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[
8] See Supporting Information.
9] Crystallographic study for compound 2: Intensity data were
collected on a Rigaku RAXIS-RAPID imaging plate diffrac-
tometer with CuKa radiation at a temperature of 93.2 K. The
[
10]
program of PROCESS-AUTO was used during data collec-
tion. The structure was solved by direct methods with SIR97
and refined by least-squares methods with CRYSTALS.
[
11]
[
12]
2:
crystallized from MeOH/CHCl , C H F N O S, M = 516.50,
3
24 22
6
2
2
r
colorless block 0.30 0.20 0.10 mm, monoclinic, P2 (4), a =
1
1
1.6363(11), b = 8.2929(9), c = 12.4374(13) , b = 96.404(6)8,
3
À3
V= 1192.7(2) , Z = 2, 1
= 1.438 gcm , 2qmax 136.58, mea-
calcd
sured reflections = 12702, independent reflections = 4013 (Rint
.029), R1 = 0.0307 for 3797 reflections with I > 2s(I), wR2 =
.0812 for all reflections with I > 2s(I), GOF = 1.054. The
=
0
0
absolute configuration was determined based on the Flack
parameter (0.004(14)) refined using 1684 Friedel pairs. CCDC-
269460 (2) contains the supplementary crystallographic data for
this paper. These data can be obtained free of charge from the
Cambridge Crystallographic Data Centre via www.ccdc.cam.
ac.uk/data_request/cif.
[
[
10] Rigaku (1998) PROCESS-AUTO: Automatic data acquisition
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Angew. Chem. Int. Ed. 2005, 44, 5838 –5841ꢀ 2005 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
5841