#------------------------------------------------------------------------------ #$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003095.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_2003095 loop_ _publ_author_name 'Krebs, Frederik C.' 'Laursen, Bo W.' 'Johannsen, Ib' 'Faldt, Andr\'e' 'Bechgaard, Klaus' 'Jacobsen, Claus S.' 'Thorup, Niels' 'Boubekeur, Kamal' _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 13.131(2) _cell_length_b 13.131(2) _cell_length_c 16.970(3) _cell_measurement_temperature 338(2) _cell_volume 2534.0(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 .71073 _diffrn_reflns_av_R_equivalents .0708 _diffrn_reflns_av_sigmaI/netI .0244 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 8356 _diffrn_reflns_theta_max 26.39 _diffrn_reflns_theta_min 3.00 _exptl_absorpt_coefficient_mu .246 _exptl_absorpt_correction_type none _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.692 _exptl_crystal_description prism _exptl_crystal_F_000 1296 _exptl_crystal_size_max .25 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .075 _refine_diff_density_max .113 _refine_diff_density_min -.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 579 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all .1019 _refine_ls_R_factor_gt .0365 _refine_ls_shift/su_max -.028 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+1.2721P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_ref .1137 _reflns_number_observed 275 _reflns_number_total 579 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file os0007.cif _[local]_cod_data_source_block 6338K _[local]_cod_cif_authors_sg_H-M 'R -3c' _cod_database_code 2003095 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_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 .0726(8) .0726(8) .0708(10) .0363(4) .000 .000 F1 .121(2) .0923(12) .1163(15) .0475(13) -.0134(11) -.0324(9) O1 .0845(14) .122(3) .081(2) .0611(14) .0011(10) .002(2) C1 .071(2) .071(2) .045(3) .0353(12) .000 .000 C2 .082(3) .075(2) .051(2) .0411(14) .002(2) .0010(10) C3 .101(3) .098(3) .0561(15) .060(2) .000(2) -.001(2) C4 .147(4) .132(3) .075(2) .102(3) -.011(2) -.012(2) C5 .196(7) .105(2) .079(3) .098(3) -.030(4) -.015(2) 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_type_symbol P1 .0000 .0000 .0000 .0720(6) Uani d S 1 P F1 .0483(2) .11356(14) .05367(9) .1126(8) Uani d . 1 F O1 .7892(2) .0000 .2500 .0917(9) Uani d S 1 O C1 1.0000 .0000 .2500 .0620(15) Uani d S 1 C C2 1.0000 .1056(3) .2500 .0688(10) Uani d S 1 C C3 .8935(3) .1050(3) .25159(13) .0800(8) Uani d . 1 C C4 .8925(3) .2090(4) .2537(2) .1036(12) Uani d . 1 C H4 .8226 .2104 .2574 .124 Uiso calc . 1 H C5 1.0000 .3114(4) .2500 .117(2) Uani d S 1 C H5 1.0000 .3822 .2500 .140 Uiso calc S 1 H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle F1 P1 F1 19 . 180.0 F1 P1 F1 19 21 90.24(9) F1 P1 F1 . 21 89.76(9) F1 P1 F1 19 2 89.76(9) F1 P1 F1 . 2 90.24(9) F1 P1 F1 21 2 89.76(9) F1 P1 F1 19 3 89.76(9) F1 P1 F1 . 3 90.24(9) F1 P1 F1 21 3 180.0 F1 P1 F1 2 3 90.24(9) F1 P1 F1 19 20 90.24(9) F1 P1 F1 . 20 89.76(9) F1 P1 F1 21 20 90.24(9) F1 P1 F1 2 20 180.0 F1 P1 F1 3 20 89.76(9) C3 O1 C3 5 . 120.6(3) C2 C1 C2 2_645 . 120.0 C2 C1 C2 2_645 3_765 120.0 C2 C1 C2 . 3_765 120.0000(10) C1 C2 C3 . 6_765 119.7(2) C1 C2 C3 . . 119.7(2) C3 C2 C3 6_765 . 120.6(5) C4 C3 O1 . . 119.8(3) C4 C3 C2 . . 120.2(4) O1 C3 C2 . . 120.0(3) C3 C4 C5 . . 117.0(4) C4 C5 C4 . 6_765 124.8(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance P1 F1 19 1.584(2) P1 F1 . 1.584(2) P1 F1 21 1.584(2) P1 F1 2 1.584(2) P1 F1 3 1.584(2) P1 F1 20 1.584(2) O1 C3 5 1.374(4) O1 C3 . 1.374(4) C1 C2 2_645 1.387(4) C1 C2 . 1.387(4) C1 C2 3_765 1.387(4) C2 C3 6_765 1.394(3) C2 C3 . 1.394(3) C3 C4 . 1.373(4) C4 C5 . 1.381(4) C5 C4 6_765 1.381(4)