Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) and (μ-H)2Ru3(μ3-CPh)(μ-CO)(CO)6(η5-C5H5). Crystal Structures of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) and Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3

Leigh R. Nevinger; Jerome B. Keister; Charles H. Lake; Melvyn Rowen Churchill

doi:10.1021/om00041a015

Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and (μ-H)₂Ru₃(μ₃-CPh)(μ-CO)(CO)₆(η⁵-C₅H₅). Crystal Structures of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and Ru₃(μ₃-CPh)(μ-CO)₃(η⁵-C₅H₅)₃

Leigh R. Nevinger
, Jerome B. Keister
, Charles H. Lake
, Melvyn Rowen Churchill

Chemistry

University at Buffalo

SUNY Buffalo

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

7 Scopus citations

Abstract

The reaction of (µ-H)₃Ru₃(μ₃-CPh) (CO)_9-n(NCMe)_n (n= 1, 2) with cyclopentadiene produces the new cluster Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅), in addition to Ru₃(μ₃-CPh)(μ-CO)₃(η⁵-C₅H₅)₃. Hydrogenation of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) gives (μ-H)₂Ru₃(μ₃-CPh)(μ-CO)(CO)₆(η⁵-C₅H₅). The compound Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) crystallizes in the centrosymmetric monocfinic space group P2₁/n, with a = 9.039 (2) Å, b = 20.496 (5) Å, c = 11.896 (3)Å, β = 92.80 (2)°, V = 2201 (1) Å³, and Z = 4. Diffraction data (Mo Kα 2θ = 5-50°) were collected with a Siemens R3m/V diffractometer, and the structure was solved and refined to R = 5.09% for all 3901 data (R = 2.69% for those 2659 data hwith F > 6.0σ(F)). The structure contains a triangular arrangement of ruthenium atoms (Ru-Ru = 2.738 (1)-2.749 (1) Å) capped by a μ₃-CPh ligand (Ru-C = 2.055 (5)-2.086 (5) Å). Atoms Ru(1) and Ru(2) are each bound to three terminal CO ligands, while Ru(3) is linked to an η⁵-C₅H₅ ligand. The structure is completed by two bridging CO ligands bonded more strongly to Ru(3) and somewhat less strongly to the remaining Ru atoms (Ru(3)-C(31) = 1.993 (6) Å, Ru(1)-C(31) = 2.167 (6) Å; Ru(3)-C(32) = 1.972 (6) Å, Ru(2)-C(32) = 2.225 (6) Å). The compound Ru₃(μ₃-CPh)(μ-CO)₃(η⁵-C₅H₅)₃ crystallizes in the centrosymmetric monoclinic space group P2₁/c, with a = 10.465 (2) Å, b = 11.192 (2) Å, c = 18.444 (3) Å β = 92.00 (2)°, V = 2158.8 (7) Å³, and Z = 4. Diffraction data (Mo Kα 2θ = 5-45°) were collected with a Siemens R3m/V diffractometer, and the structure was solved and refined to R_F = 3.24% for all 2716 unique data (R_F = 2.02% for those 2110 μμμdata with |F₀|> 6 σ(|F₀|)). The three ruthenium atoms in the structure form an almost perfect equilateral triangle (Ru-Ru = 2.690 (1)-2.705 (1) Å), which is capped by a μ₃-CPh ligand (Ru-C = 2.019 (4)-2.023 (4) Å). Each edge of the triangle has a symmetrically bridging carbonyl attached. The structure is then completed by one η⁵-C₅H₆ ring bonded to each ruthenium.

Original language	English
Pages (from-to)	1819-1824
Number of pages	6
Journal	Organometallics
Volume	11
Issue number	5
DOIs	https://doi.org/10.1021/om00041a015
State	Published - May 1 1992

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Nevinger, L. R., Keister, J. B., Lake, C. H., & Churchill, M. R. (1992). Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and (μ-H)₂Ru₃(μ₃-CPh)(μ-CO)(CO)₆(η⁵-C₅H₅). Crystal Structures of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and Ru₃(μ₃-CPh)(μ-CO)₃(η⁵-C₅H₅)₃. Organometallics, 11(5), 1819-1824. https://doi.org/10.1021/om00041a015

Nevinger, Leigh R. ; Keister, Jerome B. ; Lake, Charles H. et al. / Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and (μ-H)₂Ru₃(μ₃-CPh)(μ-CO)(CO)₆(η⁵-C₅H₅). Crystal Structures of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and Ru₃(μ₃-CPh)(μ-CO)₃(η⁵-C₅H₅)₃. In: Organometallics. 1992 ; Vol. 11, No. 5. pp. 1819-1824.

@article{4d15f22bc29742f499d6b518d369fdf6,

title = "Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) and (μ-H)2Ru3(μ3-CPh)(μ-CO)(CO)6(η5-C5H5). Crystal Structures of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) and Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3",

abstract = "The reaction of (µ-H)3Ru3(μ3-CPh) (CO)9-n(NCMe)n (n= 1, 2) with cyclopentadiene produces the new cluster Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5), in addition to Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3. Hydrogenation of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) gives (μ-H)2Ru3(μ3-CPh)(μ-CO)(CO)6(η5-C5H5). The compound Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) crystallizes in the centrosymmetric monocfinic space group P21/n, with a = 9.039 (2) {\AA}, b = 20.496 (5) {\AA}, c = 11.896 (3){\AA}, β = 92.80 (2)°, V = 2201 (1) {\AA}3, and Z = 4. Diffraction data (Mo Kα 2θ = 5-50°) were collected with a Siemens R3m/V diffractometer, and the structure was solved and refined to R = 5.09\% for all 3901 data (R = 2.69\% for those 2659 data hwith F > 6.0σ(F)). The structure contains a triangular arrangement of ruthenium atoms (Ru-Ru = 2.738 (1)-2.749 (1) {\AA}) capped by a μ3-CPh ligand (Ru-C = 2.055 (5)-2.086 (5) {\AA}). Atoms Ru(1) and Ru(2) are each bound to three terminal CO ligands, while Ru(3) is linked to an η5-C5H5 ligand. The structure is completed by two bridging CO ligands bonded more strongly to Ru(3) and somewhat less strongly to the remaining Ru atoms (Ru(3)-C(31) = 1.993 (6) {\AA}, Ru(1)-C(31) = 2.167 (6) {\AA}; Ru(3)-C(32) = 1.972 (6) {\AA}, Ru(2)-C(32) = 2.225 (6) {\AA}). The compound Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3 crystallizes in the centrosymmetric monoclinic space group P21/c, with a = 10.465 (2) {\AA}, b = 11.192 (2) {\AA}, c = 18.444 (3) {\AA} β = 92.00 (2)°, V = 2158.8 (7) {\AA}3, and Z = 4. Diffraction data (Mo Kα 2θ = 5-45°) were collected with a Siemens R3m/V diffractometer, and the structure was solved and refined to RF = 3.24\% for all 2716 unique data (RF = 2.02\% for those 2110 μμμdata with |F0|> 6 σ(|F0|)). The three ruthenium atoms in the structure form an almost perfect equilateral triangle (Ru-Ru = 2.690 (1)-2.705 (1) {\AA}), which is capped by a μ3-CPh ligand (Ru-C = 2.019 (4)-2.023 (4) {\AA}). Each edge of the triangle has a symmetrically bridging carbonyl attached. The structure is then completed by one η5-C5H6 ring bonded to each ruthenium.",

author = "Nevinger, \{Leigh R.\} and Keister, \{Jerome B.\} and Lake, \{Charles H.\} and Churchill, \{Melvyn Rowen\}",

year = "1992",

month = may,

day = "1",

doi = "10.1021/om00041a015",

language = "English",

volume = "11",

pages = "1819--1824",

journal = "Organometallics",

issn = "0276-7333",

publisher = "American Chemical Society",

number = "5",

}

Nevinger, LR, Keister, JB, Lake, CH & Churchill, MR 1992, 'Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and (μ-H)₂Ru₃(μ₃-CPh)(μ-CO)(CO)₆(η⁵-C₅H₅). Crystal Structures of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and Ru₃(μ₃-CPh)(μ-CO)₃(η⁵-C₅H₅)₃', Organometallics, vol. 11, no. 5, pp. 1819-1824. https://doi.org/10.1021/om00041a015

Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and (μ-H)₂Ru₃(μ₃-CPh)(μ-CO)(CO)₆(η⁵-C₅H₅). Crystal Structures of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and Ru₃(μ₃-CPh)(μ-CO)₃(η⁵-C₅H₅)₃. / Nevinger, Leigh R.; Keister, Jerome B.; Lake, Charles H. et al.
In: Organometallics, Vol. 11, No. 5, 01.05.1992, p. 1819-1824.

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

TY - JOUR

T1 - Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) and (μ-H)2Ru3(μ3-CPh)(μ-CO)(CO)6(η5-C5H5). Crystal Structures of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) and Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3

AU - Nevinger, Leigh R.

AU - Keister, Jerome B.

AU - Lake, Charles H.

AU - Churchill, Melvyn Rowen

PY - 1992/5/1

Y1 - 1992/5/1

N2 - The reaction of (µ-H)3Ru3(μ3-CPh) (CO)9-n(NCMe)n (n= 1, 2) with cyclopentadiene produces the new cluster Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5), in addition to Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3. Hydrogenation of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) gives (μ-H)2Ru3(μ3-CPh)(μ-CO)(CO)6(η5-C5H5). The compound Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) crystallizes in the centrosymmetric monocfinic space group P21/n, with a = 9.039 (2) Å, b = 20.496 (5) Å, c = 11.896 (3)Å, β = 92.80 (2)°, V = 2201 (1) Å3, and Z = 4. Diffraction data (Mo Kα 2θ = 5-50°) were collected with a Siemens R3m/V diffractometer, and the structure was solved and refined to R = 5.09% for all 3901 data (R = 2.69% for those 2659 data hwith F > 6.0σ(F)). The structure contains a triangular arrangement of ruthenium atoms (Ru-Ru = 2.738 (1)-2.749 (1) Å) capped by a μ3-CPh ligand (Ru-C = 2.055 (5)-2.086 (5) Å). Atoms Ru(1) and Ru(2) are each bound to three terminal CO ligands, while Ru(3) is linked to an η5-C5H5 ligand. The structure is completed by two bridging CO ligands bonded more strongly to Ru(3) and somewhat less strongly to the remaining Ru atoms (Ru(3)-C(31) = 1.993 (6) Å, Ru(1)-C(31) = 2.167 (6) Å; Ru(3)-C(32) = 1.972 (6) Å, Ru(2)-C(32) = 2.225 (6) Å). The compound Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3 crystallizes in the centrosymmetric monoclinic space group P21/c, with a = 10.465 (2) Å, b = 11.192 (2) Å, c = 18.444 (3) Å β = 92.00 (2)°, V = 2158.8 (7) Å3, and Z = 4. Diffraction data (Mo Kα 2θ = 5-45°) were collected with a Siemens R3m/V diffractometer, and the structure was solved and refined to RF = 3.24% for all 2716 unique data (RF = 2.02% for those 2110 μμμdata with |F0|> 6 σ(|F0|)). The three ruthenium atoms in the structure form an almost perfect equilateral triangle (Ru-Ru = 2.690 (1)-2.705 (1) Å), which is capped by a μ3-CPh ligand (Ru-C = 2.019 (4)-2.023 (4) Å). Each edge of the triangle has a symmetrically bridging carbonyl attached. The structure is then completed by one η5-C5H6 ring bonded to each ruthenium.

AB - The reaction of (µ-H)3Ru3(μ3-CPh) (CO)9-n(NCMe)n (n= 1, 2) with cyclopentadiene produces the new cluster Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5), in addition to Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3. Hydrogenation of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) gives (μ-H)2Ru3(μ3-CPh)(μ-CO)(CO)6(η5-C5H5). The compound Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) crystallizes in the centrosymmetric monocfinic space group P21/n, with a = 9.039 (2) Å, b = 20.496 (5) Å, c = 11.896 (3)Å, β = 92.80 (2)°, V = 2201 (1) Å3, and Z = 4. Diffraction data (Mo Kα 2θ = 5-50°) were collected with a Siemens R3m/V diffractometer, and the structure was solved and refined to R = 5.09% for all 3901 data (R = 2.69% for those 2659 data hwith F > 6.0σ(F)). The structure contains a triangular arrangement of ruthenium atoms (Ru-Ru = 2.738 (1)-2.749 (1) Å) capped by a μ3-CPh ligand (Ru-C = 2.055 (5)-2.086 (5) Å). Atoms Ru(1) and Ru(2) are each bound to three terminal CO ligands, while Ru(3) is linked to an η5-C5H5 ligand. The structure is completed by two bridging CO ligands bonded more strongly to Ru(3) and somewhat less strongly to the remaining Ru atoms (Ru(3)-C(31) = 1.993 (6) Å, Ru(1)-C(31) = 2.167 (6) Å; Ru(3)-C(32) = 1.972 (6) Å, Ru(2)-C(32) = 2.225 (6) Å). The compound Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3 crystallizes in the centrosymmetric monoclinic space group P21/c, with a = 10.465 (2) Å, b = 11.192 (2) Å, c = 18.444 (3) Å β = 92.00 (2)°, V = 2158.8 (7) Å3, and Z = 4. Diffraction data (Mo Kα 2θ = 5-45°) were collected with a Siemens R3m/V diffractometer, and the structure was solved and refined to RF = 3.24% for all 2716 unique data (RF = 2.02% for those 2110 μμμdata with |F0|> 6 σ(|F0|)). The three ruthenium atoms in the structure form an almost perfect equilateral triangle (Ru-Ru = 2.690 (1)-2.705 (1) Å), which is capped by a μ3-CPh ligand (Ru-C = 2.019 (4)-2.023 (4) Å). Each edge of the triangle has a symmetrically bridging carbonyl attached. The structure is then completed by one η5-C5H6 ring bonded to each ruthenium.

UR - https://www.scopus.com/pages/publications/0242445370

U2 - 10.1021/om00041a015

DO - 10.1021/om00041a015

M3 - Article

SN - 0276-7333

VL - 11

SP - 1819

EP - 1824

JO - Organometallics

JF - Organometallics

IS - 5

ER -

Nevinger LR, Keister JB, Lake CH, Churchill MR. Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and (μ-H)₂Ru₃(μ₃-CPh)(μ-CO)(CO)₆(η⁵-C₅H₅). Crystal Structures of Ru₃(μ₃-CPh)(μ-CO)₂(CO)₆(η⁵-C₅H₅) and Ru₃(μ₃-CPh)(μ-CO)₃(η⁵-C₅H₅)₃. Organometallics. 1992 May 1;11(5):1819-1824. doi: 10.1021/om00041a015

Reaction of Cyclopentadiene with (Alkylidyne)triruthenium Clusters. Syntheses of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) and (μ-H)2Ru3(μ3-CPh)(μ-CO)(CO)6(η5-C5H5). Crystal Structures of Ru3(μ3-CPh)(μ-CO)2(CO)6(η5-C5H5) and Ru3(μ3-CPh)(μ-CO)3(η5-C5H5)3

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