2.4. X-ray crystal structure analysis of compounds 1 and 4
Colorless crystals of 1 and 4were obtained fromMeOH. The intensity
data were collected on an Xcalibur Onyx Nova diffractometer with CuKα radiation. The crystal structures of 1 and 4 were solved by the direct
method (SHLXS-97), expanded using difference Fourier technique,
and refined by the program and the full-matrix least-squares calculations.
The nonhydrogen atoms were refined anisotropically, and
hydrogen atoms were fixed at calculated positions. Crystallographic
data for the structures of 1 and 4 have been deposited in the Cambridge
Crystallographic Data Centre (deposition numbers: CCDC 1402275 and
1402261). Copies of these data can be obtained free of charge via
www.ccdc.cam.ac.uk (or from the Cambridge Crystallographic Data
Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: (+44) 1223-
336-033; or desposit@ccdc.cam.ac.uk).
Crystal data of 1: C19H20O6·CH4O,Mr. = 376.39, monoclinic, space
group, P21, a = 7.76825 (7) Å, b = 12.07112 (12) Å, c = 9.55484
(9) Å; α = 90.00°, β = 99.5128 (9)°, γ = 90.00°, V = 883.65 (1) Å3,
Z = 2, μ(Cu Kα) = 0.89 mm−1, DX = 1.415 Mg/m3, F(000) = 400,
3419 reflections independent and 3394 reflections observed [I N 2σ(I)].
Fig. 1.