´
´
B. Wrackmeyer, Z. Garcıa Hernandez, R. Kempe, M. Herberhold
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Table 4 Crystal data [25] for the compounds 2 and 3.
2
3
Empirical formula
Formula mass
Crystal size /mm
Crystal system
Space group
C8H15B10PSe2
408.19
0.20x0.14x0.05
monoclinic
P21/c
9.0450(7)
10.8030(10)
16.3520(13)
101.188(6)
1567.4(2)
4
C8H15B10PSSe2
440.25
0.39x0.30x0.14
monoclinic
P21/c
7.3055(9)
22.160(3)
10.6480(12)
93.726(10)
1720.2(4)
4
˚
a /A
˚
b /A
˚
c /A
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Chem. Rev. 2006, 250, 259.
β /°
˚
Volume /A
Z
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Jones, J. Chem. Soc. Dalton Trans. 1998, 2163. (b) K. Base,
M. W. Grinstaff, Inorg. Chem. 1998, 37, 1432. (c) O. Crespo,
M. C. Gimeno, P. G. Jones, A. Laguna, J. Organomet. Chem.
1999, 547, 89.
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S.-I. Cho, S. O. Kang, Inorg. Chim. Acta. 1999, 289, 141. (c)
J.-Y. Bae, Y.-J. Lee, S.-J. Kim, J. Ko, S. Cho, S. O. Kang, Or-
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Dcalcd. /g cmϪ3
1.730
4.797
784
1.700
4.495
848
M(Mo-Kα) /mmϪ1
F(000)
Data collection range Θ /°
Reflections collected
Independent reflections
Data/restraints/parameters
Goodness-of-fit on F2
R1 [I>2σ(I)]
2.27-25.74
2960
1635
1635/0/250
0.734
0.0860
1.84-25.77
3252
2245
3252/0/199
1.050
0.1119
wR2 (all data)
0.0638
0.694/Ϫ0.375
0.1962
1.578/Ϫ1.191
Ϫ3
˚
Max./min. ∆F /e A
3-Phenyl-2,2-bis(triphenylphosphane)-3-seleno-4,5-
[1,2(1,2-dicarba-closo-dodecaborano)]-1-selena-3-λ5-
phospha-2-platina-cyclopentane (9)
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Eur. J. 2000, 6, 3026. (c) M. Herberhold, H. Yan, W. Milius,
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Chem. Commun. 2004, 7, 1174. (c) S. Lu, G.-X. Jin, St. Eibl,
M. Herberhold, Y. Xin, Organometallics 2002, 21, 2533. (d) J.-
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2005, 24, 5280.
To a solution of (ethene)bis(triphenylphosphane)platinum (0.2 g,
0.27 mmol) in CD2Cl2 (0.5 mL) was added a solution of 2 (0.11 g,
0.27 mmol) in CD2Cl2 (0.5 mL) at Ϫ78 °C. An orange-red solution
was obtained and immediately analysed by 31P NMR spectroscopy
at Ϫ40 °C. The NMR analysis indicated the presence of complex
9 as the main product (see Table 3 and Figures 2 to 4), Ph3PϭSe
and the starting material [(Ph3P)2Pt(CH2ϭCH2)]. At room tem-
perature, the 31P NMR spectrum showed the presence of Ph3Pϭ
Se, (1,2-C2B10H10-1,2-Se2)Pt(PPh3)2 [15] [δ31P
ϭ
15.7 (s),
2J(77Se,31P)cis/trans ϭ 51 Hz, 1J(195Pt,31P) ϭ 2972.5 Hz] and other
unidentified compounds in low concentration [δ31P ϭ 15.0 (s),
1
1J(195Pt,31P) ϭ 3679 Hz; 22.6 (s), J(195Pt,31P) ϭ 2963 Hz; 19.7 (s),
1J(195Pt,31P) ϭ 3248 Hz]. 9: 1H NMR (400 MHz; CD2Cl2; Ϫ40 °C):
δ> ϭ 7.00-7.67 (m, 35H, 7Ph), 1.40-2.60 (m (broad), 10H, B10H10).
Crystal structure determinations of the phosphane 2
and its sulphide 3
Details pertinent to the crystal structure determinations are listed
in Table 4. The X-ray crystal structure analyses were carried out
for single crystals using a STOE IPDS II system equipped with an
Oxford Cryostream low-temperature unit. Crystals of appropriate
size were selected in perfluorinated oil at room temperature, and
the data collections were carried out at 193(2) K [25]. Structure
solution and refinement were accomplished using SIR97 [26],
SHELXL-97 [27], and WinGX [28].
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2005, 690, 249. (b) S. Cai, X. Hou, L.-H. Weng, G.-X. Jin, J.
Organomet. Chem. 2005, 690, 910.
Acknowledgement. This work was supported by the Deutsche
Forschungsgemeinschaft.
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yer, J. Organomet. Chem. 1999, 587, 252. (b) M. Herberhold,
W. Milius, G.-X. Jin, W. Kremnitz, B. Wrackmeyer, Z. Anorg.
Allg. Chem. 2006, 632, 2031.
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