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Reactions of 6,6'-Bis(nido-decaboranyl) Oxide and 6-Hydroxy-nido-decaborane with Dihalogenobis(phosphine) Complexes of Nickel , Palladium, and Platinum, and some Related Chemistry; Nuclear Magnetic Resonance Investigations and the Crystal and Molecular Structures of Bis(dimethylphosph...

DOI: 10.1039/DT9850000953

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 953 - 972 (1985)

Update date:2022-08-04

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Authors:

Greenwood, Norman N.Greenwood, Norman N.

Hails, Michael J.Hails, Michael J.

Kennedy, John D.Kennedy, John D.

McDonald, Walter S.McDonald, Walter S.

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Article abstract of DOI:10.1039/DT9850000953

A modified procedure for the preparation and isolation of 6,6'-(B10H13)2O leads also to the isolation of the new compound 6-B10H13OH, which has been fully characterised by 11B and 1H n.m.r. and mass spectroscopy.The structures and some chemistry of these two related oxyboranes are compared.The reaction of either 6,6'-(B10H13)2O or 6-B10H13OH with cis- (L = PMe2Ph or PPh3) gives three platinaboranes, arachno- (1), nido-, and 3-B6H9)2L2> (2).The yellow needles of (2) (L = PMe2Ph) are monoclinic, space group P21/c, with a = 1014.0(2), b = 586.8(2), c = 2316.9(6) pm, β = 91.66(2) deg, Z = 2 and the molecular structure is that of a centrosymmetric 14-vertex arachno-diplatinaborane in which two B6H9 clusters are bonded above and below an almost linear P-Pt-Pt-P system.The bonding of each B6H9 unit is symmetrical trihapto.In sharp contrast the reaction of 6,6'-(B10H13)2O with the corresponding nickel complex cis- gives mainly phosphine-boranes of known type, viz.PhMe2P*BH3, PhMe2P*B3H7, and PhMe2P*B9H13, together with a low yield of the new metallaborane closo-<(PhMe2P)2NiB9H7Cl2> (3).The red crystals of (3) are monoclinic, space group C2/c, with a = 1341.2(2), b = 1321.5(2), c = 1476.3(2) pm, β = 109.50(1) deg, Z = 4 and the molecular structure is that of a bicapped square antiprismatic 10-vertex closo-nickelaborane in which the Ni(PMe2Ph)2 group takes up a capping four-connected site.The reaction of 6,6'-(B10H13)2O with cis- (L = PMe2Ph or PPh3) gives phosphine-boranes analogous to those from the reaction with cis-, together with arachno-, the palladium analogues of (1).Treatment of (1) with KH followed by cis- gives the moderately stable heterodimetallaborane cluster compound, <(PhMe2P)4PdPtB8H10>, an arachno-palladaplatinaborane species and the first metallaborane of any kind to contain metals from two different periods in the Periodic Table.Treatment of (2) with base followed by cis- gives the 15-vertex trimetallaborane cluster compound 3-B6H9)(μ-(η3-B6H8-η2-PtH(PMe2Ph)2))(PMe2Ph)2>.The 1H, 11B, and 31P n.m.r. behaviour of these compounds have been investigated in detail using both single- and double-resonance techniques, and a number of interesting patterns emerge.

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