#------------------------------------------------------------------------------ #$Date: 2008-01-26 17:25:03 +0000 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003586.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003586 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1211 _journal_page_last 1213 _publ_section_title ; 3-(4-Butoxycarbonylphenyloxycarbonyl)-9H-xanthen-9-one ; _chemical_formula_moiety 'C25 H20 O6' _chemical_formula_sum 'C25 H20 O6' _chemical_formula_weight 416.43 _symmetry_space_group_name_H-M 'P -1' _cell_length_a 7.590(1) _cell_length_b 11.640(1) _cell_length_c 11.748(3) _cell_angle_alpha 88.00(1) _cell_angle_beta 88.08(1) _cell_angle_gamma 80.02(1) _cell_volume 1021(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_meas 1.34(1) _exptl_crystal_density_method ; flotation in a carbon tetrachloride-heptane solution ; _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.4 _cell_measurement_theta_max 27.0 _exptl_absorpt_coefficient_mu 0.759 _cell_measurement_temperature 295 _exptl_crystal_description prism _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_colour colorless _diffrn_measurement_device 'Enraf-Nonius' _diffrn_measurement_method '\w/\q scans' _exptl_absorpt_correction_type 'none' _diffrn_reflns_number 4206 _reflns_number_total 4206 _reflns_number_observed 3780 _reflns_observed_criterion I>3.0\s(I) _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 75.0 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 2 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1.4 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.044 _refine_ls_wR_factor_obs 0.067 _refine_ls_goodness_of_fit_obs 3.021 _refine_ls_number_reflns 3780 _refine_ls_number_parameters 361 _refine_ls_hydrogen_treatment 'refall' _refine_ls_weighting_scheme ; calc w = 4F~o~^2^/[\s^2^(F~o~^2^) + (0.03F~o~^2^)^2^] ; _refine_ls_shift/esd_max 0.03 _refine_diff_density_max 0.337 _refine_diff_density_min -0.177 _refine_ls_extinction_method 'Stout & Jensen (1989)' _refine_ls_extinction_coef 3.7E-6(4) loop_ _atom_type_symbol _atom_type_scat_source 'C' IntTabIV 'H' IntTabIV 'O' IntTabIV ; ORTEPII (Johnson, 1976) and PLUTO (Motherwell & Clegg, 1978) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O1 0.7279(1) -0.76053(8) 0.49544(8) 0.0501(3) O2 0.8505(2) -0.6330(1) 0.59065(9) 0.0730(4) O3 0.5099(1) -0.30803(8) 0.18237(8) 0.0467(3) O4 0.6286(2) -0.39855(8) 0.02368(9) 0.0530(3) O5 0.2084(2) 0.10123(9) -0.28217(8) 0.0592(3) O6 0.1615(1) 0.06297(7) 0.06533(7) 0.0397(2) C1 0.7650(3) -1.1769(1) 0.5971(2) 0.0661(5) C2 0.8046(2) -1.0609(1) 0.6333(1) 0.0563(4) C3 0.7339(2) -0.9607(1) 0.5514(1) 0.0546(4) C4 0.7858(2) -0.8482(1) 0.5840(1) 0.0508(4) C5 0.7690(2) -0.6554(1) 0.5104(1) 0.0450(4) C6 0.7027(2) -0.5686(1) 0.4190(1) 0.0408(4) C7 0.7341(2) -0.4556(1) 0.4282(1) 0.0503(4) C8 0.6724(2) -0.3705(1) 0.3467(1) 0.0485(4) C9 0.5798(2) -0.4006(1) 0.2568(1) 0.0405(3) C10 0.5467(2) -0.5118(1) 0.2448(1) 0.0511(4) C11 0.6090(2) -0.5963(1) 0.3274(1) 0.0494(4) C12 0.5413(2) -0.3164(1) 0.0686(1) 0.0383(3) C13 0.4535(2) -0.2082(1) 0.0073(1) 0.0350(3) C14 0.3459(2) -0.1195(1) 0.0648(1) 0.0353(3) C15 0.2635(2) -0.0217(1) 0.0026(1) 0.0333(3) C16 0.2855(2) -0.0129(1) -0.1152(1) 0.0348(3) C17 0.3959(2) -0.1037(1) -0.1710(1) 0.0410(3) C18 0.4803(2) -0.2000(1) -0.1108(1) 0.0403(3) C19 0.1948(2) 0.0915(1) -0.1785(1) 0.0400(3) C20 0.0926(2) 0.1815(1) -0.1069(1) 0.0382(3) C21 0.0830(2) 0.1647(1) 0.0109(1) 0.0369(3) C22 -0.0085(2) 0.2499(1) 0.0813(1) 0.0462(4) C23 -0.0913(2) 0.3540(1) 0.0325(1) 0.0527(4) C24 -0.0866(2) 0.3724(1) -0.0848(1) 0.0523(4) C25 0.0032(2) 0.2875(1) -0.1545(1) 0.0464(4) H1C1 0.796(3) -1.239(2) 0.650(2) 0.052(6) H2C1 0.822(3) -1.195(2) 0.522(2) 0.060(6) H3C1 0.631(2) -1.174(2) 0.588(2) 0.046(5) H1C2 0.936(3) -1.067(2) 0.641(2) 0.054(6) H2C2 0.754(2) -1.044(2) 0.706(2) 0.042(5) H1C3 0.782(2) -0.980(2) 0.471(1) 0.042(5) H2C3 0.597(3) -0.950(2) 0.555(2) 0.051(6) H1C4 0.915(3) -0.854(2) 0.591(2) 0.053(6) H2C4 0.729(2) -0.819(1) 0.657(1) 0.030(4) HC7 0.800(3) -0.437(2) 0.496(2) 0.067(6) HC8 0.695(2) -0.292(1) 0.354(1) 0.035(5) HC10 0.483(2) -0.531(1) 0.181(1) 0.035(5) HC11 0.581(3) -0.675(2) 0.324(2) 0.046(5) HC14 0.323(2) -0.119(1) 0.142(1) 0.015(4) HC17 0.415(2) -0.098(1) -0.254(1) 0.030(4) HC18 0.562(2) -0.262(1) -0.151(1) 0.033(5) HC22 -0.011(2) 0.231(2) 0.159(1) 0.035(5) HC23 -0.157(2) 0.414(1) 0.090(1) 0.035(5) HC24 -0.138(3) 0.448(2) -0.116(1) 0.042(5) HC25 0.013(2) 0.299(1) -0.234(1) 0.029(4) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O1 0.0651(5) -0.0065(4) -0.0175(4) 0.0385(4) 0.0101(4) 0.0448(4) O2 0.1005(7) -0.0234(5) -0.0451(5) 0.0555(6) 0.0177(5) 0.0631(6) O3 0.0613(5) 0.0086(4) -0.0091(4) 0.0334(4) 0.0050(4) 0.0410(4) O4 0.0634(6) 0.0130(4) -0.0024(5) 0.0378(4) 0.0009(4) 0.0523(5) O5 0.0894(7) 0.0040(5) -0.0093(5) 0.0478(5) 0.0073(4) 0.0353(4) O6 0.0476(4) 0.0087(4) -0.0037(4) 0.0331(4) 0.0024(3) 0.0343(4) C1 0.088(1) -0.0132(8) 0.0002(9) 0.0446(7) 0.0034(7) 0.0635(9) C2 0.0782(9) -0.0115(7) -0.0098(7) 0.0440(6) 0.0086(6) 0.0449(7) C3 0.0677(8) -0.0110(6) -0.0156(6) 0.0441(6) 0.0081(6) 0.0505(7) C4 0.0676(8) -0.0060(6) -0.0138(6) 0.0399(6) 0.0108(5) 0.0427(6) C5 0.0504(7) -0.0052(5) -0.0107(5) 0.0416(6) 0.0061(5) 0.0412(6) C6 0.0425(6) -0.0024(5) -0.0079(5) 0.0380(6) 0.0057(5) 0.0397(6) C7 0.0606(7) -0.0134(5) -0.0183(5) 0.0445(6) 0.0065(5) 0.0453(6) C8 0.0621(7) -0.0099(5) -0.0114(6) 0.0355(6) 0.0042(5) 0.0466(6) C9 0.0457(6) 0.0036(5) -0.0067(5) 0.0330(5) 0.0054(5) 0.0396(6) C10 0.0655(7) -0.0076(6) -0.0233(6) 0.0381(6) 0.0057(5) 0.0483(6) C11 0.0632(7) -0.0087(5) -0.0186(6) 0.0336(5) 0.0058(5) 0.0501(7) C12 0.0394(5) -0.0004(4) -0.0075(5) 0.0315(5) 0.0010(5) 0.0421(6) C13 0.0356(5) -0.0021(4) -0.0077(4) 0.0287(5) 0.0017(4) 0.0393(5) C14 0.0391(5) -0.0004(4) -0.0064(4) 0.0314(5) 0.0031(4) 0.0333(5) C15 0.0336(5) -0.0011(4) -0.0052(4) 0.0294(5) 0.0003(4) 0.0353(5) C16 0.0377(5) -0.0042(4) -0.0061(4) 0.0309(5) 0.0030(4) 0.0343(5) C17 0.0493(6) -0.0029(5) -0.0021(5) 0.0370(5) 0.0012(5) 0.0345(5) C18 0.0450(6) 0.0005(5) -0.0024(5) 0.0341(5) -0.0025(5) 0.0392(6) C19 0.0475(6) -0.0061(5) -0.0107(5) 0.0351(5) 0.0060(5) 0.0358(5) C20 0.0370(5) -0.0036(4) -0.0102(5) 0.0323(5) 0.0057(5) 0.0437(6) C21 0.0340(5) 0.0002(4) -0.0076(5) 0.0305(5) 0.0033(5) 0.0442(6) C22 0.0457(6) 0.0035(5) -0.0040(6) 0.0388(6) -0.0024(5) 0.0508(7) C23 0.0460(7) 0.0052(6) -0.0037(7) 0.0366(6) -0.0040(6) 0.0717(9) C24 0.0468(7) 0.0037(5) -0.0112(6) 0.0329(6) 0.0103(6) 0.0738(9) C25 0.0442(6) -0.0030(5) -0.0127(5) 0.0381(6) 0.0116(5) 0.0548(7)