| Differential ECD, 1:1 (v/v) water/methanol, 25 °C | On adding rac-[Ir(nBuBQ)₂Cl], the band around 460 nm changed its intensity in the positive or negative direction in the presence of Δ- or Λ-[Ru(phen)₃]²⁺, respectively. The change around 380 nm, where the Ru(II) complex showed no absorption, was assigned to induced ECD of rac-[Ir(nBuBQ)₂Cl]. No ECD change occurred in a homogeneous solution containing Δ- or Λ-[Ru(phen)₃]Cl₂ without SAP |
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Akihiko Yamagishi, Kazuyoshi Takimoto, Jun Yoshida, Kyaw Naing, Hisako Sato. “Enantiomeric enrichment at a microcavity embedded in a modified clay: In-column reactions of a coordinatively unsaturated racemic iridium(III) complex.” ChemRxiv (). https://doi.org/10.26434/chemrxiv.15007907/v1
Values presented only in spectra, chromatograms, or other plots or images were not transcribed. The main paper refers to supporting information, but no separate supporting information file was available on the ChemRxiv article page
| UV–visible absorption spectroscopy, Na₂BPS added to [Ir(nBuBQ)₂Cl] in methanol, 25 °C | The 440 nm peak decreased while absorbance below 450 nm increased; a nearly isosbestic point was present around 460 nm; and the spectral change saturated above [Na₂BPS]/[Ir(nBuBQ)₂Cl] = 1 |
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| MS, product solution | Experimental molecular weight: 1151.2; calculated molecular weight: 1151.2 |
| ECD, product eluted after injection of rac-[Ir(nBuBQ)₂Cl] | Δ/Λ = 82/18; e.e. of Δ = 0.64 |
| ECD, product eluted after injection of Λ-[Ir(nBuBQ)₂Cl] | Δ/Λ = 22/78; e.e. of Λ = 0.55 |
| ECD, product eluted after injection of Δ-[Ir(nBuBQ)₂Cl] | Δ/Λ = 82/18; e.e. of Δ = 0.64 |
| ECD, product eluted after injection of Na⁺ Λ-[Ir(nBuBQ)₂(BPS)] | Δ/Λ = 2/98; e.e. of Λ = 0.96 |
| ECD, product eluted after injection of Na⁺ Δ-[Ir(nBuBQ)₂(BPS)] | Δ/Λ = 96/4; e.e. of Δ = 0.92 |
| Solid-state VCD | Strong peaks were observed at 1420 cm⁻¹ as bisignate couplets and at 1500 cm⁻¹ as a negative peak. Two low-intensity peaks of opposite sign were present in the 1500–1600 cm⁻¹ region for both samples and were assigned to bending vibrations of the BQ ligands |
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| Solid-state VCD | Several small peaks were present in the 1500–1600 cm⁻¹ region, with opposite signs between the two samples |
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