Discrete Mixed-Valence Metal Chains: Iridium Pyridonate Blues
2001; Wiley; Volume: 113; Issue: 21 Linguagem: Inglês
10.1002/1521-3757(20011105)113
ISSN1521-3757
AutoresCristina Tejel, Miguel A. Ciriano, B. Eva Villarroya, Raquel Gelpi, José A. López, Fernando J. Lahoz, Luis A. Oro,
Tópico(s)Ferrocene Chemistry and Applications
ResumoAngewandte ChemieVolume 113, Issue 21 p. 4208-4210 Zuschrift Discrete Mixed-Valence Metal Chains: Iridium Pyridonate Blues Cristina Tejel Dr., Cristina Tejel Dr. Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorMiguel A. Ciriano Dr., Miguel A. Ciriano Dr. [email protected] Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorB. Eva Villarroya Dr., B. Eva Villarroya Dr. Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorRaquel Gelpi, Raquel Gelpi Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorJosé A. López Dr., José A. López Dr. Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorFernando J. Lahoz Dr., Fernando J. Lahoz Dr. Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorLuis A. Oro Prof., Luis A. Oro Prof. [email protected] Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this author Cristina Tejel Dr., Cristina Tejel Dr. Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorMiguel A. Ciriano Dr., Miguel A. Ciriano Dr. [email protected] Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorB. Eva Villarroya Dr., B. Eva Villarroya Dr. Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorRaquel Gelpi, Raquel Gelpi Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorJosé A. López Dr., José A. López Dr. Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorFernando J. Lahoz Dr., Fernando J. Lahoz Dr. Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this authorLuis A. Oro Prof., Luis A. Oro Prof. [email protected] Departamento de Química Inorgánica Instituto de Ciencia de Materiales de Aragón Universidad de Zaragoza-C.S.I.C., 50009-Zaragoza (Spain) Fax: (+34) 976761143Search for more papers by this author First published: 31 October 2001 https://doi.org/10.1002/1521-3757(20011105)113:21 3.0.CO;2-DCitations: 10 The generous financial support from DGES and MCyT-PNI (Projects PB98-641 and BQU2000-1170) is gratefully acknowledged. Read the full textAboutPDF ToolsRequest permissionAdd to favorites 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 Zweikernige Komplexe mit Kopf-Schwanz-Anordnung der Liganden (head-to-tail, HT) eignen sich für den Aufbau von viergliedrigen Iridiumketten, ganz im Widerspruch zu früheren Vorhersagen. Beim Erhitzen lagern sich die erhaltenen HT,HH-Spezies in die thermodynamisch stabileren HH,HH-Verbindungen um (siehe Schema). References 1 For leading references see: Google Scholar 1a R. Clérac, F. A. Cotton, K. R. Dunbar, T. B. Lu, C. A. Murillo, X. P. Wang, J. Am. Chem. Soc. 2000, 122, 2272; 10.1021/ja994051b CASWeb of Science®Google Scholar 1b Y. H. Chen, C. C. Lee, C. C. Wang, G. H. Lee, S. Y. Lai, F. Y. Li, C. Y. Mou, S. M. Peng, Chem. Commun. 1999, 1667; 10.1039/a905001i CASWeb of Science®Google Scholar 1c S. Y. Lai, T. W. Lin, Y. H. Chen, C. C. Wang, G. H. Lee, M. H. Yang, M. K. Leung, S. M. Peng, J. Am. Chem. Soc. 1999, 121, 250; 10.1021/ja982065w CASWeb of Science®Google Scholar 1d F. A. 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Google Scholar 5 Selected analytical and spectroscopic data for the new complexes: Complex 1: elemental analysis (%) calcd for C14H8N2O6Ir2: C 24.56, H 1.18, N 4.09; found: C 24.95, H 1.47, N 4.18; IR (toluene): =ν(CO)=2079 (s), 2048 (m), 2002 (s) cm−1; 1H NMR (C6D6, 333 K): HH isomer: δ=7.64 (d, J=6.9 Hz, 2 H), 6.60 (ddd, J=8.7, 6.9, 1.8 Hz, 2 H), 6.36 (d, J=8.7 Hz, 2 H), 5.77 (t, J=6.9 Hz, 2 H); HT isomer δ=7.53 (d, J=6.9 Hz, 2 H), 6.60 (ddd, J=8.7, 6.9, 1.8 Hz, 2 H), 6.31 (d, J=8.7 Hz, 2 H), 5.77 (t, J=6.9 Hz, 2 H). Complex 2: elemental analysis (%) calcd for C28H16N4O12Ir4I2: C 20.72, H 0.99, N 3.45; found: C 20.94, H 1.18, N 3.25; IR (toluene): =ν(CO)=2110 (w), 2093 (s), 2066 (m), 2052 (s), 2027 (w) cm−1; 1H NMR (C6D6, 295 K): δ=9.52 (dd, 4 H), 6.47 (ddd, 4 H), 6.26 (dd, 4 H), 5.73 (td); 13C{1H} NMR (C6D6, 295 K): δ=175.3, 167.2 (CO), 165.5 (CO), 152.7, 139.8, 116.7, 115.7. Complex 3: elemental analysis (%) calcd for C28H16N4O12Ir4I2: C 20.72, H 0.99, N 3.45; found: C 20.52, H 0.78, N 3.44; IR (nujol): =ν(CO)=2087 (s), 2071 (m) 2050 (sh), 2041 (s) 2006 (m) cm−1; 1H NMR: δ=9.65 (dd, 1 H), 9.52 (dd (1 H), 9.48 (dd, 1 H), 9.21 (dd, 1 H), 6.56 (m, 2 H), 6.53 (m (1 H), 6.45 (m, 1 H), 6.38 (dd, 1 H), 6.33 (dd, 1 H), 6.20 (dd, 1 H), 6.10 (dd, 1 H), 5.90 (td, 1 H), 5.86 (td, 1 H), 5.74 (m, 2 H). Google Scholar 6 Google Scholar 6a Crystallographically imposed twofold symmetry was observed relating the two halves of the tetranuclear complex. Crystal data for 2: C28H16I2Ir4N4O12, Mr=1623.04, laminar crystal (0.14×0.11×0.06 mm), monoclinic, space group C2/c, a=27.709(3), b=9.2163(10), c=16.9592(17) Å, β=124.274(2)°, V=3578.9(6) Å−3, Z=4, ρcalcd=3.012 g cm−3, F(000)=2888, T=150(2) K, MoKα radiation (λ=0.71073 Å, μ=16.615 mm−1). Data collected with a Bruker SMART APEX CCD diffractometer. Of 5545 measured reflections (2θ: 5–50°, ω scans 0.3°), 2662 were unique (Rint=0.0808); a multiscan absorption correction was applied (PLATON program) with min./max. transmission factors of 0.204/0.436. Structure solved by Patterson and difference-Fourier maps; refined using SHELXTL. Final agreement factors were R1=0.0808 (1965 observed reflections, F 2>4σ(F 2)) and wR2=0.2264; data/restrains/parameters 2662/72/227; GOF=1.039. Largest peak and hole in the final difference map 6.084 and −3.483 e Å−3. The limited quality of the structural data (also the merging and agreement factors, and the high residuals) should be necessarily associated to the diffracting weakness, to the anisotropic morphology, and to the high absorption of the crystals. Google Scholar 6b Crystallographic data (excluding structure factors) for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication nos. CCDC-165456 (2) and CCDC-165457 (3⋅2 CH4O). Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax: (+44) 1223-336-033; e-mail: [email protected]). Google Scholar 7 Crystal data for 3⋅2 CH4O: C28H16I2Ir4N4O12⋅2 CH4O, Mr=1687.13, triclinic, space group P, a=10.2440(8), b=13.4751(10), c=15.2437 (11) Å, α=75.8696(15), β=71.2963(13), γ=78.1790(15)°, V=1914.4(2) Å−3, Z=2, ρcalcd=2.927 g cm−3, F(000)=1516, T=150(2) K, MoKα radiation (λ=0.71073 Å, μ=15.541 mm−1). Data collected as described for 3 with an elongated block (0.20×0.06×0.04 mm). Of 10 303 measured reflections (2θ: 5–50°, ω scans 0.3°), 6555 were unique; a multiscan absorption correction was performed (SADABS program) with min./max. transmission factors of 0.119/0.583. Structure solution and refinement as described for 2. Final agreement factors were R1=0.0656 (4735 observed reflections) and wR2=0.1606. Data/restrains/parameters 6555/61/487; GOF=1.049. Largest peak and hole in the final difference map 3.638 and −2.464 e Å−3.[6b] Google Scholar Citing Literature Volume113, Issue21November 5, 2001Pages 4208-4210 This is the German version of Angewandte Chemie. Note for articles published since 1962: Do not cite this version alone. Take me to the International Edition version with citable page numbers, DOI, and citation export. We apologize for the inconvenience. ReferencesRelatedInformation
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