The co-crystallization of Ru((R)-binap)(eta(3)-Me-allyl)(2) and binap dioxide, and synthesis of Ru(Ph2P(CH2)(4)PPh2)(eta(3)-Me-allyl)(2)


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Authors: MacFarlane, KS; Rettig, SJ; Liu, ZQ; James, BR
Year: 1998
Journal: Journal of Organometallic Chemistry 557: 213-219   Article Link (DOI)
Title: The co-crystallization of Ru((R)-binap)(eta(3)-Me-allyl)(2) and binap dioxide, and synthesis of Ru(Ph2P(CH2)(4)PPh2)(eta(3)-Me-allyl)(2)
Abstract: The molecular structure of the 2-methylallyl species Ru((R)-binap)(eta(3)-Me-allyl)(2) (3) was established by X-ray crystallography of a crystal of 3a, the asymmetric unit of which is composed of half of a molecule of 3 and half of a (R)-(+)-2,2'-bis(-diphenylphosphinoyl)-1,1'-binaphthyl(binap dioxide) molecule, co-crystallized with two disordered deuterobenzenes; crystals of 3a are tetragonal, space group I422, with Z = 8, a = 21.344(1) Angstrom and c = 36.453(2) A. The structure was solved by direct methods and refined by full-matrix least-squares procedures to R = 0.034 and R-w = 0.032 for 3431 reflections with I greater than or equal to 3 sigma(I). The 1,4-bis(diphenylphosphino)butane (dppb) analogue (2) of 3 was also prepared and characterized by H-1 and P-31{H-1}-NMR spectroscopy and elemental analysis, and the reactivities of 2 and 3 toward halogen acids are discussed. (C) 1998 Elsevier Science S.A. All rights reserved.
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