10
JHOU ET AL.
5
1
.69 (s, 1H), 3.15–3.20 (m, 2H), 2.46 (s, 3H), 1.64–1.72 (m,
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13
H), 1.51–1.60 (m, 2H), 0.94–0.96 (m, 6H); C NMR
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2
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16
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3
.6.4 | Spectroscopic data for 6a
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[
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6
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2
13
H), 0.74–0.75 (d, J = 6.8 Hz, 3H); C NMR (100 MHz,
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3
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3
.7 | X-ray crystallographic studies
[
Crystals of 3d_O, 3e, 4b, 4c, 4d, 5b, and 6a were obtained
by placing samples in crystal-growing glassware, which
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ꢀ
CH Cl ), in an environment of 25 C for a few days. Suit-
2
2
able crystals of these compounds were sealed in thin-
walled glass capillaries under nitrogen atmosphere and
mounted on a Bruker AXS SMART 1000 diffractometer.
Intensity data were collected in 1350 frames with increas-
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ꢀ
ing ω (width of 0.3 per frame). The absorption correction
was based on the symmetry-equivalent reflections using
the SADABS program. The space group determination
was based on a check of the Laue symmetry and system-
atic absences and was confirmed using the structure solu-
tion. The structure was solved by direct methods using a
SHELXTL package. All non-H atoms were located from
successive Fourier maps, and hydrogen atoms were
refined using a riding model. Anisotropic thermal param-
eters were used for all non-H atoms, and fixed isotropic
parameters were used for H atoms.
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[
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ACKNOWLEDGMENTS
We thank the Ministry of Science and Technology of the
ROC (Grant MOST 107-2113-M-005-006) for financial
support.
[33] Crystal growing for this newly obtained 3b was carried out in
different mixed solvents, CH Cl /hexanes. Interestingly, differ-
2
2
ent crystal systems were observed in two cases; yet, the main
structure are almost identical. See Supporting Information for
detail data of the crystal structure of 3b.
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