The reaction of Ru3(CO)12 with 1,4-dichloro-but-2-yne in basic methanolic solution. Synthesis and crystal structure of (μ-H) 2Ru3(CO)9{μ3-η2- [H2C=C(H)C≡CC(=O)OCH3]}

Giuliana Gervasio; Domenica Marabello; Enrico Sappa; Andrea Secco

doi:10.1016/j.jorganchem.2004.12.033

The reaction of Ru₃(CO)₁₂ with 1,4-dichloro-but-2-yne in basic methanolic solution. Synthesis and crystal structure of (μ-H) ₂Ru₃(CO)₉{μ₃-η²- [H₂C=C(H)C≡CC(=O)OCH₃]}

Giuliana Gervasio
, Domenica Marabello
, Enrico Sappa
, Andrea Secco

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

Abstract

The title complex is obtained by reacting Ru₃(CO)₁₂ with 1,4-dichloro-but-2-yne (ClCH₂C≡CCH₂Cl, DCB) in CH₃OH/KOH solution (followed by acidification with HCl). The X-ray structure analysis shows that (μ-H)₂Ru₃(CO) ₉{μ₃-η²-[H₂C=C(H)CCC(=O) OCH₃]} complex contains a "parallel" ene-yne acetyl substituent, H₂C=C(H)C≡CC(=O)OCH₃; the formation of such a ligand starting from DCB is - to our knowledge - unprecedented. The synthesis of complex (μ-H)₂Ru₃(CO)₉{μ ₃-η²-[H₂C=C(H)CCC(=O)OCH₃]} occurs through the activation of CO and methanol. This process has been found for other reactions of functionalized alkynes with M₃(CO) ₁₂ carbonyls (M = Fe, Ru) under basic methanolic conditions. The known hydridic cluster, (μ-H)Ru₃(CO)₉[μ₃- η³-(MeCCHCH)] has been identified as the minor reaction product.

Original language	English
Pages (from-to)	1594-1599
Number of pages	6
Journal	Journal of Organometallic Chemistry
Volume	690
Issue number	6
DOIs	https://doi.org/10.1016/j.jorganchem.2004.12.033
Publication status	Published - 15 Mar 2005
Externally published	Yes

Keywords

Acetyl ligands
Ene-yne ligands
Methanol and CO activation
Parallel alkynes
Triruthenium clusters
X-ray structure analysis

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10.1016/j.jorganchem.2004.12.033

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@article{d1990d03bf59470d9640e97c234e012a,

title = "The reaction of Ru3(CO)12 with 1,4-dichloro-but-2-yne in basic methanolic solution. Synthesis and crystal structure of (μ-H) 2Ru3(CO)9\{μ3-η2- [H2C=C(H)C≡CC(=O)OCH3]\}",

abstract = "The title complex is obtained by reacting Ru3(CO)12 with 1,4-dichloro-but-2-yne (ClCH2C≡CCH2Cl, DCB) in CH3OH/KOH solution (followed by acidification with HCl). The X-ray structure analysis shows that (μ-H)2Ru3(CO) 9\{μ3-η2-[H2C=C(H)CCC(=O) OCH3]\} complex contains a {"}parallel{"} ene-yne acetyl substituent, H2C=C(H)C≡CC(=O)OCH3; the formation of such a ligand starting from DCB is - to our knowledge - unprecedented. The synthesis of complex (μ-H)2Ru3(CO)9\{μ 3-η2-[H2C=C(H)CCC(=O)OCH3]\} occurs through the activation of CO and methanol. This process has been found for other reactions of functionalized alkynes with M3(CO) 12 carbonyls (M = Fe, Ru) under basic methanolic conditions. The known hydridic cluster, (μ-H)Ru3(CO)9[μ3- η3-(MeCCHCH)] has been identified as the minor reaction product.",

keywords = "Acetyl ligands, Ene-yne ligands, Methanol and CO activation, Parallel alkynes, Triruthenium clusters, X-ray structure analysis",

author = "Giuliana Gervasio and Domenica Marabello and Enrico Sappa and Andrea Secco",

year = "2005",

month = mar,

day = "15",

doi = "10.1016/j.jorganchem.2004.12.033",

language = "English",

volume = "690",

pages = "1594--1599",

journal = "Journal of Organometallic Chemistry",

issn = "0022-328X",

publisher = "Elsevier B.V.",

number = "6",

}

The reaction of Ru₃(CO)₁₂ with 1,4-dichloro-but-2-yne in basic methanolic solution. Synthesis and crystal structure of (μ-H) ₂Ru₃(CO)₉{μ₃-η²- [H₂C=C(H)C≡CC(=O)OCH₃]}. / Gervasio, Giuliana; Marabello, Domenica; Sappa, Enrico et al.
In: Journal of Organometallic Chemistry, Vol. 690, No. 6, 15.03.2005, p. 1594-1599.

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

TY - JOUR

T1 - The reaction of Ru3(CO)12 with 1,4-dichloro-but-2-yne in basic methanolic solution. Synthesis and crystal structure of (μ-H) 2Ru3(CO)9{μ3-η2- [H2C=C(H)C≡CC(=O)OCH3]}

AU - Gervasio, Giuliana

AU - Marabello, Domenica

AU - Sappa, Enrico

AU - Secco, Andrea

PY - 2005/3/15

Y1 - 2005/3/15

N2 - The title complex is obtained by reacting Ru3(CO)12 with 1,4-dichloro-but-2-yne (ClCH2C≡CCH2Cl, DCB) in CH3OH/KOH solution (followed by acidification with HCl). The X-ray structure analysis shows that (μ-H)2Ru3(CO) 9{μ3-η2-[H2C=C(H)CCC(=O) OCH3]} complex contains a "parallel" ene-yne acetyl substituent, H2C=C(H)C≡CC(=O)OCH3; the formation of such a ligand starting from DCB is - to our knowledge - unprecedented. The synthesis of complex (μ-H)2Ru3(CO)9{μ 3-η2-[H2C=C(H)CCC(=O)OCH3]} occurs through the activation of CO and methanol. This process has been found for other reactions of functionalized alkynes with M3(CO) 12 carbonyls (M = Fe, Ru) under basic methanolic conditions. The known hydridic cluster, (μ-H)Ru3(CO)9[μ3- η3-(MeCCHCH)] has been identified as the minor reaction product.

AB - The title complex is obtained by reacting Ru3(CO)12 with 1,4-dichloro-but-2-yne (ClCH2C≡CCH2Cl, DCB) in CH3OH/KOH solution (followed by acidification with HCl). The X-ray structure analysis shows that (μ-H)2Ru3(CO) 9{μ3-η2-[H2C=C(H)CCC(=O) OCH3]} complex contains a "parallel" ene-yne acetyl substituent, H2C=C(H)C≡CC(=O)OCH3; the formation of such a ligand starting from DCB is - to our knowledge - unprecedented. The synthesis of complex (μ-H)2Ru3(CO)9{μ 3-η2-[H2C=C(H)CCC(=O)OCH3]} occurs through the activation of CO and methanol. This process has been found for other reactions of functionalized alkynes with M3(CO) 12 carbonyls (M = Fe, Ru) under basic methanolic conditions. The known hydridic cluster, (μ-H)Ru3(CO)9[μ3- η3-(MeCCHCH)] has been identified as the minor reaction product.

KW - Acetyl ligands

KW - Ene-yne ligands

KW - Methanol and CO activation

KW - Parallel alkynes

KW - Triruthenium clusters

KW - X-ray structure analysis

UR - https://www.scopus.com/pages/publications/14644440500

U2 - 10.1016/j.jorganchem.2004.12.033

DO - 10.1016/j.jorganchem.2004.12.033

M3 - Article

SN - 0022-328X

VL - 690

SP - 1594

EP - 1599

JO - Journal of Organometallic Chemistry

JF - Journal of Organometallic Chemistry

IS - 6

ER -

The reaction of Ru₃(CO)₁₂ with 1,4-dichloro-but-2-yne in basic methanolic solution. Synthesis and crystal structure of (μ-H) ₂Ru₃(CO)₉{μ₃-η²- [H₂C=C(H)C≡CC(=O)OCH₃]}

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