#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/30/2003079.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003079 loop_ _publ_author_name ; Frederik C. Krebs ; _publ_section_title ; The geometry and structural properties of the 4,8,12-trioxa-4,8,12,12c-tetrahydrodibenzo[cd,mn]pyrene system in the cationic state. Structures of a planar organic cation with various monovalent and divalent anions ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 410 _journal_page_last 423 _journal_paper_doi 10.1107/S0108768198016140 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C19 H9 O3,B F4' _chemical_formula_sum 'C19 H9 B F4 O3' _chemical_formula_weight 372.07 _chemical_name_systematic ; 4,8,12-trioxa-4,8,12,12c-tetrahydro-dibenzo[cd,mn]pyrenium tetrafluoroborate ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 12.817(3) _cell_length_b 15.196(3) _cell_length_c 15.396(3) _cell_measurement_temperature 120(2) _cell_volume 2998.6(11) _computing_cell_refinement 'SAINT Siemens' _computing_data_collection 'SMART Siemens' _computing_data_reduction 'SAINT Siemens' _computing_molecular_graphics 'SHELXTL (Sheldrick)' _computing_publication_material 'XCIF (Sheldrick)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'omega scan, frame data integration' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 29798 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 2.46 _exptl_absorpt_coefficient_mu 0.143 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_type empirical _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.648 _exptl_crystal_description needle _exptl_crystal_F_000 1504 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.562 _refine_diff_density_min -0.517 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 3054 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0437 _refine_ls_shift/su_max -0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+2.6840P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1239 _reflns_number_observed 2381 _reflns_number_total 3056 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file os0007.cif _[local]_cod_data_source_block 4 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+2.6840P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+2.6840P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2998.6(10) _cod_database_code 2003079 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' 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 F1 0.0356(7) 0.0934(12) 0.0424(8) -0.0078(8) -0.0117(6) 0.0125(8) F2 0.0386(7) 0.0632(9) 0.0430(8) 0.0050(7) 0.0037(6) -0.0017(7) F3 0.0446(8) 0.0503(8) 0.0306(6) -0.0112(6) -0.0075(6) 0.0073(6) F4 0.130(2) 0.0245(8) 0.1011(15) 0.0137(9) 0.0267(13) 0.0071(8) O1 0.0288(7) 0.0320(8) 0.0296(7) -0.0031(6) -0.0012(6) -0.0057(6) O2 0.0343(8) 0.0283(7) 0.0233(7) -0.0029(6) -0.0038(6) -0.0004(6) O3 0.0284(7) 0.0337(8) 0.0279(7) 0.0039(6) -0.0010(6) 0.0036(6) B1 0.0313(12) 0.0271(11) 0.0324(12) 0.0005(9) 0.0001(10) 0.0054(9) C1 0.0194(9) 0.0294(10) 0.0233(9) 0.0017(7) 0.0034(7) -0.0021(8) C2 0.0227(9) 0.0268(10) 0.0244(9) 0.0011(7) 0.0027(7) -0.0015(8) C3 0.0218(9) 0.0311(10) 0.0262(9) 0.0004(8) 0.0031(7) -0.0043(8) C4 0.0290(10) 0.0269(10) 0.0356(11) -0.0007(8) 0.0069(9) -0.0024(9) C5 0.0302(10) 0.0296(11) 0.0323(11) 0.0033(8) 0.0060(8) 0.0048(9) C6 0.0281(10) 0.0347(11) 0.0252(9) 0.0016(8) 0.0018(8) 0.0027(8) C7 0.0245(9) 0.0299(10) 0.0238(9) -0.0019(8) 0.0026(7) -0.0036(8) C8 0.0222(9) 0.0274(10) 0.0233(9) 0.0015(7) 0.0043(7) -0.0012(8) C9 0.0275(10) 0.0275(10) 0.0226(9) 0.0010(8) 0.0045(8) -0.0017(8) C10 0.0329(11) 0.0348(11) 0.0243(9) -0.0040(9) 0.0036(8) -0.0045(8) C11 0.0331(11) 0.0272(10) 0.0340(11) -0.0036(9) 0.0111(9) -0.0056(9) C12 0.0274(10) 0.0281(10) 0.0359(11) 0.0042(8) 0.0076(8) 0.0028(9) C13 0.0213(9) 0.0323(11) 0.0265(10) 0.0034(8) 0.0051(8) 0.0010(8) C14 0.0188(9) 0.0348(11) 0.0242(9) 0.0009(8) 0.0017(7) -0.0017(8) C15 0.0211(9) 0.0378(11) 0.0260(9) 0.0017(8) 0.0032(8) 0.0004(8) C16 0.0253(10) 0.0498(13) 0.0270(10) 0.0037(9) 0.0000(8) 0.0049(9) C17 0.0251(10) 0.0625(15) 0.0245(10) -0.0032(10) -0.0032(8) -0.0022(10) C18 0.0257(10) 0.0461(12) 0.0293(10) -0.0047(9) -0.0001(8) -0.0073(9) C19 0.0214(9) 0.0359(11) 0.0265(9) -0.0006(8) 0.0027(8) -0.0023(8) 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 F1 0.53697(11) 0.58286(12) 0.59875(9) 0.0571(4) Uani d . 1 . F F2 0.71216(11) 0.59357(10) 0.58733(9) 0.0483(4) Uani d . 1 . F F3 0.63652(10) 0.58242(9) 0.71954(8) 0.0418(3) Uani d . 1 . F F4 0.6204(2) 0.70674(10) 0.64035(14) 0.0853(7) Uani d . 1 . F O1 0.68793(11) 0.30995(9) 0.80019(9) 0.0301(3) Uani d . 1 . O O2 0.52205(11) 0.12281(9) 0.58920(8) 0.0286(3) Uani d . 1 . O O3 0.67891(11) -0.00380(9) 0.84489(9) 0.0300(3) Uani d . 1 . O B1 0.6263(2) 0.6169(2) 0.6367(2) 0.0302(5) Uani d . 1 . B C1 0.62937(14) 0.14304(12) 0.74483(12) 0.0240(4) Uani d . 1 . C C2 0.60645(14) 0.21643(13) 0.69395(12) 0.0247(4) Uani d . 1 . C C3 0.63884(14) 0.30015(13) 0.72109(12) 0.0264(4) Uani d . 1 . C C4 0.6192(2) 0.37264(13) 0.67007(14) 0.0305(4) Uani d . 1 . C H4 0.6411 0.4285 0.6869 0.037 Uiso calc . 1 . H C5 0.5656(2) 0.35974(13) 0.59238(13) 0.0307(5) Uani d . 1 . C H5 0.5514 0.4086 0.5580 0.037 Uiso calc . 1 . H C6 0.5321(2) 0.27747(14) 0.56355(13) 0.0293(4) Uani d . 1 . C H6 0.4967 0.2714 0.5112 0.035 Uiso calc . 1 . H C7 0.55303(15) 0.20557(13) 0.61505(12) 0.0261(4) Uani d . 1 . C C8 0.60070(14) 0.05953(13) 0.71712(12) 0.0243(4) Uani d . 1 . C C9 0.54533(15) 0.05006(13) 0.63893(12) 0.0259(4) Uani d . 1 . C C10 0.5149(2) -0.03224(14) 0.61179(13) 0.0307(5) Uani d . 1 . C H10 0.4756 -0.0395 0.5616 0.037 Uiso calc . 1 . H C11 0.5448(2) -0.10424(13) 0.66169(14) 0.0314(5) Uani d . 1 . C H11 0.5264 -0.1601 0.6424 0.038 Uiso calc . 1 . H C12 0.6006(2) -0.09739(13) 0.73885(14) 0.0305(5) Uani d . 1 . C H12 0.6195 -0.1472 0.7702 0.037 Uiso calc . 1 . H C13 0.62709(14) -0.01423(13) 0.76747(12) 0.0267(4) Uani d . 1 . C C14 0.68214(14) 0.15331(13) 0.82334(12) 0.0259(4) Uani d . 1 . C C15 0.70531(15) 0.07872(14) 0.87366(13) 0.0283(4) Uani d . 1 . C C16 0.7550(2) 0.0885(2) 0.95264(13) 0.0340(5) Uani d . 1 . C H16 0.7711 0.0400 0.9870 0.041 Uiso calc . 1 . H C17 0.7800(2) 0.1737(2) 0.97895(13) 0.0373(5) Uani d . 1 . C H17 0.8125 0.1808 1.0325 0.045 Uiso calc . 1 . H C18 0.7594(2) 0.2488(2) 0.93008(13) 0.0337(5) Uani d . 1 . C H18 0.7782 0.3044 0.9499 0.040 Uiso calc . 1 . H C19 0.71009(15) 0.23784(14) 0.85112(12) 0.0279(4) Uani d . 1 . C 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C19 O1 C3 120.7(2) C9 O2 C7 120.64(15) C15 O3 C13 120.3(2) F4 B1 F2 108.8(2) F4 B1 F3 110.2(2) F2 B1 F3 109.5(2) F4 B1 F1 110.1(2) F2 B1 F1 109.2(2) F3 B1 F1 109.0(2) C8 C1 C14 119.8(2) C8 C1 C2 120.2(2) C14 C1 C2 120.0(2) C1 C2 C3 119.7(2) C1 C2 C7 119.7(2) C3 C2 C7 120.6(2) C4 C3 O1 120.1(2) C4 C3 C2 120.2(2) O1 C3 C2 119.8(2) C3 C4 C5 117.9(2) C6 C5 C4 123.5(2) C7 C6 C5 117.9(2) C6 C7 O2 120.1(2) C6 C7 C2 120.0(2) O2 C7 C2 119.9(2) C1 C8 C13 119.8(2) C1 C8 C9 119.4(2) C13 C8 C9 120.9(2) C10 C9 O2 120.0(2) C10 C9 C8 119.8(2) O2 C9 C8 120.2(2) C9 C10 C11 118.0(2) C10 C11 C12 123.7(2) C13 C12 C11 117.9(2) O3 C13 C12 120.1(2) O3 C13 C8 120.2(2) C12 C13 C8 119.7(2) C1 C14 C19 119.5(2) C1 C14 C15 119.4(2) C19 C14 C15 121.2(2) O3 C15 C16 119.7(2) O3 C15 C14 120.5(2) C16 C15 C14 119.8(2) C15 C16 C17 117.5(2) C18 C17 C16 124.1(2) C19 C18 C17 117.6(2) O1 C19 C18 120.0(2) O1 C19 C14 120.2(2) C18 C19 C14 119.8(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance F1 B1 1.386(3) F2 B1 1.384(3) F3 B1 1.385(3) F4 B1 1.369(3) O1 C19 1.377(2) O1 C3 1.379(2) O2 C9 1.377(2) O2 C7 1.378(2) O3 C15 1.372(3) O3 C13 1.374(2) C1 C8 1.388(3) C1 C14 1.394(3) C1 C2 1.394(3) C2 C3 1.402(3) C2 C7 1.404(3) C3 C4 1.376(3) C4 C5 1.394(3) C5 C6 1.394(3) C6 C7 1.376(3) C8 C13 1.404(3) C8 C9 1.405(3) C9 C10 1.375(3) C10 C11 1.391(3) C11 C12 1.391(3) C12 C13 1.381(3) C14 C19 1.400(3) C14 C15 1.405(3) C15 C16 1.380(3) C16 C17 1.395(3) C17 C18 1.392(3) C18 C19 1.380(3)