2852
L. Ja´nosi et al. / Journal of Organometallic Chemistry 691 (2006) 2846–2852
Table 4
Crystallographic data for the structural analysis has
been deposited with the Cambridge Crystallographic Data
Centre, CCDC No. 287350 for compound 3a and CCDC
No. 287351 for compound 4.
Crystal data and data collection parameters
Identification code
[Pt{(S,S)-bdpp}I2] Æ [Pt{(S,S)-bdpp}-
1/3 MeCN Æ
(Me)I] (3a)
1/3 CH2I2 (4)
Empirical formula
C30H31.67 2.67
I
-
C
30H33IP2Pt
Acknowledgements
N0.33P2Pt
992.32
293(2)
0.71069
P21
Formula weight
Temperature (K)
777.49
293(2)
0.71069
P21
The authors thank the Hungarian Research Fund
(TS044800) for the financial support.
˚
Wavelength (A)
Crystal system,
space group
References
Unit cell dimensions
˚
a (A)
11.316(5)
14.305(5)
29.717(5)
100.381(5)
4732(3)
11.1302(10)
14.5032(13)
18.6585(16)
106.229(2)
2891.9(4)
[1] C.D. Frohning, C.W. Kohlpainter, in: B. Cornils, W.A. Herrmann
(Eds.), Applied Homogeneous Catalysis with Organometallic Com-
pounds, vol. 1, VCH, Weinheim, 1996, p. 29 ff;
˚
b (A)
˚
c (A)
b (ꢁ)
I. Ojima, C.-Y. Tsai, M. Tzamarioudaki, D. Bonafoux, The Hydro-
formylation Reaction, in: L. Overman et al. (Eds.), Organic Reac-
tions, Wiley, New York, 2000, pp. 1–354.
3
˚
Volume (A )
Z, calculated
density (Mg/m3)
Absorption
coefficient (mmꢀ1
F(000)
Crystal size (mm)
6, 2.089
4, 1.786
´
[2] S. Gladiali, J.C. Bayon, C. Claver, Tetrahedron: Asymmetry 6 (1996)
7.178
2780
0.3 · 0.2 · 0.1
0.70 to 31.38
6.047
1453;
)
F. Agbossou, J.-F. Carpentier, A. Mortreux, Chem. Rev. 95 (1995)
2485.
1496
0.2 · 0.15 · 0.1
1.81 to 32.76
[3] K.G. Anderson, R.J. Cross, Acc. Chem. Res. 17 (1984) 67;
h Range for
data collection (ꢁ)
´
M. Gomez, G. Muller, D. Sainz, J. Sales, Organometallics 10 (1991)
4036.
Limiting indices
ꢀ15 6 h 6 15,
ꢀ20 6 k 6 20,
ꢀ 43 6 l 6 43
76998/28580
[Rint = 0.0391]
94.3%
None
Full-matrix
least-squares on F2 least-squares on F2
28580/3/981
1.023
R1 = 0.0371,
wR2 = 0.0796
R1 = 0.0530,
wR2 = 0.0857
ꢀ16 6 h 6 16,
ꢀ21 6 k 6 21,
ꢀ 28 6 l 6 27
52539/19671
[Rint = 0.0286]
94.2%
´
´
´
[4] I. Toth, T. Kegl, C.J. Elsevier, L. Kollar, Inorg. Chem. 33 (1994)
5708;
´
´
T. Kegl, L. Kollar, L. Radics, Inorg. Chim. Acta 265 (1997) 249.
[5] G. Consiglio, P. Pino, L.I. Flowers, C.U. Pittmann Jr., J. Chem.
Soc., Chem. Commun. (1983) 612;
Reflections collected/unique
Completeness to h = 31ꢁ
Absorption correction
Refinement method
P. Haelg, G. Consiglio, P. Pino, J. Organomet. Chem. 296 (1985) 281;
G. Consiglio, F. Morandini, M. Scalone, P. Pino, J. Organomet.
Chem. 279 (1985) 193;
None
Full-matrix
´
L. Kollar, G. Consiglio, P. Pino, J. Organomet. Chem. 330 (1987)
Data/restraints/parameters
Goodness-of-fit on F2
Final R indices [I > 2r(I)]
19671/1/619
0.999
305;
´
´
L. Kollar, J. Bakos, I. Toth, B. Heil, J. Organomet. Chem. 370 (1989)
R1 = 0.0288,
wR2 = 0.0685
R1 = 0.0427,
wR2 = 0.0738
ꢀ0.001(3)
257;
G. Consiglio, S.C.A. Nefkens, A. Borer, Organometallics 10 (1991)
2046;
R indices (all data)
´
I. Toth, I. Guo, B. Hanson, Organometallics 12 (1993) 848;
Absolute structure parameter ꢀ0.010(2)
Largest difference in peak
1.375 and ꢀ1.357
and hole (e Aꢀ3
G. Parrinello, J.K. Stille, J. Am. Chem. Soc. 109 (1987) 7122.
1.821 and ꢀ1.103
´
[6] E. Farkas, L. Kollar, M. Moret, A. Sironi, Organometallics 15 (1996)
)
1345.
[7] C. Eaborn, K.J. Odell, A. Pidcock, J.C.S. Dalton (1978) 357.
[8] H.C. Clark, L.E. Manzer, J. Organomet. Chem. 59 (1973) 411.
[9] The fact that d-skew conformations have a smaller ‘bite’ angle than
the other ones can be also verified in the crystal structure determi-
nations of [Rh(BDPP)(NBD)]+ [(chair) P-Rh–P 95.1(3)ꢁ] and
after integration, of ca. 8000 reflections. The intensity data
were collected within the limits 2h < 62.8ꢁ (4) and
2h < 65.5ꢁ (3a) in the full sphere (x scan method), with
sample-detector distance fixed at 4.72 and 3.86 cm., respec-
tively; 2400 frames (20 s per frame; Dx = 0.3ꢁ) were col-
lected for both crystals; an empirical absorption
correction was applied (SADABS [11]). The structures were
solved by direct methods (SIR97 [12]) and refined with
full-matrix least-squares (SHELX97 [13]) on the basis of
28,580 and 19,671 independent reflections, respectively;
anisotropic temperature factors were assigned to all non-
hydrogen atoms. Hydrogens were riding on their carbon
atoms. The absolute configuration was determined by
internal comparison and subsequently confirmed by the
refined Flack parameter.
[Rh(BDPP)(COD)]+ [(d-skew) P-Rh–P 88.6(1)ꢁ] J. Bakos, I. Toth,
´
´
´
B. Heil, G. Szalontai, L. Parkanyi, V. Fulo¨p, J. Organomet. Chem.
¨
370 (1989) 263.
[10] H.B. Burgi, J.D. Dunitz, Acc. Chem. Res. 16 (1983) 153.
¨
[11] G.M. Sheldrick, SADABS, University of Go¨ttingen, Germany, 1996.
[12] A. Altomare, M.C. Burla, M. Camalli, G.L. Cascarano, C. Giaco-
vazzo, A. Guagliardi, A.G.G. Moliterni, G. Polidori, R. Spagna, J.
Appl. Cryst. 32 (1999) 115–119.
[13] G.M. Sheldrick, Programs for Crystal Structure Analysis (Release 97-
2), Institut fur Anorganische Chemie der Universita¨t, Tammanst-
¨
rasse4, D-3400 Go¨ttingen, Germany, 1998.
[14] J.L. Portscheller, S.E. Lilly, H.C. Malinakova, Organometallics 22
(2003) 2961.
´
[15] I. Toth, C.J. Elsevier, J.D. De Vries, J. Bakos, W.J.J. Smeets, A.L.
Spek, J. Organomet. Chem. 540 (1997) 15.