[12] J. CaÂmpora, JA LoÂpez, P. Palma, P. Valerga, E. Carmona, Angew. Chem. 1999, 111, 199; Angew. Chem. Int. Ed. Engl. 1999, 38, 147.[13] Crystal data for 4: C48H41BF24P2Pd, Mr 1252.96, monoclinic, space group Pn, a 10.3940 (9), b 9.9127 (8), c 24.819 (2), b 94.565 (2) 8, V 2549.0 (4) 3, Z 2, 1calcd 1.632 Mg mÀ3, T 173 (2) K, l 0.71073, m 0.549 mmÀ1, F (000) 1252, crystal size 0.4 Â 0.2 Â 0.15 mm, V range 2.63 to 23.308; À11 h 11, À 2 k 11, À23 l 23; 6033 reflections (4624 independent, Rint 0.02) were collected at 177 K on a Brucker±Siemens Smart CCD diffractometer, GOF 1.02, R1 0.026 and wR2 0.06 for [I> 2 (I)], R and R1 0.031 and wR2 0.062 for all data. Data were collected over a hemisphere of the reciprocal space by a combination of three exposure sets. Each exposure of 10 s covered 0.38 in w. The unit cell dimensions were determined by a least-squares refinement using reflections with I> 20s and 68< 2q< 468. The distance between the crystal and the detector was 6.05 cm. Coverage of the unique set was over 92% complete to at least 238 in q. The first 50 frames were recollected at the end of the data collection to monitor crystal decay. The structure was solved by Multan and Fourier methods. Full-matrix least-squares refinement was carried out minimizing w (F2 o À F2 c 2. Hydrogen atoms were included in their calculated positions. Refinement on F 2 for all reflections. Weighted R factors (Rw) and all goodnesses of fit S were based on F 2, conventional R factors (R) were based on F. Most of the calculations were carried out with the SHELXTL program.[18] Crystallographic data (excluding structure factors) for the structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publication no. CCDC-162439. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK (fax:(44) 1223-336-033; e-mail: deposit@ ccdc. cam. ac. uk).[14] a) LR Falvello, J. FornieÂs, R. Navarro, V. Sicilia, M. TomaÂs, Angew. Chem. 1990, 102, 952; Angew. Chem. Int. Ed. Engl. 1990, 29, 891; b) LR Falvello, J. FornieÂs, R. Navarro, V. Sicilia, M. TomaÂs, J. Chem. Soc. Dalton Trans. 1994, 3143; c) CC Li, CH Cheng, FL Liao, SL Wang, J. Chem. Soc. Chem. Commun. 1991, 710; d) H. Ossor, M. Pfeffer, JTBH Jastrzsbki, CH Stam, Inorg. Chem. 1987, 26, 1169.[15] K. Albert, P. Gisdakis, N. Rösch, Organometallics 1998, 17, 1608.[16] a) F. Kawataka, Y. Kayaki, I. Shimizu, A. Yamamoto, Organometallics 1994, 13, 3517; b) F. Ozawa, T. Ito, A. Yamamoto, J. Am. Chem. Soc. 1980, 102, 6457.[17] a) A. Michalak, T. Ziegler, Organometallics 2000, 19, 1850; b) DL Thorn, R. Hoffmann, J. Am. Chem. Soc. 1978, 100, 2079.[18] SHELXTL, Siemens Energy & Automation, Inc., Analytical Instrumentation, 1996.