Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of...

Melvyn Rowen Churchill; Charles H. Lake; Romana A. Lashewycz-Rubycz; Huirong Yao; Robert D. McCargar; Jerome B. Keister

doi:10.1016/0022-328X(93)83184-W

Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of...

Melvyn Rowen Churchill
, Charles H. Lake
, Romana A. Lashewycz-Rubycz
, Huirong Yao
, Robert D. McCargar
, Jerome B. Keister

Chemistry

SUNY Buffalo

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

20 Scopus citations

Abstract

Title full: Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of (μ-H)Ru₃(μ₃-η³-XCCRCR′) (CO)_9-n(PPh₃)_n complexes. Crystal structures of (μ-H)Ru₃(μ₃-η³-Et₂ NCCHCMe)(CO)₈(PPh₃) and (μ-H)Ru₃(μ₃-η³-MeOCCMeCMe)(CO )₇(PPh₃)₂·2CH₂Cl₂. Substitution products HRu₃(μ₃-η³-XCCRCR′)(CO) _9-n(PPh₃)_n (X OMe, R R′ Me, n = 1-3; X OMe, R H, R′ OEt, n = 2, 3; X NEt₂, R H, R′ Me, n = 1, 2) were prepared by using ONMe₃-induced ligand substitution. The products were characterized by spectroscopic methods. In addition, (μ-H)Ru₃(μ₃-η³-Et₂ NCCHMe)(CO)₈(PPh₃) (Mo Kα, 2θ 5.0-50.0°, R_f 5.22% for all 6,374 reflections, 2.62% for those 4,306 reflections with | F_o | ≫ 6σ( | F_o | )) and (μ-H)Ru₃(μ₃-η³-MeOCCMeCMe)(CO )₇(PPh₃)₂·2CH₂Cl₂ (Mo Kα, 2θ 8.0-45.0°, R_F 9.52% for all 6,798 reflections, 6.69% for those 3,795 reflections with | F_o | ≫ 6σ( | F_o |)) were characterized by single-crystal X-ray diffraction. Both compounds crystallize in the triclinic space group P1, with a 11.277(2) Å, b 11.899(1)Å, c 15.638(2)Å, α = 70.56(1)°,β = 85.23(1)°, γ = 66.00(1)°, V = 1802.8(4) Å³, and Z = 2 for the former and a = 12.960(2) Å, b = 13.040(2) Å, c = 17.683(3) Å, α = 98.81(1)°, β = 94.50(1)°, γ = 116.50(1)Å, V = 2606.2(8) Å³, and Z = 2 for the latter. In each case the PPh₃ ligands are coordinated cis to the bridging hydride and to the sigma RuC bond.

Original language	English
Pages (from-to)	151-160
Number of pages	10
Journal	Journal of Organometallic Chemistry
Volume	452
Issue number	1-2
DOIs	https://doi.org/10.1016/0022-328X(93)83184-W
State	Published - Jun 15 1993

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10.1016/0022-328X(93)83184-W

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@article{e726a02ef86d44778ddb1279547cfc90,

title = "Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of...",

abstract = "Title full: Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of (μ-H)Ru3(μ3-η3-XCCRCR′) (CO)9-n(PPh3)n complexes. Crystal structures of (μ-H)Ru3(μ3-η3-Et2 NCCHCMe)(CO)8(PPh3) and (μ-H)Ru3(μ3-η3-MeOCCMeCMe)(CO )7(PPh3)2·2CH2Cl 2. Substitution products HRu3(μ3-η3-XCCRCR′)(CO) 9-n(PPh3)n (X OMe, R R′ Me, n = 1-3; X OMe, R H, R′ OEt, n = 2, 3; X NEt2, R H, R′ Me, n = 1, 2) were prepared by using ONMe3-induced ligand substitution. The products were characterized by spectroscopic methods. In addition, (μ-H)Ru3(μ3-η3-Et2 NCCHMe)(CO)8(PPh3) (Mo Kα, 2θ 5.0-50.0°, Rf 5.22\% for all 6,374 reflections, 2.62\% for those 4,306 reflections with | Fo | ≫ 6σ( | Fo | )) and (μ-H)Ru3(μ3-η3-MeOCCMeCMe)(CO )7(PPh3)2·2CH2Cl 2 (Mo Kα, 2θ 8.0-45.0°, RF 9.52\% for all 6,798 reflections, 6.69\% for those 3,795 reflections with | Fo | ≫ 6σ( | Fo |)) were characterized by single-crystal X-ray diffraction. Both compounds crystallize in the triclinic space group P1, with a 11.277(2) {\AA}, b 11.899(1){\AA}, c 15.638(2){\AA}, α = 70.56(1)°,β = 85.23(1)°, γ = 66.00(1)°, V = 1802.8(4) {\AA}3, and Z = 2 for the former and a = 12.960(2) {\AA}, b = 13.040(2) {\AA}, c = 17.683(3) {\AA}, α = 98.81(1)°, β = 94.50(1)°, γ = 116.50(1){\AA}, V = 2606.2(8) {\AA}3, and Z = 2 for the latter. In each case the PPh3 ligands are coordinated cis to the bridging hydride and to the sigma RuC bond.",

author = "Churchill, \{Melvyn Rowen\} and Lake, \{Charles H.\} and Lashewycz-Rubycz, \{Romana A.\} and Huirong Yao and McCargar, \{Robert D.\} and Keister, \{Jerome B.\}",

year = "1993",

month = jun,

day = "15",

doi = "10.1016/0022-328X(93)83184-W",

language = "English",

volume = "452",

pages = "151--160",

journal = "Journal of Organometallic Chemistry",

issn = "0022-328X",

publisher = "Elsevier B.V.",

number = "1-2",

}

TY - JOUR

T1 - Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of...

AU - Churchill, Melvyn Rowen

AU - Lake, Charles H.

AU - Lashewycz-Rubycz, Romana A.

AU - Yao, Huirong

AU - McCargar, Robert D.

AU - Keister, Jerome B.

PY - 1993/6/15

Y1 - 1993/6/15

N2 - Title full: Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of (μ-H)Ru3(μ3-η3-XCCRCR′) (CO)9-n(PPh3)n complexes. Crystal structures of (μ-H)Ru3(μ3-η3-Et2 NCCHCMe)(CO)8(PPh3) and (μ-H)Ru3(μ3-η3-MeOCCMeCMe)(CO )7(PPh3)2·2CH2Cl 2. Substitution products HRu3(μ3-η3-XCCRCR′)(CO) 9-n(PPh3)n (X OMe, R R′ Me, n = 1-3; X OMe, R H, R′ OEt, n = 2, 3; X NEt2, R H, R′ Me, n = 1, 2) were prepared by using ONMe3-induced ligand substitution. The products were characterized by spectroscopic methods. In addition, (μ-H)Ru3(μ3-η3-Et2 NCCHMe)(CO)8(PPh3) (Mo Kα, 2θ 5.0-50.0°, Rf 5.22% for all 6,374 reflections, 2.62% for those 4,306 reflections with | Fo | ≫ 6σ( | Fo | )) and (μ-H)Ru3(μ3-η3-MeOCCMeCMe)(CO )7(PPh3)2·2CH2Cl 2 (Mo Kα, 2θ 8.0-45.0°, RF 9.52% for all 6,798 reflections, 6.69% for those 3,795 reflections with | Fo | ≫ 6σ( | Fo |)) were characterized by single-crystal X-ray diffraction. Both compounds crystallize in the triclinic space group P1, with a 11.277(2) Å, b 11.899(1)Å, c 15.638(2)Å, α = 70.56(1)°,β = 85.23(1)°, γ = 66.00(1)°, V = 1802.8(4) Å3, and Z = 2 for the former and a = 12.960(2) Å, b = 13.040(2) Å, c = 17.683(3) Å, α = 98.81(1)°, β = 94.50(1)°, γ = 116.50(1)Å, V = 2606.2(8) Å3, and Z = 2 for the latter. In each case the PPh3 ligands are coordinated cis to the bridging hydride and to the sigma RuC bond.

AB - Title full: Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of (μ-H)Ru3(μ3-η3-XCCRCR′) (CO)9-n(PPh3)n complexes. Crystal structures of (μ-H)Ru3(μ3-η3-Et2 NCCHCMe)(CO)8(PPh3) and (μ-H)Ru3(μ3-η3-MeOCCMeCMe)(CO )7(PPh3)2·2CH2Cl 2. Substitution products HRu3(μ3-η3-XCCRCR′)(CO) 9-n(PPh3)n (X OMe, R R′ Me, n = 1-3; X OMe, R H, R′ OEt, n = 2, 3; X NEt2, R H, R′ Me, n = 1, 2) were prepared by using ONMe3-induced ligand substitution. The products were characterized by spectroscopic methods. In addition, (μ-H)Ru3(μ3-η3-Et2 NCCHMe)(CO)8(PPh3) (Mo Kα, 2θ 5.0-50.0°, Rf 5.22% for all 6,374 reflections, 2.62% for those 4,306 reflections with | Fo | ≫ 6σ( | Fo | )) and (μ-H)Ru3(μ3-η3-MeOCCMeCMe)(CO )7(PPh3)2·2CH2Cl 2 (Mo Kα, 2θ 8.0-45.0°, RF 9.52% for all 6,798 reflections, 6.69% for those 3,795 reflections with | Fo | ≫ 6σ( | Fo |)) were characterized by single-crystal X-ray diffraction. Both compounds crystallize in the triclinic space group P1, with a 11.277(2) Å, b 11.899(1)Å, c 15.638(2)Å, α = 70.56(1)°,β = 85.23(1)°, γ = 66.00(1)°, V = 1802.8(4) Å3, and Z = 2 for the former and a = 12.960(2) Å, b = 13.040(2) Å, c = 17.683(3) Å, α = 98.81(1)°, β = 94.50(1)°, γ = 116.50(1)Å, V = 2606.2(8) Å3, and Z = 2 for the latter. In each case the PPh3 ligands are coordinated cis to the bridging hydride and to the sigma RuC bond.

UR - https://www.scopus.com/pages/publications/0000443098

U2 - 10.1016/0022-328X(93)83184-W

DO - 10.1016/0022-328X(93)83184-W

M3 - Article

AN - SCOPUS:0000443098

SN - 0022-328X

VL - 452

SP - 151

EP - 160

JO - Journal of Organometallic Chemistry

JF - Journal of Organometallic Chemistry

IS - 1-2

ER -

Structural studies on ruthenium carbonyl hydrides. XVIII. Synthesis and characterization of...

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