Abstract
Electronic and geometrical structures of NO-Na+ and Cu(I)-NO complexes formed in zeolites are discussed based on the g and the 14N and 23Na hf values evaluated by multi-frequency ESR, pulsed ENDOR and HYSCORE methods. The structure of (NO)2 bi-radical formed in zeolites is discussed based on X- and Q-band ESR spectra. Microenvironment effects on the molecular dynamics and the thermal stability of triethyl- and tripropyl-amine radical cations as spin probes are presented referring to the CW-X-band ESR results and theoretical DFT calculations. X- and Q-band ESR studies on nitrogen-doped TiO2 semiconductor reveal that the diamagnetic N– ion in the system absorbs visible light so as to excite an electron of N– to the conduction band. The photo-catalytic reactions of TiO2 are modified by introducing O2 molecules which scavenge a fraction of photoexcited electrons to generate O2 –. ESR spectral characteristics of adsorbed O2 –, g-tensor and hf structure of labeled 17O (I = 7/2), are presented.
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Appendices
Appendices
1.1 A6.1 Isotropic Hyperfine Splittings of β-Hydrogens
The isotropic hf splitting of β-hydrogens, a β-H, arises, in principle, due to a hyperconjugative mechanism [56b]. To illustrate the general ideas here we consider triethylamine radical cation, (CH3CH2)3N· +, described in Section 6.4. The hydrogens of (CH3CH2)3N· + are conventionally labeled with Greek letters: β for one bonded to carbon adjacent to the π-radical center (α-position; N atom) and γ for a hydrogen one carbon further out as CγH3-CβH2-Nα · +-(CH3CH2)2. It is found experimentally that the β-hydrogen hf splitting is formulated as follows [127]:
where θ is the angle between the unpaired electron 2p z orbital at the π-radical center and the C(β)-H bond and ρ is the spin density on the nitrogen 2p z orbital, see Fig. 6.8(c). Coefficient B reflects the spin density arising from hyperconjugation and should be positive; the positive sign has been confirmed by NMR experiments. On the other hand coefficient A accounts for that arising from orientation-independent mechanisms such as spin polarization. If there is free rotation about the Cβ—Nα bond then we observe an orientationally averaged hf splitting:
Studies of many systems suggest that the value of A is much smaller than B, i.e., less than ca. 0.3 mT and Eq. (6.10) can be approximated as:
From the ESR spectral analysis of (CH3CH2)3N· + in AlPO4-5 the following isotropic hf splittings have been identified: a β-H = 2.0 mT for six equivalent β-hydrogens at 300 K corresponding to an averaged structure and a β-H = 3.6 mT for three equivalent hydrogens, one from each β-methylene group, at a low temperature of 77 K corresponding to a rigid limit structure, see Fig. 6.8(a) and (b). Combining Eq. (6.12) with the experimental β-hydrogen hf splittings at 77 and 300 K, we have the following four equations:
By solving the equations we obtain: Bρ= 6.9 mT, a β H(2) = 0.4 mT, θ(1) = 44° and θ(2) = 76°, see Fig. 6.8(c). Consistent with the experimental result the value evaluated for a βH(2), 0.4 mT, is much smaller than the experimental line-width of 1.2 mT at 77 K and too small to be resolved in the spectrum.
We close this section by repeating that Eq. (6.10) for the angular dependence on β-hydrogens is very useful in discussing geometrical structures (conformations) of not only the amine radical cations exemplified here but also for other many alkyl-type radicals [56b] including those stabilized in organic solid polymers as described in Chapter 7.
1.2 A6.2 Anatase and Rutile TiO2
Titanium dioxide has several polymorphs. Among them, rutile (P42/mnm space group, D 4 h) and anatase (I41/amd space group, D 4 h) are well known from viewpoint of crystal structure [128] and have been intensively studied for photocatalysis. Experimentally, anatase has a slightly larger band gaps than rutile, 3.2 vs. 3.0 eV [129, 130]. Ab-initio calculations show that the primary structural difference between the anatase and rutile phases is that the former is 9% less dense than the latter, and has larger Ti-Ti distances, a more pronounced localization of the Ti 3d states and a narrower 3d band [131]. This can be a reason why the carrier (electron) generated in anatase by UV excitation is less mobile than in rutile. Also the O 2p-Ti 3d hybridization is different in the two structures (more covalent mixing in rutile), with anatase exhibiting a valence and a conduction band with more pronounced O 2p and Ti 3d characters, respectively [131]. In rutile the greater Pauli repulsion among the oxygen 2p electrons results in a larger O 2p bandwidth. Experimentally, the bandwidth in rutile is 6 eV while it is 4.7 eV in anatase [132, 133]. The calculated values are 5.3 and 4.5 eV, respectively; the values nicely reflect the important difference in the electronic structures [105].
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Lund, A., Shiotani, M., Shimada, S. (2011). Applications to Catalysis and Environmental Science . In: Principles and Applications of ESR Spectroscopy. Springer, Dordrecht. https://doi.org/10.1007/978-1-4020-5344-3_6
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