#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/30/2003081.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_2003081 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_volume 55 _journal_year 1999 _chemical_formula_moiety 'C19 H9 O3,F6 P' _chemical_formula_sum 'C19 H9 F6 O3 P' _chemical_formula_weight 430.23 _chemical_name_systematic ;4,8,12-trioxa-4,8,12,12c-tetrahydro-dibenzo[cd,mn]pyrenium hexafluorophosphate ; _space_group_IT_number 167 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-R 3 2"c' _symmetry_space_group_name_H-M 'R -3 c :H' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 6 _cell_length_a 12.946(2) _cell_length_b 12.946(2) _cell_length_c 16.806(3) _cell_measurement_temperature 120(2) _cell_volume 2439.3(7) _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 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 8019 _diffrn_reflns_theta_max 26.32 _diffrn_reflns_theta_min 3.03 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_type none _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.757 _exptl_crystal_description prism _exptl_crystal_F_000 1296 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.075 _refine_diff_density_max 0.185 _refine_diff_density_min -0.301 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 557 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0261 _refine_ls_shift/su_max -0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+2.6625P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref 0.0819 _reflns_number_observed 474 _reflns_number_total 557 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file os0007.cif _[local]_cod_data_source_block 6120K _[local]_cod_cif_authors_sg_H-M 'R -3c' _cod_original_cell_volume 2439.4(7) _cod_database_code 2003081 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 P1 0.0000 0.0000 0.0000 0.0213(3) Uani d S 1 . P F1 0.04986(8) 0.11667(8) 0.05520(5) 0.0319(3) Uani d . 1 . F O1 0.78471(10) 0.0000 0.2500 0.0267(4) Uani d S 1 . O C1 1.0000 0.0000 0.2500 0.0202(7) Uani d S 1 . C C2 1.0000 0.10771(15) 0.2500 0.0221(4) Uani d S 1 . C C3 0.89117(12) 0.10668(12) 0.25162(7) 0.0241(4) Uani d . 1 . C C4 0.89034(14) 0.21302(14) 0.25388(8) 0.0299(4) Uani d . 1 . C H4 0.8193 0.2142 0.2578 0.036 Uiso calc . 1 . H C5 1.0000 0.3184(2) 0.2500 0.0322(5) Uani d S 1 . C H5 1.0000 0.3903 0.2500 0.039 Uiso calc S 1 . H 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 P1 0.0200(3) 0.0200(3) 0.0239(4) 0.0100(2) 0.000 0.000 F1 0.0322(5) 0.0258(5) 0.0363(5) 0.0134(4) -0.0033(4) -0.0081(4) O1 0.0231(5) 0.0318(8) 0.0280(7) 0.0159(4) 0.0008(3) 0.0016(6) C1 0.0226(10) 0.0226(10) 0.0152(14) 0.0113(5) 0.000 0.000 C2 0.0262(10) 0.0245(8) 0.0161(8) 0.0131(5) 0.0010(7) 0.0005(4) C3 0.0280(8) 0.0272(8) 0.0190(6) 0.0153(7) 0.0005(5) 0.0006(5) C4 0.0401(9) 0.0371(9) 0.0233(7) 0.0273(8) -0.0028(6) -0.0022(6) C5 0.0528(14) 0.0280(7) 0.0239(9) 0.0264(7) -0.0052(9) -0.0026(5) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle F1 P1 F1 19 . 180.0 F1 P1 F1 19 2 89.98(5) F1 P1 F1 . 2 90.02(5) F1 P1 F1 19 3 89.98(5) F1 P1 F1 . 3 90.02(5) F1 P1 F1 2 3 90.02(5) F1 P1 F1 19 21 90.02(5) F1 P1 F1 . 21 89.98(5) F1 P1 F1 2 21 89.98(5) F1 P1 F1 3 21 180.0 F1 P1 F1 19 20 90.02(5) F1 P1 F1 . 20 89.98(5) F1 P1 F1 2 20 180.0 F1 P1 F1 3 20 89.98(5) F1 P1 F1 21 20 90.02(5) C3 O1 C3 . 5 120.22(15) C2 C1 C2 2_645 3_765 120.0 C2 C1 C2 2_645 . 120.0 C2 C1 C2 3_765 . 120.0 C1 C2 C3 . 6_765 119.52(9) C1 C2 C3 . . 119.52(9) C3 C2 C3 6_765 . 121.0(2) O1 C3 C4 . . 119.74(13) O1 C3 C2 . . 120.33(13) C4 C3 C2 . . 119.93(15) C3 C4 C5 . . 117.54(14) C4 C5 C4 . 6_765 124.0(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance P1 F1 19 1.6074(8) P1 F1 . 1.6074(8) P1 F1 2 1.6074(8) P1 F1 3 1.6074(8) P1 F1 21 1.6074(8) P1 F1 20 1.6074(8) O1 C3 . 1.380(2) O1 C3 5 1.380(2) C1 C2 2_645 1.394(2) C1 C2 3_765 1.394(2) C1 C2 . 1.394(2) C2 C3 6_765 1.403(2) C2 C3 . 1.403(2) C3 C4 . 1.383(2) C4 C5 . 1.395(2) C5 C4 6_765 1.395(2) _journal_paper_doi 10.1107/S0108768198016140