414
A. Mack et al. / Journal of Organometallic Chemistry 643–644 (2002) 409–415
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8] (a) Review: M. Regitz, U. Bergstr a¨ ßer, Science of Synthesis, vol.
, Thieme, Stuttgart, 2001, p. 172ff;
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08 (1996) 1616; Angew. Chem. Int. Ed. Engl. 35 (1996) 1512;
c) T. Hofmann, PhD Thesis, University of Kaiserslautern, 2000.
Data Centre, CCDC nos. 174178 and 174179 for com-
pounds 14 and 16b, respectively. Copies of this infor-
9
(
1
(
1
EZ, UK (Fax: +44-1223-336033; e-mail: deposit@
[9] (a) T. Wettling, B. Geißler, R. Schneider, S. Barth, P. Binger,
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1992) 758;
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(
Acknowledgements
This work was supported by the Deutschen
Forschungsgemeinschaft (Graduate College ‘Phospho-
rus as Connecting Link Between Various Chemical
Disciplines’) and the Fonds der Chemischen Industrie
[
[
10] Review: A. Mack, M. Regitz, Chem. Ber./Recl. 130 (1997) 823.
11] See also: (a) A. Mack, PhD Thesis, University of Kaiserslautern,
1
(
998;
b) A. Mack, M. Regitz, Adv. Str. Int. Org. Mol. (1999) 199
(Suppl. 1);
(
postgraduate grant to A.M.).
(
(
c) M. Regitz, U. Bergstr a¨ ßer, Pol. J. Chem. 73 (1999) 135;
d) A. Mack, U. Bergstr a¨ ßer, M. Regitz, Synthesis (1999) 639.
[
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[
(
1
990, p. 157ff.
15] Single crystals (red needles) of 14 were obtained from an n-pen-
tane solution at −30 °C. Data collection with a Siemens P4
9
(
diffractometer, Mo–Ka radiation, u=0.71073 A
monochromator; C30H38N O P W , M=1016.26 g mol , tri-
,
with graphite
[
−1
2
10
2
2
9
(
clinic, space group P1, a=10.157(2) A
7.935(3) h=99.187(13)°, i=103.22(2)°, k=91.86(2)°,
Z=2; V=1888.3(5) A
, b=10.8142(15) A, c=
, ,
1
A,
,
M. Regitz, Angew. Chem. 98 (1986) 645; Angew. Chem. Int. Ed.
Engl. 25 (1986) 644;
3
−3
−1
,
, zcalc=1.787 g cm , v=6.223 mm
,
F(000)=980; absorption correction: semi-empirical from c-
scans, max and min transmission 1.0000 and 0.6733; 9052
collected reflections with 7412 independent reflections [Rint
0
full-matrix least-squares method on F
ness-of-fit=1.073. The structure model converged with R =
0
(c) P.B. Hitchcock, M.J. Maah, J.F. Nixon, J. Chem. Soc. Chem.
Commun. (1986) 737;
=
(
(
(
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2
(SHELXL-93 [25]); good-
1
Bruckmann, C. Kr u¨ ger, Angew. Chem. 107 (1995) 2411; Angew.
Chem. Int. Ed. Engl. 34 (1995) 2227.
.0519, wR =0.0806 (R =0.1068, wR =0.1185 for all data).
2 1 2
The final Fourier difference analysis showed a maximum of
[
[
[
5] (a) Review: M. Regitz, U. Bergstr a¨ ßer, Science of Synthesis, vol.
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−3
0
.927 e A
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and a minimum of −0.637 e A
,
.
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Ber./Recl. 130 (1997) 1491.
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from an n-pentane–diethyl ether (10:1) solution at −30 °C.
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258;
(IPDS-STOE), Mo–Ka radiation, u=0.71073 A with a graphite
monochromator; C28H36O P , M=498.51 g mol , orthorhom-
4 2
bic, space group Ccca, a=10.342(2) A
15.734(3)
,
−
1
,
, b=31.861(6) A
h=90.00°, i=90.00°, k=90.00°, Z=8;
,
, c=
(
(
(
c) B. Neum u¨ ller, E. Fluck, Phosphorus Sulfur Relat. Elem. 29
1987) 23;
d) H. Keller, G. Maas, M. Regitz, Tetrahedron Lett. 27 (1986)
A,
,
A
,
3, zcalc=1.277 g cm
−3
,
v=0.200 mm
−1
,
V=5185(2)
F(000)=2128; 19 318 collected reflections with 2543 independent
1
903;
reflections [Rint=0.0464] and 1899 reflections with I]2|(I)
2
(e) G. Bertrand, in: M. Regitz, O.J. Scherer (Eds.), Multiple
were refined by full-matrix least-squares method on F
(
SHELXL
-
Bonds and Low Coordination in Phosphorus Chemistry,
Thieme, Stuttgart, 1990, p. 443ff;
93 [25]); goodness-of-fit=1.204. The structure model converged
with R =0.0436, wR =0.0935 (R =0.0592, wR =0.0977 for
1
2
1
2
(
6
f) E. Fluck, G. Heckmann, K. Lange, Z. Anorg. Allg. Chem.
19 (1993) 1551.
all data). The final Fourier difference analysis showed a maxi-
−
3
−3
mum of 0.307 e A
,
and a minimum of −0.261 e A
,
.