Co-ordination chemistry of higher oxidation states. Part 35. Synthetic, spectroscopic, and electrochemical studies of some mer- and fac-[OsL3X3]/[OsL3X3]+ systems (L = PR3, AsR3, SbR3, or pyridine; X = Cl or Br): crystal structure of fac-[Os(PEt2Ph)3Cl3]·CH2Cl2
作者： Robert A. Cipriano , William Levason , Roy A. S. Mould , Derek Pletcher , Michael Webster
DOI: 10.1039/DT9900002609
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摘要: The complexes mer-[OsL3X3](L = PMe3,PEt3, PEt2Ph, PEtPh2, or AsEt3; X Cl Br) are oxidised by HNO3–HBF4 to mer-[OsL3X3]BF4; fac- and mer-[Os(py)3X3]BF4(py pyridine) were obtained similarly, but attempts oxidise fac-[OsL′3Cl3](L′= PR3 AsR3) mer-[Os(SbPh3)3X3] OsIV failed. osmium(IV) characterised i.r., u.v.-visible, 31P n.m.r. spectroscopies, magnetic conductance measurements, their properties compared with those of the osmium(III) analogues. Cyclic voltammetry showed that most mer-[OsL3X3]0/+ fac-[Os(py)3X3]0/+ couples electrochemically reversible, fac-[OsL′3Cl3] exhibited only completely irreversible oxidation waves at highly positive potentials. X-ray structure fac-[Os(PEt2Ph)3Cl3]·CH2Cl2 has been determined: space group P a= 18.606(2), b= 10.088(2), c= 10.011 (4)A;, α= 107.91 (3), β= 97.23(3), γ= 94.85(1)°, Z= 2; Os–Cl 2.442(3)–2.449(2), Os–P 2.375(2)–2.380(3)A.
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sci-hub.se 参考文章(30)
James A. Ibers, Lonsdale, Kathleen, Dame, John S. Kasper, Gerard D. Rieck, Walter C. Hamilton, Norman Fordyce McKerron Henry, Caroline H. MacGillavry, International tables for X-ray crystallography UT Back-in-Print Service. ,(1962)
J. Lewis, F. E. Mabbs, R. A. Walton, The preparation, infrared spectra, and magnetic properties of some ruthenium(II), ruthenium(III), and osmium(III) complexes Journal of the Chemical Society A: Inorganic, Physical, Theoretical. pp. 1366- 1370 ,(1967) , 10.1039/J19670001366
C. C. Hinckley, M. Matusz, P. D. Robinson, Structure of mer-tribromotris(triphenylstibine)osmium(III) Acta Crystallographica Section C-crystal Structure Communications. ,vol. 44, pp. 1829- 1831 ,(1988) , 10.1107/S0108270188007218
John D. Buhr, Jay R. Winkler, Henry Taube, Characterization and reactions of osmium(IV) ammines Inorganic Chemistry. ,vol. 11, pp. 2416- 2425 ,(1980) , 10.1021/IC50210A048
Robert A. Cipriano, William Levason, Derek Pletcher, Nigel A. Powell, Michael Webster, Co-ordination chemistry of higher oxidation states. Part 23. Synthesis and properties of tetrahalogenoiridium(IV) complexes, [IrL2X4][X = Cl or Br; L = pyridine, PR3, AsR3, SbR3, SR2, or SeR2]. Crystal and molecular structure of trans-[Ir(AsEt3)2Br4] Journal of the Chemical Society, Dalton Transactions. pp. 1901- 1910 ,(1987) , 10.1039/DT9870001901
Bernard Bell, Joseph Chatt, G. Jeffery Leigh, Hydrido-complexes of osmium(II) and osmium(IV) Journal of The Chemical Society-dalton Transactions. pp. 997- 1004 ,(1973) , 10.1039/DT9730000997
Rusmidah Ali, Simon J. Higgins, William Levason, Osmium(III) and Osmium(IV) complexes of bi- and polydentate thioethers Inorganica Chimica Acta. ,vol. 84, pp. 65- 69 ,(1984) , 10.1016/S0020-1693(00)87670-7
Robert A. Cipriano, Lyall R. Hanton, William Levason, Derek Pletcher, Nigel A. Powell, Michael Webster, Co-ordination chemistry of higher oxidation states. Part 27. Synthesis, properties, and electrochemistry of some cis-tetrahalogenoiridium(IV) complexes: crystal structure of [Ir(phen)Cl4] Journal of the Chemical Society, Dalton Transactions. pp. 2483- 2490 ,(1988) , 10.1039/DT9880002483
Phillip E. Fanwick, Iain F. Fraser, Stephen M. Tetrick, Richard A. Walton, Multiply bonded octahalodiosmate(III) anions. 4. Reactions with nitrogen and phosphorus donor ligands that lead to cleavage of the osmium-osmium triple bond Inorganic Chemistry. ,vol. 26, pp. 3786- 3791 ,(1987) , 10.1021/IC00269A032
Eric G. Hope, William Levason, Stephen G. Murray, Gregory L. Marshall, Synthesis, properties, and 77Se nuclear magnetic resonance studies of platinum metal complexes of two isomeric tris(selenoethers), MeC(CH2SeMe)3 and Se(CH2CH2CH2SeMe)2 Journal of The Chemical Society-dalton Transactions. pp. 2185- 2190 ,(1985) , 10.1039/DT9850002185