| 15360258 |
Tutusaus O, Nunez R, Vinas C, Teixidor F, Mata I, Molins E: Synthesis, characterization, and dynamic studies of 12-vertex eta5-ruthenium (II) closo-phosphine complexes with monoanionic [10-L-nido-7-R-7,8-C2B9H9]- ligands. Inorg Chem. 2004 Sep 20;43(19):6067-74.
Ruthenacarborane complexes of formula [3-H-3,3-(PPh3) 2-8-L-closo-3,1,2-RuC2B9H10)] (L = SMe2 (2a), SEt2 (2b), S (CH2) 4 (2c), SEtPh (2d)) and [1-Me-3-H-3,3-(PPh3) 2-8-L-closo-3,1,2-RuC2B9H9)] (L = SMe2 (2e), SEt2 (2f)) were prepared by reaction of the respective monoanionic charge-compensated ligands [10-L-nido-7,8-C2B9H10]- and [7-Me-10-L-nido-7,8-C2B9H9]- with [RuCl2 (PPh3) 3]. Similary, complexes [3-H-3,3,8-(PPh3) 3-closo-3,1,2-RuC2B9H10)] (4a) and [3-H-3,3-(PPh3) 2-8-PPh2Me-closo-3,1,2-RuC2B9H10)] (4b) were prepared from the corresponding phosphonium ligands. The reaction is done in one pot by reacting the ligand with the Ru (II) complex in a 1.5:1 ratio. All compounds have been fully characterized by multinuclear NMR spectroscopy, and the molecular structures for 2a and 4a have been elucidated by single-crystal X-ray diffraction analysis. The Ru (II) atom in this complex is on the open face of the monoanionic charge-compensated ligand adopting a pseudooctahedral coordination. Formally, three positions are supplied by the C2B3 open face, two PPh3 groups occupy two other positions, and a hydride fulfills the remaining one. The hydride complexes were generated with no special reagent. They result from a dehalogenation in the presence of ethanol. |
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