#------------------------------------------------------------------------------ #$Date: 2008-03-08 13:08:03 +0000 (Sat, 08 Mar 2008) $ #$Revision: 247 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003079.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_2003079 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1999 _journal_volume B55 _journal_page_first 410 _journal_page_last 423 _publ_author_name ; Frederik C. Krebs ; _chemical_name_systematic ; 4,8,12-trioxa-4,8,12,12c-tetrahydro-dibenzo[cd,mn]pyrenium tetrafluoroborate ; _chemical_formula_moiety 'C19 H9 O3,B F4' _chemical_formula_sum 'C19 H9 B F4 O3' _chemical_formula_weight 372.07 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.817(3) _cell_length_b 15.196(3) _cell_length_c 15.396(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2998.6(10) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 120(2) _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.143 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.980 _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 29798 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 3056 _reflns_number_observed 2381 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1239 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.035 _refine_ls_number_reflns 3054 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+2.6840P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.004 _refine_diff_density_max 0.562 _refine_diff_density_min -0.517 _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' 'B' 'B' 0.0013 0.0007 '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' 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 F1 0.53697(11) 0.58286(12) 0.59875(9) 0.0571(4) Uani d . 1 . F F2 0.71216(11) 0.59357(10) 0.58733(9) 0.0483(4) Uani d . 1 . F F3 0.63652(10) 0.58242(9) 0.71954(8) 0.0418(3) Uani d . 1 . F F4 0.6204(2) 0.70674(10) 0.64035(14) 0.0853(7) Uani d . 1 . F O1 0.68793(11) 0.30995(9) 0.80019(9) 0.0301(3) Uani d . 1 . O O2 0.52205(11) 0.12281(9) 0.58920(8) 0.0286(3) Uani d . 1 . O O3 0.67891(11) -0.00380(9) 0.84489(9) 0.0300(3) Uani d . 1 . O B1 0.6263(2) 0.6169(2) 0.6367(2) 0.0302(5) Uani d . 1 . B C1 0.62937(14) 0.14304(12) 0.74483(12) 0.0240(4) Uani d . 1 . C C2 0.60645(14) 0.21643(13) 0.69395(12) 0.0247(4) Uani d . 1 . C C3 0.63884(14) 0.30015(13) 0.72109(12) 0.0264(4) Uani d . 1 . C C4 0.6192(2) 0.37264(13) 0.67007(14) 0.0305(4) Uani d . 1 . C H4 0.6411 0.4285 0.6869 0.037 Uiso calc . 1 . H C5 0.5656(2) 0.35974(13) 0.59238(13) 0.0307(5) Uani d . 1 . C H5 0.5514 0.4086 0.5580 0.037 Uiso calc . 1 . H C6 0.5321(2) 0.27747(14) 0.56355(13) 0.0293(4) Uani d . 1 . C H6 0.4967 0.2714 0.5112 0.035 Uiso calc . 1 . H C7 0.55303(15) 0.20557(13) 0.61505(12) 0.0261(4) Uani d . 1 . C C8 0.60070(14) 0.05953(13) 0.71712(12) 0.0243(4) Uani d . 1 . C C9 0.54533(15) 0.05006(13) 0.63893(12) 0.0259(4) Uani d . 1 . C C10 0.5149(2) -0.03224(14) 0.61179(13) 0.0307(5) Uani d . 1 . C H10 0.4756 -0.0395 0.5616 0.037 Uiso calc . 1 . H C11 0.5448(2) -0.10424(13) 0.66169(14) 0.0314(5) Uani d . 1 . C H11 0.5264 -0.1601 0.6424 0.038 Uiso calc . 1 . H C12 0.6006(2) -0.09739(13) 0.73885(14) 0.0305(5) Uani d . 1 . C H12 0.6195 -0.1472 0.7702 0.037 Uiso calc . 1 . H C13 0.62709(14) -0.01423(13) 0.76747(12) 0.0267(4) Uani d . 1 . C C14 0.68214(14) 0.15331(13) 0.82334(12) 0.0259(4) Uani d . 1 . C C15 0.70531(15) 0.07872(14) 0.87366(13) 0.0283(4) Uani d . 1 . C C16 0.7550(2) 0.0885(2) 0.95264(13) 0.0340(5) Uani d . 1 . C H16 0.7711 0.0400 0.9870 0.041 Uiso calc . 1 . H C17 0.7800(2) 0.1737(2) 0.97895(13) 0.0373(5) Uani d . 1 . C H17 0.8125 0.1808 1.0325 0.045 Uiso calc . 1 . H C18 0.7594(2) 0.2488(2) 0.93008(13) 0.0337(5) Uani d . 1 . C H18 0.7782 0.3044 0.9499 0.040 Uiso calc . 1 . H C19 0.71009(15) 0.23784(14) 0.85112(12) 0.0279(4) Uani d . 1 . C 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 F1 0.0356(7) 0.0934(12) 0.0424(8) -0.0078(8) -0.0117(6) 0.0125(8) F2 0.0386(7) 0.0632(9) 0.0430(8) 0.0050(7) 0.0037(6) -0.0017(7) F3 0.0446(8) 0.0503(8) 0.0306(6) -0.0112(6) -0.0075(6) 0.0073(6) F4 0.130(2) 0.0245(8) 0.1011(15) 0.0137(9) 0.0267(13) 0.0071(8) O1 0.0288(7) 0.0320(8) 0.0296(7) -0.0031(6) -0.0012(6) -0.0057(6) O2 0.0343(8) 0.0283(7) 0.0233(7) -0.0029(6) -0.0038(6) -0.0004(6) O3 0.0284(7) 0.0337(8) 0.0279(7) 0.0039(6) -0.0010(6) 0.0036(6) B1 0.0313(12) 0.0271(11) 0.0324(12) 0.0005(9) 0.0001(10) 0.0054(9) C1 0.0194(9) 0.0294(10) 0.0233(9) 0.0017(7) 0.0034(7) -0.0021(8) C2 0.0227(9) 0.0268(10) 0.0244(9) 0.0011(7) 0.0027(7) -0.0015(8) C3 0.0218(9) 0.0311(10) 0.0262(9) 0.0004(8) 0.0031(7) -0.0043(8) C4 0.0290(10) 0.0269(10) 0.0356(11) -0.0007(8) 0.0069(9) -0.0024(9) C5 0.0302(10) 0.0296(11) 0.0323(11) 0.0033(8) 0.0060(8) 0.0048(9) C6 0.0281(10) 0.0347(11) 0.0252(9) 0.0016(8) 0.0018(8) 0.0027(8) C7 0.0245(9) 0.0299(10) 0.0238(9) -0.0019(8) 0.0026(7) -0.0036(8) C8 0.0222(9) 0.0274(10) 0.0233(9) 0.0015(7) 0.0043(7) -0.0012(8) C9 0.0275(10) 0.0275(10) 0.0226(9) 0.0010(8) 0.0045(8) -0.0017(8) C10 0.0329(11) 0.0348(11) 0.0243(9) -0.0040(9) 0.0036(8) -0.0045(8) C11 0.0331(11) 0.0272(10) 0.0340(11) -0.0036(9) 0.0111(9) -0.0056(9) C12 0.0274(10) 0.0281(10) 0.0359(11) 0.0042(8) 0.0076(8) 0.0028(9) C13 0.0213(9) 0.0323(11) 0.0265(10) 0.0034(8) 0.0051(8) 0.0010(8) C14 0.0188(9) 0.0348(11) 0.0242(9) 0.0009(8) 0.0017(7) -0.0017(8) C15 0.0211(9) 0.0378(11) 0.0260(9) 0.0017(8) 0.0032(8) 0.0004(8) C16 0.0253(10) 0.0498(13) 0.0270(10) 0.0037(9) 0.0000(8) 0.0049(9) C17 0.0251(10) 0.0625(15) 0.0245(10) -0.0032(10) -0.0032(8) -0.0022(10) C18 0.0257(10) 0.0461(12) 0.0293(10) -0.0047(9) -0.0001(8) -0.0073(9) C19 0.0214(9) 0.0359(11) 0.0265(9) -0.0006(8) 0.0027(8) -0.0023(8)