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R.C.J. Atkinson et al. / Journal of Organometallic Chemistry 692 (2007) 2076–2085
4.6. Synthesis of [{Co2(CO)6}2{l-g2:l-g2-
OCH2C2C2CH2OGePh2}] (6)
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To a solution of 1a (0.50 g, 0.733 mmol) and Cl2GePh2
(0.20 mL, 0.950 mmol) in tetrahydrofuran (150 mL) at
ꢀ78 ꢁC, was added n-BuLi (1.84 mL, 2.932 mmol). The
solution was allowed to warm to room temperature and
after 16 h the mixture was filtered through a florisil pad
(2 · 5 cm). The solvent was removed on a rotary evapora-
tor, the residue dissolved in dichloromethane and adsorbed
onto florisil. The florisil was pumped dry and added to the
top of a chromatography column. Elution with hexane
afforded brown crystalline 6 (0.33 g, 50%). 13C {1H}
NMR (CDCl3): d 199.4 (CO), 134.4–128.6 (Ph), 101.0,
94.5 (C„C), 65.7 (CH2).
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4.7. Crystallographic studies
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Single crystal X-ray diffraction data for 2, 3, 5a, 5b and 6
were collected using a Nonius-Kappa CCD diffractometer,
equipped with an Oxford Cryosystems cryostream and
˚
employing Mo Ka (k = 0.71073 A) irradiation from a
(f) F. Demirhan, S. Irisli, S.N. Salek, O.S. Senturk, M.J. Went, J.C.
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sealed tube X-ray source. Cell refinement, data collection
and data reduction were performed with the programs
DENZO [18] and COLLECT [19] and multi-scan absorption cor-
rections were applied to all intensity data with the program
SORTAV [20]. All structures were solved and refined with the
programs SHELXS97 and SHELXL97 [21], respectively. Hydro-
gen atoms were included in calculated positions (C–
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˚
H = 0.96 A) riding on the bonded atom with isotropic dis-
[7] (a) J.E. Davies, L.J. Hope-Weeks, M.J. Mays, P.R. Raithby, Chem.
Commun. (2000) 1411;
placement parameters set to 1.5 Ueq(C) for methyl H atoms
and 1.2 Ueq(C) for all other H atoms. Details of the data
collection, refinement and crystal data are listed in Table 6.
(b) L.J. Hope-Weeks, M.J. Mays, A.D. Woods, J. Chem. Soc.,
Dalton Trans. (2002) 1812.
[8] V.B. Golovko, L.J. Hope-Weeks, M.J. Mays, M. McPartlin, A.M.
Sloan, A.D. Woods, New J. Chem. 28 (2004) 527.
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(1994) 241;
Acknowledgements
We acknowledge the financial support of the EPSRC
(L.J.H.-W) and Dstl. Fort Halstead (L.J.H.-W). The help
of the EPSRC mass spectrometry service, Swansea is grate-
fully acknowledged. Dr. John E. Davies is thanked for
crystal structure determinations.
(b) A. Osella, L. Milone, C. Nervi, M. Ravera, Eur. J. Inorg. Chem.
(1998) 1473;
(c) H. Amouri, C. Da Silva, B. Malezieux, R. Andres, J. Vaissermann,
M. Gruselle, Inorg. Chem. 39 (2000) 5053.
[10] L.J. Hope-Weeks, M.J. Mays, G.A. Solan, Eur. J. Inorg. Chem.,
submitted for publication.
[11] (a) X.-N. Chen, J. Zhang, S.-L. Wu, Y.-Q. Yin, W.-L. Wang, J. Sun,
J. Chem. Soc., Dalton Trans. (1999) 1987;
Appendix A. Supplementary material
(b) C.E. Housecroft, B.F.G. Johnson, M.S. Khan, J. Lewis, P.R.
Raithby, M.E. Robson, D.A. Wilkinson, Dalton (1992) 3171.
[12] (a) V.B. Golovko, M.J. Mays, A.D. Woods, New J. Chem. 26 (2002)
1706;
CCDC 626871, 626872, 626873, 626874 and 626875 con-
tain the supplementary crystallographic data for 2, 3, 5a,
5b and 6. These data can be obtained free of charge via
the Cambridge Crystallographic Data Centre, 12 Union
Road, Cambridge CB2 1EZ, UK; fax: (+44) 1223-336-
033; or e-mail: deposit@ccdc.cam.ac.uk. Supplementary
data associated with this article can be found, in the online
(b) B.F.G. Johnson, J. Lewis, P.R. Raithby, D.A. Wilkinson, J.
Organomet. Chem. 408 (1991) C9;
(c) E. Champeil, S.M. Draper, J. Chem. Soc., Dalton Trans. (2001)
1440;
(d) M.B. Nielsen, N.F. Utesch, N.N.P. Moonen, C. Boudon, J.-P.
Gisselbrecht, S. Concilio, S.P. Piotto, P. Seiler, P. Gunter, M. Gross,
F. Diederich, Chem.-Eur. J. 8 (2002) 3601;
(e) M.I. Bruce, B.W. Skelton, M.E. Smith, A.H. White, Aust. J.
Chem. 52 (1999) 431;
(f) Quan-Ling Suo, Li-Min Han, Yi-Bing Wang, Jie-Hui Ye, Ning
Zhu, Xue-Bing Leng, Jie Sun, J. Coord. Chem. 57 (2004) 1591.
[13] Calculated from a CCDC search, F.H. Allen, O. Kennard, Chemical
Design Automation News 8 (1993) 31.
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