6 K. Hashizume, Y. Mizobe and M. Hidai, Organometallics, 1996, 15,
data collection parameters are summarized in Table 5. For 8,
space group P21 with Z = 4 was chosen, because additional
centers of symmetry could not be found. The correctness of
this choice has been suggested by the Flack parameter of
Ϫ0.017(10).
3303.
7 H. Seino, Y. Mizobe and M. Hidai, New J. Chem., 2000, 24, 907.
8 (a) T. Masumori, H. Seino, Y. Mizobe and M. Hidai, Inorg. Chem.,
2000, 39, 5002; (b) T. Kochi, Y. Nomura, Z. Tang, Y. Ishii, Y. Mizobe
and M. Hidai, J. Chem. Soc., Dalton Trans., 1999, 2575; (c) Z. Tang,
Y. Nomura, S. Kuwata, Y. Ishii, Y. Mizobe and M. Hidai, Inorg.
Chem., 1998, 37, 4909; (d ) S. Kuwata, M. Andou, K. Hashizume,
Y. Mizobe and M. Hidai, Organometallics, 1998, 17, 3429;
(e) Z. Tang, Y. Nomura, Y. Ishii, Y. Mizobe and M. Hidai,
Organometallics, 1997, 16, 151.
9 (a) S. Kuwata, S. Kabashima, Y. Ishii and M. Hidai, J. Am. Chem.
Soc., 2001, 123, 3826; (b) S. Kuwata, S. Kabashima, N. Sugiyama,
Y. Ishii and M. Hidai, Inorg. Chem., 2001, 40, 2034; (c) S.
Kabashima, S. Kuwata, K. Ueno, M. Shiro and M. Hidai, Angew.
Chem., Int. Ed., 2000, 39, 1128; (d ) S. Kabashima, S. Kuwata and
M. Hidai, J. Am. Chem. Soc., 1999, 121, 7837.
10 T. Nagano, S. Kuwata, Y. Ishii and M. Hidai, Organometallics, 2000,
19, 4176.
11 R. R. Schrock and J. A. Osborn, J. Am. Chem. Soc., 1971, 93, 2397.
12 C. K. Johnson, ORTEP, Report ORNL-5138, Oak Ridge National
Laboratory, Oak Ridge, TN, 1976.
13 R. A. Sánchez-Delgado, V. Herrera, C. Bianchini, D. Masi and
C. Mealli, Inorg. Chem., 1993, 32, 3766.
14 V. Herrera, A. Fuentes, M. Rosales, R. A. Sánchez-Delgado,
C. Bianchini, A. Meli and F. Vizza, Organometallics, 1997, 16,
2465.
Structure solution and refinements were conducted using
the TEXSAN program package.27 The positions of the non-
hydrogen atoms were determined by DIRDIF PATTY28 and
were refined anisotropically. Hydrogen atoms were placed at
calculated positions and included at the final stages of refine-
ments with fixed parameters. For 4ЈؒMe2CO, the BPh4 anion
occupies two disordered positions with the same occupancies.
The carbon atoms in the solvating Me2CO as well as the hydride
hydrogens found in the Fourier map were refined isotropically.
However, the hydrosulfido protons could not be located at
reasonable positions and were not included in the refinements.
The hydrosulfido hydrogens in 7 were located from the Fourier
map and refined isotropically, while the carbon atoms in the
solvating Me2CO with 50% occupancy for 8ؒ0.75Me2CO were
refined using isotropic parameters.
Crystal data for 10ؒ0.5CH2Cl2 are as follows. C46.5H41F6P3-
S2ClWIr, M = 1282.39, monoclinic, space group P21/a (no. 14),
a = 15.155(4), b = 19.601(4), c = 17.635(4) Å, β = 112.51(2)Њ, V =
4839.2(2) Å3, room temperature, Z = 4, µ(Mo-Kα) = 54.28 cmϪ1
,
15 K. Prout and G. V. Rees, Acta Crystallogr., Sect. B, 1974, 30, 2249.
16 C. J. Casewit, D. E. Coons, L. L. Wright, W. K. Miller and
M. Rakowski DuBois, Organometallics, 1986, 5, 951.
17 C. Bianchini, C. Mealli, A. Meli and M. Sabat, Inorg. Chem., 1986,
25, 4617.
18 Z. K. Sweeney, J. L. Polse, R. G. Bergman and R. A. Andersen,
Organometallics, 1999, 18, 5502.
SHELX-97,29 R1 = 0.053, wR2 = 0.170 for 7311 reflections with
I > 3.00σ(I ) and 601 variables.
CCDC reference numbers 170943–170946.
tallographic data in CIF or other electronic format.
19 (a) J. C. Bayón, C. Claver and A. M. Masdeu-Bultó, Coord. Chem.
Rev., 1999, 193–195, 73; (b) M. Rakowski DuBois, Chem. Rev., 1989,
89, 1.
20 For some unique examples reported recently, see for example:
(a) Y. Nishibayashi, M. Yamanashi, I. Wakiji and M. Hidai, Angew.
Chem., Int. Ed., 2000, 39, 2909; (b) T. Wakabayashi, Y. Ishii,
K. Ishikawa and M. Hidai, Angew. Chem., Int. Ed. Engl., 1996, 35,
2123.
Acknowledgements
This work was supported by the JSPS FY2000 and 2001
“Research for the Future Program”.
21 D. I. Gilmour, M. A. Luke and D. M. P. Mingos, J. Chem. Soc.,
Dalton Trans., 1987, 335.
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