Preparation and Structural Characterization of [(Ph3P)2N][HFeRu3(CO)13] and [(Ph3P)2N][HFe2Ru2(CO)13]

F. Takusagawa; A. Fumagalli; T. F. Koetzle; G. R. Steinmetz; R. P. Rosen; W. L. Gladfelter; G. L. Geoffroy; M. A. Bruck; R. Bau

doi:10.1021/ic50225a045

Preparation and Structural Characterization of [(Ph₃P)₂N][HFeRu₃(CO)₁₃] and [(Ph₃P)₂N][HFe₂Ru₂(CO)₁₃]

F. Takusagawa, A. Fumagalli, T. F. Koetzle, G. R. Steinmetz, R. P. Rosen, W. L. Gladfelter, G. L. Geoffroy, M. A. Bruck, R. Bau

Chemistry (Twin Cities)

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Abstract

Reaction of [(Ph₃P)₂N][HFe(CO)₄] with Ru₃(CO)₁₂ and Fe₂Ru(CO)₁₂ in refluxing THF gives the new clusters [(Ph₃P)₂N] [HFeRu₃(CO)₁₃] and [(Ph₃P)₂N][HFe₂Ru₂(CO)₁₃] in 47% and 4% yields, respectively. [(Ph₃P)₂N]-[HFeRu₃(CO)₁₃] has been characterized by its spectroscopic properties and by complete single-crystal X-ray and neutron diffraction studies. [(Ph₃P)₂N][HFeRu₃(CO)₁₃] crystallizes in the space group PI with Z = 2. Unit cell dimensions from the neutron diffraction study at 15 K are a = 15.053 (2) Å, b = 9.073 (1) Å, c = 18.992 (3) Å, α = 104.75 (2)°, β = 109.58 (2)6, and = 86.95 (2)°. The structure was refined to RiF²) = 0.052 and P(wP²) = 0.057 with measured intensities of 8354 independent reflections. The [HFeRu₃(CO)₁₃]^- anion has a closed pseudotetrahedral structure with each Ru bearing three terminal carbonyls. Two terminal carbonyls are attached to Fe with two additional carbonyls occupying semibridging positions between Fe and two Ru atoms. The hydride ligand symmetrically bridges one of the Ru-Ru bonds. [(Ph₃P)₂N] [HFe₂Ru₂(CO)₁₃] has also been characterized crystallographically. It crystallizes in the space group PI with Z = 2. The unit cell dimensions at room temperature are a = 14.955 (2) Å, b= 18.144 (3) Å, c = 9.290 (2) Å, α = 101.54 (2)°, β = 95.03 (4)°, and = 84.04 (3)°. The structure was solved and refined to P(P) = 0.056 and P(wF) = 0.042 for 5886 independent reflections with I ≥ 3.0σ(I). The structure of [HFe₂Ru₂(CO)₁₃]^- is similar to that of [HFeRu₃(CO)₁₃]^- except that the anion possesses a full-bridging CO between the two Fe atoms and no semibridging CO's.

Original language	English (US)
Pages (from-to)	3823-3828
Number of pages	6
Journal	Inorganic chemistry
Volume	20
Issue number	11
DOIs	https://doi.org/10.1021/ic50225a045
State	Published - Nov 1981

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@article{fa43e55c1a0a4206940a7eee9d40330e,

title = "Preparation and Structural Characterization of [(Ph3P)2N][HFeRu3(CO)13] and [(Ph3P)2N][HFe2Ru2(CO)13]",

abstract = "Reaction of [(Ph3P)2N][HFe(CO)4] with Ru3(CO)12 and Fe2Ru(CO)12 in refluxing THF gives the new clusters [(Ph3P)2N] [HFeRu3(CO)13] and [(Ph3P)2N][HFe2Ru2(CO)13] in 47% and 4% yields, respectively. [(Ph3P)2N]-[HFeRu3(CO)13] has been characterized by its spectroscopic properties and by complete single-crystal X-ray and neutron diffraction studies. [(Ph3P)2N][HFeRu3(CO)13] crystallizes in the space group PI with Z = 2. Unit cell dimensions from the neutron diffraction study at 15 K are a = 15.053 (2) {\AA}, b = 9.073 (1) {\AA}, c = 18.992 (3) {\AA}, α = 104.75 (2)°, β = 109.58 (2)6, and = 86.95 (2)°. The structure was refined to RiF2) = 0.052 and P(wP2) = 0.057 with measured intensities of 8354 independent reflections. The [HFeRu3(CO)13]- anion has a closed pseudotetrahedral structure with each Ru bearing three terminal carbonyls. Two terminal carbonyls are attached to Fe with two additional carbonyls occupying semibridging positions between Fe and two Ru atoms. The hydride ligand symmetrically bridges one of the Ru-Ru bonds. [(Ph3P)2N] [HFe2Ru2(CO)13] has also been characterized crystallographically. It crystallizes in the space group PI with Z = 2. The unit cell dimensions at room temperature are a = 14.955 (2) {\AA}, b= 18.144 (3) {\AA}, c = 9.290 (2) {\AA}, α = 101.54 (2)°, β = 95.03 (4)°, and = 84.04 (3)°. The structure was solved and refined to P(P) = 0.056 and P(wF) = 0.042 for 5886 independent reflections with I ≥ 3.0σ(I). The structure of [HFe2Ru2(CO)13]- is similar to that of [HFeRu3(CO)13]- except that the anion possesses a full-bridging CO between the two Fe atoms and no semibridging CO's.",

author = "F. Takusagawa and A. Fumagalli and Koetzle, {T. F.} and Steinmetz, {G. R.} and Rosen, {R. P.} and Gladfelter, {W. L.} and Geoffroy, {G. L.} and Bruck, {M. A.} and R. Bau",

year = "1981",

month = nov,

doi = "10.1021/ic50225a045",

language = "English (US)",

volume = "20",

pages = "3823--3828",

journal = "Inorganic chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "11",

}

TY - JOUR

T1 - Preparation and Structural Characterization of [(Ph3P)2N][HFeRu3(CO)13] and [(Ph3P)2N][HFe2Ru2(CO)13]

AU - Takusagawa, F.

AU - Fumagalli, A.

AU - Koetzle, T. F.

AU - Steinmetz, G. R.

AU - Rosen, R. P.

AU - Gladfelter, W. L.

AU - Geoffroy, G. L.

AU - Bruck, M. A.

AU - Bau, R.

PY - 1981/11

Y1 - 1981/11

N2 - Reaction of [(Ph3P)2N][HFe(CO)4] with Ru3(CO)12 and Fe2Ru(CO)12 in refluxing THF gives the new clusters [(Ph3P)2N] [HFeRu3(CO)13] and [(Ph3P)2N][HFe2Ru2(CO)13] in 47% and 4% yields, respectively. [(Ph3P)2N]-[HFeRu3(CO)13] has been characterized by its spectroscopic properties and by complete single-crystal X-ray and neutron diffraction studies. [(Ph3P)2N][HFeRu3(CO)13] crystallizes in the space group PI with Z = 2. Unit cell dimensions from the neutron diffraction study at 15 K are a = 15.053 (2) Å, b = 9.073 (1) Å, c = 18.992 (3) Å, α = 104.75 (2)°, β = 109.58 (2)6, and = 86.95 (2)°. The structure was refined to RiF2) = 0.052 and P(wP2) = 0.057 with measured intensities of 8354 independent reflections. The [HFeRu3(CO)13]- anion has a closed pseudotetrahedral structure with each Ru bearing three terminal carbonyls. Two terminal carbonyls are attached to Fe with two additional carbonyls occupying semibridging positions between Fe and two Ru atoms. The hydride ligand symmetrically bridges one of the Ru-Ru bonds. [(Ph3P)2N] [HFe2Ru2(CO)13] has also been characterized crystallographically. It crystallizes in the space group PI with Z = 2. The unit cell dimensions at room temperature are a = 14.955 (2) Å, b= 18.144 (3) Å, c = 9.290 (2) Å, α = 101.54 (2)°, β = 95.03 (4)°, and = 84.04 (3)°. The structure was solved and refined to P(P) = 0.056 and P(wF) = 0.042 for 5886 independent reflections with I ≥ 3.0σ(I). The structure of [HFe2Ru2(CO)13]- is similar to that of [HFeRu3(CO)13]- except that the anion possesses a full-bridging CO between the two Fe atoms and no semibridging CO's.

AB - Reaction of [(Ph3P)2N][HFe(CO)4] with Ru3(CO)12 and Fe2Ru(CO)12 in refluxing THF gives the new clusters [(Ph3P)2N] [HFeRu3(CO)13] and [(Ph3P)2N][HFe2Ru2(CO)13] in 47% and 4% yields, respectively. [(Ph3P)2N]-[HFeRu3(CO)13] has been characterized by its spectroscopic properties and by complete single-crystal X-ray and neutron diffraction studies. [(Ph3P)2N][HFeRu3(CO)13] crystallizes in the space group PI with Z = 2. Unit cell dimensions from the neutron diffraction study at 15 K are a = 15.053 (2) Å, b = 9.073 (1) Å, c = 18.992 (3) Å, α = 104.75 (2)°, β = 109.58 (2)6, and = 86.95 (2)°. The structure was refined to RiF2) = 0.052 and P(wP2) = 0.057 with measured intensities of 8354 independent reflections. The [HFeRu3(CO)13]- anion has a closed pseudotetrahedral structure with each Ru bearing three terminal carbonyls. Two terminal carbonyls are attached to Fe with two additional carbonyls occupying semibridging positions between Fe and two Ru atoms. The hydride ligand symmetrically bridges one of the Ru-Ru bonds. [(Ph3P)2N] [HFe2Ru2(CO)13] has also been characterized crystallographically. It crystallizes in the space group PI with Z = 2. The unit cell dimensions at room temperature are a = 14.955 (2) Å, b= 18.144 (3) Å, c = 9.290 (2) Å, α = 101.54 (2)°, β = 95.03 (4)°, and = 84.04 (3)°. The structure was solved and refined to P(P) = 0.056 and P(wF) = 0.042 for 5886 independent reflections with I ≥ 3.0σ(I). The structure of [HFe2Ru2(CO)13]- is similar to that of [HFeRu3(CO)13]- except that the anion possesses a full-bridging CO between the two Fe atoms and no semibridging CO's.

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JO - Inorganic chemistry

JF - Inorganic chemistry

IS - 11

ER -

Preparation and Structural Characterization of [(Ph₃P)₂N][HFeRu₃(CO)₁₃] and [(Ph₃P)₂N][HFe₂Ru₂(CO)₁₃]

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