#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003088.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_2003088 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1999 _journal_volume B55 _journal_page_first 410 _journal_page_last 423 ; Frederik C. Krebs ; _chemical_name_systematic ; 4,8,12-trioxa-4,8,12,12c-tetrahydro-dibenzo[cd,mn]pyrenium hexafluorophosphate ; _chemical_name_common ? _chemical_formula_moiety 'C19 H9 O3,F6 P' _chemical_formula_sum 'C19 H9 F6 O3 P' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 430.23 _chemical_melting_point ? _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3c' _symmetry_space_group_name_Hall '-R 3 2"c' 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' _cell_length_a 12.964(2) _cell_length_b 12.964(2) _cell_length_c 16.813(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2447.3(7) _cell_formula_units_Z 6 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 160(2) _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.075 _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.255 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 8102 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 561 _reflns_number_observed 425 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0902 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_number_reflns 561 _refine_ls_number_parameters 47 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _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_shift/su_max -0.007 _refine_diff_density_max 0.178 _refine_diff_density_min -0.298 _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' '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 0.0292(3) Uani d S 1 . P F1 0.04964(11) 0.11613(9) 0.05494(6) 0.0436(4) Uani d . 1 . F O1 0.78529(13) 0.0000 0.2500 0.0366(5) Uani d S 1 . O C1 1.0000 0.0000 0.2500 0.0262(9) Uani d S 1 . C C2 1.0000 0.1072(2) 0.2500 0.0293(6) Uani d S 1 . C C3 0.8916(2) 0.1065(2) 0.25166(9) 0.0317(4) Uani d . 1 . C C4 0.8909(2) 0.2123(2) 0.25376(10) 0.0410(5) Uani d . 1 . C H4 0.8199 0.2136 0.2576 0.049 Uiso calc . 1 . H C5 1.0000 0.3171(2) 0.2500 0.0439(8) Uani d S 1 . C H5 1.0000 0.3888 0.2500 0.053 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 0.0277(4) 0.0277(4) 0.0323(6) 0.0138(2) 0.000 0.000 F1 0.0444(7) 0.0351(7) 0.0492(7) 0.0183(6) -0.0053(5) -0.0117(5) O1 0.0324(7) 0.0458(11) 0.0360(10) 0.0229(6) 0.0012(4) 0.0025(9) C1 0.0296(13) 0.0296(13) 0.020(2) 0.0148(7) 0.000 0.000 C2 0.0348(14) 0.0317(10) 0.0226(11) 0.0174(7) 0.0004(10) 0.0002(5) C3 0.0374(11) 0.0357(11) 0.0249(8) 0.0204(9) 0.0006(7) 0.0007(7) C4 0.0561(13) 0.0514(13) 0.0312(10) 0.0387(11) -0.0043(9) -0.0037(9) C5 0.071(2) 0.0389(11) 0.0324(14) 0.0357(11) -0.0084(14) -0.0042(7)