V.G. Albano et al. / Journal of Organometallic Chemistry 649 (2002) 64–69
69
(
(
b) H. Endres, in: G. Wilkinson, R.D. Gillard, J.A. McCleverty
Eds.), Comprehensive Coordination Chemistry, vol. 2, Perga-
3.7. X-ray crystallographic study of 3a
mon, Oxford, 1987, p. 261.
Crystal data and details of the data collection for
[
2] (a) N.M. Doherty, J.A.K. Howard, S.A.R. Knox, N.J. Terril,
M.I. Yates, J. Chem. Soc., Chem. Commun. (1989) 638;
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Yates, J. Chem. Soc., Chem. Commun. (1989) 1680;
complex
[Fe (m-CNMe )(m-CO)(CO)(CH CN)(Cp) ]
2
2
2
2
(
3a) are given in Table 2. The diffraction experiments
were carried out at room temperature on a fully
automated Enraf–Nonius CAD-4 diffractometer using
(
c) M. Akita, R. Hua, S.A.R. Knox, Y. Moro-oka, S. Nakanishi,
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graphite-monochromated Mo–K radiation. The unit
a
cell parameters were determined by a least-squares
fitting procedure using 25 reflections. Data were
corrected for Lorentz and polarization effects. No
decay correction and no absorption correction were
applied. The positions of the metal atoms were found
by direct methods using the SHELXS-86 program [17]
and all the non-hydrogen atoms located from difference
Fourier syntheses. Two fold orientational disorder of
one of the Cp ligands [bound to Fe(1)] around the
metal-ring axis was detected and the site occupation
factors were refined for this ligand, yielding the values
(
d) M. Akita, R. Hua, S. Nakanishi, M. Tanaka, Y. Moro-oka,
Organometallics 16 (1997) 5572.
[3] V.G. Albano, L. Busetto, M. Monari, V. Zanotti, J. Organomet.
Chem. 606 (2000) 163.
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Serra, V.G. Albano, M. Monari, F. Prestopino, F. Laschi, P.
Zanello, Organometallics 14 (1995) 5232.
[
[
5] K. Boss, M.G. Cox, C. Dowling, A.R. Manning, J. Organomet.
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nated Ligands, vol. 2, Plenum Press, New York, 1989, p. 280;
c) D.A. Garnovskii, V.Y. Kukushkin, M. Haukka, G. Wagner,
1
(
0.54 and 0.46, respectively. The hydrogen atoms of the
(
methyl and methylene groups were located from
successive Fourier-difference maps but were added in
calculated positions. The final refinement on F
A.J.L. Pombeiro, J. Chem. Soc. Dalton Trans. (2001) 560 and
reference therein;
2
(
d) R. Bertani, D. Catanese, R.A. Michelin, M. Mozzon, G.
Bandoli, A. Dolmella, Inorg. Chem. Commun. 3 (2000) 16;
e) C.S. Chin, D. Chong, B. Lee, H. Jeong, G. Wong, Y. Do,
proceeded by full-matrix least-squares calculations
(
(SHELXL-97) [18] using anisotropic thermal parameters
Y.J. Park, Organometallics 19 (2000) 638.
for all the non-hydrogen atoms. The cyclopentadienyl
the methyl and the methylene H atoms were assigned
an isotropic thermal parameter 1.2, 1.3 and 1.5 times
Ueq of the carbon atoms to which they were attached.
[
7] V.G. Albano, S. Bordoni, L. Busetto, C. Camiletti, M. Monari,
A. Palazzi, F. Prestopino, V. Zanotti, J. Chem. Soc. Dalton
Trans., (1997) 4665.
8] V.G. Albano, L. Busetto, C. Camiletti, C. Castellari, M. Monari,
V. Zanotti, J. Chem. Soc. Dalton Trans. (1997) 4671.
9] (a) G. Cox, C. Dowling, A.R. Manning, P. McArdle, D. Cun-
ningham, J. Organomet. Chem. 438 (1992) 143;
[
[
4. Supplementary material
(
5
b) K. Boss, C. Dowling, A.R. Manning, J. Organomet. Chem.
09 (1996) 197.
Crystallographic data for the structural analysis have
[10] V.G. Albano, L. Busetto, C. Camiletti, M. Monari, V. Zanotti,
J. Organomet. Chem. 563 (1998) 153.
been deposited with the Cambridge Crystallographic
Data Centre, CCDC no. 174241 for 3a. Copies of this
[
11] S. Bordoni, L. Busetto, C. Camiletti, V. Zanotti, V.G. Albano,
M. Monari, F. Prestopino, Organometallics 16 (1997) 1224.
12] (a) S.I. Murahashi, T. Naota, H. Taki, M. Mizuno, H. Takaya,
S. Komiya, Y. Mizuho, N. Oyasato, M. Hiraoka, M. Hirano, A.
Fukuoka, J. Am. Chem. Soc. 117 (1995) 12436;
[
1
EZ, UK (fax: +44-1233-336033; e-mail: deposit@
ccdc.cam.ac.uk or www: http://www.ccdc.cam.ac.uk).
(b) B.M. Trost, F.D. Toste, A.B. Pinkerton, Chem. Rev. 101
(
2001) 2067.
[
[
[
13] P. Schollhammer, M. Pichon, K.W. Muir, F.Y. P e´ tillon, R.
Pichon, J. Talarmin, Eur. J. Inorg. Chem. (1999) 221.
14] B.T. Sterenberg, R.W. Hilts, G. Moro, R. McDonald, M.
Cowie, J. Am. Chem. Soc. 117 (1995) 245.
15] (a) J.R. Matachek, R.J. Angelici, K.A. Schugart, K. Haller, R.F.
Fenske, Organometallics 3 (1984) 1038;
Acknowledgements
We thank the Ministero dell’Universita’ e della
Ricerca Scientifica e Tecnologica (M.I.U.R.) (project:
‘
New strategies for the control of reactions: interactions
(b) J.R. Matachek, R.J. Angelici, Inorg. Chem. 25 (1986) 2877;
(
c) L. Busetto, V. Zanotti, L. Norfo, A. Palazzi, V.G. Albano,
D. Braga, Organometallics 12 (1993) 190;
d) V.G. Albano, S. Bordoni, L. Busetto, C. Camiletti, M.
Monari, F. Prestopino, V. Zanotti, J. Chem. Soc. Dalton Trans.
1996) 3693.
16] M.H. Quick, R.J. Angelici, Inorg. Chem. 20 (1981) 1123.
of molecular fragments with metallic sites in unconven-
tional species’) and the University of Bologna (‘Funds
for Selected Research Topics’) for financial support.
(
(
[
References
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tion, University of G o¨ ttingen, Germany, 1986.
[
1] (a) B.N. Storhoff, H.C. Lewis Jr., Coord. Chem. Rev. 23 (1977)
[18] G.M. Sheldrick, SHELXL-97, Program for Crystal Structure
Refinement, University of G o¨ ttingen, Germany, 1997.
1
;