Heterobimetallic Di-tert-butylphosphido-Bridged Complexes of Cr-Ni and Cr-Rh. Synthesis and X-ray Structures of (CO)4(PMe3)Cr(μ-t-Bu2P)Ni(PMe3)CI(Cr-Ni) and (CO)4(PMe3)Cr(μ-t-Bu2P)Rh(PMe3)CO(Cr-Rh)

Richard A. Jones, Jon G. Lasch, Nicholas C. Norman, Anthony L. Stuart, Thomas C. Wright, Bruce R. Whittlesey

Research output: Contribution to journalArticle

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Abstract

Reaction of (CO)5CrP(t-Bu)2Li, prepared in situ from (CO)5CrP(t-Bu)2H and n-BuLi (1:1) in THF, with NiCl2(PMe3)2 at-100 °C yields (CO)4(PMe3)Cr(μ-t-Bu2P)Ni(PMe3)Cl(Cr-Ni) (1) in 60% yield. A similar reaction with Rh(PMe3)3Cl yields (CO)4(PMe3)Cr(μ-t-Bu2P)Rh(PMe3)CO(Cr-Rh) (2) in 70% yield. Both 1 and 2 contain a metal-metal bond bridged by a single di-tert-butylphosphido (μ-t-Bu2P) unit. In both cases a PMe3 group from the Ni and Rh starting complexes becomes bound to the Cr atom in 1 and 2, respectively. In 1 the Cr-PMe3 group is trans to the phosphorus atom of μ-t-Bu2P while in 2 it occupies a cis coordination site. Crystal data for 1: C18H36ClCrNiP3O4, Mr = 555.56, monoclinic, P21/n, a = 17.682 (2) Å, b = 11.323 (2) Å c = 13.231 (1) Å, s = 92.582 (1)°, U = 2646.6 (5) Å3 23, Dcalcd = 1.394 g cm-3, Z = 4, λ(Mo Kα) = 0.71069 Å, μ(Mo Kα) = 14.2 cm-1, final R = 0.0544, Rw = 0.0681, from 2714 observed reflections (4683 measured). Crystal data for 2: C19H36CrO5P3Rh, Mr = 592.31, monoclinic, P21/n, a = 8.459 (3) Å, b = 18.687 (3) Å, c = 17.113 (2) Å, β = 101.42 (2)°, U = 2677.1 (1)Å3, Dcalcd = 1.47 g cm-3, Z = 4, λ(Mo Kα) = 0.71069 Å, μ(Mo Kα) = 12.0 cm-1, final R = 0.041, Rw = 0.052, from 2806 observed reflections (4854 measured).

Original languageEnglish
Pages (from-to)114-119
Number of pages6
JournalOrganometallics
Volume3
Issue number1
DOIs
StatePublished - Oct 1984

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