# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Hiroki Takahashi' _publ_contact_author_email TAKAHASHI@MBOX.KUDPC.KYOTO-U.AC.JP _publ_section_title ; Low-temperature-induced reversible single-crystal-to-single-crystal phase transition of 3,4-dichloro-2',4',6'-triethylbenzophenone ; loop_ _publ_author_name 'Hiroki Takahashi' 'Yoshikatsu Ito' # Attachment 'compound_1_beta.cif' data_1-beta _database_code_depnum_ccdc_archive 'CCDC 751183' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C19 H23 Cl2 O ' _chemical_formula_moiety 'C19 H23 Cl2 O ' _chemical_formula_weight 338.30 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,+Z #------------------------------------------------------------------------------ _cell_length_a 10.861(2) _cell_length_b 17.249(2) _cell_length_c 18.531(2) _cell_angle_alpha 90.0000 _cell_angle_beta 96.916(4) _cell_angle_gamma 90.0000 _cell_volume 3446.2(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 23046 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 108.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432.00 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 45425 _diffrn_reflns_av_R_equivalents 0.180 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.916 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7240 _reflns_number_gt 4157 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1868 _refine_ls_wR_factor_ref 0.5145 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7240 _refine_ls_number_parameters 398 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.3000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0050 _refine_diff_density_max 1.67 _refine_diff_density_min -1.09 _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 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl(1) Cl -0.0501(2) 0.59491(12) 0.08211(12) 0.0441(6) Uani 1.00 1 d . . . Cl(2) Cl 0.2406(2) 0.57419(15) 0.10760(17) 0.0608(8) Uani 1.00 1 d . . . O(1) O -0.2051(5) 0.3057(3) 0.0768(3) 0.0505(16) Uani 1.00 1 d . . . C(1) C -0.0448(7) 0.2209(4) 0.1244(4) 0.0357(17) Uani 1.00 1 d . . . C(2) C -0.0097(6) 0.1671(5) 0.0748(4) 0.0347(17) Uani 1.00 1 d . . . C(3) C 0.0261(8) 0.0918(5) 0.1000(5) 0.043(2) Uani 1.00 1 d . . . C(4) C 0.0289(7) 0.0720(4) 0.1724(4) 0.0368(17) Uani 1.00 1 d . . . C(5) C -0.0005(8) 0.1288(4) 0.2207(4) 0.0388(18) Uani 1.00 1 d . . . C(6) C -0.0361(8) 0.2024(4) 0.2003(4) 0.0389(18) Uani 1.00 1 d . . . C(7) C -0.0943(7) 0.2982(4) 0.0968(4) 0.0359(17) Uani 1.00 1 d . . . C(8) C -0.0092(7) 0.3649(4) 0.1010(4) 0.0359(17) Uani 1.00 1 d . . . C(9) C -0.0615(7) 0.4394(5) 0.0898(4) 0.0349(17) Uani 1.00 1 d . . . C(10) C 0.0166(8) 0.5028(4) 0.0929(4) 0.0350(16) Uani 1.00 1 d . . . C(11) C 0.1456(8) 0.4951(5) 0.1049(4) 0.0409(19) Uani 1.00 1 d . . . C(12) C 0.1954(7) 0.4216(4) 0.1136(4) 0.0374(18) Uani 1.00 1 d . . . C(13) C 0.1177(7) 0.3578(5) 0.1117(4) 0.0379(18) Uani 1.00 1 d . . . C(14) C -0.0186(8) 0.1865(6) -0.0053(4) 0.046(2) Uani 1.00 1 d . . . C(15) C -0.1435(9) 0.1612(7) -0.0456(5) 0.055(2) Uani 1.00 1 d . . . C(16) C 0.0640(9) -0.0091(5) 0.1985(5) 0.045(2) Uani 1.00 1 d . . . C(17) C 0.2026(9) -0.0177(6) 0.2190(5) 0.054(2) Uani 1.00 1 d . . . C(18) C -0.0665(8) 0.2614(5) 0.2546(4) 0.0427(19) Uani 1.00 1 d . . . C(19) C -0.2040(9) 0.2630(7) 0.2655(5) 0.059(2) Uani 1.00 1 d . . . H(1) H 0.0487 0.0543 0.0665 0.052 Uiso 1.00 1 c R . . H(2) H 0.0045 0.1157 0.2708 0.047 Uiso 1.00 1 c R . . H(3) H -0.1488 0.4459 0.0803 0.042 Uiso 1.00 1 c R . . H(4) H 0.2828 0.4147 0.1207 0.045 Uiso 1.00 1 c R . . H(5) H 0.1533 0.3076 0.1181 0.045 Uiso 1.00 1 c R . . H(6) H -0.0084 0.2431 -0.0112 0.055 Uiso 1.00 1 c R . . H(7) H 0.0493 0.1602 -0.0269 0.055 Uiso 1.00 1 c R . . H(8) H -0.2036 0.2034 -0.0449 0.066 Uiso 1.00 1 c R . . H(9) H -0.1333 0.1483 -0.0960 0.066 Uiso 1.00 1 c R . . H(10) H -0.1737 0.1155 -0.0216 0.066 Uiso 1.00 1 c R . . H(11) H 0.0210 -0.0214 0.2412 0.054 Uiso 1.00 1 c R . . H(12) H 0.0358 -0.0466 0.1596 0.054 Uiso 1.00 1 c R . . H(13) H 0.2237 -0.0059 0.2707 0.064 Uiso 1.00 1 c R . . H(14) H 0.2273 -0.0711 0.2095 0.064 Uiso 1.00 1 c R . . H(15) H 0.2464 0.0181 0.1899 0.064 Uiso 1.00 1 c R . . H(16) H -0.0168 0.2504 0.3018 0.051 Uiso 1.00 1 c R . . H(17) H -0.0422 0.3133 0.2384 0.051 Uiso 1.00 1 c R . . H(18) H -0.2177 0.2293 0.3064 0.071 Uiso 1.00 1 c R . . H(19) H -0.2284 0.3161 0.2759 0.071 Uiso 1.00 1 c R . . H(20) H -0.2539 0.2445 0.2213 0.071 Uiso 1.00 1 c R . . Cl(3) Cl 0.0816(2) -0.09184(12) 0.58337(11) 0.0401(5) Uani 1.00 1 d . . . Cl(4) Cl -0.2091(2) -0.07348(12) 0.58058(13) 0.0457(6) Uani 1.00 1 d . . . O(2) O 0.2396(5) 0.1924(3) 0.6226(4) 0.0517(16) Uani 1.00 1 d . . . C(20) C 0.0744(7) 0.2831(4) 0.6236(4) 0.0324(16) Uani 1.00 1 d . . . C(21) C 0.0293(7) 0.3231(4) 0.5593(4) 0.0332(16) Uani 1.00 1 d . . . C(22) C -0.0130(7) 0.3973(4) 0.5646(4) 0.0345(16) Uani 1.00 1 d . . . C(23) C -0.0176(8) 0.4351(4) 0.6317(4) 0.0376(18) Uani 1.00 1 d . . . C(24) C 0.0279(8) 0.3939(4) 0.6942(4) 0.0398(18) Uani 1.00 1 d . . . C(25) C 0.0747(7) 0.3187(4) 0.6908(4) 0.0370(17) Uani 1.00 1 d . . . C(26) C 0.1268(7) 0.2041(4) 0.6198(4) 0.0349(17) Uani 1.00 1 d . . . C(27) C 0.0415(6) 0.1357(4) 0.6114(4) 0.0298(15) Uani 1.00 1 d . . . C(28) C 0.0934(8) 0.0620(4) 0.6020(4) 0.0359(17) Uani 1.00 1 d . . . C(29) C 0.0160(8) -0.0008(4) 0.5935(4) 0.0370(17) Uani 1.00 1 d . . . C(30) C -0.1119(8) 0.0063(4) 0.5936(4) 0.0349(17) Uani 1.00 1 d . . . C(31) C -0.1637(8) 0.0792(4) 0.6032(4) 0.0367(18) Uani 1.00 1 d . . . C(32) C -0.0866(6) 0.1435(4) 0.6111(4) 0.0320(15) Uani 1.00 1 d . . . C(33) C 0.0317(8) 0.2840(4) 0.4860(4) 0.0405(18) Uani 1.00 1 d . . . C(34) C 0.1558(9) 0.2891(5) 0.4583(4) 0.046(2) Uani 1.00 1 d . . . C(35) C -0.0621(9) 0.5170(4) 0.6341(5) 0.0424(19) Uani 1.00 1 d . . . C(36) C -0.1151(9) 0.5394(5) 0.7035(5) 0.051(2) Uani 1.00 1 d . . . C(37) C 0.1210(8) 0.2780(5) 0.7619(4) 0.0420(19) Uani 1.00 1 d . . . C(38) C 0.0148(11) 0.2354(5) 0.7943(5) 0.057(2) Uani 1.00 1 d . . . H(21) H -0.0405 0.4246 0.5212 0.041 Uiso 1.00 1 c R . . H(22) H 0.0270 0.4178 0.7403 0.048 Uiso 1.00 1 c R . . H(23) H 0.1803 0.0561 0.6017 0.043 Uiso 1.00 1 c R . . H(24) H -0.2505 0.0846 0.6043 0.044 Uiso 1.00 1 c R . . H(25) H -0.1213 0.1934 0.6165 0.038 Uiso 1.00 1 c R . . H(26) H -0.0315 0.3084 0.4501 0.049 Uiso 1.00 1 c R . . H(27) H 0.0091 0.2287 0.4902 0.049 Uiso 1.00 1 c R . . H(28) H 0.2052 0.2433 0.4741 0.055 Uiso 1.00 1 c R . . H(29) H 0.1441 0.2915 0.4051 0.055 Uiso 1.00 1 c R . . H(30) H 0.1991 0.3358 0.4778 0.055 Uiso 1.00 1 c R . . H(31) H 0.0080 0.5521 0.6278 0.051 Uiso 1.00 1 c R . . H(32) H -0.1267 0.5255 0.5924 0.051 Uiso 1.00 1 c R . . H(33) H -0.0487 0.5599 0.7388 0.061 Uiso 1.00 1 c R . . H(34) H -0.1791 0.5792 0.6926 0.061 Uiso 1.00 1 c R . . H(35) H -0.1517 0.4936 0.7239 0.061 Uiso 1.00 1 c R . . H(36) H 0.1861 0.2401 0.7532 0.050 Uiso 1.00 1 c R . . H(37) H 0.1586 0.3167 0.7974 0.050 Uiso 1.00 1 c R . . H(38) H 0.0078 0.1823 0.7754 0.068 Uiso 1.00 1 c R . . H(39) H 0.0327 0.2340 0.8474 0.068 Uiso 1.00 1 c R . . H(40) H -0.0635 0.2629 0.7806 0.068 Uiso 1.00 1 c R . . 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 Cl(1) 0.0478(13) 0.0325(11) 0.0531(12) 0.0071(8) 0.0100(9) 0.0001(8) Cl(2) 0.0479(14) 0.0403(13) 0.094(2) -0.0117(10) 0.0095(13) 0.0007(11) O(1) 0.028(3) 0.040(3) 0.082(4) -0.001(2) 0.000(2) 0.013(3) C(1) 0.030(3) 0.033(4) 0.045(4) -0.004(3) 0.009(3) 0.002(3) C(2) 0.018(3) 0.043(4) 0.044(4) 0.001(3) 0.009(2) 0.000(3) C(3) 0.035(4) 0.046(5) 0.048(4) -0.004(3) 0.007(3) 0.004(3) C(4) 0.029(4) 0.030(3) 0.051(4) 0.002(3) 0.002(3) -0.000(3) C(5) 0.045(4) 0.030(4) 0.042(4) -0.004(3) 0.007(3) 0.009(3) C(6) 0.041(4) 0.032(4) 0.045(4) -0.007(3) 0.009(3) 0.000(3) C(7) 0.033(4) 0.032(4) 0.045(4) -0.010(3) 0.017(3) -0.002(3) C(8) 0.032(4) 0.034(4) 0.043(4) -0.002(3) 0.011(3) -0.001(3) C(9) 0.029(3) 0.040(4) 0.036(4) 0.008(3) 0.006(3) 0.004(3) C(10) 0.038(4) 0.031(3) 0.038(4) 0.002(3) 0.012(3) -0.004(3) C(11) 0.035(4) 0.039(4) 0.051(4) -0.011(3) 0.011(3) 0.004(3) C(12) 0.023(3) 0.038(4) 0.050(4) -0.003(3) 0.002(3) 0.006(3) C(13) 0.036(4) 0.032(4) 0.047(4) 0.008(3) 0.012(3) 0.003(3) C(14) 0.047(5) 0.052(5) 0.041(4) -0.005(4) 0.013(3) 0.004(3) C(15) 0.046(5) 0.071(7) 0.050(5) 0.001(5) 0.009(4) -0.001(4) C(16) 0.047(5) 0.034(4) 0.052(5) 0.005(3) 0.003(3) 0.010(3) C(17) 0.047(5) 0.053(5) 0.064(6) 0.015(4) 0.020(4) 0.005(4) C(18) 0.038(4) 0.045(4) 0.047(4) -0.004(3) 0.009(3) 0.001(3) C(19) 0.047(5) 0.070(7) 0.062(6) -0.002(5) 0.015(4) -0.013(5) Cl(3) 0.0407(11) 0.0299(10) 0.0500(12) 0.0039(7) 0.0063(8) -0.0031(7) Cl(4) 0.0371(11) 0.0342(11) 0.0656(14) -0.0088(8) 0.0058(9) -0.0041(9) O(2) 0.028(2) 0.036(3) 0.091(4) -0.001(2) 0.007(2) 0.002(3) C(20) 0.029(3) 0.024(3) 0.045(4) -0.002(2) 0.008(3) 0.000(2) C(21) 0.026(3) 0.027(3) 0.047(4) 0.001(2) 0.009(3) 0.002(3) C(22) 0.029(3) 0.029(3) 0.045(4) 0.004(3) 0.002(3) 0.004(3) C(23) 0.038(4) 0.027(3) 0.047(4) -0.001(3) 0.004(3) 0.004(3) C(24) 0.042(4) 0.029(4) 0.048(4) -0.001(3) 0.004(3) -0.003(3) C(25) 0.030(3) 0.035(4) 0.047(4) 0.005(3) 0.007(3) 0.004(3) C(26) 0.036(4) 0.025(3) 0.045(4) 0.003(3) 0.009(3) -0.004(3) C(27) 0.027(3) 0.022(3) 0.041(4) -0.000(2) 0.004(2) -0.001(2) C(28) 0.033(4) 0.030(4) 0.045(4) 0.010(3) 0.005(3) -0.005(3) C(29) 0.043(4) 0.030(3) 0.038(4) 0.001(3) 0.007(3) -0.001(3) C(30) 0.043(4) 0.019(3) 0.044(4) -0.006(3) 0.011(3) 0.004(2) C(31) 0.029(4) 0.032(4) 0.048(4) 0.006(3) 0.000(3) -0.007(3) C(32) 0.026(3) 0.025(3) 0.047(4) -0.000(2) 0.013(3) -0.000(3) C(33) 0.052(5) 0.032(4) 0.038(4) -0.003(3) 0.005(3) 0.002(3) C(34) 0.051(5) 0.045(5) 0.042(4) -0.003(4) 0.008(3) -0.003(3) C(35) 0.047(4) 0.028(4) 0.054(5) 0.000(3) 0.012(3) 0.001(3) C(36) 0.058(5) 0.038(4) 0.053(5) 0.013(4) -0.004(4) -0.003(3) C(37) 0.043(4) 0.042(4) 0.041(4) 0.004(3) 0.006(3) 0.003(3) C(38) 0.074(7) 0.040(5) 0.058(5) -0.020(4) 0.011(4) 0.005(4) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(10) 1.748(8) yes . . Cl(2) C(11) 1.707(9) yes . . O(1) C(7) 1.223(9) yes . . C(1) C(2) 1.392(11) yes . . C(1) C(6) 1.434(11) yes . . C(1) C(7) 1.504(11) yes . . C(2) C(3) 1.418(12) yes . . C(2) C(14) 1.513(11) yes . . C(3) C(4) 1.381(12) yes . . C(4) C(5) 1.389(12) yes . . C(4) C(16) 1.513(11) yes . . C(5) C(6) 1.367(11) yes . . C(6) C(18) 1.496(12) yes . . C(7) C(8) 1.472(11) yes . . C(8) C(9) 1.411(12) yes . . C(8) C(13) 1.374(11) yes . . C(9) C(10) 1.380(11) yes . . C(10) C(11) 1.398(12) yes . . C(11) C(12) 1.380(12) yes . . C(12) C(13) 1.384(12) yes . . C(14) C(15) 1.532(13) yes . . C(16) C(17) 1.514(13) yes . . C(18) C(19) 1.531(14) yes . . Cl(3) C(29) 1.743(8) yes . . Cl(4) C(30) 1.734(8) yes . . O(2) C(26) 1.236(10) yes . . C(20) C(21) 1.411(10) yes . . C(20) C(25) 1.387(11) yes . . C(20) C(26) 1.483(10) yes . . C(21) C(22) 1.368(11) yes . . C(21) C(33) 1.521(11) yes . . C(22) C(23) 1.409(12) yes . . C(23) C(24) 1.396(11) yes . . C(23) C(35) 1.496(11) yes . . C(24) C(25) 1.398(11) yes . . C(25) C(37) 1.525(11) yes . . C(26) C(27) 1.495(10) yes . . C(27) C(28) 1.410(11) yes . . C(27) C(32) 1.397(10) yes . . C(28) C(29) 1.369(11) yes . . C(29) C(30) 1.395(12) yes . . C(30) C(31) 1.397(11) yes . . C(31) C(32) 1.388(11) yes . . C(33) C(34) 1.500(13) yes . . C(35) C(36) 1.522(14) yes . . C(37) C(38) 1.548(15) yes . . C(3) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(9) H(3) 0.950 no . . C(12) H(4) 0.950 no . . C(13) H(5) 0.950 no . . C(14) H(6) 0.990 no . . C(14) H(7) 0.990 no . . C(15) H(8) 0.980 no . . C(15) H(9) 0.980 no . . C(15) H(10) 0.980 no . . C(16) H(11) 0.990 no . . C(16) H(12) 0.990 no . . C(17) H(13) 0.980 no . . C(17) H(14) 0.980 no . . C(17) H(15) 0.980 no . . C(18) H(16) 0.990 no . . C(18) H(17) 0.990 no . . C(19) H(18) 0.980 no . . C(19) H(19) 0.980 no . . C(19) H(20) 0.980 no . . C(22) H(21) 0.950 no . . C(24) H(22) 0.950 no . . C(28) H(23) 0.950 no . . C(31) H(24) 0.950 no . . C(32) H(25) 0.950 no . . C(33) H(26) 0.990 no . . C(33) H(27) 0.990 no . . C(34) H(28) 0.980 no . . C(34) H(29) 0.980 no . . C(34) H(30) 0.980 no . . C(35) H(31) 0.990 no . . C(35) H(32) 0.990 no . . C(36) H(33) 0.980 no . . C(36) H(34) 0.980 no . . C(36) H(35) 0.980 no . . C(37) H(36) 0.990 no . . C(37) H(37) 0.990 no . . C(38) H(38) 0.980 no . . C(38) H(39) 0.980 no . . C(38) H(40) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(2) C(1) C(6) 120.5(7) yes . . . C(2) C(1) C(7) 118.8(7) yes . . . C(6) C(1) C(7) 120.7(7) yes . . . C(1) C(2) C(3) 118.6(7) yes . . . C(1) C(2) C(14) 120.6(7) yes . . . C(3) C(2) C(14) 120.6(7) yes . . . C(2) C(3) C(4) 121.3(8) yes . . . C(3) C(4) C(5) 118.1(7) yes . . . C(3) C(4) C(16) 120.9(7) yes . . . C(5) C(4) C(16) 121.0(7) yes . . . C(4) C(5) C(6) 123.8(7) yes . . . C(1) C(6) C(5) 117.5(7) yes . . . C(1) C(6) C(18) 120.9(7) yes . . . C(5) C(6) C(18) 121.6(7) yes . . . O(1) C(7) C(1) 119.8(7) yes . . . O(1) C(7) C(8) 121.5(7) yes . . . C(1) C(7) C(8) 118.5(6) yes . . . C(7) C(8) C(9) 117.7(7) yes . . . C(7) C(8) C(13) 123.5(7) yes . . . C(9) C(8) C(13) 118.7(7) yes . . . C(8) C(9) C(10) 118.8(7) yes . . . Cl(1) C(10) C(9) 118.1(6) yes . . . Cl(1) C(10) C(11) 119.9(6) yes . . . C(9) C(10) C(11) 122.1(7) yes . . . Cl(2) C(11) C(10) 121.3(6) yes . . . Cl(2) C(11) C(12) 120.3(6) yes . . . C(10) C(11) C(12) 118.4(8) yes . . . C(11) C(12) C(13) 119.9(7) yes . . . C(8) C(13) C(12) 122.1(7) yes . . . C(2) C(14) C(15) 111.3(7) yes . . . C(4) C(16) C(17) 112.1(7) yes . . . C(6) C(18) C(19) 113.5(7) yes . . . C(21) C(20) C(25) 120.3(7) yes . . . C(21) C(20) C(26) 120.3(7) yes . . . C(25) C(20) C(26) 119.3(6) yes . . . C(20) C(21) C(22) 118.8(7) yes . . . C(20) C(21) C(33) 119.8(6) yes . . . C(22) C(21) C(33) 121.4(7) yes . . . C(21) C(22) C(23) 123.0(7) yes . . . C(22) C(23) C(24) 116.7(7) yes . . . C(22) C(23) C(35) 120.6(7) yes . . . C(24) C(23) C(35) 122.6(7) yes . . . C(23) C(24) C(25) 121.9(7) yes . . . C(20) C(25) C(24) 119.3(7) yes . . . C(20) C(25) C(37) 122.5(7) yes . . . C(24) C(25) C(37) 118.2(7) yes . . . O(2) C(26) C(20) 122.2(7) yes . . . O(2) C(26) C(27) 118.3(7) yes . . . C(20) C(26) C(27) 119.6(6) yes . . . C(26) C(27) C(28) 118.2(6) yes . . . C(26) C(27) C(32) 121.9(6) yes . . . C(28) C(27) C(32) 119.9(6) yes . . . C(27) C(28) C(29) 118.6(7) yes . . . Cl(3) C(29) C(28) 118.2(6) yes . . . Cl(3) C(29) C(30) 120.0(6) yes . . . C(28) C(29) C(30) 121.8(7) yes . . . Cl(4) C(30) C(29) 121.3(6) yes . . . Cl(4) C(30) C(31) 118.9(6) yes . . . C(29) C(30) C(31) 119.8(7) yes . . . C(30) C(31) C(32) 119.0(7) yes . . . C(27) C(32) C(31) 120.8(7) yes . . . C(21) C(33) C(34) 113.1(6) yes . . . C(23) C(35) C(36) 114.9(7) yes . . . C(25) C(37) C(38) 111.7(7) yes . . . C(2) C(3) H(1) 119.4 no . . . C(4) C(3) H(1) 119.3 no . . . C(4) C(5) H(2) 118.1 no . . . C(6) C(5) H(2) 118.1 no . . . C(8) C(9) H(3) 120.6 no . . . C(10) C(9) H(3) 120.6 no . . . C(11) C(12) H(4) 120.1 no . . . C(13) C(12) H(4) 120.1 no . . . C(8) C(13) H(5) 119.0 no . . . C(12) C(13) H(5) 118.9 no . . . C(2) C(14) H(6) 109.4 no . . . C(2) C(14) H(7) 109.4 no . . . C(15) C(14) H(6) 109.4 no . . . C(15) C(14) H(7) 109.4 no . . . H(6) C(14) H(7) 108.0 no . . . C(14) C(15) H(8) 109.5 no . . . C(14) C(15) H(9) 109.5 no . . . C(14) C(15) H(10) 109.5 no . . . H(8) C(15) H(9) 109.5 no . . . H(8) C(15) H(10) 109.5 no . . . H(9) C(15) H(10) 109.5 no . . . C(4) C(16) H(11) 109.2 no . . . C(4) C(16) H(12) 109.2 no . . . C(17) C(16) H(11) 109.2 no . . . C(17) C(16) H(12) 109.2 no . . . H(11) C(16) H(12) 107.9 no . . . C(16) C(17) H(13) 109.5 no . . . C(16) C(17) H(14) 109.5 no . . . C(16) C(17) H(15) 109.5 no . . . H(13) C(17) H(14) 109.5 no . . . H(13) C(17) H(15) 109.5 no . . . H(14) C(17) H(15) 109.5 no . . . C(6) C(18) H(16) 108.9 no . . . C(6) C(18) H(17) 108.9 no . . . C(19) C(18) H(16) 108.9 no . . . C(19) C(18) H(17) 108.9 no . . . H(16) C(18) H(17) 107.7 no . . . C(18) C(19) H(18) 109.5 no . . . C(18) C(19) H(19) 109.5 no . . . C(18) C(19) H(20) 109.5 no . . . H(18) C(19) H(19) 109.5 no . . . H(18) C(19) H(20) 109.5 no . . . H(19) C(19) H(20) 109.5 no . . . C(21) C(22) H(21) 118.5 no . . . C(23) C(22) H(21) 118.5 no . . . C(23) C(24) H(22) 119.0 no . . . C(25) C(24) H(22) 119.0 no . . . C(27) C(28) H(23) 120.7 no . . . C(29) C(28) H(23) 120.7 no . . . C(30) C(31) H(24) 120.5 no . . . C(32) C(31) H(24) 120.5 no . . . C(27) C(32) H(25) 119.6 no . . . C(31) C(32) H(25) 119.6 no . . . C(21) C(33) H(26) 109.0 no . . . C(21) C(33) H(27) 109.0 no . . . C(34) C(33) H(26) 109.0 no . . . C(34) C(33) H(27) 109.0 no . . . H(26) C(33) H(27) 107.8 no . . . C(33) C(34) H(28) 109.5 no . . . C(33) C(34) H(29) 109.5 no . . . C(33) C(34) H(30) 109.5 no . . . H(28) C(34) H(29) 109.5 no . . . H(28) C(34) H(30) 109.5 no . . . H(29) C(34) H(30) 109.5 no . . . C(23) C(35) H(31) 108.5 no . . . C(23) C(35) H(32) 108.5 no . . . C(36) C(35) H(31) 108.5 no . . . C(36) C(35) H(32) 108.5 no . . . H(31) C(35) H(32) 107.5 no . . . C(35) C(36) H(33) 109.5 no . . . C(35) C(36) H(34) 109.5 no . . . C(35) C(36) H(35) 109.5 no . . . H(33) C(36) H(34) 109.5 no . . . H(33) C(36) H(35) 109.5 no . . . H(34) C(36) H(35) 109.5 no . . . C(25) C(37) H(36) 109.3 no . . . C(25) C(37) H(37) 109.3 no . . . C(38) C(37) H(36) 109.3 no . . . C(38) C(37) H(37) 109.3 no . . . H(36) C(37) H(37) 107.9 no . . . C(37) C(38) H(38) 109.5 no . . . C(37) C(38) H(39) 109.5 no . . . C(37) C(38) H(40) 109.5 no . . . H(38) C(38) H(39) 109.5 no . . . H(38) C(38) H(40) 109.5 no . . . H(39) C(38) H(40) 109.5 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(2) C(1) C(6) C(5) -4.3(12) ? . . . . C(2) C(1) C(6) C(18) 176.4(7) ? . . . . C(6) C(1) C(2) C(3) 4.5(11) ? . . . . C(6) C(1) C(2) C(14) -179.9(6) ? . . . . C(2) C(1) C(7) O(1) 87.7(10) ? . . . . C(2) C(1) C(7) C(8) -97.9(9) ? . . . . C(7) C(1) C(2) C(3) -174.3(7) ? . . . . C(7) C(1) C(2) C(14) 1.3(11) ? . . . . C(6) C(1) C(7) O(1) -91.1(10) ? . . . . C(6) C(1) C(7) C(8) 83.3(10) ? . . . . C(7) C(1) C(6) C(5) 174.4(7) ? . . . . C(7) C(1) C(6) C(18) -4.9(12) ? . . . . C(1) C(2) C(3) C(4) -1.2(12) ? . . . . C(1) C(2) C(14) C(15) -92.2(10) ? . . . . C(3) C(2) C(14) C(15) 83.3(10) ? . . . . C(14) C(2) C(3) C(4) -176.8(8) ? . . . . C(2) C(3) C(4) C(5) -2.1(12) ? . . . . C(2) C(3) C(4) C(16) 178.4(7) ? . . . . C(3) C(4) C(5) C(6) 2.3(13) ? . . . . C(3) C(4) C(16) C(17) 88.5(10) ? . . . . C(5) C(4) C(16) C(17) -90.9(10) ? . . . . C(16) C(4) C(5) C(6) -178.2(8) ? . . . . C(4) C(5) C(6) C(1) 0.8(13) ? . . . . C(4) C(5) C(6) C(18) -179.9(6) ? . . . . C(1) C(6) C(18) C(19) 87.9(10) ? . . . . C(5) C(6) C(18) C(19) -91.4(10) ? . . . . O(1) C(7) C(8) C(9) 7.6(12) ? . . . . O(1) C(7) C(8) C(13) -169.2(8) ? . . . . C(1) C(7) C(8) C(9) -166.7(7) ? . . . . C(1) C(7) C(8) C(13) 16.5(12) ? . . . . C(7) C(8) C(9) C(10) -179.5(7) ? . . . . C(7) C(8) C(13) C(12) 178.3(8) ? . . . . C(9) C(8) C(13) C(12) 1.5(12) ? . . . . C(13) C(8) C(9) C(10) -2.5(11) ? . . . . C(8) C(9) C(10) Cl(1) -177.8(6) ? . . . . C(8) C(9) C(10) C(11) 1.7(12) ? . . . . Cl(1) C(10) C(11) Cl(2) -1.2(10) ? . . . . Cl(1) C(10) C(11) C(12) 179.7(5) ? . . . . C(9) C(10) C(11) Cl(2) 179.3(6) ? . . . . C(9) C(10) C(11) C(12) 0.3(10) ? . . . . Cl(2) C(11) C(12) C(13) 179.6(6) ? . . . . C(10) C(11) C(12) C(13) -1.3(13) ? . . . . C(11) C(12) C(13) C(8) 0.4(10) ? . . . . C(21) C(20) C(25) C(24) 1.1(12) ? . . . . C(21) C(20) C(25) C(37) 179.3(7) ? . . . . C(25) C(20) C(21) C(22) 0.5(10) ? . . . . C(25) C(20) C(21) C(33) 178.9(7) ? . . . . C(21) C(20) C(26) O(2) 96.9(9) ? . . . . C(21) C(20) C(26) C(27) -82.3(10) ? . . . . C(26) C(20) C(21) C(22) -176.9(7) ? . . . . C(26) C(20) C(21) C(33) 1.4(11) ? . . . . C(25) C(20) C(26) O(2) -80.6(11) ? . . . . C(25) C(20) C(26) C(27) 100.3(9) ? . . . . C(26) C(20) C(25) C(24) 178.5(7) ? . . . . C(26) C(20) C(25) C(37) -3.2(11) ? . . . . C(20) C(21) C(22) C(23) -2.2(12) ? . . . . C(20) C(21) C(33) C(34) -81.9(9) ? . . . . C(22) C(21) C(33) C(34) 96.5(9) ? . . . . C(33) C(21) C(22) C(23) 179.4(7) ? . . . . C(21) C(22) C(23) C(24) 2.3(12) ? . . . . C(21) C(22) C(23) C(35) 178.6(8) ? . . . . C(22) C(23) C(24) C(25) -0.6(11) ? . . . . C(22) C(23) C(35) C(36) 154.7(8) ? . . . . C(24) C(23) C(35) C(36) -29.2(12) ? . . . . C(35) C(23) C(24) C(25) -176.9(8) ? . . . . C(23) C(24) C(25) C(20) -1.0(13) ? . . . . C(23) C(24) C(25) C(37) -179.3(8) ? . . . . C(20) C(25) C(37) C(38) -91.3(9) ? . . . . C(24) C(25) C(37) C(38) 87.0(9) ? . . . . O(2) C(26) C(27) C(28) -4.2(11) ? . . . . O(2) C(26) C(27) C(32) 177.0(7) ? . . . . C(20) C(26) C(27) C(28) 175.0(7) ? . . . . C(20) C(26) C(27) C(32) -3.8(11) ? . . . . C(26) C(27) C(28) C(29) -179.3(7) ? . . . . C(26) C(27) C(32) C(31) 180.0(7) ? . . . . C(28) C(27) C(32) C(31) 1.2(12) ? . . . . C(32) C(27) C(28) C(29) -0.5(9) ? . . . . C(27) C(28) C(29) Cl(3) -179.0(6) ? . . . . C(27) C(28) C(29) C(30) 0.1(10) ? . . . . Cl(3) C(29) C(30) Cl(4) -2.3(10) ? . . . . Cl(3) C(29) C(30) C(31) 178.7(6) ? . . . . C(28) C(29) C(30) Cl(4) 178.5(6) ? . . . . C(28) C(29) C(30) C(31) -0.5(10) ? . . . . Cl(4) C(30) C(31) C(32) -177.8(6) ? . . . . C(29) C(30) C(31) C(32) 1.2(12) ? . . . . C(30) C(31) C(32) C(27) -1.6(12) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) C(8) 3.596(8) ? . 3_565 Cl(1) C(9) 3.591(8) ? . 3_565 Cl(1) C(15) 3.506(10) ? . 2_455 O(1) C(2) 3.337(9) ? . 4_455 O(1) C(3) 3.482(11) ? . 4_455 O(1) C(13) 3.518(10) ? . 4_455 O(1) C(14) 3.560(10) ? . 4_455 C(2) O(1) 3.337(9) ? . 4_555 C(3) O(1) 3.482(11) ? . 4_555 C(8) Cl(1) 3.596(8) ? . 3_565 C(9) Cl(1) 3.591(8) ? . 3_565 C(10) C(10) 3.421(11) ? . 3_565 C(13) O(1) 3.518(10) ? . 4_555 C(14) O(1) 3.560(10) ? . 4_555 C(15) Cl(1) 3.506(10) ? . 2_445 C(17) C(24) 3.514(13) ? . 2_546 C(17) C(31) 3.535(14) ? . 3_556 O(2) C(21) 3.498(10) ? . 4_555 O(2) C(22) 3.385(10) ? . 4_555 O(2) C(23) 3.421(10) ? . 4_555 O(2) C(24) 3.574(10) ? . 4_555 O(2) C(32) 3.424(9) ? . 4_555 C(21) O(2) 3.498(10) ? . 4_455 C(22) O(2) 3.385(10) ? . 4_455 C(23) O(2) 3.421(10) ? . 4_455 C(24) C(17) 3.514(13) ? . 2_556 C(24) O(2) 3.574(10) ? . 4_455 C(29) C(29) 3.439(11) ? . 3_556 C(31) C(17) 3.535(14) ? . 3_556 C(32) O(2) 3.424(9) ? . 4_455 Cl(1) H(6) 3.184 ? . 3_565 Cl(1) H(8) 3.269 ? . 2_455 Cl(1) H(9) 3.599 ? . 2_455 Cl(1) H(10) 3.094 ? . 2_455 Cl(1) H(22) 3.277 ? . 3_566 Cl(1) H(37) 3.055 ? . 3_566 Cl(1) H(39) 3.224 ? . 3_566 Cl(2) H(3) 3.522 ? . 3_565 Cl(2) H(7) 3.236 ? . 2_555 Cl(2) H(12) 3.270 ? . 4_555 Cl(2) H(35) 3.575 ? . 3_566 O(1) H(1) 3.590 ? . 4_455 O(1) H(5) 2.656 ? . 4_455 O(1) H(6) 3.595 ? . 4_455 O(1) H(7) 3.149 ? . 4_455 C(1) H(4) 2.992 ? . 4_455 C(1) H(5) 3.304 ? . 4_455 C(1) H(20) 3.492 ? . 4_555 C(2) H(4) 2.873 ? . 4_455 C(3) H(4) 2.718 ? . 4_455 C(4) H(4) 2.738 ? . 4_455 C(5) H(4) 2.913 ? . 4_455 C(5) H(19) 3.155 ? . 4_555 C(5) H(20) 3.456 ? . 4_555 C(6) H(4) 3.070 ? . 4_455 C(6) H(5) 3.535 ? . 4_455 C(6) H(19) 3.480 ? . 4_555 C(6) H(20) 3.178 ? . 4_555 C(7) H(5) 3.355 ? . 4_455 C(8) H(33) 3.231 ? . 3_566 C(9) H(15) 3.044 ? . 4_455 C(9) H(33) 3.255 ? . 3_566 C(10) H(22) 3.465 ? . 3_566 C(10) H(33) 3.278 ? . 3_566 C(10) H(35) 3.533 ? . 3_566 C(11) H(3) 3.585 ? . 3_565 C(11) H(33) 3.336 ? . 3_566 C(11) H(35) 3.171 ? . 3_566 C(12) H(10) 3.092 ? . 4_555 C(12) H(20) 3.497 ? . 4_555 C(12) H(33) 3.343 ? . 3_566 C(12) H(35) 3.433 ? . 3_566 C(13) H(10) 3.577 ? . 4_555 C(13) H(20) 2.916 ? . 4_555 C(13) H(33) 3.278 ? . 3_566 C(14) H(39) 2.966 ? . 1_554 C(15) H(4) 3.528 ? . 4_455 C(15) H(12) 3.214 ? . 3_555 C(15) H(14) 3.436 ? . 3_555 C(15) H(37) 3.425 ? . 4_454 C(15) H(39) 3.177 ? . 1_554 C(16) H(9) 3.207 ? . 3_555 C(16) H(38) 3.141 ? . 3_556 C(17) H(3) 3.426 ? . 4_555 C(17) H(9) 3.228 ? . 3_555 C(17) H(22) 3.146 ? . 2_546 C(17) H(24) 3.452 ? . 3_556 C(17) H(37) 3.260 ? . 2_546 C(18) H(20) 3.525 ? . 4_555 C(18) H(29) 3.427 ? . . C(18) H(33) 3.323 ? . 3_566 C(19) H(5) 3.214 ? . 4_455 C(19) H(16) 3.549 ? . 4_455 C(19) H(29) 3.365 ? . 4_455 C(19) H(34) 3.536 ? . 2_446 H(1) O(1) 3.590 ? . 4_555 H(1) H(1) 3.173 ? . 3_555 H(1) H(3) 3.264 ? . 4_555 H(1) H(4) 3.215 ? . 4_455 H(1) H(10) 3.373 ? . 3_555 H(2) H(4) 3.491 ? . 4_455 H(2) H(19) 3.122 ? . 4_555 H(2) Cl(3) 2.993 ? . 3_556 H(2) Cl(4) 3.403 ? . 3_556 H(2) C(29) 3.231 ? . 3_556 H(2) C(30) 3.377 ? . 3_556 H(3) Cl(2) 3.522 ? . 3_565 H(3) C(11) 3.585 ? . 3_565 H(3) C(17) 3.426 ? . 4_455 H(3) H(1) 3.264 ? . 4_455 H(3) H(10) 3.599 ? . 2_455 H(3) H(15) 2.522 ? . 4_455 H(4) C(1) 2.992 ? . 4_555 H(4) C(2) 2.873 ? . 4_555 H(4) C(3) 2.718 ? . 4_555 H(4) C(4) 2.738 ? . 4_555 H(4) C(5) 2.913 ? . 4_555 H(4) C(6) 3.070 ? . 4_555 H(4) C(15) 3.528 ? . 4_555 H(4) H(1) 3.215 ? . 4_555 H(4) H(2) 3.491 ? . 4_555 H(4) H(10) 2.785 ? . 4_555 H(4) H(12) 3.573 ? . 4_555 H(4) H(20) 3.369 ? . 4_555 H(5) O(1) 2.656 ? . 4_555 H(5) C(1) 3.304 ? . 4_555 H(5) C(6) 3.535 ? . 4_555 H(5) C(7) 3.355 ? . 4_555 H(5) C(19) 3.214 ? . 4_555 H(5) H(8) 3.563 ? . 4_555 H(5) H(20) 2.240 ? . 4_555 H(6) Cl(1) 3.184 ? . 3_565 H(6) O(1) 3.595 ? . 4_555 H(6) H(8) 3.563 ? . 4_555 H(6) H(39) 2.716 ? . 1_554 H(7) Cl(2) 3.236 ? . 2_545 H(7) O(1) 3.149 ? . 4_555 H(7) H(12) 3.193 ? . 3_555 H(7) C(38) 3.536 ? . 1_554 H(7) H(39) 2.642 ? . 1_554 H(8) Cl(1) 3.269 ? . 2_445 H(8) H(5) 3.563 ? . 4_455 H(8) H(6) 3.563 ? . 4_455 H(8) H(37) 3.139 ? . 4_454 H(8) H(39) 3.477 ? . 1_554 H(8) H(39) 3.460 ? . 4_454 H(9) Cl(1) 3.599 ? . 2_445 H(9) C(16) 3.207 ? . 3_555 H(9) C(17) 3.228 ? . 3_555 H(9) H(12) 2.426 ? . 3_555 H(9) H(14) 2.593 ? . 3_555 H(9) H(15) 3.503 ? . 3_555 H(9) C(38) 3.124 ? . 1_554 H(9) H(37) 2.881 ? . 4_454 H(9) H(38) 3.042 ? . 1_554 H(9) H(39) 2.643 ? . 1_554 H(9) H(40) 3.182 ? . 1_554 H(10) Cl(1) 3.094 ? . 2_445 H(10) C(12) 3.092 ? . 4_455 H(10) C(13) 3.577 ? . 4_455 H(10) H(1) 3.373 ? . 3_555 H(10) H(3) 3.599 ? . 2_445 H(10) H(4) 2.785 ? . 4_455 H(10) H(12) 3.333 ? . 3_555 H(10) H(14) 3.544 ? . 3_555 H(11) C(27) 3.502 ? . 3_556 H(11) C(28) 3.368 ? . 3_556 H(11) C(29) 3.161 ? . 3_556 H(11) C(30) 3.112 ? . 3_556 H(11) C(31) 3.261 ? . 3_556 H(11) C(32) 3.458 ? . 3_556 H(11) H(38) 2.806 ? . 3_556 H(12) Cl(2) 3.270 ? . 4_455 H(12) C(15) 3.214 ? . 3_555 H(12) H(4) 3.573 ? . 4_455 H(12) H(7) 3.193 ? . 3_555 H(12) H(9) 2.426 ? . 3_555 H(12) H(10) 3.333 ? . 3_555 H(12) C(38) 3.428 ? . 3_556 H(12) H(38) 2.701 ? . 3_556 H(12) H(39) 3.316 ? . 3_556 H(13) H(19) 3.313 ? . 4_555 H(13) Cl(4) 3.099 ? . 3_556 H(13) C(24) 3.204 ? . 2_546 H(13) C(30) 2.922 ? . 3_556 H(13) C(31) 2.802 ? . 3_556 H(13) H(22) 3.039 ? . 2_546 H(13) H(24) 2.671 ? . 3_556 H(13) H(31) 3.422 ? . 2_546 H(14) C(15) 3.436 ? . 3_555 H(14) H(9) 2.593 ? . 3_555 H(14) H(10) 3.544 ? . 3_555 H(14) C(24) 3.078 ? . 2_546 H(14) C(25) 3.271 ? . 2_546 H(14) C(37) 3.092 ? . 2_546 H(14) H(22) 2.725 ? . 2_546 H(14) H(24) 3.437 ? . 3_556 H(14) H(36) 3.437 ? . 2_546 H(14) H(37) 2.310 ? . 2_546 H(14) H(38) 3.234 ? . 3_556 H(15) C(9) 3.044 ? . 4_555 H(15) H(3) 2.522 ? . 4_555 H(15) H(9) 3.503 ? . 3_555 H(15) H(19) 3.267 ? . 4_555 H(15) H(22) 3.156 ? . 2_546 H(15) H(33) 3.463 ? . 2_546 H(16) C(19) 3.549 ? . 4_555 H(16) H(18) 3.257 ? . 4_555 H(16) H(19) 3.424 ? . 4_555 H(16) H(20) 3.379 ? . 4_555 H(16) Cl(3) 3.587 ? . 3_556 H(16) C(33) 3.438 ? . . H(16) C(34) 3.325 ? . . H(16) H(26) 2.947 ? . . H(16) H(27) 3.488 ? . . H(16) H(29) 2.532 ? . . H(16) H(33) 3.450 ? . 3_566 H(17) H(20) 3.338 ? . 4_555 H(17) C(36) 3.176 ? . 3_566 H(17) H(29) 3.503 ? . . H(17) H(31) 3.384 ? . 3_566 H(17) H(33) 2.416 ? . 3_566 H(17) H(34) 3.180 ? . 3_566 H(18) H(16) 3.257 ? . 4_455 H(18) Cl(3) 3.355 ? . 3_556 H(18) C(34) 3.294 ? . 4_455 H(18) H(26) 3.429 ? . . H(18) H(28) 3.348 ? . 4_455 H(18) H(29) 2.527 ? . 4_455 H(18) H(30) 3.586 ? . 4_455 H(18) H(34) 2.822 ? . 2_446 H(19) C(5) 3.155 ? . 4_455 H(19) C(6) 3.480 ? . 4_455 H(19) H(2) 3.122 ? . 4_455 H(19) H(13) 3.313 ? . 4_455 H(19) H(15) 3.267 ? . 4_455 H(19) H(16) 3.424 ? . 4_455 H(19) Cl(4) 3.405 ? . 2_456 H(19) H(29) 3.449 ? . 4_455 H(20) C(1) 3.492 ? . 4_455 H(20) C(5) 3.456 ? . 4_455 H(20) C(6) 3.178 ? . 4_455 H(20) C(12) 3.497 ? . 4_455 H(20) C(13) 2.916 ? . 4_455 H(20) C(18) 3.525 ? . 4_455 H(20) H(4) 3.369 ? . 4_455 H(20) H(5) 2.240 ? . 4_455 H(20) H(16) 3.379 ? . 4_455 H(20) H(17) 3.338 ? . 4_455 H(20) H(34) 3.390 ? . 2_446 Cl(3) H(2) 2.993 ? . 3_556 Cl(3) H(16) 3.587 ? . 3_556 Cl(3) H(18) 3.355 ? . 3_556 Cl(3) H(27) 2.842 ? . 3_556 Cl(3) H(29) 3.580 ? . 2_546 Cl(3) H(30) 3.027 ? . 2_546 Cl(3) H(32) 3.353 ? . 4_555 Cl(3) H(34) 3.103 ? . 4_555 Cl(4) H(2) 3.403 ? . 3_556 Cl(4) H(13) 3.099 ? . 3_556 Cl(4) H(19) 3.405 ? . 2_446 Cl(4) H(21) 3.117 ? . 2_446 Cl(4) H(23) 3.443 ? . 3_556 Cl(4) H(26) 3.468 ? . 2_446 Cl(4) H(28) 3.101 ? . 3_556 Cl(4) H(31) 3.315 ? . 4_455 O(2) H(25) 2.494 ? . 4_555 O(2) H(40) 3.498 ? . 4_555 C(20) H(24) 3.019 ? . 4_555 C(20) H(25) 3.348 ? . 4_555 C(21) H(24) 2.910 ? . 4_555 C(22) H(21) 3.539 ? . 3_566 C(22) H(23) 3.573 ? . 4_455 C(22) H(24) 2.874 ? . 4_555 C(23) H(23) 3.264 ? . 4_455 C(23) H(24) 3.024 ? . 4_555 C(24) H(13) 3.204 ? . 2_556 C(24) H(14) 3.078 ? . 2_556 C(24) H(24) 3.109 ? . 4_555 C(25) H(14) 3.271 ? . 2_556 C(25) H(24) 3.113 ? . 4_555 C(26) H(25) 3.265 ? . 4_555 C(27) H(11) 3.502 ? . 3_556 C(28) H(11) 3.368 ? . 3_556 C(28) H(32) 3.418 ? . 4_555 C(28) H(35) 3.489 ? . 4_555 C(29) H(2) 3.231 ? . 3_556 C(29) H(11) 3.161 ? . 3_556 C(30) H(2) 3.377 ? . 3_556 C(30) H(11) 3.112 ? . 3_556 C(30) H(13) 2.922 ? . 3_556 C(31) H(11) 3.261 ? . 3_556 C(31) H(13) 2.802 ? . 3_556 C(31) H(30) 2.990 ? . 4_455 C(32) H(11) 3.458 ? . 3_556 C(32) H(30) 3.205 ? . 4_455 C(33) H(16) 3.438 ? . . C(33) H(28) 3.557 ? . 4_455 C(33) H(31) 3.523 ? . 3_566 C(34) H(16) 3.325 ? . . C(34) H(18) 3.294 ? . 4_555 C(34) H(24) 3.526 ? . 4_555 C(34) H(25) 3.582 ? . 4_555 C(34) H(31) 3.540 ? . 3_566 C(34) H(32) 3.337 ? . 3_566 C(35) H(21) 3.362 ? . 3_566 C(35) H(23) 3.061 ? . 4_455 C(35) H(26) 3.593 ? . 3_566 C(35) H(29) 3.475 ? . 3_566 C(35) H(30) 3.493 ? . 3_566 C(36) H(17) 3.176 ? . 3_566 C(36) H(23) 3.193 ? . 4_455 C(36) H(29) 3.536 ? . 3_566 C(37) H(14) 3.092 ? . 2_556 C(37) H(40) 3.475 ? . 4_555 C(38) H(7) 3.536 ? . 1_556 C(38) H(9) 3.124 ? . 1_556 C(38) H(12) 3.428 ? . 3_556 C(38) H(36) 3.584 ? . 4_455 H(21) Cl(4) 3.117 ? . 2_456 H(21) C(22) 3.539 ? . 3_566 H(21) C(35) 3.362 ? . 3_566 H(21) H(21) 2.884 ? . 3_566 H(21) H(23) 3.553 ? . 4_455 H(21) H(24) 3.339 ? . 4_555 H(21) H(31) 2.854 ? . 3_566 H(21) H(32) 3.064 ? . 3_566 H(22) Cl(1) 3.277 ? . 3_566 H(22) C(10) 3.465 ? . 3_566 H(22) C(17) 3.146 ? . 2_556 H(22) H(13) 3.039 ? . 2_556 H(22) H(14) 2.725 ? . 2_556 H(22) H(15) 3.156 ? . 2_556 H(23) Cl(4) 3.443 ? . 3_556 H(23) C(22) 3.573 ? . 4_555 H(23) C(23) 3.264 ? . 4_555 H(23) C(35) 3.061 ? . 4_555 H(23) C(36) 3.193 ? . 4_555 H(23) H(21) 3.553 ? . 4_555 H(23) H(32) 2.548 ? . 4_555 H(23) H(34) 3.160 ? . 4_555 H(23) H(35) 2.862 ? . 4_555 H(24) C(17) 3.452 ? . 3_556 H(24) H(13) 2.671 ? . 3_556 H(24) H(14) 3.437 ? . 3_556 H(24) C(20) 3.019 ? . 4_455 H(24) C(21) 2.910 ? . 4_455 H(24) C(22) 2.874 ? . 4_455 H(24) C(23) 3.024 ? . 4_455 H(24) C(24) 3.109 ? . 4_455 H(24) C(25) 3.113 ? . 4_455 H(24) C(34) 3.526 ? . 4_455 H(24) H(21) 3.339 ? . 4_455 H(24) H(30) 2.715 ? . 4_455 H(24) H(31) 3.592 ? . 4_455 H(25) O(2) 2.494 ? . 4_455 H(25) C(20) 3.348 ? . 4_455 H(25) C(26) 3.265 ? . 4_455 H(25) C(34) 3.582 ? . 4_455 H(25) H(28) 3.242 ? . 4_455 H(25) H(30) 3.076 ? . 4_455 H(26) H(16) 2.947 ? . . H(26) H(18) 3.429 ? . . H(26) Cl(4) 3.468 ? . 2_456 H(26) C(35) 3.593 ? . 3_566 H(26) H(28) 3.078 ? . 4_455 H(26) H(31) 2.833 ? . 3_566 H(26) H(32) 3.479 ? . 3_566 H(27) H(16) 3.488 ? . . H(27) Cl(3) 2.842 ? . 3_556 H(27) H(28) 3.314 ? . 4_455 H(27) H(30) 3.528 ? . 4_455 H(28) H(18) 3.348 ? . 4_555 H(28) Cl(4) 3.101 ? . 3_556 H(28) C(33) 3.557 ? . 4_555 H(28) H(25) 3.242 ? . 4_555 H(28) H(26) 3.078 ? . 4_555 H(28) H(27) 3.314 ? . 4_555 H(29) C(18) 3.427 ? . . H(29) C(19) 3.365 ? . 4_555 H(29) H(16) 2.532 ? . . H(29) H(17) 3.503 ? . . H(29) H(18) 2.527 ? . 4_555 H(29) H(19) 3.449 ? . 4_555 H(29) Cl(3) 3.580 ? . 2_556 H(29) C(35) 3.475 ? . 3_566 H(29) C(36) 3.536 ? . 3_566 H(29) H(31) 3.184 ? . 3_566 H(29) H(32) 3.163 ? . 3_566 H(29) H(34) 2.926 ? . 3_566 H(30) H(18) 3.586 ? . 4_555 H(30) Cl(3) 3.027 ? . 2_556 H(30) C(31) 2.990 ? . 4_555 H(30) C(32) 3.205 ? . 4_555 H(30) C(35) 3.493 ? . 3_566 H(30) H(24) 2.715 ? . 4_555 H(30) H(25) 3.076 ? . 4_555 H(30) H(27) 3.528 ? . 4_555 H(30) H(31) 3.400 ? . 3_566 H(30) H(32) 2.789 ? . 3_566 H(30) H(34) 3.463 ? . 3_566 H(31) H(13) 3.422 ? . 2_556 H(31) H(17) 3.384 ? . 3_566 H(31) Cl(4) 3.315 ? . 4_555 H(31) C(33) 3.523 ? . 3_566 H(31) C(34) 3.540 ? . 3_566 H(31) H(21) 2.854 ? . 3_566 H(31) H(24) 3.592 ? . 4_555 H(31) H(26) 2.833 ? . 3_566 H(31) H(29) 3.184 ? . 3_566 H(31) H(30) 3.400 ? . 3_566 H(32) Cl(3) 3.353 ? . 4_455 H(32) C(28) 3.418 ? . 4_455 H(32) C(34) 3.337 ? . 3_566 H(32) H(21) 3.064 ? . 3_566 H(32) H(23) 2.548 ? . 4_455 H(32) H(26) 3.479 ? . 3_566 H(32) H(29) 3.163 ? . 3_566 H(32) H(30) 2.789 ? . 3_566 H(33) C(8) 3.231 ? . 3_566 H(33) C(9) 3.255 ? . 3_566 H(33) C(10) 3.278 ? . 3_566 H(33) C(11) 3.336 ? . 3_566 H(33) C(12) 3.343 ? . 3_566 H(33) C(13) 3.278 ? . 3_566 H(33) C(18) 3.323 ? . 3_566 H(33) H(15) 3.463 ? . 2_556 H(33) H(16) 3.450 ? . 3_566 H(33) H(17) 2.416 ? . 3_566 H(34) C(19) 3.536 ? . 2_456 H(34) H(17) 3.180 ? . 3_566 H(34) H(18) 2.822 ? . 2_456 H(34) H(20) 3.390 ? . 2_456 H(34) Cl(3) 3.103 ? . 4_455 H(34) H(23) 3.160 ? . 4_455 H(34) H(29) 2.926 ? . 3_566 H(34) H(30) 3.463 ? . 3_566 H(35) Cl(2) 3.575 ? . 3_566 H(35) C(10) 3.533 ? . 3_566 H(35) C(11) 3.171 ? . 3_566 H(35) C(12) 3.433 ? . 3_566 H(35) C(28) 3.489 ? . 4_455 H(35) H(23) 2.862 ? . 4_455 H(36) H(14) 3.437 ? . 2_556 H(36) C(38) 3.584 ? . 4_555 H(36) H(40) 2.706 ? . 4_555 H(37) Cl(1) 3.055 ? . 3_566 H(37) C(15) 3.425 ? . 4_556 H(37) C(17) 3.260 ? . 2_556 H(37) H(8) 3.139 ? . 4_556 H(37) H(9) 2.881 ? . 4_556 H(37) H(14) 2.310 ? . 2_556 H(37) H(40) 3.364 ? . 4_555 H(38) C(16) 3.141 ? . 3_556 H(38) H(9) 3.042 ? . 1_556 H(38) H(11) 2.806 ? . 3_556 H(38) H(12) 2.701 ? . 3_556 H(38) H(14) 3.234 ? . 3_556 H(39) Cl(1) 3.224 ? . 3_566 H(39) C(14) 2.966 ? . 1_556 H(39) C(15) 3.177 ? . 1_556 H(39) H(6) 2.716 ? . 1_556 H(39) H(7) 2.642 ? . 1_556 H(39) H(8) 3.477 ? . 1_556 H(39) H(8) 3.460 ? . 4_556 H(39) H(9) 2.643 ? . 1_556 H(39) H(12) 3.316 ? . 3_556 H(40) H(9) 3.182 ? . 1_556 H(40) O(2) 3.498 ? . 4_455 H(40) C(37) 3.475 ? . 4_455 H(40) H(36) 2.706 ? . 4_455 H(40) H(37) 3.364 ? . 4_455 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== data__4_140C _database_code_depnum_ccdc_archive 'CCDC 751184' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C19 H21 Cl O ' _chemical_formula_moiety 'C19 H21 Cl O ' _chemical_formula_weight 300.83 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 10.3663(3) _cell_length_b 15.8579(4) _cell_length_c 10.7014(3) _cell_angle_alpha 90.0000 _cell_angle_beta 110.9847(9) _cell_angle_gamma 90.0000 _cell_volume 1642.49(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15669 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 133.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.216 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640.00 _exptl_absorpt_coefficient_mu 0.229 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.934 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 25281 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_theta_max 27.45 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3734 _reflns_number_gt 2523 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.2626 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3734 _refine_ls_number_parameters 191 _refine_ls_goodness_of_fit_ref 1.231 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1323P)^2^+1.0073P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 0.61 _refine_diff_density_min -0.64 _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 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl(1) Cl 0.18919(9) 0.60734(5) 0.25214(9) 0.0458(3) Uani 1.00 1 d . . . O(1) O 0.1334(2) 0.31616(15) -0.2165(2) 0.0479(6) Uani 1.00 1 d . . . C(1) C 0.2307(3) 0.22511(18) -0.0305(3) 0.0331(6) Uani 1.00 1 d . . . C(2) C 0.1410(3) 0.16636(19) -0.0082(3) 0.0330(6) Uani 1.00 1 d . . . C(3) C 0.1945(3) 0.0891(2) 0.0495(3) 0.0355(7) Uani 1.00 1 d . . . C(4) C 0.3328(3) 0.0696(2) 0.0837(3) 0.0387(7) Uani 1.00 1 d . . . C(5) C 0.4199(3) 0.1295(2) 0.0614(3) 0.0428(8) Uani 1.00 1 d . . . C(6) C 0.3723(3) 0.2070(2) 0.0044(3) 0.0406(7) Uani 1.00 1 d . . . C(7) C 0.1765(3) 0.30896(19) -0.0946(3) 0.0341(6) Uani 1.00 1 d . . . C(8) C 0.1805(3) 0.38220(18) -0.0065(3) 0.0313(6) Uani 1.00 1 d . . . C(9) C 0.2040(3) 0.3714(2) 0.1291(3) 0.0332(6) Uani 1.00 1 d . . . C(10) C 0.2074(3) 0.44077(19) 0.2093(3) 0.0353(6) Uani 1.00 1 d . . . C(11) C 0.1867(3) 0.52018(19) 0.1520(3) 0.0336(6) Uani 1.00 1 d . . . C(12) C 0.1628(3) 0.53268(19) 0.0177(3) 0.0361(7) Uani 1.00 1 d . . . C(13) C 0.1578(3) 0.46330(19) -0.0616(3) 0.0348(6) Uani 1.00 1 d . . . C(14) C -0.0113(3) 0.1846(2) -0.0479(3) 0.0385(7) Uani 1.00 1 d . . . C(15) C -0.0927(3) 0.1603(2) -0.1921(3) 0.0483(8) Uani 1.00 1 d . . . C(16) C 0.3923(4) -0.0129(2) 0.1506(3) 0.0511(9) Uani 1.00 1 d . . . C(17) C 0.4462(4) -0.0067(2) 0.3021(3) 0.0553(10) Uani 1.00 1 d . . . C(18) C 0.4727(4) 0.2705(2) -0.0145(5) 0.0638(12) Uani 1.00 1 d . . . C(19) C 0.5317(8) 0.2517(3) -0.1110(7) 0.123(3) Uani 1.00 1 d . . . H(1) H 0.1344 0.0489 0.0657 0.043 Uiso 1.00 1 c R . . H(2) H 0.5154 0.1168 0.0863 0.051 Uiso 1.00 1 c R . . H(3) H 0.2178 0.3164 0.1668 0.040 Uiso 1.00 1 c R . . H(4) H 0.2236 0.4338 0.3019 0.042 Uiso 1.00 1 c R . . H(5) H 0.1500 0.5879 -0.0192 0.043 Uiso 1.00 1 c R . . H(6) H 0.1389 0.4707 -0.1546 0.042 Uiso 1.00 1 c R . . H(7) H -0.0242 0.2456 -0.0359 0.046 Uiso 1.00 1 c R . . H(8) H -0.0480 0.1532 0.0120 0.046 Uiso 1.00 1 c R . . H(9) H -0.0965 0.2085 -0.2508 0.058 Uiso 1.00 1 c R . . H(10) H -0.1868 0.1442 -0.2007 0.058 Uiso 1.00 1 c R . . H(11) H -0.0474 0.1127 -0.2179 0.058 Uiso 1.00 1 c R . . H(12) H 0.4687 -0.0303 0.1211 0.061 Uiso 1.00 1 c R . . H(13) H 0.3199 -0.0570 0.1217 0.061 Uiso 1.00 1 c R . . H(14) H 0.5438 0.0098 0.3345 0.066 Uiso 1.00 1 c R . . H(15) H 0.4369 -0.0615 0.3403 0.066 Uiso 1.00 1 c R . . H(16) H 0.3928 0.0357 0.3295 0.066 Uiso 1.00 1 c R . . H(17) H 0.4242 0.3253 -0.0385 0.077 Uiso 1.00 1 c R . . H(18) H 0.5487 0.2781 0.0727 0.077 Uiso 1.00 1 c R . . H(19) H 0.6173 0.2198 -0.0690 0.147 Uiso 1.00 1 c R . . H(20) H 0.5521 0.3043 -0.1484 0.147 Uiso 1.00 1 c R . . H(21) H 0.4667 0.2180 -0.1828 0.147 Uiso 1.00 1 c R . . 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 Cl(1) 0.0454(5) 0.0339(4) 0.0525(5) 0.0025(3) 0.0105(4) -0.0118(3) O(1) 0.0752(18) 0.0376(12) 0.0369(13) 0.0082(11) 0.0272(12) 0.0023(9) C(1) 0.0414(17) 0.0245(14) 0.0353(15) 0.0008(11) 0.0160(13) -0.0028(11) C(2) 0.0363(16) 0.0311(15) 0.0338(15) -0.0001(11) 0.0151(12) -0.0036(11) C(3) 0.0463(18) 0.0282(14) 0.0366(16) -0.0008(12) 0.0204(14) -0.0003(11) C(4) 0.0481(19) 0.0319(16) 0.0357(16) 0.0036(13) 0.0146(14) -0.0044(12) C(5) 0.0381(18) 0.0342(16) 0.055(2) 0.0019(13) 0.0147(15) -0.0082(14) C(6) 0.0428(18) 0.0297(15) 0.0501(19) -0.0001(12) 0.0178(15) -0.0077(13) C(7) 0.0427(17) 0.0307(15) 0.0340(16) -0.0016(12) 0.0197(13) 0.0003(11) C(8) 0.0332(15) 0.0279(14) 0.0356(16) -0.0007(11) 0.0157(12) 0.0003(11) C(9) 0.0386(16) 0.0281(14) 0.0313(15) 0.0022(11) 0.0107(12) 0.0018(11) C(10) 0.0371(16) 0.0331(15) 0.0367(16) 0.0022(12) 0.0143(13) 0.0003(12) C(11) 0.0302(15) 0.0312(15) 0.0370(16) -0.0010(11) 0.0089(12) -0.0049(11) C(12) 0.0345(16) 0.0290(14) 0.0436(17) 0.0008(11) 0.0126(13) 0.0043(12) C(13) 0.0373(16) 0.0294(14) 0.0389(16) 0.0022(11) 0.0152(13) 0.0044(11) C(14) 0.0381(17) 0.0359(16) 0.0424(17) 0.0006(12) 0.0156(14) -0.0024(12) C(15) 0.0432(19) 0.048(2) 0.045(2) -0.0012(15) 0.0056(15) -0.0049(15) C(16) 0.064(2) 0.0381(18) 0.050(2) 0.0166(16) 0.0182(17) 0.0073(15) C(17) 0.051(2) 0.065(2) 0.053(2) 0.0251(18) 0.0231(18) 0.0216(18) C(18) 0.055(2) 0.0363(19) 0.113(3) -0.0085(16) 0.047(2) -0.012(2) C(19) 0.193(7) 0.056(3) 0.196(7) -0.034(3) 0.163(6) -0.017(3) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(11) 1.743(3) yes . . O(1) C(7) 1.224(3) yes . . C(1) C(2) 1.396(4) yes . . C(1) C(6) 1.408(4) yes . . C(1) C(7) 1.509(4) yes . . C(2) C(3) 1.394(4) yes . . C(2) C(14) 1.509(4) yes . . C(3) C(4) 1.382(4) yes . . C(4) C(5) 1.389(5) yes . . C(4) C(16) 1.513(4) yes . . C(5) C(6) 1.382(4) yes . . C(6) C(18) 1.513(6) yes . . C(7) C(8) 1.487(4) yes . . C(8) C(9) 1.393(4) yes . . C(8) C(13) 1.399(4) yes . . C(9) C(10) 1.388(4) yes . . C(10) C(11) 1.383(4) yes . . C(11) C(12) 1.383(4) yes . . C(12) C(13) 1.379(4) yes . . C(14) C(15) 1.520(4) yes . . C(16) C(17) 1.518(5) yes . . C(18) C(19) 1.408(11) yes . . C(3) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(9) H(3) 0.950 no . . C(10) H(4) 0.950 no . . C(12) H(5) 0.950 no . . C(13) H(6) 0.950 no . . C(14) H(7) 0.990 no . . C(14) H(8) 0.990 no . . C(15) H(9) 0.980 no . . C(15) H(10) 0.980 no . . C(15) H(11) 0.980 no . . C(16) H(12) 0.990 no . . C(16) H(13) 0.990 no . . C(17) H(14) 0.980 no . . C(17) H(15) 0.980 no . . C(17) H(16) 0.980 no . . C(18) H(17) 0.990 no . . C(18) H(18) 0.990 no . . C(19) H(19) 0.980 no . . C(19) H(20) 0.980 no . . C(19) H(21) 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(2) C(1) C(6) 120.9(2) yes . . . C(2) C(1) C(7) 120.2(2) yes . . . C(6) C(1) C(7) 118.9(3) yes . . . C(1) C(2) C(3) 118.6(2) yes . . . C(1) C(2) C(14) 121.2(2) yes . . . C(3) C(2) C(14) 120.2(3) yes . . . C(2) C(3) C(4) 121.6(3) yes . . . C(3) C(4) C(5) 118.5(2) yes . . . C(3) C(4) C(16) 121.9(3) yes . . . C(5) C(4) C(16) 119.5(3) yes . . . C(4) C(5) C(6) 122.2(3) yes . . . C(1) C(6) C(5) 118.2(3) yes . . . C(1) C(6) C(18) 122.0(2) yes . . . C(5) C(6) C(18) 119.8(3) yes . . . O(1) C(7) C(1) 120.0(2) yes . . . O(1) C(7) C(8) 121.3(2) yes . . . C(1) C(7) C(8) 118.6(2) yes . . . C(7) C(8) C(9) 121.2(2) yes . . . C(7) C(8) C(13) 119.2(2) yes . . . C(9) C(8) C(13) 119.5(2) yes . . . C(8) C(9) C(10) 120.2(2) yes . . . C(9) C(10) C(11) 118.8(3) yes . . . Cl(1) C(11) C(10) 118.9(2) yes . . . Cl(1) C(11) C(12) 118.9(2) yes . . . C(10) C(11) C(12) 122.2(2) yes . . . C(11) C(12) C(13) 118.6(2) yes . . . C(8) C(13) C(12) 120.7(3) yes . . . C(2) C(14) C(15) 112.5(3) yes . . . C(4) C(16) C(17) 112.4(3) yes . . . C(6) C(18) C(19) 117.2(4) yes . . . C(2) C(3) H(1) 119.2 no . . . C(4) C(3) H(1) 119.2 no . . . C(4) C(5) H(2) 118.9 no . . . C(6) C(5) H(2) 118.9 no . . . C(8) C(9) H(3) 119.9 no . . . C(10) C(9) H(3) 119.9 no . . . C(9) C(10) H(4) 120.6 no . . . C(11) C(10) H(4) 120.6 no . . . C(11) C(12) H(5) 120.7 no . . . C(13) C(12) H(5) 120.7 no . . . C(8) C(13) H(6) 119.7 no . . . C(12) C(13) H(6) 119.7 no . . . C(2) C(14) H(7) 109.1 no . . . C(2) C(14) H(8) 109.1 no . . . C(15) C(14) H(7) 109.1 no . . . C(15) C(14) H(8) 109.1 no . . . H(7) C(14) H(8) 107.8 no . . . C(14) C(15) H(9) 109.5 no . . . C(14) C(15) H(10) 109.5 no . . . C(14) C(15) H(11) 109.5 no . . . H(9) C(15) H(10) 109.5 no . . . H(9) C(15) H(11) 109.5 no . . . H(10) C(15) H(11) 109.5 no . . . C(4) C(16) H(12) 109.1 no . . . C(4) C(16) H(13) 109.1 no . . . C(17) C(16) H(12) 109.1 no . . . C(17) C(16) H(13) 109.1 no . . . H(12) C(16) H(13) 107.9 no . . . C(16) C(17) H(14) 109.5 no . . . C(16) C(17) H(15) 109.5 no . . . C(16) C(17) H(16) 109.5 no . . . H(14) C(17) H(15) 109.5 no . . . H(14) C(17) H(16) 109.5 no . . . H(15) C(17) H(16) 109.5 no . . . C(6) C(18) H(17) 108.0 no . . . C(6) C(18) H(18) 108.0 no . . . C(19) C(18) H(17) 108.0 no . . . C(19) C(18) H(18) 108.0 no . . . H(17) C(18) H(18) 107.2 no . . . C(18) C(19) H(19) 109.5 no . . . C(18) C(19) H(20) 109.5 no . . . C(18) C(19) H(21) 109.5 no . . . H(19) C(19) H(20) 109.5 no . . . H(19) C(19) H(21) 109.5 no . . . H(20) C(19) H(21) 109.5 no . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(2) C(1) C(6) C(5) -0.1(3) ? . . . . C(2) C(1) C(6) C(18) -177.9(3) ? . . . . C(6) C(1) C(2) C(3) -0.0(4) ? . . . . C(6) C(1) C(2) C(14) -178.7(3) ? . . . . C(2) C(1) C(7) O(1) -88.6(4) ? . . . . C(2) C(1) C(7) C(8) 93.0(3) ? . . . . C(7) C(1) C(2) C(3) 179.1(2) ? . . . . C(7) C(1) C(2) C(14) 0.4(4) ? . . . . C(6) C(1) C(7) O(1) 90.6(4) ? . . . . C(6) C(1) C(7) C(8) -87.8(4) ? . . . . C(7) C(1) C(6) C(5) -179.2(3) ? . . . . C(7) C(1) C(6) C(18) 2.9(5) ? . . . . C(1) C(2) C(3) C(4) -0.5(4) ? . . . . C(1) C(2) C(14) C(15) 87.0(3) ? . . . . C(3) C(2) C(14) C(15) -91.6(3) ? . . . . C(14) C(2) C(3) C(4) 178.3(3) ? . . . . C(2) C(3) C(4) C(5) 1.0(5) ? . . . . C(2) C(3) C(4) C(16) 177.9(3) ? . . . . C(3) C(4) C(5) C(6) -1.1(5) ? . . . . C(3) C(4) C(16) C(17) -91.3(4) ? . . . . C(5) C(4) C(16) C(17) 85.6(4) ? . . . . C(16) C(4) C(5) C(6) -178.1(3) ? . . . . C(4) C(5) C(6) C(1) 0.7(5) ? . . . . C(4) C(5) C(6) C(18) 178.6(3) ? . . . . C(1) C(6) C(18) C(19) -112.8(4) ? . . . . C(5) C(6) C(18) C(19) 69.4(5) ? . . . . O(1) C(7) C(8) C(9) 167.6(3) ? . . . . O(1) C(7) C(8) C(13) -11.4(5) ? . . . . C(1) C(7) C(8) C(9) -14.1(4) ? . . . . C(1) C(7) C(8) C(13) 166.9(3) ? . . . . C(7) C(8) C(9) C(10) 179.9(2) ? . . . . C(7) C(8) C(13) C(12) -179.1(3) ? . . . . C(9) C(8) C(13) C(12) 2.0(5) ? . . . . C(13) C(8) C(9) C(10) -1.1(4) ? . . . . C(8) C(9) C(10) C(11) 0.2(3) ? . . . . C(9) C(10) C(11) Cl(1) 179.4(2) ? . . . . C(9) C(10) C(11) C(12) 0.0(5) ? . . . . Cl(1) C(11) C(12) C(13) -178.6(2) ? . . . . C(10) C(11) C(12) C(13) 0.8(5) ? . . . . C(11) C(12) C(13) C(8) -1.8(5) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) O(1) 3.448(3) ? . 3_565 O(1) Cl(1) 3.448(3) ? . 3_565 O(1) C(2) 3.162(4) ? . 4_554 O(1) C(3) 3.172(4) ? . 4_554 O(1) C(14) 3.319(3) ? . 4_554 C(2) O(1) 3.162(4) ? . 4_555 C(3) O(1) 3.172(4) ? . 4_555 C(11) C(12) 3.523(4) ? . 3_565 C(11) C(13) 3.359(4) ? . 3_565 C(12) C(11) 3.523(4) ? . 3_565 C(12) C(12) 3.419(4) ? . 3_565 C(12) C(13) 3.520(5) ? . 3_565 C(13) C(11) 3.359(4) ? . 3_565 C(13) C(12) 3.520(5) ? . 3_565 C(14) O(1) 3.319(3) ? . 4_555 Cl(1) H(2) 2.932 ? . 2_655 Cl(1) H(6) 3.412 ? . 3_565 Cl(1) H(7) 3.300 ? . 3_565 Cl(1) H(8) 3.418 ? . 2_555 Cl(1) H(9) 3.073 ? . 3_565 Cl(1) H(14) 3.571 ? . 2_655 Cl(1) H(20) 3.539 ? . 3_665 O(1) H(1) 3.166 ? . 4_554 O(1) H(3) 2.743 ? . 4_554 O(1) H(7) 3.363 ? . 4_554 O(1) H(8) 2.881 ? . 4_554 O(1) H(16) 3.470 ? . 4_554 C(1) H(3) 3.261 ? . 4_554 C(1) H(4) 3.079 ? . 4_554 C(2) H(4) 2.939 ? . 4_554 C(3) H(4) 2.797 ? . 4_554 C(3) H(6) 3.545 ? . 4_555 C(4) H(4) 2.817 ? . 4_554 C(4) H(12) 3.558 ? . 3_655 C(4) H(20) 3.566 ? . 4_555 C(5) H(4) 2.969 ? . 4_554 C(5) H(12) 3.040 ? . 3_655 C(5) H(20) 3.095 ? . 4_555 C(5) H(21) 3.553 ? . 4_555 C(6) H(3) 3.407 ? . 4_554 C(6) H(4) 3.109 ? . 4_554 C(6) H(20) 3.515 ? . 4_555 C(6) H(21) 3.352 ? . 4_555 C(7) H(3) 3.382 ? . 4_554 C(8) H(5) 3.565 ? . 3_565 C(8) H(14) 3.448 ? . 2_655 C(8) H(16) 3.519 ? . 4_554 C(9) H(5) 3.489 ? . 3_565 C(9) H(11) 3.548 ? . 4_555 C(9) H(14) 3.328 ? . 2_655 C(9) H(21) 3.090 ? . 4_555 C(10) H(5) 3.560 ? . 3_565 C(10) H(11) 3.127 ? . 4_555 C(10) H(12) 3.227 ? . 2_655 C(10) H(14) 2.990 ? . 2_655 C(10) H(21) 3.560 ? . 4_555 C(11) H(6) 3.388 ? . 3_565 C(11) H(14) 2.751 ? . 2_655 C(12) H(11) 3.253 ? . 2_554 C(12) H(14) 2.906 ? . 2_655 C(13) H(11) 3.249 ? . 2_554 C(13) H(14) 3.261 ? . 2_655 C(13) H(16) 3.053 ? . 4_554 C(15) H(5) 3.146 ? . 2_544 C(15) H(6) 3.377 ? . 2_544 C(15) H(13) 3.174 ? . 3_555 C(16) H(2) 3.434 ? . 3_655 C(16) H(10) 3.159 ? . 3_555 C(16) H(19) 3.387 ? . 3_655 C(16) H(21) 3.531 ? . 3_655 C(17) H(6) 3.427 ? . 4_555 C(17) H(10) 3.328 ? . 3_555 C(17) H(17) 3.587 ? . 2_645 C(17) H(17) 3.393 ? . 4_555 C(17) H(20) 3.372 ? . 4_555 C(18) H(15) 3.193 ? . 2_655 C(18) H(16) 3.453 ? . 4_554 C(18) H(21) 3.577 ? . 4_555 C(19) H(3) 3.445 ? . 4_554 C(19) H(12) 3.513 ? . 3_655 C(19) H(13) 3.470 ? . 3_655 C(19) H(18) 3.484 ? . 4_554 H(1) O(1) 3.166 ? . 4_555 H(1) H(1) 3.056 ? . 3_555 H(1) H(4) 3.283 ? . 4_554 H(1) H(6) 2.993 ? . 4_555 H(1) H(8) 3.351 ? . 3_555 H(1) H(10) 3.346 ? . 3_555 H(1) H(11) 3.330 ? . 3_555 H(2) Cl(1) 2.932 ? . 2_645 H(2) C(16) 3.434 ? . 3_655 H(2) H(4) 3.530 ? . 4_554 H(2) H(12) 2.664 ? . 3_655 H(2) H(13) 3.389 ? . 3_655 H(2) H(20) 3.000 ? . 4_555 H(3) O(1) 2.743 ? . 4_555 H(3) C(1) 3.261 ? . 4_555 H(3) C(6) 3.407 ? . 4_555 H(3) C(7) 3.382 ? . 4_555 H(3) C(19) 3.445 ? . 4_555 H(3) H(11) 3.574 ? . 4_555 H(3) H(21) 2.563 ? . 4_555 H(4) C(1) 3.079 ? . 4_555 H(4) C(2) 2.939 ? . 4_555 H(4) C(3) 2.797 ? . 4_555 H(4) C(4) 2.817 ? . 4_555 H(4) C(5) 2.969 ? . 4_555 H(4) C(6) 3.109 ? . 4_555 H(4) H(1) 3.283 ? . 4_555 H(4) H(2) 3.530 ? . 4_555 H(4) H(11) 2.839 ? . 4_555 H(4) H(12) 3.049 ? . 2_655 H(4) H(14) 3.451 ? . 2_655 H(4) H(21) 3.446 ? . 4_555 H(5) C(8) 3.565 ? . 3_565 H(5) C(9) 3.489 ? . 3_565 H(5) C(10) 3.560 ? . 3_565 H(5) C(15) 3.146 ? . 2_554 H(5) H(7) 3.094 ? . 3_565 H(5) H(9) 3.007 ? . 2_554 H(5) H(10) 3.278 ? . 2_554 H(5) H(11) 2.656 ? . 2_554 H(5) H(14) 3.320 ? . 2_655 H(5) H(20) 3.422 ? . 3_665 H(6) Cl(1) 3.412 ? . 3_565 H(6) C(3) 3.545 ? . 4_554 H(6) C(11) 3.388 ? . 3_565 H(6) C(15) 3.377 ? . 2_554 H(6) C(17) 3.427 ? . 4_554 H(6) H(1) 2.993 ? . 4_554 H(6) H(10) 3.281 ? . 2_554 H(6) H(11) 2.629 ? . 2_554 H(6) H(15) 3.427 ? . 4_554 H(6) H(16) 2.700 ? . 4_554 H(7) Cl(1) 3.300 ? . 3_565 H(7) O(1) 3.363 ? . 4_555 H(7) H(5) 3.094 ? . 3_565 H(7) H(9) 3.470 ? . 4_555 H(8) Cl(1) 3.418 ? . 2_545 H(8) O(1) 2.881 ? . 4_555 H(8) H(1) 3.351 ? . 3_555 H(8) H(9) 3.524 ? . 4_555 H(8) H(13) 3.071 ? . 3_555 H(8) H(19) 3.427 ? . 1_455 H(9) Cl(1) 3.073 ? . 3_565 H(9) H(5) 3.007 ? . 2_544 H(9) H(7) 3.470 ? . 4_554 H(9) H(8) 3.524 ? . 4_554 H(9) H(18) 3.487 ? . 4_454 H(10) C(16) 3.159 ? . 3_555 H(10) C(17) 3.328 ? . 3_555 H(10) H(1) 3.346 ? . 3_555 H(10) H(5) 3.278 ? . 2_544 H(10) H(6) 3.281 ? . 2_544 H(10) H(13) 2.317 ? . 3_555 H(10) H(15) 2.810 ? . 3_555 H(10) H(16) 3.534 ? . 3_555 H(10) H(18) 3.186 ? . 4_454 H(10) H(19) 3.098 ? . 1_455 H(11) C(9) 3.548 ? . 4_554 H(11) C(10) 3.127 ? . 4_554 H(11) C(12) 3.253 ? . 2_544 H(11) C(13) 3.249 ? . 2_544 H(11) H(1) 3.330 ? . 3_555 H(11) H(3) 3.574 ? . 4_554 H(11) H(4) 2.839 ? . 4_554 H(11) H(5) 2.656 ? . 2_544 H(11) H(6) 2.629 ? . 2_544 H(11) H(13) 3.451 ? . 3_555 H(12) C(4) 3.558 ? . 3_655 H(12) C(5) 3.040 ? . 3_655 H(12) C(10) 3.227 ? . 2_645 H(12) C(19) 3.513 ? . 3_655 H(12) H(2) 2.664 ? . 3_655 H(12) H(4) 3.049 ? . 2_645 H(12) H(12) 3.046 ? . 3_655 H(12) H(19) 3.127 ? . 3_655 H(12) H(21) 3.070 ? . 3_655 H(13) C(15) 3.174 ? . 3_555 H(13) C(19) 3.470 ? . 3_655 H(13) H(2) 3.389 ? . 3_655 H(13) H(8) 3.071 ? . 3_555 H(13) H(10) 2.317 ? . 3_555 H(13) H(11) 3.451 ? . 3_555 H(13) H(19) 2.770 ? . 3_655 H(13) H(21) 3.287 ? . 3_655 H(14) Cl(1) 3.571 ? . 2_645 H(14) C(8) 3.448 ? . 2_645 H(14) C(9) 3.328 ? . 2_645 H(14) C(10) 2.990 ? . 2_645 H(14) C(11) 2.751 ? . 2_645 H(14) C(12) 2.906 ? . 2_645 H(14) C(13) 3.261 ? . 2_645 H(14) H(4) 3.451 ? . 2_645 H(14) H(5) 3.320 ? . 2_645 H(14) H(15) 3.511 ? . 3_656 H(14) H(16) 3.491 ? . 3_656 H(14) H(17) 3.595 ? . 2_645 H(14) H(17) 3.381 ? . 4_555 H(14) H(20) 2.953 ? . 4_555 H(15) C(18) 3.193 ? . 2_645 H(15) H(6) 3.427 ? . 4_555 H(15) H(10) 2.810 ? . 3_555 H(15) H(14) 3.511 ? . 3_656 H(15) H(16) 3.362 ? . 3_656 H(15) H(17) 2.758 ? . 2_645 H(15) H(18) 2.694 ? . 2_645 H(15) H(21) 3.347 ? . 3_655 H(16) O(1) 3.470 ? . 4_555 H(16) C(8) 3.519 ? . 4_555 H(16) C(13) 3.053 ? . 4_555 H(16) C(18) 3.453 ? . 4_555 H(16) H(6) 2.700 ? . 4_555 H(16) H(10) 3.534 ? . 3_555 H(16) H(14) 3.491 ? . 3_656 H(16) H(15) 3.362 ? . 3_656 H(16) H(17) 2.575 ? . 4_555 H(16) H(20) 2.990 ? . 4_555 H(17) C(17) 3.587 ? . 2_655 H(17) C(17) 3.393 ? . 4_554 H(17) H(14) 3.595 ? . 2_655 H(17) H(14) 3.381 ? . 4_554 H(17) H(15) 2.758 ? . 2_655 H(17) H(16) 2.575 ? . 4_554 H(18) C(19) 3.484 ? . 4_555 H(18) H(9) 3.487 ? . 4_655 H(18) H(10) 3.186 ? . 4_655 H(18) H(15) 2.694 ? . 2_655 H(18) H(20) 3.247 ? . 4_555 H(18) H(21) 3.028 ? . 4_555 H(19) C(16) 3.387 ? . 3_655 H(19) H(8) 3.427 ? . 1_655 H(19) H(10) 3.098 ? . 1_655 H(19) H(12) 3.127 ? . 3_655 H(19) H(13) 2.770 ? . 3_655 H(20) Cl(1) 3.539 ? . 3_665 H(20) C(4) 3.566 ? . 4_554 H(20) C(5) 3.095 ? . 4_554 H(20) C(6) 3.515 ? . 4_554 H(20) C(17) 3.372 ? . 4_554 H(20) H(2) 3.000 ? . 4_554 H(20) H(5) 3.422 ? . 3_665 H(20) H(14) 2.953 ? . 4_554 H(20) H(16) 2.990 ? . 4_554 H(20) H(18) 3.247 ? . 4_554 H(21) C(5) 3.553 ? . 4_554 H(21) C(6) 3.352 ? . 4_554 H(21) C(9) 3.090 ? . 4_554 H(21) C(10) 3.560 ? . 4_554 H(21) C(16) 3.531 ? . 3_655 H(21) C(18) 3.577 ? . 4_554 H(21) H(3) 2.563 ? . 4_554 H(21) H(4) 3.446 ? . 4_554 H(21) H(12) 3.070 ? . 3_655 H(21) H(13) 3.287 ? . 3_655 H(21) H(15) 3.347 ? . 3_655 H(21) H(18) 3.028 ? . 4_554 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================