Synthesis and Characterization of the Stable Dicarbonyl(cyclopentadienyl)iron Radical [(C5R5)Fe(CO)2] (R CHMe2)†‡
Corresponding Author
Dr. Helmut Sitzmann
FB Chemie der Universität, Erwin-Schrödinger-Strasse, D-67663 Kaiserslautern (Germany), Fax: Int. code +(631)205-2187, e-mail: [email protected]
FB Chemie der Universität, Erwin-Schrödinger-Strasse, D-67663 Kaiserslautern (Germany), Fax: Int. code +(631)205-2187, e-mail: [email protected]Search for more papers by this authorDipl.-Chem. Thomas Dezember
FB Chemie der Universität, Erwin-Schrödinger-Strasse, D-67663 Kaiserslautern (Germany), Fax: Int. code +(631)205-2187, e-mail: [email protected]
Search for more papers by this authorProf. Dr. Wolfgang Kaim
Institut für Anorganische Chemie der Universität Stuttgart (Germany)
Search for more papers by this authorDipl.-Chem. Frank Baumann
Institut für Anorganische Chemie der Universität Stuttgart (Germany)
Search for more papers by this authorProf. Dr. Dietmar Stalke
Institut für Anorganische Chemie der Universität Würzburg (Germany)
Search for more papers by this authorDipl.-Chem. Joerg Kärcher
Institut für Anorganische Chemie der Universität Göttingen (Germany)
Search for more papers by this authorProf. Dr. Elmar Dormann
Physikalisches Institut der Universität Karlsruhe (Germany)
Search for more papers by this authorDr. Hubert Winter
Physikalisches Institut der Universität Karlsruhe (Germany)
Search for more papers by this authorDipl.-Phys. Christoph Wachter
Physikalisches Institut der Universität Karlsruhe (Germany)
Search for more papers by this authorDipl.-Phys. Marc Kelemen
Physikalisches Institut der Universität Karlsruhe (Germany)
Search for more papers by this authorCorresponding Author
Dr. Helmut Sitzmann
FB Chemie der Universität, Erwin-Schrödinger-Strasse, D-67663 Kaiserslautern (Germany), Fax: Int. code +(631)205-2187, e-mail: [email protected]
FB Chemie der Universität, Erwin-Schrödinger-Strasse, D-67663 Kaiserslautern (Germany), Fax: Int. code +(631)205-2187, e-mail: [email protected]Search for more papers by this authorDipl.-Chem. Thomas Dezember
FB Chemie der Universität, Erwin-Schrödinger-Strasse, D-67663 Kaiserslautern (Germany), Fax: Int. code +(631)205-2187, e-mail: [email protected]
Search for more papers by this authorProf. Dr. Wolfgang Kaim
Institut für Anorganische Chemie der Universität Stuttgart (Germany)
Search for more papers by this authorDipl.-Chem. Frank Baumann
Institut für Anorganische Chemie der Universität Stuttgart (Germany)
Search for more papers by this authorProf. Dr. Dietmar Stalke
Institut für Anorganische Chemie der Universität Würzburg (Germany)
Search for more papers by this authorDipl.-Chem. Joerg Kärcher
Institut für Anorganische Chemie der Universität Göttingen (Germany)
Search for more papers by this authorProf. Dr. Elmar Dormann
Physikalisches Institut der Universität Karlsruhe (Germany)
Search for more papers by this authorDr. Hubert Winter
Physikalisches Institut der Universität Karlsruhe (Germany)
Search for more papers by this authorDipl.-Phys. Christoph Wachter
Physikalisches Institut der Universität Karlsruhe (Germany)
Search for more papers by this authorDipl.-Phys. Marc Kelemen
Physikalisches Institut der Universität Karlsruhe (Germany)
Search for more papers by this authorHigh-Spin Cyclopentadienyl Complexes, Part 1. This work was supported by Fonds der Chemischen Industrie. H. S. is grateful to Prof. Dr. O. J. Scherer, Kaiserslautern, for his generous support, and to Prof. Dr. R. Gleiter, Heidelberg, for recording photoelectron spectra.
Dedicated to Professor Max Herberhold on the occasion of his 60th birthday
Graphical Abstract
Monomeric in solution, dimeric in the crystal is the dicarbonyl(pentaisopropyl-cyclopentadienyl)iron(I) radical 2, which is formed from the high-spin iron(II) complex 1 by carbonylation and reduction.
References
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X-ray crystal structure data for 7: C22H35FeO2: T = 193 K, triclinic space group P1, a = 1.0392(2), b = 1.0489(2), c = 1.0536(2) Å, α = 105.44(3), β = 106.30(3), γ = 101.22(3)°, V = 1016.5(4) Å33, Z = 2, ρcalcd = 1.265 g cm−1, F(000) = 418, λ = 71.073 pm, μ(MoKα) = 0.754 mm−1. Data were collected on a Stoe-Siemens-AED-diffractometer. Intensities were measured on a rapidly cooled crystal (0.3 × 0.1 × 0.05 mm) in an oil drop [19] with 2θ/ω scans in the range 8° ≤ 2θ ≤ 45°. Of 2660 collected reflections, 2660 were independent and 2659 were used in refinement of 296 parameters (84 restraints); maximum and minimum of the difference fourier map 0.534 and 0.477 eÅ−3, R1 [F > 2σ(F)] = 0.0595, wR2 (all data) = 0.1281, R1 = Σ||Fo|–|Fc||/Σ|Fo| and wR2 = ΣW(F
–F
)2/ΣW(F
2)0.5. The structure was solved with direct methods (SHELXS92) [20] and refined by full-matrix least squares on F2 (SHELXL-93) [21]. Hydrogen atoms were refined by using a riding model. Crystallographic data (excluding structure factors) for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CCDC-179-121. Copies of the data can be obtained free of charge on application to The Director, CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: Int. code +(1223) 336-033; e-mail: [email protected]).
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