Title: A Stable η<sup>5</sup>‐Germacyclopentadienyl Complex: [(η<sup>5</sup> C<sub>5</sub>Me<sub>5</sub>)Ru{η<sup>5</sup>‐C<sub>4</sub>Me<sub>4</sub>GeSi(SiMe<sub>3</sub>)<sub>3</sub>}]
Abstract: Angewandte Chemie International Edition in EnglishVolume 32, Issue 12 p. 1744-1745 Communication A Stable η5-Germacyclopentadienyl Complex: [(η5 C5Me5)Ru{η5-C4Me4GeSi(SiMe3)3}]† William P. Freeman, William P. Freeman Department of Chemistry, 0506, University of California at San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 (USA), Telefax: Int. code + (619)534-4864Search for more papers by this authorProf. Dr. T. Don Tilley, Corresponding Author Prof. Dr. T. Don Tilley Department of Chemistry, 0506, University of California at San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 (USA), Telefax: Int. code + (619)534-4864 T. Don Tilley, Department of Chemistry, 0506, University of California at San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 (USA), Telefax: Int. code + (619)534-4864 Robert L. Ostrander, Department of Chemistry, University of Delaware, Newark, DE 19716 (USA)Search for more papers by this authorProf. Dr. Arnold L. Rheingold, Prof. Dr. Arnold L. Rheingold Department of Chemistry, University of Delaware, Newark, DE 19716 (USA)Search for more papers by this authorDr. Robert L. Ostrander, Corresponding Author Dr. Robert L. Ostrander Department of Chemistry, University of Delaware, Newark, DE 19716 (USA) T. Don Tilley, Department of Chemistry, 0506, University of California at San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 (USA), Telefax: Int. code + (619)534-4864 Robert L. Ostrander, Department of Chemistry, University of Delaware, Newark, DE 19716 (USA)Search for more papers by this author William P. Freeman, William P. Freeman Department of Chemistry, 0506, University of California at San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 (USA), Telefax: Int. code + (619)534-4864Search for more papers by this authorProf. Dr. T. Don Tilley, Corresponding Author Prof. Dr. T. Don Tilley Department of Chemistry, 0506, University of California at San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 (USA), Telefax: Int. code + (619)534-4864 T. Don Tilley, Department of Chemistry, 0506, University of California at San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 (USA), Telefax: Int. code + (619)534-4864 Robert L. Ostrander, Department of Chemistry, University of Delaware, Newark, DE 19716 (USA)Search for more papers by this authorProf. Dr. Arnold L. Rheingold, Prof. Dr. Arnold L. Rheingold Department of Chemistry, University of Delaware, Newark, DE 19716 (USA)Search for more papers by this authorDr. Robert L. Ostrander, Corresponding Author Dr. Robert L. Ostrander Department of Chemistry, University of Delaware, Newark, DE 19716 (USA) T. Don Tilley, Department of Chemistry, 0506, University of California at San Diego, 9500 Gilman Drive, La Jolla, CA 92093-0506 (USA), Telefax: Int. code + (619)534-4864 Robert L. Ostrander, Department of Chemistry, University of Delaware, Newark, DE 19716 (USA)Search for more papers by this author First published: December 1993 https://doi.org/10.1002/anie.199317441Citations: 67 † This research was supported by the National Science Foundation. AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onEmailFacebookTwitterLinkedInRedditWechat Graphical Abstract A planar five-membered C4Ge ring with a delocalized π system stabilized by a [Cp*Ru] fragment is the key feature of the title compound 1. This compound can be prepared from [(Cp*RuCl)4] and the lithiated germole Li[C4Me4Ge{Si(SiMe3)3}]. References 1(a) G. Raabe, J. Michl, Chem. Rev. 1985, 85, 419; J. Barrau, J. Escudié, J. Satgé, Chem. Rev. 1990, 90, 283; A. H. Cowley, N. C. Norman, Prog. Inorg. Chem. 1986, 34, 1; A. G. Brook, K. M. Baines, Adv. Organomet, Chem. 1986, 25, 1; A. Berndt, H. Meyer, G. Baum, W. Massa, S. Berger, Pure Appl. Chem. 1987, 59, 1011; R. West, Angew. Chem. 1987, 99, 1231; Angew. Chem. Int. Ed. Engl. 1987, 26, 1201; N. Wiberg, J. Organomet. Chem. 1984, 273, 141. 2(a) G. Maier, G. Mihm, H. P. Reisenauer, Angew. Chem. 1980, 92, 58; Angew. Chem. Int. Ed. Engl. 1980. 19, 52; P. Jutzi, M. Meyer, H. P. Reisenauer, G. Maier, Chem. Ber. 1989, 122, 1227; G. Märkl, W. Schlosser, Angew. Chem. 1988, 100, 1009; Angew. Chem. Int. Ed. Engl. 1988, 27, 963; J. D. Rich, R. West, J. Am. Chem. Soc. 1982, 104, 6884; H. B. Schlegel, B. Coleman, M. Jones, Jr., J. Am. Chem. Soc. 1978, 100, 6499. 3 E. Colomer, R. J. P. Corriu, M. Lheureux, Chem. Rev. 1990, 90, 265. 4 P. Jutzi, A. Karl, P. Hofmann, Angew. Chem. 1980, 92, 496; Angew. Chem. Int, Ed. Engl. 1980, 19, 484. 5 P. J. Fagan, M. D. Ward, J. C. Calabrese, J. Am. Chem. Soc. 1989, 111, 1698. 6 X-ray structure analysis of 1: C18H27C13GeRu, Mr = 523.4, monoclinic, c, a = 8.345(2), b = 17.831(4), c = 14.612(4) Å, β = 103.90(2)°, V = 2110.5(10) Å3, Z = 4, ϱcalcd = 1.647 gcm−3, μ(MoKα) = 25.17 cm−1, T = 296 K; 2518 independent reflections with 4° ≤ 2θ ≤ 55° were collected, of which 2219 reflections with Fo greater than 5σ(Fo) were used in refinement. R(F) = 0.0277, Rw (F) = 0.0353, GOF = 0.89. The acentric space group was chosen on the initial basis of E values and retained on the basis of the refinement statistics and the symmetry of the molecule. A Rogers test indicated the choice of absolute configuration was correct, η = 1.05(6). A semiempirical absorption correction based on 216 data (6 reflections, 10° increments) was applied, T(max)/T(min) = 1.30. All the non-hydrogen atoms were refined anisotropically with the hydrogen atoms treated as idealized isotropic contributions. Further details of the crystal structure investigation are available on request from the Director of the Cambridge Crystallographic Data Centre, 12 Union Road, GB-Cambridge CB21EZ (UK), on quoting the full journal citation. 7 P. Dufour, J. Dubac, M. Dartiguenave, Y. Dartiguenave, Organometallics 1990, 9, 3001. 8 X-ray structure analysis of 4: C27H27CI3GeRu, Mr = 664.7, triclinic, P1, a = 9.848(6), b = 12.192(7), c = 15.854(9) Å, α = 93.83(5), β = 90.54(5), γ = 107.89(4)°, V = 1806.5(18)Å3, Z = 2. ϱcalcd = 1.222 gcm−3, μ(MoKα) = 13.95 cm−1, T = 295 K; 6370 independent reflections with 4° < 2θ < 55° were collected (Siemens P4), of which 3684 reflections with Fo greater than 6σ(Fo) were used in refinement. R(F) = 0.0443, Rw(F) = 0.0539, GOF = 1.13. The centrosymmetric space group was chosen on the initial basis of E values and retained on the basis of the refinement statistics and the molecular symmetry. The absorption coefficient was small and the crystal well-shaped, therefore no absorption correction was applied. All other non-hydrogen atoms were refined anisotropically with the hydrogen atoms treated as idealized isotropic contributions. Further details of the crystal structure investigation are available on request from the Director of the Cambridge Crystallographic Data Centre, 12 Union Road, GB-Cambridge CB21EZ (UK), on quoting the full journal citation. 9(a) R. Ball, M. J. Bennett, Inorg. Chem. 1972, 11, 1806; J. Howard, P. Woodward, J. Chem. Soc. (A) 1971, 3648; J. A. K. Howard, P. Woodward, J. Chem. Soc. Dalton trans. 1978, 412; L. Y. Y. Chan, W. A. G. Graham, Inorg. Chem. 1975, 14, 1773. 10 P. G. Gassman, C. H. Winter, J. Am Chem. Soc. 1988, 110, 6130. 11 P. J. Fagan, W. A. Nugent, J. Am. Chem. Soc. 1988, 110, 2310. 12 G. Gutekunst, A. G. Brook, J. Organomet. Chem. 1982, 225, 1. Citing Literature Volume32, Issue12December 1993Pages 1744-1745 ReferencesRelatedInformation
Publication Year: 1993
Publication Date: 1993-12-01
Language: en
Type: article
Indexed In: ['crossref']
Access and Citation
Cited By Count: 75
AI Researcher Chatbot
Get quick answers to your questions about the article from our AI researcher chatbot