Spin Density Distribution after Electron Transfer from Triethylamine to an [Ir(ppy) 2 (bpy)] + Photosensitizer during Photocatalytic Water Reduction
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1 Spin Density Distribution after Electron Transfer from Triethylamine to an [Ir(ppy) 2 (bpy)] + Photosensitizer during Photocatalytic Water Reduction Sergey I. Bokarev,* Dirk Hollmann, Alexandra Pazidis, Antje Neubauer, Jörg Radnik, Oliver Kühn, Stefan Lochbrunner, Henrik Junge, Matthias Beller, and Angelika Brückner* The photoreduction of the bis(2-phenylpyridinato-)(2,2 -bipyridine)iridium(iii) ion ([Ir(ppy) 2 (bpy)] + ), used as photosensitizer in photocatalytic water splitting, by triethylamine was studied by means of UV/VIS, XANES, and EPR spectroscopies, supported by theoretical calculations on density functional theory (DFT) and complete active space self-consistent field (CASSCF/CASPT2) levels. The combination of these methods suggests a predominant bpy localization of the spin-density of the unpaired electron with notable delocalization to the Ir center. This is particularly evident from EPR and theoretical results and leads to broad EPR lines and a large anisotropy of the g-factor. Supplementary Material Figure S1. XANES measurements of [Ir] +3 ([Ir(H 2 )(TFP)(P ipr 3 ) 2 ]), [Ir] +2 (*Ir(Cl){µ es -Diimin}(CN tbu)]), [Ir] +1 (*Ir(µ- Cl)(COOEt) 2 ] 2 ) and [Ir] 0 (iridium foil) and the sample ([Ir(ppy) 2 (bpy)]pf 6 ). 1
2 Figure S2. In situ EPR spectroelectrochemistry performed by Cyclovoltametrie (0 to -1.7V) combined with EPR spectroscopy for IrPS. 2
3 Figure S3. MOs most important for electronic spectrum. 3
4 Table S1. Vertical electronic transitions of [Ir(ppy) 2 (bpy)] 0 as predicted by TDDFT (LC-BLYP, ω=0.18 bohr -1 ) in THF (PCM). State nr. Energy / cm -1 Osc. str. Configuration Weight π1*(bpy) π2*(bpy) π1*(bpy) π1*(ppy) π1*(bpy) π2*(ppy) π1*(bpy) π3*(bpy) π1*(bpy) π3*(ppy) π1*(bpy) π4*(ppy) dx2-y2 π1*(ppy) π1*(bpy) π4*(bpy) dx2-y2 π1*(ppy) dx2-y2 π1*(ppy) dx2-y2 π2*(ppy) dyz π2*(ppy) 0.16 dxz π1*(bpy) 0.16 dxz π1*(ppy) dyz π1*(ppy) 0.2 dyz π1*(bpy) π1*(bpy) σ*(dz2) π1*(bpy) π5*(ppy) dx2-y2 π2*(ppy) dyz π1*(bpy) 0.15 dx2-y2 π3*(ppy) 0.15 dx2-y2 π3*(ppy) dyz π1*(ppy) 0.16 dyz π2*(ppy) 0.15 π1(bpy) π1*(ppy) 0.08 dx2-y2 π4*(ppy) 0.06 dx2-y2 π4*(ppy) dx2-y2 π2*(ppy) 0.2 dyz π1*(bpy) dyz π2*(ppy) 0.13 dx2-y2 π2*(ppy) 0.12 dyz π1*(ppy) 0.11 dx2-y2 π3*(ppy) dxz π1*(bpy) 0.34 dx2-y2 π4*(ppy) dyz π1*(ppy) π1*(bpy) diff π1*(bpy) diff 0.22 dxz π1*(bpy)
5 dx2-y2 π4*(ppy) π1*(bpy) π6*(ppy) dxz π2*(ppy) dxz π1*(ppy) 0.33 π1*(bpy) π6*(ppy) dyz π2*(ppy) dx2-y2 π3*(ppy) dxz π2*(ppy) dxz π2*(ppy) 0.25 dxz π1*(ppy) π1*(bpy) diff π1*(bpy) diff dx2-y2 π4*(ppy) dyz π3*(ppy) 0.17 π1(ppy) π2*(ppy) 0.14 dyz π3*(ppy) 0.09 π1(bpy) π3*(ppy) π1(ppy) π2*(ppy) dyz π3*(ppy) 0.12 dyz π3*(ppy) 0.11 π1(bpy)+π5(ppy) π1*(ppy) 0.11 π1(ppy) π2*(ppy) π1(ppy) π1*(ppy) 0.13 π1(bpy)+π5(ppy) π1*(bpy) 0.12 dxz π3*(ppy) 0.12 dxz π3*(ppy) dyz π4*(ppy) 0.1 dyz π4*(ppy) 0.09 dxz π3*(ppy) 0.09 π1(bpy) π4*(ppy) 0.05 dxz π3*(ppy) 0.04 dx2-y2 π6*(ppy) 0.03 π3(ppy) π3*(ppy) 0.03 π3(ppy) π3*(ppy) π1*(bpy) π7*(ppy) π1*(bpy) π8*(ppy) dyz π3*(ppy) 0.28 dyz π3*(ppy) dx2-y2 π6*(ppy) 0.18 dx2-y2 π6*(ppy) 0.16 π3(ppy) π1*(ppy) 0.06 π1(bpy)+π5(ppy) π5*(ppy) dyz π2*(bpy) 0.14 π1(ppy) π2*(bpy)
6 π1(ppy) π3*(ppy) 0.12 dyz π3*(ppy) π1(ppy) π1*(ppy) 0.21 dxz π3*(ppy) 0.14 dyz π4*(ppy) dx2-y2 π5*(ppy) 0.16 dx2-y2 π5*(ppy) 0.16 π1(ppy) π2*(ppy) 0.07 π3(ppy) π1*(ppy) dxz π3*(ppy) 0.2 dxz π3*(ppy) 0.12 dyz π4*(ppy) π1*(bpy) σ*(dxy) dxz π4*(ppy) 0.29 dxz π4*(ppy) 0.07 dx2-y2 π3*(ppy) 0.06 π1(ppy) π2*(ppy) dyz π3*(ppy) 0.18 π1(bpy)+π5(ppy) π1*(ppy) 0.17 dxz π4*(ppy) dyz π4*(ppy) 0.17 π1(ppy) π3*(bpy) 0.07 dxz π3*(ppy) 0.06 dx2-y2 π4*(ppy) 0.04 π1(bpy) π3*(bpy) 0.04 dx2-y2 π4*(ppy) 0.04 π1(ppy) π4*(ppy) dxz π3*(ppy) 0.18 dxz π3*(ppy) 0.15 dyz π3*(bpy) dxz π3*(ppy) 0.15 dyz π3*(bpy) 0.13 dyz π3*(bpy) 0.1 π1(bpy)+π5(ppy) π1*(bpy) dyz π3*(ppy) 0.17 dxz π4*(ppy) 0.13 π1(ppy) π2*(ppy) dyz π4*(ppy) dx2-y2 π2*(bpy) 0.33 dxz π4*(ppy) dyz π4*(ppy) 0.11 dxz π3*(ppy) 0.09 dxz π2*(bpy) 0.09 dx2-y2 π3*(bpy)
7 dyz π3*(bpy) dxz π4*(ppy) 0.36 π1(ppy) π2*(ppy) dx2-y2 π2*(bpy) π3(ppy) π1*(bpy) 0.19 π3(ppy) π1*(ppy) 0.19 π1(ppy) π1*(ppy) π1(ppy) π1*(bpy) 0.34 dyz π1*(bpy) 0.08 π1(ppy) π2*(ppy) dx2-y2 σ*(dz2) 0.2 dx2-y2 σ*(dz2) dx2-y2 π3*(bpy) π6(ppy) π1*(ppy) 0.07 π6(ppy) π1*(bpy) 0.06 π(lig) π1*(ppy) 0.06 dx2-y2 π5*(ppy) 0.06 π3(ppy) π2*(ppy) 0.04 π(lig) π2*(ppy) 0.04 π1(bpy)+π5(ppy) diff 0.03 π(bpy) π1*(bpy) 0.03 π1(ppy) π7*(ppy) π1(ppy) π1*(bpy) 0.19 π1(bpy) π1*(bpy) 0.08 dxz π4*(ppy) 0.06 π3(ppy) π1*(ppy) dx2-y2 π3*(bpy) 0.13 π1(ppy) π1*(bpy) 0.04 π(lig) π1*(bpy) 0.03 dx2-y2 π3*(bpy) 0.03 π6(ppy) π2*(ppy) 0.03 π(lig) π1*(ppy) 0.02 dx2-y2 σ*(dz2) 0.02 π1(ppy) π1*(ppy) 0.02 π6(ppy) π1*(ppy) 0.02 σ(dxy) π1*(bpy) σ(dxy) π2*(ppy) 0.25 π1(bpy)+π5(ppy) π2*(ppy) dx2-y2 π2*(bpy) π1(ppy) π1*(ppy) σ(dxy) π1*(bpy) 0.16 σ(dxy) π1*(ppy) 0.16 σ(dxy) π2*(ppy) π1(ppy) π1*(ppy)
8 π3(bpy) π2*(ppy) 0.11 σ(dxy) π1*(bpy) 0.07 σ(dxy) π1*(ppy) 0.07 π1*(bpy) diff 0.05 π1*(bpy) π*(bpy) 0.04 σ(dxy) π2*(ppy) π1*(bpy) diff σ(dxy) π1*(ppy) 0.26 σ(dxy) π2*(ppy) dx2-y2 π3*(bpy) dyz π2*(bpy) σ(dxy) π1*(ppy) σ(dz2) π1*(ppy) 0.18 σ(dxy) π2*(ppy) 0.17 σ(dxy) π1*(ppy) dyz π3*(bpy) 0.18 dxz π2*(bpy) 0.12 π3(bpy) π2*(ppy) 0.06 dyz σ*(dz2) dyz σ*(dz2) 0.12 dyz π3*(bpy) 0.11 dyz σ*(dz2) 0.11 dyz diff 0.07 dyz π8*(ppy) π1(bpy)+π5(ppy) π3*(ppy) 0.25 π1(ppy) π3*(ppy)
9 Table S2. Vertical electronic transitions of [Ir(ppy) 2 (bpy)] + as predicted by TDDFT (LC-BLYP, ω=0.18 bohr -1 ) in THF (PCM). State Energy / nr. cm -1 Osc. str. Configuration Weight dx2-y2+π(ppy) π1*(bpy) dyz π1*(bpy) dx2-y2+π(ppy) π1*(ppy) dx2-y2+π(ppy) π2*(ppy) dx2-y2+π(ppy) π2*(ppy) dx2-y2+π(ppy) π2*(bpy) dyz π1*(ppy) dx2-y2+π(ppy) π3*(bpy) dxz+π1(ppy) π1*(ppy) dyz π2*(ppy) dxz+π1(ppy) π2*(ppy) dxz π1*(bpy) dx2-y2+π(ppy) π4*(ppy) dx2-y2+π(ppy) π3*(ppy) dyz π2*(bpy) dxz π1*(ppy) 0.36 dxz+π1(ppy) π2*(bpy) π5(ppy) π1*(bpy) dxz+π1(ppy) π2*(bpy) 0.28 dxz π2*(bpy) π5(ppy) π1*(bpy) 0.30 dxz π2*(ppy) π3(ppy) π1*(bpy) π1(bpy) π1*(bpy) 0.26 dxz+π1(ppy) π3*(bpy) dyz π3*(bpy) π3(ppy) π1*(ppy) π3(ppy) π2*(ppy) π1(bpy) π1*(bpy) dyz π4*(ppy) σ(dxy) π1*(bpy) dyz π3*(ppy) dxz+π1(ppy) π3*(ppy) dxz+π1(ppy) π4*(ppy) σ(dz2) π1*(bpy) dxz π2*(bpy) dx2-y2+π(ppy) σ*(dz2) 0.38 dx2-y2+π(ppy) π6*(ppy) dxz π3*(ppy)
10 π3(ppy) π2*(ppy) π5(ppy) π2*(ppy) 0.34 π3(ppy) π1*(ppy) π5(ppy) π1*(ppy) 0.26 dx2-y2+π(ppy) π5*(ppy) dx2-y2+π(ppy) π5*(ppy) 0.32 π5(ppy) π2*(bpy) π3(ppy) π2*(bpy) 0.18 σ(dxy) π1*(ppy) 0.18 π5(ppy) π3*(ppy) dxz π4*(ppy) 0.26 σ(dxy) π1*(ppy) dxz π3*(bpy) σ(dxy) π1*(ppy) 0.26 π3(ppy) π2*(bpy) σ(dz2) π1*(ppy) π5(ppy) π2*(bpy) 0.20 π1(bpy) π2*(bpy) 0.18 dxz π3*(ppy) π1(bpy) π3*(bpy) 0.32 π2(bpy)+π(ppy) π1*(bpy) 0.08 π3(ppy) π4*(ppy) π1(bpy) π2*(bpy) 0.42 π5(ppy) π2*(bpy) dyz σ*(dz2) dx2-y2+π(ppy) π4*(bpy) 0.30 dx2-y2+π(ppy) π6*(ppy) dx2-y2+π(ppy) π4*(bpy) 0.14 π3(ppy) π3*(ppy) 0.12 dx2-y2+π(ppy) π1*(bpy) dx2-y2+π(ppy) π4*(bpy) 0.20 π3(ppy) π3*(ppy) 0.08 π1(bpy) π3*(bpy) 0.06 π3(ppy) π4*(ppy) dxz+π1(ppy) σ*(dz2) 0.20 dxz σ*(dz2) 0.18 dxz+π1(ppy) π6*(ppy) dx2-y2+π(ppy) π1*(bpy) dx2-y2+π(ppy) σ*(dxy) 0.16 σ(dz2) π1*(ppy) 0.14 π3(ppy) π3*(ppy) σ(dz2) π2*(ppy) 0.22 σ(dxy) π2*(ppy) 0.16 σ(dz2) π1*(ppy)
11 σ(dz2) π2*(ppy) 0.20 σ(dxy) π2*(ppy) 0.16 σ(dz2) π1*(ppy) dx2-y2+π(ppy) π6*(ppy) 0.28 σ(dz2) π2*(ppy) π5(ppy) π3*(bpy) dyz π5*(ppy) π3(ppy) π3*(bpy) 0.16 σ(dxy) π3*(bpy) 0.12 π5(ppy) π3*(ppy) 0.08 σ(dxy) π2*(bpy) π5(ppy) π3*(ppy) 0.14 σ(dxy) π2*(bpy) 0.12 π3(ppy) π2*(bpy) dxz+π1(ppy) π5*(ppy) σ(dxy) π3*(bpy) 0.18 π5(ppy) π4*(ppy) 0.16 dx2-y2+π(ppy) π1*(ppy) σ(dz2) π2*(bpy) π3(ppy) π4*(ppy) 0.24 dxz π5*(ppy) 0.10 dx2-y2+π(ppy) π7*(ppy) π3(ppy) π3*(ppy) 0.22 σ(dz2) π2*(bpy) π1(bpy) π1*(ppy) π3(ppy) π4*(ppy) 0.16 π5(ppy) π3*(ppy) 0.14 dx2-y2+π(ppy) π7*(ppy) dyz π4*(bpy) dxz+π1(ppy) π4*(bpy) π6(ppy) π1*(bpy) 0.26 σ(dxy) π3*(bpy) π1(bpy) π2*(ppy) π6(ppy) π1*(bpy) 0.16 dx2-y2+π(ppy) π1*(ppy) 0.12 π7(ppy) π2*(ppy) 0.06 dx2-y2+π(ppy) π2*(bpy) 0.06 σ(dxy) π3*(bpy) π7(ppy) π1*(bpy) π6(ppy) π1*(bpy) 0.22 dx2-y2+π(ppy) π1*(ppy) dyz π6*(ppy) π7(ppy) π1*(bpy) 0.28 dyz π6*(ppy)
12 σ(dz2) π3*(bpy) π2(bpy)+π(ppy) π1*(bpy) 0.30 π2(bpy) π1*(bpy) π6(ppy) π1*(ppy) 0.26 π7(ppy) π2*(ppy) σ(dxy) π4*(ppy) 0.30 σ(dz2) π3*(bpy) π3(bpy) π1*(bpy) 0.32 π6(ppy) π1*(bpy)
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