#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003227.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_2003227 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 462 _journal_page_last 465 _publ_section_title ; 4-Methoxy-11-oxo-5-azabenzo[b]fluorene N-Oxide and its Free Base ; _chemical_formula_moiety 'C17 H11 N O3' _chemical_formula_sum 'C17 H11 N O3' _chemical_formula_weight 277.27 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _symmetry_space_group_name_H-M 'P b c a' _cell_length_a 21.023(1) _cell_length_b 14.907(1) _cell_length_c 8.2059(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2571.6(3) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 18.06 _cell_measurement_theta_max 47.15 _exptl_absorpt_coefficient_mu 0.815 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_colour red _chemical_compound_source ? _diffrn_measurement_device 'Syntex P2~1~' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1204 _reflns_number_total 1204 _reflns_number_observed 1199 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 'not determined' _diffrn_reflns_theta_max 57.28 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.4 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0380 _refine_ls_wR_factor_obs 0.0825 _refine_ls_wR_factor_all 0.0859 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_goodness_of_fit_all 1.087 _refine_ls_number_reflns 1200 _refine_ls_number_parameters 191 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0276P)^2^+1.5593P] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max <0.001 _refine_diff_density_max 0.153 _refine_diff_density_min -0.109 _refine_ls_extinction_method 'F~c~^*^ = kF~c~[1+0.001xF~c~^2^\l^3^/sin(2\q)]' _refine_ls_extinction_coef 0.0022(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0181 0.009 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0311 0.018 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0492 0.032 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 1 0.57903(13) 0.6377(2) 0.2845(3) 0.0560(7) O1 1 0.61256(10) 0.56501(12) 0.2382(3) 0.0880(7) C12 1 0.5903(2) 0.4795(2) 0.2729(5) 0.117(2) H12A 1 0.6197(2) 0.4358(2) 0.2316(5) 0.140 H12B 1 0.5495(2) 0.4711(2) 0.2223(5) 0.140 H12C 1 0.5862(2) 0.4725(2) 0.3887(5) 0.140 C2 1 0.52269(14) 0.6315(2) 0.3742(3) 0.0654(8) H2 1 0.50602(14) 0.5751(2) 0.3973(3) 0.078 C3 1 0.49124(14) 0.7066(2) 0.4292(4) 0.0684(8) H3 1 0.45393(14) 0.7001(2) 0.4890(4) 0.082 C4 1 0.51424(14) 0.7914(2) 0.3971(3) 0.0635(8) H4 1 0.49353(14) 0.8423(2) 0.4356(3) 0.076 C4a 1 0.56918(13) 0.7980(2) 0.3056(3) 0.0547(7) C5 1 0.60084(13) 0.8816(2) 0.2526(4) 0.0595(7) O5 1 0.58187(9) 0.95806(12) 0.2721(3) 0.0811(7) C5a 1 0.65757(12) 0.8533(2) 0.1595(3) 0.0515(7) C6 1 0.70319(13) 0.9033(2) 0.0868(3) 0.0594(8) H6 1 0.70275(13) 0.9656(2) 0.0943(3) 0.071 C6a 1 0.75146(14) 0.8585(2) -0.0008(3) 0.0542(7) C7 1 0.80213(14) 0.9031(2) -0.0782(4) 0.0675(8) H7 1 0.80496(14) 0.9653(2) -0.0714(4) 0.081 C8 1 0.84722(14) 0.8565(2) -0.1630(4) 0.0698(8) H8 1 0.88066(14) 0.8870(2) -0.2124(4) 0.084 C9 1 0.84325(13) 0.7635(2) -0.1757(4) 0.0643(8) H9 1 0.87372(13) 0.7325(2) -0.2355(4) 0.077 C10 1 0.79527(13) 0.7174(2) -0.1017(3) 0.0575(7) H10 1 0.79315(13) 0.6552(2) -0.1099(3) 0.069 C10a 1 0.74956(12) 0.7642(2) -0.0137(3) 0.0505(7) N11 1 0.69994(10) 0.71444(12) 0.0630(3) 0.0532(6) O11 1 0.69883(10) 0.62939(11) 0.0385(3) 0.0850(7) C11a 1 0.65651(11) 0.7581(2) 0.1522(3) 0.0478(7) C11b 1 0.60206(11) 0.72315(14) 0.2462(3) 0.0490(6) 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 C1 0.057(2) -0.0046(14) -0.0026(15) 0.0496(15) -0.0006(13) 0.061(2) O1 0.0922(15) -0.0069(11) 0.0360(14) 0.0469(11) 0.0044(12) 0.125(2) C12 0.117(3) -0.012(2) 0.038(3) 0.051(2) -0.004(2) 0.183(4) C2 0.064(2) -0.0093(15) -0.001(2) 0.061(2) 0.008(2) 0.071(2) C3 0.059(2) -0.001(2) 0.001(2) 0.083(2) 0.009(2) 0.064(2) C4 0.062(2) 0.0096(15) -0.009(2) 0.066(2) -0.002(2) 0.062(2) C4a 0.054(2) -0.0023(14) -0.0094(14) 0.056(2) 0.0014(13) 0.054(2) C5 0.061(2) 0.0011(14) -0.013(2) 0.050(2) -0.002(2) 0.067(2) O5 0.0776(14) 0.0082(10) 0.0009(14) 0.0501(11) -0.0084(12) 0.116(2) C5a 0.055(2) 0.0010(12) -0.0084(15) 0.0427(13) 0.0031(12) 0.056(2) C6 0.066(2) -0.0032(14) -0.009(2) 0.0433(14) 0.0031(14) 0.069(2) C6a 0.060(2) -0.0067(13) -0.0086(14) 0.0462(14) 0.0058(13) 0.057(2) C7 0.074(2) -0.012(2) -0.001(2) 0.052(2) 0.009(2) 0.076(2) C8 0.069(2) -0.013(2) 0.005(2) 0.066(2) 0.012(2) 0.075(2) C9 0.064(2) 0.000(2) 0.005(2) 0.067(2) 0.0026(15) 0.062(2) C10 0.061(2) -0.0038(15) 0.001(2) 0.054(2) 0.0003(14) 0.057(2) C10a 0.0537(15) -0.0057(13) -0.0073(14) 0.0496(14) 0.0044(13) 0.048(2) N11 0.0635(14) -0.0058(11) -0.0047(12) 0.0417(11) -0.0026(11) 0.0543(13) O11 0.105(2) -0.0134(10) 0.0368(14) 0.0434(11) -0.0120(11) 0.107(2) C11a 0.051(2) -0.0007(13) -0.0082(14) 0.0442(13) -0.0007(11) 0.048(2) C11b 0.0488(15) -0.0025(12) -0.0101(13) 0.0471(14) 0.0002(13) 0.0510(14) _cod_database_code 2003227