1996
DOI: 10.1021/ic9506769
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Synthesis, Molecular Structure, and Vibrational Spectra of mer-Tris(carbonyl)iridium(III) Fluorosulfate, mer-Ir(CO)3(SO3F)3

Abstract: Addition of carbon monoxide (0.5-2 atm) to iridium(III) fluorosulfate, Ir(SO(3)F)(3), dissolved in HSO(3)F over 4 days and at 60 degrees C, results in the quantitative formation of tris(carbonyl)iridium(III) fluorosulfate Ir(CO)(3)(SO(3)F)(3). Slow evaporation of the solvent produces single crystals of mer-Ir(CO)(3)(SO(3)F)(3). Crystal structure data for mer-Ir(CO)(3)(SO(3)F)(3): monoclinic, space group P2(1)/c, Z = 4, a = 8.476(1) Å, b = 12.868(2) Å, c = 12.588 (1) Å, beta = 108.24(1) degrees, V = 1304.0 Å(3)… Show more

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Cited by 29 publications
(51 citation statements)
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“…To confirm this hypothesis, we conducted infrared spectroscopy measurement (Figure S7), which revealed two vibrations at ca. 2255 and 2295 cm –1 , which closely match with CO vibration in Ir­(CO) x complexes. , Cyclic voltammetry (Figure S8) also revealed the apparition of an irreversible reduction wave at ca. −2 V vs SCE under CO, as previously observed …”
Section: Resultssupporting
confidence: 56%
See 1 more Smart Citation
“…To confirm this hypothesis, we conducted infrared spectroscopy measurement (Figure S7), which revealed two vibrations at ca. 2255 and 2295 cm –1 , which closely match with CO vibration in Ir­(CO) x complexes. , Cyclic voltammetry (Figure S8) also revealed the apparition of an irreversible reduction wave at ca. −2 V vs SCE under CO, as previously observed …”
Section: Resultssupporting
confidence: 56%
“…2255 and 2295 cm −1 , which closely match with CO vibration in Ir (CO) x complexes. 44,45 Cyclic voltammetry (Figure S8) also revealed the apparition of an irreversible reduction wave at ca. −2 V vs SCE under CO, as previously observed.…”
Section: Resultsmentioning
confidence: 98%
“…In this regard, comparison with other Ir(III) complexes with π-acceptor ligands is appropriate. For example, the tris(carbonyl) derivative Ir(SO 3 F) 3 (CO) 3 features a ν av (CO) of 2218 cm -1 , which is about 75 cm -1 higher than that found for gaseous CO (2143 cm -1 ), while in the mono(carbonyl) derivatives IrCl 3 (CO)(PR 3 ) 2 that contain the strongly basic trialkyl phosphines PEt 3 or PBu n 3 , ν(CO) appears in the proximity of 2000 cm -1 . Finally, the C(16)−O distance within the carbene fragment of 4b of 1.326(3) Å is short enough to suggest some double-bond character.…”
Section: Resultsmentioning
confidence: 85%
“…The analysis is limited by the quality of the EXAS spectra, so the useful ranges were limited to Δ k ∼ 2.0–12.5 Å –1 and Δ R ∼ 1.1–3.9 Å. In order to elucidate the possible coordination of the O–SO 2 – groups to the metal center, phases and amplitudes for Ir–O–S paths (single and multiple scattering) were calculated from the X-ray diffraction crystal data of the fluorosulfate iridium­(III) compound, mer -[Ir­(CO) 3 (OSO 2 F) 3 ] . The addition of these paths does not allow accurate fits for the CNT-2-Ir spectra thereby suggesting that sulfonate group is not present in the Ir environment in the hybrid catalysts and that this position is occupied by oxygen groups on the nanomaterial wall as it was previously observed for CNT-1-Ir .…”
Section: Resultsmentioning
confidence: 99%