#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003078.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_2003078 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 410 _journal_page_last 423 loop_ _publ_author_name ; Frederik C. Krebs ; _chemical_name_systematic ; 4,8,12-trioxa-4,8,12,12c-tetrahydro-dibenzo[cd,mn]pyrenium iodide ; _chemical_formula_moiety 'C19 H9 O3, I' _chemical_formula_sum 'C19 H9 I O3' _chemical_formula_weight 412.16 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.934(3) _cell_length_b 14.748(3) _cell_length_c 15.858(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3024.9(10) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293(2) _exptl_crystal_description cube _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.810 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 2.129 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.476 _exptl_absorpt_correction_T_max 0.603 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'omega scan, frame data integration' _diffrn_reflns_number 29370 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0116 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 3093 _reflns_number_observed 2679 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1104 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.196 _refine_ls_number_reflns 3093 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+2.1435P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.383 _refine_diff_density_min -1.740 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol C1 0.8724(2) 0.6351(2) 0.7442(2) 0.0441(7) Uani d . 1 . C C2 0.9012(3) 0.5494(2) 0.7160(2) 0.0465(7) Uani d . 1 . C C3 0.9530(3) 0.5411(3) 0.6391(2) 0.0519(8) Uani d . 1 . C C4 0.9804(4) 0.4568(3) 0.6105(2) 0.0644(10) Uani d . 1 . C H4 1.0166 0.4498 0.5602 0.077 Uiso calc . 1 . H C5 0.9525(4) 0.3824(3) 0.6584(3) 0.0641(10) Uani d . 1 . C H5 0.9697 0.3251 0.6383 0.077 Uiso calc . 1 . H C6 0.9011(3) 0.3884(3) 0.7338(3) 0.0587(9) Uani d . 1 . C H6 0.8834 0.3364 0.7638 0.070 Uiso calc . 1 . H C7 0.8763(2) 0.4731(3) 0.7639(2) 0.0512(8) Uani d . 1 . C C8 0.8207(3) 0.6440(2) 0.8205(2) 0.0476(7) Uani d . 1 . C C9 0.8002(3) 0.5673(3) 0.8695(2) 0.0541(9) Uani d . 1 . C C10 0.7532(4) 0.5760(3) 0.9466(2) 0.0687(10) Uani d . 1 . C H10 0.7396 0.5257 0.9802 0.082 Uiso calc . 1 . H C11 0.7267(3) 0.6628(4) 0.9724(3) 0.0753(12) Uani d . 1 . C H11 0.6949 0.6692 1.0247 0.090 Uiso calc . 1 . H C12 0.7441(3) 0.7402(3) 0.9260(2) 0.0650(10) Uani d . 1 . C H12 0.7242 0.7969 0.9459 0.078 Uiso calc . 1 . H C13 0.7921(3) 0.7307(3) 0.8488(2) 0.0536(8) Uani d . 1 . C C14 0.8935(2) 0.7111(2) 0.6959(2) 0.0469(7) Uani d . 1 . C C15 0.8611(3) 0.7967(3) 0.7234(2) 0.0511(8) Uani d . 1 . C C16 0.8791(3) 0.8723(2) 0.6752(3) 0.0617(10) Uani d . 1 . C H16 0.8566 0.9293 0.6921 0.074 Uiso calc . 1 . H C17 0.9324(4) 0.8600(3) 0.5997(3) 0.0645(10) Uani d . 1 . C H17 0.9463 0.9109 0.5671 0.077 Uiso calc . 1 . H C18 0.9660(3) 0.7764(3) 0.5701(2) 0.0626(10) Uani d . 1 . C H18 1.0011 0.7713 0.5191 0.075 Uiso calc . 1 . H C19 0.9454(3) 0.7018(3) 0.6186(2) 0.0531(8) Uani d . 1 . C O1 0.9754(2) 0.6168(2) 0.5923(2) 0.0605(7) Uani d . 1 . O O2 0.8272(2) 0.4824(2) 0.8404(2) 0.0581(6) Uani d . 1 . O O3 0.8128(2) 0.8055(2) 0.8003(2) 0.0579(6) Uani d . 1 . O I1 0.87640(2) 0.12899(2) 0.62911(2) 0.06149(14) Uani d . 1 . I loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.038(2) 0.049(2) 0.046(2) -0.0013(13) -0.0049(13) -0.0001(13) C2 0.047(2) 0.046(2) 0.046(2) -0.0021(14) -0.0040(13) -0.0022(13) C3 0.057(2) 0.052(2) 0.047(2) 0.004(2) -0.0028(15) -0.0004(14) C4 0.082(3) 0.061(2) 0.050(2) 0.012(2) -0.003(2) -0.010(2) C5 0.070(3) 0.051(2) 0.071(2) 0.011(2) -0.017(2) -0.011(2) C6 0.056(2) 0.047(2) 0.073(2) -0.005(2) -0.012(2) 0.004(2) C7 0.047(2) 0.052(2) 0.055(2) -0.0044(14) -0.0076(15) 0.002(2) C8 0.040(2) 0.056(2) 0.047(2) -0.0007(14) -0.0015(13) -0.0031(14) C9 0.045(2) 0.066(2) 0.051(2) -0.005(2) -0.0004(14) 0.004(2) C10 0.063(2) 0.085(3) 0.058(2) -0.003(2) 0.008(2) 0.011(2) C11 0.065(3) 0.106(4) 0.055(2) 0.007(3) 0.011(2) -0.009(2) C12 0.056(2) 0.079(3) 0.060(2) 0.008(2) 0.007(2) -0.014(2) C13 0.043(2) 0.061(2) 0.056(2) 0.003(2) -0.0013(15) -0.006(2) C14 0.043(2) 0.049(2) 0.049(2) -0.0015(14) -0.0016(13) 0.0013(14) C15 0.046(2) 0.050(2) 0.057(2) -0.0021(14) -0.0043(15) 0.000(2) C16 0.058(2) 0.048(2) 0.079(3) 0.002(2) -0.011(2) 0.003(2) C17 0.064(3) 0.058(2) 0.072(2) -0.006(2) -0.009(2) 0.017(2) C18 0.065(2) 0.066(2) 0.057(2) -0.003(2) 0.003(2) 0.014(2) C19 0.054(2) 0.054(2) 0.051(2) 0.002(2) 0.0016(15) 0.0005(15) O1 0.075(2) 0.0581(15) 0.0478(13) 0.0058(13) 0.0114(12) 0.0017(11) O2 0.061(2) 0.0552(14) 0.0579(14) -0.0067(12) 0.0051(12) 0.0083(11) O3 0.0576(15) 0.0519(14) 0.0641(15) 0.0071(12) 0.0032(12) -0.0067(11) I1 0.0620(2) 0.0500(2) 0.0724(2) 0.00363(10) 0.00786(11) 0.01283(10) _cod_database_code 2003078