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Re 2 I 2 (CO) 6 (Se 7 ), a Coordination Compound of Elemental Selenium with a Transition Metal: A Solution‐ and Solid‐State Study

1994; Wiley; Volume: 33; Issue: 2 Linguagem: Inglês

10.1002/anie.199401931

ISSN

1521-3773

Autores

Alessia Bacchi, Walter Baratta, Fausto Calderazzo, Fabio Marchetti, Giancarlo Pelizzi,

Tópico(s)

Organometallic Complex Synthesis and Catalysis

Resumo

Angewandte Chemie International Edition in EnglishVolume 33, Issue 2 p. 193-195 Communication Re2I2(CO)6(Se7), a Coordination Compound of Elemental Selenium with a Transition Metal: A Solution- and Solid-State Study† Dr. Alessia Bacchi, Dr. Alessia Bacchi Istituto di Chimica Generale ed Inorganica and Centro di Studio CNR per la Strutturistica Diffrattometrica Università di Parma (Italy)Search for more papers by this authorDr. Walter Baratta, Dr. Walter Baratta Dipartimento di Chimica e Chimica Industriale, Sezione di Chimica Inorganica, Università di Pisa, Via Risorgimento 35, I-56126 Pisa (Italy), Telefax: Int. code + (50) 918-260Search for more papers by this authorProf. Dr. Fausto Calderazzo, Corresponding Author Prof. Dr. Fausto Calderazzo Dipartimento di Chimica e Chimica Industriale, Sezione di Chimica Inorganica, Università di Pisa, Via Risorgimento 35, I-56126 Pisa (Italy), Telefax: Int. code + (50) 918-260Dipartimento di Chimica e Chimica Industriale, Sezione di Chimica Inorganica, Università di Pisa, Via Risorgimento 35, I-56126 Pisa (Italy), Telefax: Int. code + (50) 918-260Search for more papers by this authorDr. Fabio Marchetti, Dr. Fabio Marchetti Dipartimento di Chimica e Chimica Industriale, Sezione di Chimica Inorganica, Università di Pisa, Via Risorgimento 35, I-56126 Pisa (Italy), Telefax: Int. code + (50) 918-260Search for more papers by this authorProf. Dr. Giancarlo Pelizzi, Prof. Dr. Giancarlo Pelizzi Istituto di Chimica Generale ed Inorganica and Centro di Studio CNR per la Strutturistica Diffrattometrica Università di Parma (Italy)Search for more papers by this author Dr. Alessia Bacchi, Dr. Alessia Bacchi Istituto di Chimica Generale ed Inorganica and Centro di Studio CNR per la Strutturistica Diffrattometrica Università di Parma (Italy)Search for more papers by this authorDr. Walter Baratta, Dr. Walter Baratta Dipartimento di Chimica e Chimica Industriale, Sezione di Chimica Inorganica, Università di Pisa, Via Risorgimento 35, I-56126 Pisa (Italy), Telefax: Int. code + (50) 918-260Search for more papers by this authorProf. Dr. Fausto Calderazzo, Corresponding Author Prof. Dr. Fausto Calderazzo Dipartimento di Chimica e Chimica Industriale, Sezione di Chimica Inorganica, Università di Pisa, Via Risorgimento 35, I-56126 Pisa (Italy), Telefax: Int. code + (50) 918-260Dipartimento di Chimica e Chimica Industriale, Sezione di Chimica Inorganica, Università di Pisa, Via Risorgimento 35, I-56126 Pisa (Italy), Telefax: Int. code + (50) 918-260Search for more papers by this authorDr. Fabio Marchetti, Dr. Fabio Marchetti Dipartimento di Chimica e Chimica Industriale, Sezione di Chimica Inorganica, Università di Pisa, Via Risorgimento 35, I-56126 Pisa (Italy), Telefax: Int. code + (50) 918-260Search for more papers by this authorProf. Dr. Giancarlo Pelizzi, Prof. Dr. Giancarlo Pelizzi Istituto di Chimica Generale ed Inorganica and Centro di Studio CNR per la Strutturistica Diffrattometrica Università di Parma (Italy)Search for more papers by this author First published: February 1, 1994 https://doi.org/10.1002/anie.199401931Citations: 23 † This work was supported by the Consiglio Nazionale delle Ricerche (CNR, Rome), Progetto Finalizzato Materiali Speciali per Tecnologie Avanzate and by the Ministero dell'Università e della Ricerca Scientifica e Tecnologica (MURST). We thank Prof. P. S. Pregosin, Laboratorium für Anorganische Chemie der E. T. H., Zürich, for providing NMR facilities and discussing the NMR spectra during the sabbatical of W. B. 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 The cyclo-Se7 ligand is bound to two rhenium(I) centers in the title compound 1 (depicted on the right). It arises in the reaction of [Re2I2(CO)6(thf)2] with freshly sublimed elemental selenium in CS2 and is the first complex that contains a discrete molecule of an allotropic modification of selenium as a ligand. These findings add to the understanding of the mechanism of oxidation of metals and low-valent metal complexes by chalcogens. References 1 W. Baratta, F. Calderazzo, Organometallics 1993, 12, 1489. 10.1021/om00029a001 CASWeb of Science®Google Scholar 2 G. J. Kubas, Acc. Chem. Res. 1988, 21, 120. 10.1021/ar00147a005 Web of Science®Google Scholar 3 J. A. M. van Beek, G. van Koten, G. P. C. M. Dekker, E. Wissing, M. C. Zoutberg, C. H. Stam, J. Organomet, Chem. 1990, 394, 659. 10.1016/0022-328X(90)87260-K CASWeb of Science®Google Scholar 4(a) L. Linford, H. G. Raubenheimer, Adv. Organomet, Chem. 1991, 32, 1; 10.1016/S0065-3055(08)60478-5 CASWeb of Science®Google Scholar(b) A. Müller, E. Diemann, Adv. Inorg. Chem. 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The red sublimed Sen was scraped from the cold finger and kept at about −30 °C until it was used for the subsequent reaction with the rhenium (I) complex. A solution of the sublimed Sen, in CS2 at room temperature slowly deposited monoclinic α-Se8 as shown by comparison of the cell constants of the precipitate (a = 9.068, b = 9.080, c = 11.572 Å, β = 90.75) with the literature data [8]. No or incomplete reaction was observed between the rhenium (I) carbonyl complex and gray elemental selenium Commercial selenium carefully prewashed with carbon disulfide did not react. Google Scholar 8 P. Cherin, P. Unger, Acta Crystallogr. Sect. B 1972, 28, 313, 10.1107/S0567740872002249 CASWeb of Science®Google Scholar 9(a) N. P. Luthra, J. D. Odom in The Chemistry of Organic Selenium and Tellurium Compounds, Vol, 1 (Eds.: S. Patai, Z. Rappoport), Wiley, New York. 1986; Google Scholar(b) L. Christiaens, J. L. Piette, L. Laitem, M. Baiwir, J. Denoel, G. Llabres, Org. Magn. 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Structure solution with Patterson method [12a], structure refinement of F2 (224 refined parameters against 7105 reflections) with SHELX92 [12b]; empirical absorption according to Walker an Stuart [12c] applied after the last isotropic refinement. Final R values: R = 0.0573 for 4422 observed reflections |I ≥ 2 σ (I)| and 0.1172 for all data; wR2 = 0.1795 with w = 1/|σ2(F + (0.1281 P))|, where P = |max(F, O) + 2 F|; GOF = 0.955. Max./min. residual electron density 3.97/ −3.80 eÅ−3. Half a heptane molecule per asymmetric unit is present, disordered about an inversion centre. Structural parameters were calculated with PARST [12d]. Extensive use was made of the Cambridge Structural Database System and of the Crystal Structure Information System (CRYSTIN, Universität Bonn). Calculations were performed on the ENCORE-GOULD-POWERNODE 6040 and ENCORE 91 computers of the Centro di Studio per la Strutturistica Diffrattometrica del CNR, Parma and on the IBM 3081 computer of CNUCE, Pisa. 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