The preparation of [Ru(NCMe)6][7-(η6-C6Me6)-nido-7-RuB10H13]2 and its characterization by single-crystal X-ray diffraction analysis and nuclear magnetic resonance spectroscopy: a triply hydrogen-bridged eleven-vertex nido-7-metallaundecaborane
Abstract
Reaction between [{Ru(η6-C6Me6)Cl2}2] and [NEt4]2[B10H14] in MeCN solution gives an 86% yield of yellow [Ru(NCMe)6][7-(η6-C6Me6)-nido-7-RuB10H13]2. Crystals were triclinic, space group P![[1 with combining macron]](https://www.rsc.org/images/entities/char_0031_0304.gif)
, with a= 937.6(2), b= 1 005.5(2), c= 1 679.2(3) pm, α= 79.73(1), β= 105.24(2), γ= 115.59(2)°, and Z= 1; the final R factor was 0.0341 for 3 439 observed reflections. The unit cell contains two polyhedral anions, and a mononuclear cation which is situated on a centre of inversion. Each anion consists of a nido-7-metallaundecaboranyl open-faced cluster, with an η6-C6Me6 ligand bound to the metal atom, and with two Ru(7)–H–B bridges and one B(9)–H–B(10) bridge which mutually exchange very readily in solution (ΔG183‡ < 34 kJ mol–1). Geometrical and n.m.r. considerations indicate that the B10 residue of the metallaborane cluster has arachno-decaboranyl character. The homoleptic cation [Ru(NCMe)6]2+ has also not previously been characterized by X-ray structural analysis.
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