#------------------------------------------------------------------------------ #$Date: 2011-09-10 05:16:28 +0200 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003088.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_2003088 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 12.964(2) _cell_length_b 12.964(2) _cell_length_c 16.813(3) _cell_measurement_temperature 160(2) _cell_volume 2447.1(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 .0520 _diffrn_reflns_av_sigmaI/netI .0170 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 8102 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 3.03 _exptl_absorpt_coefficient_mu .255 _exptl_absorpt_correction_type none _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.752 _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 .178 _refine_diff_density_min -.298 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 47 _refine_ls_number_reflns 561 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all .0462 _refine_ls_R_factor_gt .0310 _refine_ls_shift/su_max -.007 _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 .0902 _reflns_number_observed 425 _reflns_number_total 561 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file os0007.cif _[local]_cod_data_source_block 6160K _[local]_cod_cif_authors_sg_H-M 'R -3c' _cod_original_cell_volume 2447.3(7) _cod_database_code 2003088 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 .0277(4) .0277(4) .0323(6) .0138(2) .000 .000 F1 .0444(7) .0351(7) .0492(7) .0183(6) -.0053(5) -.0117(5) O1 .0324(7) .0458(11) .0360(10) .0229(6) .0012(4) .0025(9) C1 .0296(13) .0296(13) .020(2) .0148(7) .000 .000 C2 .0348(14) .0317(10) .0226(11) .0174(7) .0004(10) .0002(5) C3 .0374(11) .0357(11) .0249(8) .0204(9) .0006(7) .0007(7) C4 .0561(13) .0514(13) .0312(10) .0387(11) -.0043(9) -.0037(9) C5 .071(2) .0389(11) .0324(14) .0357(11) -.0084(14) -.0042(7) 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 .0292(3) Uani d S 1 P F1 .04964(11) .11613(9) .05494(6) .0436(4) Uani d . 1 F O1 .78529(13) .0000 .2500 .0366(5) Uani d S 1 O C1 1.0000 .0000 .2500 .0262(9) Uani d S 1 C C2 1.0000 .1072(2) .2500 .0293(6) Uani d S 1 C C3 .8916(2) .1065(2) .25166(9) .0317(4) Uani d . 1 C C4 .8909(2) .2123(2) .25376(10) .0410(5) Uani d . 1 C H4 .8199 .2136 .2576 .049 Uiso calc . 1 H C5 1.0000 .3171(2) .2500 .0439(8) Uani d S 1 C H5 1.0000 .3888 .2500 .053 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 2 89.94(6) F1 P1 F1 . 2 90.06(6) F1 P1 F1 19 21 90.06(6) F1 P1 F1 . 21 89.94(6) F1 P1 F1 2 21 89.94(6) F1 P1 F1 19 3 89.94(6) F1 P1 F1 . 3 90.06(6) F1 P1 F1 2 3 90.06(6) F1 P1 F1 21 3 180.0 F1 P1 F1 19 20 90.06(6) F1 P1 F1 . 20 89.94(6) F1 P1 F1 2 20 180.0 F1 P1 F1 21 20 90.06(6) F1 P1 F1 3 20 89.94(6) C3 O1 C3 . 5 120.2(2) C2 C1 C2 2_645 . 120.0 C2 C1 C2 2_645 3_765 120.0 C2 C1 C2 . 3_765 120.0 C1 C2 C3 . 6_765 119.65(13) C1 C2 C3 . . 119.65(13) C3 C2 C3 6_765 . 120.7(3) O1 C3 C4 . . 119.7(2) O1 C3 C2 . . 120.2(2) C4 C3 C2 . . 120.0(2) C3 C4 C5 . . 117.5(2) C4 C5 C4 . 6_765 124.1(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance P1 F1 19 1.6017(10) P1 F1 . 1.6017(10) P1 F1 2 1.6017(10) P1 F1 21 1.6017(10) P1 F1 3 1.6017(10) P1 F1 20 1.6017(10) O1 C3 . 1.380(2) O1 C3 5 1.380(2) C1 C2 2_645 1.390(3) C1 C2 . 1.390(3) C1 C2 3_765 1.390(3) C2 C3 6_765 1.401(2) C2 C3 . 1.401(2) C3 C4 . 1.378(3) C4 C5 . 1.389(2) C5 C4 6_765 1.389(2)