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

doi:10.1021/om00079a021

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

Chemistry and Biochemistry

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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, M_r = 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, R_w = 0.0681, from 2714 observed reflections (4683 measured). Crystal data for 2: C₁₉H₃₆CrO₅P₃Rh, M_r = 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, D_calcd = 1.47 g cm^-3, Z = 4, λ(Mo Kα) = 0.71069 Å, μ(Mo Kα) = 12.0 cm^-1, final R = 0.041, R_w = 0.052, from 2806 observed reflections (4854 measured).

Original language	English
Pages (from-to)	114-119
Number of pages	6
Journal	Organometallics
Volume	3
Issue number	1
DOIs	https://doi.org/10.1021/om00079a021
State	Published - Oct 1984

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Jones, Richard A. ; Lasch, Jon G. ; Norman, Nicholas C. ; Stuart, Anthony L. ; Wright, Thomas C. ; Whittlesey, Bruce R. / 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). In: Organometallics. 1984 ; Vol. 3, No. 1. pp. 114-119.

@article{4ec2e4596b3b4da7a06cc4714fce333f,

title = "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)",

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) {\AA}, b = 11.323 (2) {\AA} c = 13.231 (1) {\AA}, s = 92.582 (1)°, U = 2646.6 (5) {\AA}3 23, Dcalcd = 1.394 g cm-3, Z = 4, λ(Mo Kα) = 0.71069 {\AA}, 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) {\AA}, b = 18.687 (3) {\AA}, c = 17.113 (2) {\AA}, β = 101.42 (2)°, U = 2677.1 (1){\AA}3, Dcalcd = 1.47 g cm-3, Z = 4, λ(Mo Kα) = 0.71069 {\AA}, μ(Mo Kα) = 12.0 cm-1, final R = 0.041, Rw = 0.052, from 2806 observed reflections (4854 measured).",

author = "Jones, {Richard A.} and Lasch, {Jon G.} and Norman, {Nicholas C.} and Stuart, {Anthony L.} and Wright, {Thomas C.} and Whittlesey, {Bruce R.}",

year = "1984",

month = oct,

doi = "10.1021/om00079a021",

language = "English",

volume = "3",

pages = "114--119",

journal = "Organometallics",

issn = "0276-7333",

publisher = "American Chemical Society",

number = "1",

}

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

In: Organometallics, Vol. 3, No. 1, 10.1984, p. 114-119.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - 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)

AU - Jones, Richard A.

AU - Lasch, Jon G.

AU - Norman, Nicholas C.

AU - Stuart, Anthony L.

AU - Wright, Thomas C.

AU - Whittlesey, Bruce R.

PY - 1984/10

Y1 - 1984/10

N2 - 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).

AB - 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).

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U2 - 10.1021/om00079a021

DO - 10.1021/om00079a021

M3 - Article

AN - SCOPUS:0038524320

VL - 3

SP - 114

EP - 119

JO - Organometallics

JF - Organometallics

SN - 0276-7333

IS - 1

ER -

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)

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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)