Crystal structures of the (η 2 :η 2 -cyclo-octa-1,5-diene)(η 6 -toluene)-iridium(I) cation and μ-chlorido-iridium(III) complexes of 2-(phosphinito)- and 2-(phosphinometh-yl)anthra-quinone ligands.

Autor: Thackeray S; Department of Chemistry State University of New York at New Paltz New Paltz NY 12561 USA., Mahoney J; Department of Chemistry State University of New York at New Paltz New Paltz NY 12561 USA., Arrington A; Department of Chemistry State University of New York at New Paltz New Paltz NY 12561 USA., Wilklow-Marnell M; Department of Chemistry State University of New York at New Paltz New Paltz NY 12561 USA., Brennessel WW; Department of Chemistry 120 Trustee Road University of Rochester,Rochester NY 14627 USA.
Jazyk: angličtina
Zdroj: Acta crystallographica. Section E, Crystallographic communications [Acta Crystallogr E Crystallogr Commun] 2024 Sep 30; Vol. 80 (Pt 10), pp. 1101-1109. Date of Electronic Publication: 2024 Sep 30 (Print Publication: 2024).
DOI: 10.1107/S2056989024008922
Abstrakt: When reacted in dry, degassed toluene, [Ir(COD)Cl] 2 (COD = cyclo-octa-1,5-diene) and 2 equivalents of 2-(di- tert -butyl-phosphinito)anthra-quinone ( tBu POAQH) were found to form a unique tri-iridium compound consisting of one monoanionic dinuclear tri-μ-chlorido complex bearing one bidentate tBu POAQ ligand per iridium, which was charge-balanced by an outer sphere [Ir(toluene)(COD)] + ion, the structure of which has not previously been reported. This product, which is a toluene solvate, namely, (η 2 :η 2 -cyclo-octa-1,5-diene)(η 6 -toluene)-iridium(I) tri-μ-chlorido-bis-({3-[(di- tert -butyl-phosphan-yl)-oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(III)) toluene monosolvate, [Ir(C 7 H 8 )(C 8 H 12 )][Ir 2 H 2 (C 22 H 24 O 3 P) 2 Cl 3 ]·C 7 H 8 or [Ir(toluene)(COD)][Ir(κ- P , C - tBu POAQ)(H)] 2 (μ-Cl) 3 ]·toluene, formed as small orange platelets at room temperature, crystallizing in the triclinic space group P . The cation and anion are linked via weak C-H⋯O inter-actions. The stronger inter-molecular attractions are likely the offset parallel π-π inter-actions, which occur between the toluene ligands of pairs of inverted cations and between pairs of inverted anthra-quinone moieties, the latter of which are capped by toluene solvate mol-ecules, making for π-stacks of four mol-ecules each. The related ligand, 2-(di- tert -butyl-phosphinometh-yl)-anthra-quinone ( tBu PCAQH), did not form crystals suitable for X-ray diffraction under analogous reaction conditions. However, when the reaction was conducted in chloro-form, yellow needles readily formed following addition of 1 atm of carbon monoxide. Diffraction studies revealed a neutral, dinuclear, di-μ-chlorido complex, di-μ-chlorido-bis-(carbon-yl{3-[(di- tert -butyl-phosphan-yl)-oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(I)), [Ir 2 H 2 (C 23 H 26 O 2 P) 2 Cl 2 (CO) 2 ] or [Ir(κ- P , C - tBu PCAQ)(H)(CO)(μ-Cl)] 2 , Ir 2 C 48 H 54 Cl 2 O 6 P 2 , again crystallizing in space group P . Offset parallel π-π inter-actions between anthra-quinone groups of adjacent mol-ecules link the mol-ecules in one dimension.
(© Thackeray et al. 2024.)
Databáze: MEDLINE
Externí odkaz: