Treatment of the activated trirhenium cluster H3Re3(CO)10(MeCN)2 with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd) in CH2Cl2 does not afford the expected cluster product H3Re3(CO)10(bpcd) but rather the mononuclear complex fac-ClRe(CO)3(bpcd). The identity of fac-ClRe(CO)3(bpcd) was determined in solution by IR and NMR (1H and 31P) spectroscopies and the solid-state structure was established by X-ray diffraction analysis. fac-ClRe(CO)3(bpcd) crystallizes in the triclinic space P-1, a = 9.958(2) Å, b = 11.991(3) Å, c = 13.676(3) Å, α = 73.230(4)°, β = 73.806(4)°, γ = 77.409(4)°, V = 1484.6(6) Å3, Z = 2, and d calc = 1.723 Mg/m3; R = 0.0367, R w = 0.0857 for 4253 reflections with I > 2σ(l).
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Wei, C.-Y.; Garlaschelli, L.; Bau, R.; Koetzle, T.F. J. Organomet. Chem. 1981, 213, 63. (b) Ciani, G.; Sironi, A.; D'Alfonso, G.; Romiti, P.; Freni, M. J. Organomet. Chem. 1983, 254, C37. (c) Beringhelli, T.; D'Alfonso, G.; Freni, M.; Ciana, G.; Moret, M.; Sironi, A. J. Chem. Soc., Dalton Trans. 1989, 1143. (d) Adams, R.D.; Falloon, S.B. J. Am. Chem. Soc. 1994, 116, 10540. (e) Adams, R.D.; Kwon, O.-S.; Perrin, J.L. J. Organomet. Chem. 2000, 596, 102.
Prest, D.W.; Mays, M.J.; Raithby, P.R.; Orpen, A.G. J. Chem. Soc., Dalton Trans. 1982, 737. (b) Prest, D.W.; Mays, M.J.; Orpen, A.G.; McMullan, R.K. J. Organomet. Chem. 1982, 240, 395.
For the structure of H3Re3(CO)9(triphos), see: Wang, S.R.; Wang, S.-L.; Cheng, C.P.; Yang, C.S. J. Organomet. Chem. 1992, 431, 215.
(a) Bott, S.G.; Shen, H.; Richmond, M.G. J. Organomet. Chem. 2004, 689, 3426. (b) Watson, W.H.; Kandala, S.; Richmond, M.G. J. Chem. Crystallogr. 2005, 35, 157. (c) Bott, S.G.; Shen, H.; Senter, R.A.; Richmond, M.G. Organometallics 2003, 22, 1953. (d) Watson, H.; Zhao, Y.; Richmond, M.G. J. Chem. Crystallogr. 2003, 33, 765.
Andrews, M.A.; Kirtley, S.W.; Kaesz, H.D. Inorg. Synth. 1975, 17, 66.
Adams, R.D.; Cortopassi, J.E.; Falloon, S.B. Organometallics 1992, 11, 3794.
(a) Fenske, D.; Becher, H. Chem. Ber. 1974,107, 117. (b) Fenske, D. Chem. Ber. 1979, 112, 363.
Shriver, D.F. The Manipulation of Air-Sensitive Compounds ; McGraw-Hill: New York, 1969.
Saint Version 6.02, Bruker Analytical X-ray Systems, Inc. Copyright 1997–1999.
SHELXTL Version 5.1, Bruker Analytical X-ray Systems, Inc. Copyright 1998.
PLATON–A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands, Speck, A.L. (2001).
Epstein, R.A.; Gaffhey, T.R.; Geoffroy, G.L.; Gladfelter, W.L.; Henderson, R.S. Am. Chem. Soc. 1979, 101, 3847.
Cotton, F.A. Chemical Applications of Group Theory ; Wiley: New York, 1971, 2nd ed.
Coltrup, N.B.; Daly, L.H.; Wiberley, S.E. Introduction to Infrared and Raman Spectroscopy ; Academic Press: New York, 1990.
(a) Bott, S.G.; Lee, S.-W.; Yang, K.; Richmond, M.G. J. Chem. Crystallogr. 2005, 35, 203. (b) Bott, S.G.; Yang, K.; Richmond, M.G. J. Chem. Crystallogr. 2005, 35, 719. (c) Yang, K.; Bott, S.G.; Richmond, M.G. Organometallics 1995, 14, 2387. (d) Frantz, S.; Rail, J.; Hartenbach, I.; Schleid, T.; Zalis, S.; Kaim, W. J. Eur. Chem. 2004, 10, 149.
Gibson, D.H.; Haiyang, H.; Mashuta, M.S. Organometallics 2001, 20, 1456. (b) Bucknor, S.; Cotton, F.A.; Falvello, L.F.; Reid, A.H.; Jr.; Schmulbach, C.D. Inorg. Chem. 1986, 25, 1021. (c) da Silva, M.F.C.G.; Ferreira, C.M.P.; da Silva, J.J.R.F.; Pombeiro, A.J.L. J. Chem. Soc., Dalton Trans. 1998, 4139. (d) Huhmann-Vincent, J.; Scott, B.L.; Kubas, G.L. Inorg. Chem. 1999, 38, 115. (e) MiUer, T.M.; Ahmed, K.J.; Wrighton, M.S. Inorg. Chem. 1989, 28, 2347.
(a) Xia, C.-G.; Bott, S.G.; Wu, G.; Richmond, M.G. J. Chem. Crystallogr. 2004, 34, 513. (b) Watson, W.H.; Huang, S.-H.; Richmond, M.G. J. Chem. Crystallogr. 2004, 34, 627.
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Financial support from the Robert A. Welch Foundation (Grants P-0074-WHW and B-1093-MGR) is appreciated.
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Watson, W.H., Kandala, S. & Richmond, M.G. Chlorine-atom abstraction and cluster fragmentation in the reaction of H3Re3(CO)10(MeCN)2 with the diphosphine ligand 4,5-bis(diphenylphosphino)-4-cyclopenten-1,3-dione (bpcd): X-ray diffraction structure of fac-ClRe(CO)3(bpcd). J Chem Crystallogr 36, 71–75 (2006). https://doi.org/10.1007/s10870-005-9029-y
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DOI: https://doi.org/10.1007/s10870-005-9029-y