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7
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33745599176
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note
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2, petroleum:EtOAc (0 to 10 %)).
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8
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33745634700
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note
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+-120, 36).
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9
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33745635434
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note
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12 space group with a=b=6.346(1), c=36.640(4) Å, and Z=4. The structure was solved from 1169 reflections with I>2σ(I) and refined to an agreement R1-factor of 0.0422. The molecule is located on a crystallographic two-fold axis that symmetry relates the two molecular halves hence resembling a two-bladed propeller. As expected, each half is planar [rms deviation of atoms from the least-squares plane of 0.042 Å]. Because of the small anomalous atomic dispersion, the correct molecular stereoisomer in the lattice could not be determined. Crystal data, data collection procedure, structure determination method and refinement results for the compound are summarized in Table S1 (Supplementary material). Atomic fractional coordinates and equivalent isotropic displacement parameters are given in Table S2. Interatomic bond distances and angles are in Table S3. Listings of atomic anisotropic displacement parameters (Table S4), hydrogen atoms positions and isotropic displacement parameters (Table S5), and calculated and observed structure factor amplitudes (Table S6) are also given.7 Crystallographic data (excluding structure factors) for the structure in this paper have been deposited at the Cambridge Crystallographic Data Centre as supplementary publication numbers CCDC 601663. Copies of the data can be obtained, free of charge, on application to CCDC, 12 Union Road, Cambridge CB2 1EZ, UK [fax: 144-(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk].
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33745590222
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note
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The alcohol 3 converts gradually into compound 7 when it is stored at room temperature.
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27
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