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85069244867
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X-ray data of syn, )-4e: crystallized from ethyl acetate/n-hexane at 20°C; C20H20N2O8 (M r, 416.38, orthorhombic; space group, P2(1)2(1)2(1, a, 7.2996(15) Å, b, 14.392(3) Å; c, 19.190(4) Å; β, 90 deg, V, 2016.0(7) Å3; Z, 4; cd, 1.372 mg m-3; μ, 0.107 mm-1; F(000, 872. A transparent crystal of 0.45 x 0.09 x 0.04 mm3 was used. 3514 [R(int, 0.1395] independent reflections were collected on a Bruker Smart CCD difractomer using graphite-monochromated Mo-Kα radiation (λ, 0.71073 Å) operating at 50 Kv and 30 mA. Data were collected over a hemisphere of the reciprocal space by combination of three exposure sets. Each exposure of 20s and 30s covered 0.3 in ω. The structure was solved by direct methods and Fourier synthesis. It was refined by full-matrix least-squares procedures on F2 SHELXL-97, All
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2 (SHELXL-97). All non-hydrogen atoms were refined anisotropically and all hydrogen atoms were included in calculated positions and refined riding on the respective carbon or oxygen atoms. Final R(Rw) values were 0.0534 (0.1166) and 0.1973 (0.1596). CCDC-610275 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via the http://www.ccdc.can.ac.uk/ conts/retrieving.html (or from the Cambridge Crystallographic Centre, 12 Union Road, Cambridge CB21EZ, UK; Fax (+44)1223-336033; or deposit@cccdc.cam.ac.uk).
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