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X-ray crystal data of 1: C22H20N2O 3, MW, 360.40; monoclinic, space group P21; a, 10.483(2) Å, b, 11.115(2) Å, c, 15.144(3) Å, V, 1764.5(6) Å3, Z, 4, Dcalcd, 1.357 g/cm 3, Mo Kα (λ, 0.71073 Å, The data were collected on a MAC DIP-2030K diffractometer, with a graphite monochromator. Mo Kα radiation was found using a colorless crystal of dimensions of 0.52 × 0.52 × 0.40 mm3 and a maximum 2θ value of 16.0°. Independent reflections: 3990. Observed number of reflections: 3653, F| 2 ≥ 8σ|F|2, The structure was solved by the direct method SHELX-8612 and expanded using difference Fourier techniques, refined by the program and method NOMCSDP13 and full-matrix, least-squares calculations. Hydrogen atoms were fixed at calculated positions. The final i
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w = 0.0756. The CCDC deposit number is 631977. Copies of these data can be obtained, free of charge, on application to the CCDC via www.ccdc.cam.ac.uk/conts/retrieving. html (or Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, U.K., fax +44 1223 336033, e-mail deposit@ccdc.cam.ac.uk).
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22
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34248339055
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Compound 2: white power; [α]D25, 140° (c, 0.05, UV (CHC13) λmax 220, 286, 293 nm; IR (KBr) νmax 3418, 1745, 1634 cm-1; 1H and 13C NMR data, see Table 1; postive FABMS m/z [M, 360 (100, HRESIMS m/z 361.1547 cacld for C22H 20N2O3, 361.1552
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3, 361.1552).
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