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Chemistry of the Metal Carbonyls. Part 77. Some Reactions of the Platinumtriosmium Complexes with Donor Molecules; X-Ray Crystal Structures of and 3-MeC2Me)>

DOI: 10.1039/DT9810000162

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 162 - 170 (1981)

Update date:2022-08-02

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Authors:

Farrugia, Louis J.Farrugia, Louis J.

Howard, Judith A. K.Howard, Judith A. K.

Mitrprachachon, PachaneeMitrprachachon, Pachanee

Stone, F. Gordon A.Stone, F. Gordon A.

Woodward, PeterWoodward, Peter

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Article abstract of DOI:10.1039/DT9810000162

The compounds react with CO, PPh3, or AsPh3 to give complexes . 1H and 31P n.m.r. data for the compounds are discussed, and single-crystal X-ray diffraction study has been carried out on the compound , crystals of wich are triclinic, space group P1, Z = 2, in a unit cell with lattice parameters a=14.427(7), b=12.793(5), c=14.151(6) Angtstroem, α=92.33(3), β=120.87(3), and γ=91.06(4)o.The structure has been refined to R 0.041 (R' 0.044) for 5 794 independent reflections (2.9 < or = 2θ < or = 60 deg, Mo-Ka X-radiation) collected at 200 K.The four metal atoms adopt a butterfly arrangement in contrast to the tetrahedral cluster structure of the 58-electron precursors .In the metal-metal bonding distance are Os-Pt 2.717(1) and 2.848(1) Angstroem, and Os-Os 2.773(1), 2.914(1), and 3.043(1) Angstorem.Evidence is presented for the two hydrido-ligands bridging the longer Os-Pt and Os-Os bonds.One triphenylphosphine ligand is attached to platinum and the other to osmium, and all the carbonyl ligands are terminally bound.Reaction of with but-2-yne affords a mixture, from which five polynuclear metal complexes were isolated and studied by IR and NMR spectroscopy.None of these products contained the Os3Pt cluster of the precursor.One of the complexes was characterised as 3-MeC2Me)> and its structure established by X-ray diffraction.Crystals are monoclinic, space group P21/c, Z=4, in a unit cell of dimensions a=11.143(8), b=17.458(12), c=23.443(15) Angstroem, and β= 113.82(5) deg.The structure has been refined to R 0.031 (R' 0.033) for 4 438 independent reflections (2.9 < or = 2θ < or = 55 deg, Mo-Kα X-radiation) collected at 200 K.The metal atoms form anisoceles triangle bridged by a face-bonding but-2-yne molecule whose orientation with respect to the triangle is μ3(η2-II).The osmium atom carries three terminal CO ligands, and each platinum a CO and PPh3 group such that there is a cisoid arragement OCPtPtCO; the Pt-Pt separation of 3.033(2) Angstroem, however, suggests that there may be little direct metal-metal interaction.

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