Complexes of hybrid ligands. Synthesis of mixed-ligand,phosphino-alkoxide complexes of Pd2+: the crystal and molecular structure of the complex Ph2 PCH2C(CF3 )2OPdCl(PPh2Me) |
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| Affiliation: | 1. Department of Chemistry, Nelson Mandela Metropolitan University, Port Elizabeth, South Africa;2. Department of Physical Chemistry, Razi University, Kermanshah, Iran;3. Department of Chemistry, Faculty of Science, University of Maragheh, Maragheh, Iran;4. Department of Science, Babol Noshiravani University of Technology, Babol, Iran;1. Institute of Organic Chemistry, Karlsruhe Institute of Technology, Kaiserstr. 12, 76131 Karlsruhe, Germany;2. Institute of Toxicology and Genetics, Karlsruhe Institute of Technology, Kaiserstr. 12, 76131 Karlsruhe, Germany;3. Department of chemistry, University of Helsinki, P.O. Box 55, FIN-00014, Finland;4. Werner-von-Siemensstraße 2-6, building 5110, 76646 Bruchsal, Germany |
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| Abstract: | The hybrid, bidentate, diarylphosphino-alkoxide ligand PPh2CH2C(CF3)2O−, L1, gives the Pd2+ bis- complex Pd(L1)2, from which the chloride-bridged dinuclear complex [(L1)Pd(μ-Cl)2Pd(L1)] is made by reaction with PdCl2(PhCN)2. Cleavage of the dinuclear complex with monodentate ligands L2 then gives Pd(L1)Cl(L2) (L2 =PPh3, PPh2Me, PPhMe2, PMe3, SMe2, or pyridine); NMR data show that PR3 is cis to the phosphine site in L1 in these complexes, but SMe2 or pyridine are probably trans.A complete crystal and molecular structural determination has been made for cis-Pd(L1)Cl(PPh2Me). Crystals are monoclinic, space group P21/c, a = 10.821(1), b = 14.600(1), c = 18.674(2) Å, β = 101.25(1)°, V = 2893 Å3, Z = 4. Least-squares refinement on F of 361 variables using 3977 observations converged at a conventional agreement factor R = 0.025. The complex is square-planar, with the two phosphines cis; the 5-membered chelate ring is in a dissymmetric envelope conformation. The PdP bonds differ in length, with that to the unidentate phosphine, 2.259(1) Å, being significantly longer than that to the phosphine on the chelating ligand, 2.231(1) Å. |
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