#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003081.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_2003081 _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 12.946(2) _cell_length_b 12.946(2) _cell_length_c 16.806(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2439.4(7) _cell_formula_units_Z 6 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 120(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 1.757 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.256 _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 8019 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.32 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 557 _reflns_number_observed 474 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0819 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.037 _refine_ls_number_reflns 557 _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 -0.002 _refine_diff_density_max 0.185 _refine_diff_density_min -0.301 _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 0.0213(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)