#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003080.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_2003080 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 410 _journal_page_last 423 loop_ _publ_author_name ; Frederik C. Krebs ; _chemical_name_systematic ; 4,8,12-trioxa-4,8,12,12c-tetrahydro-dibenzo[cd,mn]pyrenium hexafluoroarsenate ; _chemical_name_common ? _chemical_formula_moiety 'C19 H9 O3,As F6' _chemical_formula_sum 'C19 H9 As F6 O3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 474.18 _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 13.550(3) _cell_length_b 15.807(3) _cell_length_c 32.201(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6897.(2) _cell_formula_units_Z 16 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293(2) _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 2.053 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.404 _exptl_absorpt_correction_T_max 0.603 _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 69140 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 26.32 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 7003 _reflns_number_observed 4567 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1779 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.070 _refine_ls_number_reflns 7000 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+14.1168P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.376 _refine_diff_density_max 1.046 _refine_diff_density_min -0.968 _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' 'As' 'As' 0.0499 2.0058 '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 As1 0.60399(4) 0.22916(3) 0.31861(2) 0.0437(2) Uani d . 1 . As F1 0.5238(3) 0.3152(2) 0.31736(13) 0.0792(11) Uani d . 1 . F F2 0.6881(3) 0.1470(3) 0.31872(14) 0.0949(14) Uani d . 1 . F F3 0.5041(3) 0.1599(3) 0.32144(14) 0.0912(13) Uani d . 1 . F F4 0.7005(3) 0.2992(3) 0.31359(14) 0.0941(13) Uani d . 1 . F F5 0.5989(3) 0.2223(3) 0.26548(12) 0.0956(14) Uani d . 1 . F F6 0.6123(3) 0.2389(3) 0.37213(12) 0.0969(14) Uani d . 1 . F As2 0.39514(4) 0.03844(3) 0.43634(2) 0.0498(2) Uani d . 1 . As F7 0.3975(12) 0.1003(6) 0.4764(3) 0.334(9) Uani d . 1 . F F8 0.3493(4) -0.0378(3) 0.4681(2) 0.149(3) Uani d . 1 . F F9 0.5065(5) -0.0003(8) 0.4437(3) 0.278(7) Uani d . 1 . F F10 0.4375(5) 0.1167(4) 0.4051(2) 0.165(3) Uani d . 1 . F F11 0.3951(9) -0.0211(6) 0.3967(3) 0.275(6) Uani d . 1 . F F12 0.2850(5) 0.0754(6) 0.4286(3) 0.244(6) Uani d . 1 . F O1 0.2888(3) 0.1032(3) 0.2914(2) 0.0763(14) Uani d . 1 . O O2 0.3340(3) 0.4058(3) 0.28354(14) 0.0694(12) Uani d . 1 . O O3 0.4597(3) 0.2254(2) 0.17558(12) 0.0591(11) Uani d . 1 . O C1 0.3605(4) 0.2449(4) 0.2502(2) 0.0462(12) Uani d . 1 . C C2 0.3097(4) 0.2547(4) 0.2877(2) 0.0567(15) Uani d . 1 . C C3 0.2751(4) 0.1818(6) 0.3080(2) 0.073(2) Uani d . 1 . C C4 0.2282(6) 0.1925(8) 0.3464(3) 0.100(3) Uani d . 1 . C H4 0.2045 0.1461 0.3610 0.119 Uiso calc . 1 . H C5 0.2179(7) 0.2734(9) 0.3619(3) 0.114(4) Uani d . 1 . C H5 0.1868 0.2798 0.3875 0.137 Uiso calc . 1 . H C6 0.2511(6) 0.3465(6) 0.3417(3) 0.096(3) Uani d . 1 . C H6 0.2421 0.4000 0.3532 0.115 Uiso calc . 1 . H C7 0.2981(4) 0.3353(5) 0.3039(2) 0.066(2) Uani d . 1 . C C8 0.3967(4) 0.3158(3) 0.2296(2) 0.0451(12) Uani d . 1 . C C9 0.3828(4) 0.3965(4) 0.2467(2) 0.0560(15) Uani d . 1 . C C10 0.4167(5) 0.4664(4) 0.2249(2) 0.069(2) Uani d . 1 . C H10 0.4066 0.5207 0.2350 0.083 Uiso calc . 1 . H C11 0.4652(5) 0.4541(4) 0.1882(2) 0.070(2) Uani d . 1 . C H11 0.4892 0.5012 0.1742 0.084 Uiso calc . 1 . H C12 0.4806(5) 0.3744(4) 0.1706(2) 0.064(2) Uani d . 1 . C H12 0.5132 0.3685 0.1453 0.076 Uiso calc . 1 . H C13 0.4464(4) 0.3053(3) 0.1917(2) 0.0484(13) Uani d . 1 . C C14 0.3748(4) 0.1648(4) 0.2338(2) 0.0498(13) Uani d . 1 . C C15 0.4250(5) 0.1551(4) 0.1964(2) 0.0559(14) Uani d . 1 . C C16 0.4380(6) 0.0761(4) 0.1792(2) 0.073(2) Uani d . 1 . C H16 0.4703 0.0689 0.1540 0.088 Uiso calc . 1 . H C17 0.4013(6) 0.0085(4) 0.2009(3) 0.083(2) Uani d . 1 . C H17 0.4106 -0.0451 0.1898 0.100 Uiso calc . 1 . H C18 0.3520(6) 0.0143(4) 0.2378(3) 0.080(2) Uani d . 1 . C H18 0.3286 -0.0339 0.2512 0.096 Uiso calc . 1 . H C19 0.3375(4) 0.0941(4) 0.2549(2) 0.059(2) Uani d . 1 . C O4 0.1946(3) -0.1254(3) 0.52441(13) 0.0583(10) Uani d . 1 . O O5 0.1788(3) 0.1755(3) 0.54636(13) 0.0678(12) Uani d . 1 . O O6 0.0359(3) 0.0532(2) 0.42312(12) 0.0561(10) Uani d . 1 . O C20 0.1374(4) 0.0342(3) 0.4978(2) 0.0431(12) Uani d . 1 . C C21 0.1871(4) 0.0247(4) 0.5357(2) 0.0474(13) Uani d . 1 . C C22 0.2130(4) -0.0567(4) 0.5488(2) 0.0571(15) Uani d . 1 . C C23 0.2571(6) -0.0663(5) 0.5871(2) 0.078(2) Uani d . 1 . C H23 0.2749 -0.1196 0.5967 0.094 Uiso calc . 1 . H C24 0.2743(6) 0.0049(7) 0.6109(2) 0.092(3) Uani d . 1 . C H24 0.3037 -0.0022 0.6368 0.111 Uiso calc . 1 . H C25 0.2505(6) 0.0858(6) 0.5985(2) 0.086(2) Uani d . 1 . C H25 0.2643 0.1321 0.6153 0.103 Uiso calc . 1 . H C26 0.2054(5) 0.0962(4) 0.5603(2) 0.062(2) Uani d . 1 . C C27 0.1075(4) 0.1153(3) 0.4848(2) 0.0449(12) Uani d . 1 . C C28 0.1280(4) 0.1858(4) 0.5097(2) 0.0560(15) Uani d . 1 . C C29 0.0964(5) 0.2645(4) 0.4968(3) 0.073(2) Uani d . 1 . C H29 0.1097 0.3124 0.5127 0.087 Uiso calc . 1 . H C30 0.0449(6) 0.2709(4) 0.4601(2) 0.072(2) Uani d . 1 . C H30 0.0233 0.3241 0.4518 0.086 Uiso calc . 1 . H C31 0.0237(5) 0.2024(4) 0.4350(2) 0.066(2) Uani d . 1 . C H31 -0.0113 0.2094 0.4104 0.079 Uiso calc . 1 . H C32 0.0558(4) 0.1234(3) 0.4474(2) 0.0476(13) Uani d . 1 . C C33 0.1168(4) -0.0358(3) 0.4735(2) 0.0422(12) Uani d . 1 . C C34 0.0663(4) -0.0267(3) 0.4361(2) 0.0503(13) Uani d . 1 . C C35 0.0475(5) -0.0956(4) 0.4118(2) 0.066(2) Uani d . 1 . C H35 0.0155 -0.0897 0.3864 0.079 Uiso calc . 1 . H C36 0.0770(5) -0.1739(4) 0.4258(2) 0.072(2) Uani d . 1 . C H36 0.0621 -0.2210 0.4097 0.086 Uiso calc . 1 . H C37 0.1275(5) -0.1861(4) 0.4625(2) 0.066(2) Uani d . 1 . C H37 0.1482 -0.2398 0.4705 0.079 Uiso calc . 1 . H C38 0.1466(4) -0.1165(3) 0.4871(2) 0.0495(13) 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 As1 0.0423(3) 0.0421(3) 0.0466(3) 0.0021(2) 0.0044(2) -0.0035(2) F1 0.076(3) 0.048(2) 0.114(3) 0.012(2) 0.006(2) 0.004(2) F2 0.072(3) 0.094(3) 0.119(3) 0.041(2) 0.009(2) 0.001(3) F3 0.080(3) 0.065(2) 0.129(4) -0.013(2) 0.002(2) -0.001(2) F4 0.066(3) 0.099(3) 0.118(3) -0.030(2) 0.018(2) -0.018(3) F5 0.105(3) 0.133(4) 0.049(2) -0.005(3) 0.009(2) -0.003(2) F6 0.088(3) 0.145(4) 0.057(2) 0.003(3) -0.003(2) -0.015(3) As2 0.0546(4) 0.0400(3) 0.0547(4) -0.0046(3) 0.0126(3) -0.0005(2) F7 0.67(3) 0.159(8) 0.170(8) -0.142(11) 0.008(11) -0.070(6) F8 0.110(4) 0.099(4) 0.237(7) 0.024(3) 0.087(4) 0.087(4) F9 0.081(4) 0.432(15) 0.321(12) 0.020(7) 0.044(6) 0.244(12) F10 0.169(6) 0.128(5) 0.197(6) 0.004(4) 0.078(5) 0.089(4) F11 0.405(17) 0.232(9) 0.187(8) -0.089(10) 0.079(9) -0.149(8) F12 0.101(5) 0.369(12) 0.262(9) 0.103(6) 0.093(5) 0.232(9) O1 0.057(3) 0.089(4) 0.083(3) -0.013(3) -0.001(2) 0.039(3) O2 0.062(3) 0.078(3) 0.068(3) 0.029(2) -0.005(2) -0.010(2) O3 0.074(3) 0.049(2) 0.054(2) -0.005(2) 0.010(2) 0.003(2) C1 0.038(3) 0.056(3) 0.045(3) -0.001(2) -0.005(2) 0.010(3) C2 0.038(3) 0.082(4) 0.050(3) 0.011(3) 0.001(2) 0.015(3) C3 0.040(3) 0.117(6) 0.062(4) -0.002(4) 0.002(3) 0.028(4) C4 0.054(4) 0.168(9) 0.077(5) 0.001(5) 0.013(4) 0.046(6) C5 0.068(5) 0.209(13) 0.064(5) 0.029(7) 0.019(4) 0.009(7) C6 0.071(5) 0.143(8) 0.074(5) 0.035(5) 0.006(4) -0.008(5) C7 0.045(3) 0.100(5) 0.054(3) 0.023(4) -0.001(3) 0.003(4) C8 0.040(3) 0.048(3) 0.047(3) 0.002(2) -0.006(2) 0.002(2) C9 0.053(4) 0.054(3) 0.061(4) 0.012(3) -0.007(3) 0.000(3) C10 0.078(5) 0.040(3) 0.091(5) 0.008(3) -0.020(4) 0.001(3) C11 0.064(4) 0.048(4) 0.099(5) -0.005(3) -0.008(4) 0.021(4) C12 0.068(4) 0.060(4) 0.063(4) -0.006(3) 0.004(3) 0.017(3) C13 0.053(3) 0.041(3) 0.050(3) 0.002(2) -0.002(3) 0.007(2) C14 0.045(3) 0.048(3) 0.056(3) -0.008(2) -0.009(2) 0.013(3) C15 0.060(4) 0.050(3) 0.058(3) -0.001(3) -0.007(3) 0.003(3) C16 0.095(5) 0.050(4) 0.075(4) -0.004(4) -0.004(4) -0.006(3) C17 0.097(6) 0.048(4) 0.105(6) -0.005(4) -0.017(5) -0.006(4) C18 0.077(5) 0.049(4) 0.115(6) -0.021(3) -0.031(5) 0.028(4) C19 0.042(3) 0.065(4) 0.071(4) -0.013(3) -0.011(3) 0.025(3) O4 0.051(2) 0.057(2) 0.066(3) 0.006(2) 0.000(2) 0.010(2) O5 0.067(3) 0.071(3) 0.066(3) -0.002(2) 0.000(2) -0.025(2) O6 0.064(3) 0.054(2) 0.050(2) 0.001(2) -0.007(2) 0.002(2) C20 0.036(3) 0.046(3) 0.047(3) -0.001(2) 0.008(2) -0.004(2) C21 0.035(3) 0.062(3) 0.046(3) -0.001(2) 0.004(2) -0.006(3) C22 0.043(3) 0.080(4) 0.049(3) 0.007(3) 0.001(3) 0.009(3) C23 0.066(4) 0.101(6) 0.069(4) 0.016(4) -0.005(4) 0.013(4) C24 0.071(5) 0.147(8) 0.060(4) 0.015(5) -0.016(4) -0.002(5) C25 0.079(5) 0.117(7) 0.061(4) 0.007(5) -0.014(4) -0.026(4) C26 0.052(4) 0.079(4) 0.055(4) 0.004(3) 0.003(3) -0.013(3) C27 0.038(3) 0.048(3) 0.050(3) 0.000(2) 0.010(2) -0.003(2) C28 0.053(3) 0.052(3) 0.063(4) -0.005(3) 0.016(3) -0.011(3) C29 0.078(5) 0.043(3) 0.098(5) -0.007(3) 0.020(4) -0.014(3) C30 0.079(5) 0.047(4) 0.091(5) 0.005(3) 0.014(4) 0.015(4) C31 0.073(4) 0.057(4) 0.067(4) 0.003(3) 0.010(3) 0.016(3) C32 0.049(3) 0.041(3) 0.052(3) -0.003(2) 0.010(3) 0.007(2) C33 0.037(3) 0.042(3) 0.048(3) -0.003(2) 0.005(2) 0.002(2) C34 0.050(3) 0.041(3) 0.059(3) -0.005(2) 0.002(3) 0.001(3) C35 0.066(4) 0.072(4) 0.059(4) -0.010(3) -0.010(3) -0.010(3) C36 0.074(5) 0.054(4) 0.087(5) -0.008(3) 0.001(4) -0.022(4) C37 0.064(4) 0.043(3) 0.091(5) -0.001(3) 0.008(3) -0.006(3) C38 0.038(3) 0.045(3) 0.065(4) -0.001(2) 0.007(3) 0.003(3)