Angewandte
Chemie
7.2 Hz, 2JHH = 3.2 Hz) and 3.24 (dd, 3JHH = 7.1 Hz, 2JHH = 3.1 Hz)
the Cambridge Crystallographic Data Centre, 12, Union Road,
3
2
(each 1Hsyn, butadiene), 1.28 (dd, JHH = 16.2 Hz, JHH = 3.2 Hz) and
Cambridge CB21EZ, UK; fax: (+ 44)1223-336-033; or deposit@
ccdc.cam.ac.uk). 6a: C24H22Cl2Zr, monoclinic, space group P21/
n, a = 10.862(1), b = 13.507(1), c = 14.264(1) , b = 93.23(1)8,
V= 2089.4(3) 3, 1calcd = 1.502 gcmꢀ3, m = 7.88 cmꢀ1, Z = 4, T=
198 K, 5775 reflections collected, 3498 independent and 2383
observed, 246 refined parameters, R = 0.056, wR2 = 0.127. Due
to the small size, the crystal diffracted very weakly. 6c:
C34H38Cl2Zr, orthorhombic, space group P212121, a = 9.391(1),
1.11 (dd, 3JHH = 16.2 Hz, 2JHH = 3.1 Hz) (each 1Hanti, butadiene),
3
ꢀ1.45 (dt, 3JHH = 16.2 Hz, 3JHH = 7.2 Hz) and ꢀ1.55 (dt, JHH
=
3
16.2 Hz, JHH = 7.1 Hz) (each 1Hmeso, butadiene), 2.76/1.69 and 2.32/
1.82 (each 1H, cyclobutylene CH2), 1.29, 1.25 ppm (each s, each 3H,
CH3). 13C NM R (CD6, 298 K, 150.6 MHz): d = 137.8, 123.1, 123.5,
6
122.6, 121.9, 121.6, 119.7, 83.2, 82.8 (indenylB), 137.2, 123.7, 123.6,
123.3, 122.7, 121.5, 118.0, 83.7, 81.2 (indenylA), 114.1, 113.5, 73.5, 71.0
(butadiene), 49.1, 48.9, 31.9, 29.9 (cyclobutylene), 27.2, 23.8 ppm
(CH3).
b = 11.494(1),
c = 26.995(1) ,
V= 2913.8(4) 3,
1calcd =
1.388 gcmꢀ3, m = 5.82 cmꢀ1, Z = 4, T= 198 K, 20454 reflections
collected, 7080 independent and 5824 observed, 334 refined
parameters, R = 0.037, wR2 = 0.067, Flack parameter ꢀ0.06(4).
7c: C34H38Cl2Zr·CH2Cl2, monoclinic, space group P21/n, a =
10.694(1), b = 7.880(1), c = 37.258(1) , b = 94.11(1)8, V=
Received: May 13, 2003
Revised: September 8, 2003 [Z51886]
3131.6(3) 3, 1calcd = 1.471 gcmꢀ3
, , Z = 4, T=
m = 7.16 cmꢀ1
Keywords: indenyl ligands · metallocenes · photolysis ·
.
198 K, 11911 reflections collected, 7160 independent, 4785
observed reflections, 362 refined parameters, R = 0.054, wR2 =
0.156.
polymerization · zirconium
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graphic data for this paper. These data can be obtained free of
Angew. Chem. Int. Ed. 2004, 43, 310 –313
ꢀ 2004 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
313