W2(μ-H)2Cl4(μ-dppm)2: the bulk synthesis of a bridging hydride
作者： Thomas E. Concolino , Judith L. Eglin , Edward J. Valente , Jeffrey D. Zubkowski
DOI: 10.1016/S0277-5387(97)00167-8
关键词: Singlet state 、 Analytical chemistry 、 Hydride 、 Infrared spectroscopy 、 Proton NMR 、 Crystallography 、 Bond length 、 Bridging (networking) 、 NMR spectra database 、 Chemistry
摘要: Abstract The synthesis of the ditungsten species W2(μ-H)2Cl4(μ-dppm)2 marks first bulk preparation a bridging hydride W(III–III) species. compound retains characteristic edge-sharing bioctahedral (ESBO) geometry with W bond distance 2.3918(7)A. Although several Group VI ESBO complesxes have been prepared, only two groups, and W2(μ-H)2(μ-O2CC6H5)2 Cl2(P(C6H5)3)2, reported to date. complex has characterized with31P1H,1H NMR, UV-vis, IR spectroscopic techniques. A singlet is observed in the31P1H NMR spectra at δ = 20.464 ppm JP−W 126Hz includes tungsten-hydride symmetric stretch 1602 cm−1.
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sci-hub.se 参考文章(34)
F. Albert Cotton, Judith L. Eglin, Bo Hong, Chris A. James, Singlet-triplet separations measured by phosphorus-31{proton} NMR; applications to quadruply-bonded dimolybdenum and ditungsten complexes Inorganic Chemistry. ,vol. 32, pp. 2104- 2106 ,(1993) , 10.1021/IC00062A037
James P. Collman, Louis S. Hegedus, Principles and applications of organotransition metal chemistry ,(1980)
V. Katovic, R. E. McCarley, Preparation of the new heteronuclear hydride-bridged anion MoWCl8H3- and determination of the metal-hydrogen bond distance in Mo2X8H3- (X = chlorine, bromine) by infrared spectroscopy Inorganic Chemistry. ,vol. 17, pp. 1268- 1270 ,(1978) , 10.1021/IC50183A034
F. Albert Cotton, Judith L. Eglin, Bo Hong, Chris A. James, Singlet-triplet separations measured by phosphorus-31 nuclear magnetic resonance spectroscopy. Applications to the molybdenum-molybdenum quadruple bond and to edge-sharing bioctahedral complexes Journal of the American Chemical Society. ,vol. 114, pp. 4915- 4917 ,(1992) , 10.1021/JA00038A074
Kathryn M. Carlson-Day, Thomas E. Concolino, Judith L. Eglin, Chun Lin, Tong Ren, Edward J. Valente, Jeffrey D. Zubkowski, The evaluation of singlet-triplet separations for [W2(μ-H)(μ-Cl)Cl4(μ-dppm)2] and [W2(μ-H)2 (μ-O2CC6H5)2(P(C6H5)3)2] based on 31P NMR and crystallographic data Polyhedron. ,vol. 15, pp. 4469- 4478 ,(1996) , 10.1016/0277-5387(96)00207-0
Jun. Okuda, Robert C. Murray, John C. Dewan, Richard R. Schrock, Peralkylcyclopentadienyl tungsten polyhydride complexes Organometallics. ,vol. 5, pp. 1681- 1690 ,(1986) , 10.1021/OM00139A028
Jo Ann M. Canich, F.Albert Cotton, Synthesis, characterization, and molecular structure of the quadruply bonded ditungsten(ll) complex, W2Cl4(dppm)2 Inorganica Chimica Acta. ,vol. 142, pp. 69- 74 ,(1988) , 10.1016/S0020-1693(00)80660-X
Jo Ann M. Canich, F. Albert Cotton, Lee M. Daniels, Diane B. Lewis, Further study of metal-metal bond lengths in homologous edge-sharing bioctahedral complexes Inorganic Chemistry. ,vol. 26, pp. 4046- 4050 ,(1987) , 10.1021/IC00271A017
William E. Streib, Richard B. Jackson, Crystal and molecular structure of the di-.mu.-chloro ditungsten(III) complex W2Cl6(C5H5N)4.x(CH3)2CO Inorganic Chemistry. ,vol. 10, pp. 1760- 1763 ,(1971) , 10.1021/IC50102A046
Phillip E. Fanwick, William S. Harwood, Richard A. Walton, Bis(diphenylphosphino)methane complexes of the multiply bonded ditungsten(III) core. Structure of W2(.mu.-H)(.mu.-Cl)Cl4(.mu.-dppm)2 Inorganic Chemistry. ,vol. 26, pp. 242- 247 ,(1987) , 10.1021/IC00249A008