#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003091.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_2003091 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 410 _journal_page_last 423 _space_group_IT_number 167 _symmetry_space_group_name_Hall '-R 3 2"c' _symmetry_space_group_name_H-M 'R -3 c :H' _[local]_cod_cif_authors_sg_H-M 'R -3c' loop_ _publ_author_name ; 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 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 13.040(2) _cell_length_b 13.040(2) _cell_length_c 16.884(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2486.5(7) _cell_formula_units_Z 6 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 243(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 1.724 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.251 _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 8207 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _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 569 _reflns_number_observed 352 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0953 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.948 _refine_ls_number_reflns 569 _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 -0.023 _refine_diff_density_max 0.145 _refine_diff_density_min -0.201 _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 0.0470(4) Uani d S 1 . P F1 0.04927(13) 0.11510(11) 0.05442(8) 0.0707(5) Uani d . 1 . F O1 0.7870(2) 0.0000 0.2500 0.0589(6) Uani d S 1 . O C1 1.0000 0.0000 0.2500 0.0402(10) Uani d S 1 . C C2 1.0000 0.1067(2) 0.2500 0.0463(7) Uani d S 1 . C C3 0.8924(2) 0.1059(2) 0.25163(11) 0.0518(6) Uani d . 1 . C C4 0.8918(2) 0.2111(2) 0.25370(12) 0.0664(7) Uani d . 1 . C H4 0.8214 0.2126 0.2574 0.080 Uiso calc . 1 . H C5 1.0000 0.3145(3) 0.2500 0.0711(11) Uani d S 1 . C H5 1.0000 0.3858 0.2500 0.085 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 0.0463(5) 0.0463(5) 0.0484(7) 0.0231(2) 0.000 0.000 F1 0.0743(10) 0.0576(8) 0.0751(10) 0.0292(8) -0.0084(7) -0.0195(6) O1 0.0533(9) 0.076(2) 0.0554(13) 0.0378(8) 0.0018(6) 0.0036(12) C1 0.046(2) 0.046(2) 0.029(2) 0.0229(8) 0.000 0.000 C2 0.056(2) 0.0509(13) 0.0334(13) 0.0281(9) 0.0022(14) 0.0011(7) C3 0.061(2) 0.0635(15) 0.0388(10) 0.0375(12) -0.0001(11) 0.0008(10) C4 0.092(2) 0.085(2) 0.0501(13) 0.065(2) -0.0075(13) -0.0068(13) C5 0.118(4) 0.0630(15) 0.051(2) 0.059(2) -0.018(2) -0.0091(10) _cod_database_code 2003091