Exact Reported	5127 · Results and Discussion · Figure 4
ESR A/B ratio for TTF-Pb microwires	A/B approaches to 1.4 for the TTF microwires	—	—	Text Rounded Reported	5127-5128 · Results and Discussion · Figure 4
ESR A/B ratio for TTF-Zn spherical particles	1.3 for the spherical particles	—	—	Text Rounded Reported	5128 · Results and Discussion · Figure 4

FT-IR spectroscopy

Infrared spectroscopy

TTF-Pb coordination-polymer microwires · Powder

KBr IR spectra recorded before and after polymer formation; coordination inferred from C=N and C=C stretch shifts and ClO4- band.

Context: pristine Pb2+-linked target sample
Measurement source: 5126 · Results and Discussion · Figure S6 referenced

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
ClO4- FT-IR band	1116 cm-1	—	—	Text Exact Reported	5126 · Results and Discussion · Figure S6 referenced
C=C stretch shift on Pb coordination	1534 to 1493 cm-1	—	—	Text Exact Reported	5126 · Results and Discussion · Figure S6 referenced
C=N stretch shift on Pb coordination	1552 to 1526 cm-1	—	—	Text Exact Reported	5126 · Results and Discussion · Figure S6 referenced