#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003562.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_2003562 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1180 _journal_page_last 1182 _publ_section_title ; Pyrylium Salts. Part VII. 2,4,6-Triphenylpyrylium Trichloroacetate ; _chemical_formula_sum 'C25 H17 Cl3 O3' _chemical_formula_weight 471.77 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 12.513(2) _cell_length_b 17.356(3) _cell_length_c 10.172(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.660(3) _cell_angle_gamma 90.00 _cell_volume 2155.4(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 28 _exptl_absorpt_coefficient_mu 4.062 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_colour yellow _chemical_compound_source ? _diffrn_measurement_device 'Kuma KM-4' _diffrn_measurement_method '\w/2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2563 _reflns_number_total 2563 _reflns_number_observed 2454 _reflns_observed_criterion I>2\s(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 59.99 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <5 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0681 _refine_ls_wR_factor_obs 0.1770 _refine_ls_wR_factor_all 0.1844 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_number_reflns 2558 _refine_ls_number_parameters 298 _refine_ls_hydrogen_treatment refU _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0956P)^2^ + 5.1989P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.568 _refine_diff_density_min -0.835 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1994)' _refine_ls_extinction_coef 0.0007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0181 0.009 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0492 0.032 'Cl' 'Cl' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3639 0.7 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Cl1 1 0.8280(2) 0.52119(14) 0.4160(2) 0.1387(11) Cl3 1 0.78493(12) 0.64852(8) 0.2389(2) 0.0700(5) Cl2 1 0.89305(14) 0.52002(11) 0.1583(3) 0.1130(9) O2 1 0.5987(3) 0.5494(2) 0.1741(5) 0.0725(12) O3 1 0.6849(3) 0.4387(2) 0.1530(4) 0.0622(10) C7 1 0.6783(4) 0.5070(3) 0.1834(5) 0.0440(11) C8 1 0.7918(4) 0.5468(3) 0.2445(5) 0.0466(12) O1 1 0.7690(2) 0.3686(2) 0.7057(3) 0.0340(7) C2 1 0.7026(3) 0.4012(2) 0.7785(4) 0.0314(9) C3 1 0.6340(3) 0.3566(2) 0.8324(4) 0.0352(10) H3 1 0.5892(3) 0.3792(2) 0.8833(4) 0.047(13) C4 1 0.6304(3) 0.2768(2) 0.8118(4) 0.0332(10) C5 1 0.6981(3) 0.2456(2) 0.7316(4) 0.0342(10) H5 1 0.6953(3) 0.1932(2) 0.7127(4) 0.043(12) C6 1 0.7678(3) 0.2918(2) 0.6815(4) 0.0329(9) C21 1 0.7173(3) 0.4847(2) 0.7922(4) 0.0341(10) C22 1 0.8086(4) 0.5202(3) 0.7619(5) 0.0440(11) H22 1 0.8600(4) 0.4910(3) 0.7303(5) 0.050(14) C23 1 0.8231(5) 0.5989(3) 0.7787(5) 0.0558(14) H23 1 0.8841(5) 0.6226(3) 0.7584(5) 0.073(18) C24 1 0.7475(5) 0.6418(3) 0.8252(5) 0.0551(14) H24 1 0.7577(5) 0.6946(3) 0.8373(5) 0.068(16) C25 1 0.6557(4) 0.6071(3) 0.8545(5) 0.0499(12) H25 1 0.6039(4) 0.6369(3) 0.8844(5) 0.062(16) C26 1 0.6410(4) 0.5287(3) 0.8394(4) 0.0394(11) H26 1 0.5801(4) 0.5053(3) 0.8608(4) 0.043(13) C41 1 0.5628(3) 0.2266(2) 0.8764(4) 0.0334(10) C42 1 0.4717(4) 0.2557(3) 0.9178(5) 0.0436(11) H42 1 0.4503(4) 0.3066(3) 0.8994(5) 0.073(18) C43 1 0.4128(4) 0.2084(3) 0.9866(5) 0.0539(13) H43 1 0.3517(4) 0.2277(3) 1.0136(5) 0.076(18) C44 1 0.4442(5) 0.1336(3) 1.0151(5) 0.0547(13) H44 1 0.4052(5) 0.1026(3) 1.0627(5) 0.071(18) C45 1 0.5336(4) 0.1041(3) 0.9731(5) 0.0498(13) H45 1 0.5549(4) 0.0533(3) 0.9927(5) 0.062(16) C46 1 0.5914(4) 0.1498(2) 0.9022(5) 0.0407(11) H46 1 0.6500(4) 0.1291(2) 0.8715(5) 0.045(13) C61 1 0.8448(3) 0.2688(2) 0.6002(4) 0.0351(10) C62 1 0.8616(4) 0.1910(3) 0.5766(4) 0.0412(11) H62 1 0.8236(4) 0.1535(3) 0.6131(4) 0.055(15) C63 1 0.9341(4) 0.1697(3) 0.4995(5) 0.0503(12) H63 1 0.9448(4) 0.1178(3) 0.4836(5) 0.038(12) C64 1 0.9914(4) 0.2250(4) 0.4455(5) 0.0578(14) H64 1 1.0406(4) 0.2102(4) 0.3937(5) 0.074(18) C65 1 0.9755(5) 0.3013(3) 0.4681(6) 0.063(2) H65 1 1.0135(5) 0.3384(3) 0.4308(6) 0.081(20) C66 1 0.9036(4) 0.3235(3) 0.5457(5) 0.0558(14) H66 1 0.8943(4) 0.3756(3) 0.5618(5) 0.072(18) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Cl1 0.183(2) -0.044(2) -0.0477(14) 0.130(2) 0.0457(12) 0.0680(12) Cl3 0.0639(9) -0.0063(6) 0.0135(8) 0.0469(8) -0.0047(7) 0.0973(12) Cl2 0.0584(10) -0.0137(9) 0.0659(13) 0.0943(13) -0.0523(14) 0.203(2) O2 0.043(2) -0.003(2) 0.022(2) 0.070(2) -0.020(2) 0.107(3) O3 0.068(2) -0.006(2) 0.018(2) 0.044(2) -0.001(2) 0.075(3) C7 0.046(3) -0.001(2) 0.017(2) 0.045(3) 0.003(2) 0.045(3) C8 0.044(3) -0.001(2) 0.005(2) 0.048(3) 0.005(2) 0.045(3) O1 0.036(2) -0.0002(12) 0.0085(13) 0.037(2) -0.0011(12) 0.030(2) C2 0.033(2) 0.003(2) 0.002(2) 0.037(2) 0.001(2) 0.023(2) C3 0.036(2) 0.001(2) 0.006(2) 0.038(2) -0.003(2) 0.031(2) C4 0.034(2) 0.002(2) 0.000(2) 0.036(2) 0.000(2) 0.027(2) C5 0.041(2) 0.000(2) 0.005(2) 0.035(2) 0.000(2) 0.026(2) C6 0.038(2) 0.002(2) 0.002(2) 0.034(2) -0.002(2) 0.025(2) C21 0.036(2) -0.003(2) 0.001(2) 0.035(2) 0.000(2) 0.029(2) C22 0.044(3) -0.006(2) 0.013(2) 0.049(3) -0.003(2) 0.040(3) C23 0.064(3) -0.021(3) 0.020(3) 0.050(3) -0.002(2) 0.057(3) C24 0.080(4) -0.007(2) 0.013(3) 0.035(3) -0.001(2) 0.049(3) C25 0.062(3) 0.003(2) 0.014(3) 0.040(3) -0.006(2) 0.049(3) C26 0.038(2) -0.003(2) 0.005(2) 0.043(2) -0.002(2) 0.036(3) C41 0.034(2) -0.004(2) 0.002(2) 0.040(2) -0.001(2) 0.025(2) C42 0.043(3) -0.001(2) 0.014(2) 0.043(3) -0.001(2) 0.047(3) C43 0.057(3) -0.004(2) 0.030(3) 0.058(3) -0.005(3) 0.055(3) C44 0.063(3) -0.017(3) 0.016(3) 0.059(3) 0.003(2) 0.045(3) C45 0.055(3) -0.008(2) 0.005(2) 0.042(3) 0.006(2) 0.050(3) C46 0.042(3) -0.001(2) 0.006(2) 0.040(2) -0.003(2) 0.039(3) C61 0.033(2) 0.002(2) 0.005(2) 0.047(3) 0.000(2) 0.025(2) C62 0.044(3) 0.004(2) 0.007(2) 0.047(3) 0.001(2) 0.032(3) C63 0.054(3) 0.015(2) 0.013(2) 0.055(3) -0.006(2) 0.043(3) C64 0.045(3) 0.006(3) 0.017(2) 0.088(4) -0.012(3) 0.044(3) C65 0.066(4) -0.013(3) 0.037(3) 0.072(4) -0.007(3) 0.061(4) C66 0.070(4) -0.007(3) 0.032(3) 0.051(3) -0.004(2) 0.055(3)