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Improved Synthesis of the Hexanuclear Clusters (2-), (1-), and H2Ru6(CO)18. The X-Ray Analysis of (1-), a Polynuclear Carbonyl containing an Interstitial Hydrogen Ligand

DOI: 10.1039/DT9800000383

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 383 - 392 (1980)

Update date:2022-08-11

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Authors:

Eady, Colin R.Eady, Colin R.

Jackson, Peter F.Jackson, Peter F.

Johnson, Brian F. G.Johnson, Brian F. G.

Lewis, JackLewis, Jack

Malatesta, Maria CarlottaMalatesta, Maria Carlotta

et al.et al.

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Article abstract of DOI:10.1039/DT9800000383

The X-ray analyses of two crystalline modifications, (I) and (II), of are reported, together with improved synthetic routes to this and the related clusters (2-) and H2Ru6(CO)18.Crystals of (I) are triclinic, space group P1-, with a=18.083(4), b=19.101(4), c=19.238(5) Angstroem, α=117.70(4), β=78.13(2), γ=97.05(2) deg, and Z=4.Crystals of (II) are monoclinic, space group P21/n, with a=33.82(8) b=52.55(10), c=9.832(2) Angstroem, β=92.66(2) deg, and Z=12.Least square refinement using diffractometer data (Mo-Kα) has given an R of 0.0681 for 9165 reflections for (I) and an R of 0.23 (Ru only) for 1485 reflections for (II).The unit cell in (I) contains two independent molecules of (1-), cluster (1) which is ordered and cluster (2) which is disordered between two sites (2A) and (2B) that are related by a non-crystallographic two-fold axis.The combined evidence of the X-ray analyses, 1H n.m.r. studies, i.r. <ν(CO)> spectra, and variable-temperature 13C n.m.r. is only consistent with the hydrogen ligand lying inside the Ru6 octahedron.

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