#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003228.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_2003228 _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 O2' _chemical_formula_sum 'C17 H11 N O2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 261.27 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.470(1) _cell_length_b 20.033(2) _cell_length_c 8.970(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.91(1) _cell_angle_gamma 90.00 _cell_volume 1245.4(4) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.393 _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 13.31 _cell_measurement_theta_max 25.73 _exptl_absorpt_coefficient_mu 0.744 _cell_measurement_temperature 293(2) _exptl_crystal_description 'thin prism' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_colour 'pale yellow' _chemical_compound_source ? _diffrn_measurement_device 'Syntex P2~1~' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.10 _diffrn_reflns_number 1203 _reflns_number_total 1203 _reflns_number_observed 743 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 'not determined' _diffrn_reflns_theta_max 57.33 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0771 _refine_ls_wR_factor_obs 0.1561 _refine_ls_wR_factor_all 0.1765 _refine_ls_goodness_of_fit_obs 2.423 _refine_ls_goodness_of_fit_all 1.875 _refine_ls_number_reflns 1195 _refine_ls_number_parameters 182 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0300P)^2^] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max <0.001 _refine_diff_density_max 0.216 _refine_diff_density_min -0.210 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 0.9814(9) 0.3958(4) 0.2138(8) 0.057(2) O1 1 1.0062(7) 0.4402(2) 0.3369(6) 0.076(2) C12 1 1.1103(10) 0.4170(4) 0.5003(8) 0.079(2) H12A 1 1.1035(10) 0.4472(4) 0.5868(8) 0.064 H12B 1 1.2557(10) 0.3972(4) 0.4960(8) 0.063 H12C 1 1.0590(10) 0.3722(4) 0.5134(8) 0.133 C2 1 1.0595(10) 0.3318(4) 0.2325(9) 0.070(2) H2 1 1.1630(10) 0.3148(4) 0.3358(9) 0.128 C3 1 1.0271(10) 0.2911(4) 0.0975(10) 0.069(2) H3 1 1.0939(10) 0.2412(4) 0.1208(10) 0.053 C4 1 0.9145(10) 0.3122(3) -0.0512(9) 0.066(2) H4 1 0.8979(10) 0.2780(3) -0.1613(9) 0.043 C4a 1 0.8405(9) 0.3759(3) -0.0743(8) 0.049(2) C5 1 0.7155(11) 0.4131(4) -0.2189(9) 0.070(2) O5 1 0.6556(8) 0.3896(3) -0.3592(6) 0.093(2) C5a 1 0.6766(10) 0.4769(3) -0.1690(7) 0.051(2) C6 1 0.5691(9) 0.5310(3) -0.2535(8) 0.057(2) H6 1 0.5072(9) 0.5288(3) -0.3646(8) 0.068 C6a 1 0.5550(9) 0.5882(3) -0.1709(8) 0.054(2) C7 1 0.4523(9) 0.6466(4) -0.2457(9) 0.065(2) H7 1 0.3878(9) 0.6474(4) -0.3567(9) 0.079 C8 1 0.4469(10) 0.7012(4) -0.1576(9) 0.067(2) H8 1 0.4123(10) 0.7466(4) -0.2124(9) 0.084 C9 1 0.5508(9) 0.7004(3) 0.0096(9) 0.064(2) H9 1 0.5425(9) 0.7298(3) 0.0724(9) 0.047 C10 1 0.6480(10) 0.6463(3) 0.0877(8) 0.054(2) H10 1 0.7332(10) 0.6414(3) 0.2103(8) 0.040 C10a 1 0.6593(9) 0.5891(3) -0.0027(8) 0.049(2) N11 1 0.7643(8) 0.5348(3) 0.0865(6) 0.053(2) C11a 1 0.7694(8) 0.4832(3) 0.0004(7) 0.049(2) C11b 1 0.8725(9) 0.4194(3) 0.0603(8) 0.048(2) 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 0.049(5) -0.006(4) 0.016(4) 0.064(5) 0.007(4) 0.054(5) O1 0.077(4) 0.002(3) 0.013(3) 0.069(4) -0.004(3) 0.070(4) C12 0.078(6) 0.004(5) 0.010(4) 0.094(6) 0.007(4) 0.054(5) C2 0.048(5) 0.002(4) 0.012(4) 0.068(6) 0.014(5) 0.082(6) C3 0.045(5) 0.000(4) 0.026(5) 0.061(5) 0.001(5) 0.100(6) C4 0.064(5) 0.000(4) 0.017(4) 0.060(5) -0.011(4) 0.068(5) C4a 0.048(4) -0.010(4) 0.015(4) 0.046(4) -0.001(3) 0.050(4) C5 0.078(6) -0.007(5) 0.040(5) 0.065(5) -0.015(5) 0.076(6) O5 0.115(5) 0.014(3) 0.019(3) 0.080(4) -0.023(3) 0.069(4) C5a 0.058(5) -0.010(4) 0.016(4) 0.046(4) -0.004(3) 0.046(4) C6 0.059(5) -0.001(4) 0.013(4) 0.069(5) -0.001(4) 0.037(4) C6a 0.053(5) -0.004(4) 0.019(4) 0.054(5) 0.015(4) 0.053(5) C7 0.055(5) 0.004(4) 0.017(4) 0.081(6) 0.003(5) 0.057(5) C8 0.057(5) 0.013(4) 0.013(4) 0.069(6) 0.014(4) 0.065(5) C9 0.058(5) 0.007(4) 0.037(4) 0.061(5) -0.015(4) 0.084(6) C10 0.067(5) -0.011(4) 0.017(4) 0.039(4) -0.011(4) 0.052(4) C10a 0.050(4) -0.005(3) 0.022(4) 0.034(4) 0.014(3) 0.064(5) N11 0.057(4) -0.009(3) 0.025(3) 0.046(4) -0.011(3) 0.059(4) C11a 0.032(4) -0.004(3) 0.025(4) 0.064(5) -0.006(4) 0.059(5) C11b 0.036(4) -0.002(3) 0.013(3) 0.056(4) 0.007(3) 0.050(4)