Asymmetry, 1997, 8, 991; (c) M. Pabel, A. C. Willis and S. B.
Wild, Inorg. Chem., 1996, 35, 1244.
J. M. Vila, M. T. Pereira, J. M. Ortiguera, J. J. Fernandez, A.
Fernandez, M. Lopez-Torres and H. Adams, Organometallics,
1999, 18, 5484.
(a) H. Brunner, Angew. Chem., Int. Ed., 1999, 38, 1195; (b) M. R.
Meneghetti, M. Grellier, M. Pfe†er, J. Dupont and J. Fischer,
Organometallics, 1999, 18, 5560.
beam time, and the orientation of the crystal was checked
after every 400 intensity measurements. Absorption
corrections26 were based on azimuthal scans of 10 (4) or 12 (7)
reÑections that have Eulerian angle s spread between 50 and
[40¡ when in their bisecting positions. Accurate unit cell
dimensions were determined from 25 centered reÑections in
the 2h range 27.2 O 2h O 31.9¡ (4) or 24.0 O 2h O 35.0¡ (7),
each centered at four distinct goniometer positions. The struc-
tures were solved and developed by Patterson and Fourier
methods.27 All non-hydrogen atoms were reÐned with aniso-
tropic displacement parameters. The hydrogen atoms were
placed in idealized positions and treated as riding atoms,
except for those of the methyl groups, which were Ðrst located
in a local slant-Fourier calculation and then reÐned as riding
atoms with the torsion angles about the OÈC(methyl) bonds
treated as variables. Each hydrogen atom was assigned an iso-
tropic displacement parameter equal to 1.2 times the equiva-
lent parameter of its parent atom. The interstitial chloroform
8
9
10 R. Navarro and E. P. Urriolabeitia, J. Chem. Soc., Dalton T rans.,
1999, 4111 and references therein.
11 R. Navarro, J. Garc•a, E. P. Urriolabeitia, C. Cativiela and M. D.
D•az-de-Villegas, J. Organomet. Chem., 1995, 490, 35.
12 (a) C. R. Baar, L. P. Carbray, M. C. Jennings and R. J. Pud-
dephatt, J. Am. Chem. Soc., 2000, 122, 176; (b) A. J. Canty, J.
Patel, B. W. Skelton and A. H. White, J. Organomet. Chem., 2000,
599, 195; (c) B. Teijido, A. Fernandez, M. Lopez-Torres, S.
CastroÈJuiz, A. Suarez, J. M. Ortigueira, J. M. Vila and J. J.
Fernandez, J. Organomet. Chem., 2000, 598, 71 and references
therein; (d) G. W. V. Cave, N. W. Alcock and J. P. Rourke,
Organometallics, 1999, 18, 1801; (e) D. J. Cardenas, A. M. Echa-
varren and M. C. Ram•rez de Arellano, Organometallics, 1999, 18,
3337; ( f ) M. Albrecht, R. A. Gossage, A. L. Spek and G. van
Kooten, J. Am. Chem. Soc., 1999, 121, 11898; (g) A. El Hatimi, M.
Gomez, S. Jansat, G. Muller, M. FontÈBardia and X. Solans, J.
Chem. Soc., Dalton T rans., 1998, 4229; (h) M. H. T. Rietveld,
D. M. Grove and G. van Koten, New J. Chem., 1997, 21, 751; (i)
P. Steenwinkel, S. L. James, D. M. Grove, H. Kooijman, A. L.
Spek and G. van Koten, Organometallics, 1997, 16, 513; ( j) P.
Dani, T. Karlen, R. A. Gossage, W. J. J. Smeets, A. L. Spek and
G. van Koten, J. Am. Chem. Soc., 1997, 119, 11317; (k) J. M. Vila,
M. Gayoso, M. T. Pereira, M. Lopez-Torres, J. J. Fernandez, A.
Fernandez and J. M. Ortigueira, J. Organomet. Chem., 1996, 506,
165 and references therein.
in 4 É CHCl was disordered and modelled as three equally
3
populated congeners and their geometrical parameters
restrained to be similar. The geometrical parameters of the
perchlorate anion in 7 were also restrained to similarity. The
structure was reÐned to F 2 and all reÑections were used in
o
the least-squares calculations.28 Data reduction was done
using the program XCAD4B.29
suppdata/nj/b0/b006140i/ for crystallographic Ðles in .cif
format.
13 (a) A. Fernandez, M. Lopez-Torres, A. Suarez, J. M. Ortigueira,
T. Pereira, J. J. Fernandez, J. M. Vila and H. Adams, J.
Organomet. Chem., 2000, 598, 1; (b) D. R. Billodeaux, F. R.
Fronczek, A. Yoneda and G. R. Newkome, Acta Crystallogr.,
Sect. C, 1998, 54, 1439; (c) P. Arndt, C. Lefeber, R. Kempe and U.
Rosenthal, Chem. Ber., 1996, 129, 207; (d) L. A. van de Kuil,
Y. S. J. Veldhuizen, D. M. Grove, J. W. Zwikker, L. W. Jennes-
kens, W. Drenth, W. J. J. Smeets, A. L. Spek and G. van Koten,
J. Organomet. Chem., 1995, 488, 191; (e) A. Yoneda, T. Hakusi,
G. R. Newkome and F. R. Fronczek, Organometallics, 1994, 13,
4912; ( f ) A. Yoneda, G. R. Newkome, Y. Morimoto, Y. Higuchi
and N. Yasuoka, Acta Crystallogr., Sect. C, 1993, 49, 476.
14 A. Bader and E. Lindner, Coord. Chem. Rev., 1991, 108, 27.
Recent references about hemilability; (a) J. C. Shi, C. H. Yueng,
D. X. Wu, Q. T. Liu and B. S. Kang, Organometallics, 1999, 18,
3796; (b) E. Lindner, M. Schmid, P. Wegner, C. Nachtigal, M.
Steimann and R. Fawzi, Inorg. Chim. Acta, 1999, 296, 103
15 (a) N. H. Kiers, B. L. Feringa, H. Kooijman, A. L. Spek and
P. W. N. M. van Leeuwen, J. Chem. Soc., Chem. Commun., 1992,
1169; (b) P. L. Alsters, J. Boersma, W. J. J. Smeets, A. L. Spek
and G. van Koten, Organometallics, 1993, 12, 1639; (c) G. H.
Quek, P. H. Leung and K. F. Mok, Inorg. Chim. Acta, 1995, 239,
185; (d) C. Price, N. H. Rees, M. R. J. Elsegood, W. Clegg and A.
Houlton, J. Chem. Soc., Dalton T rans., 1998, 2001.
Acknowledgements
Funding by the Direccion General de Ensenanza Superior e
Investigacion Cient•Ðca (Spain, projects PB98-1595-C02-01
and PB98-1593) is gratefully acknowledged, and we thank
Prof. J. Fornies for invaluable logistical support.
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351