# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Takanori Suzuki' _publ_contact_author_address ; Division of Chemistry Hokkaido University Graduate School of Science Sapporo 060-0810 JAPAN ; _publ_contact_author_email TAK@SCI.HOKUDAI.AC.JP _publ_section_title ; First stable 7,7,8,8-tetraaryl-o-quinodimethane: Isolation, X-ray structure, electrochromic response of 9,10-bis(dianisylmethylene)-9,10-dihydrophenanthrene ; loop_ _publ_author_name 'Takanori Suzuki' 'Kenshu Fujiwara' 'Hiroki Higuchi' 'Shinichi Iwashita' 'Hidetoshi Kawai' 'Eisuke Ohta' 'Kazunori Ono' ; M.Takenaka ; data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 237042' _audit_creation_date 'Fri Dec 19 18:26:50 2003' _audit_creation_method 'by teXsan' _audit_update_record ? _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (2000). teXsan. Single Crystal Structure Analysis Software. Version 1.11. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C46 H38 Cl6 O4 ' _chemical_formula_moiety ? _chemical_formula_weight 867.52 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I -4 ' _symmetry_Int_Tables_number 82 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z y,-x,-z -y,x,-z 1/2+x,1/2+y,1/2+z 1/2-x,1/2-y,1/2+z 1/2+y,1/2-x,1/2-z 1/2-y,1/2+x,1/2-z _cell_length_a 27.728(4) _cell_length_b 27.728(4) _cell_length_c 11.005(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 8461.0(1) _cell_formula_units_Z 8 _cell_measurement_reflns_used 14524 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 29.6 _cell_measurement_temperature 123.2 #------------------------------------------------------------------------------ _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.449 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_max 0.914 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 31382 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_max 29.58 _diffrn_measured_fraction_theta_max 0.9221 _diffrn_reflns_theta_full 29.58 _diffrn_measured_fraction_theta_full 0.9221 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5751 _reflns_number_gt 3232 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0683 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3232 _refine_ls_number_parameters 509 _refine_ls_goodness_of_fit_ref 1.597 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0087 _refine_diff_density_max 0.45 _refine_diff_density_min -0.61 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack 0.07(8) 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 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Cl Cl 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl(1) Cl 0.28891(5) -0.13228(6) 0.6936(2) 0.0775(5) Uani 1.00 d . . . Cl(2) Cl 0.18811(4) -0.14253(4) 0.6294(1) 0.0481(3) Uani 1.00 d . . . Cl(3) Cl 0.21503(5) -0.12971(5) 0.8801(1) 0.0678(4) Uani 1.00 d . . . Cl(4) Cl 0.12732(9) 0.0596(1) -0.0010(3) 0.173(1) Uani 1.00 d . . . Cl(5) Cl 0.13211(9) 0.04893(9) 0.2536(2) 0.1335(9) Uani 1.00 d . . . Cl(6) Cl 0.0418 0.0642 0.1295 0.210(2) Uani 0.60 d P . . Cl(7) Cl 0.0675 0.1160 0.1413 0.197(2) Uani 0.40 d P . . O(1) O 0.1320(1) 0.1703(1) 0.8760(3) 0.0442(9) Uani 1.00 d . . . O(2) O 0.2703(1) 0.19543(10) 0.0991(2) 0.0355(8) Uani 1.00 d . . . O(3) O 0.13800(10) -0.0380(1) 0.4399(3) 0.0378(8) Uani 1.00 d . . . O(4) O 0.2832(1) -0.0427(1) 1.2435(3) 0.0368(8) Uani 1.00 d . . . C(1) C 0.4082(1) 0.0702(1) 0.6096(4) 0.0219(8) Uani 1.00 d . . . C(2) C 0.3656(1) 0.0723(1) 0.5397(4) 0.0206(8) Uani 1.00 d . . . C(3) C 0.3687(1) 0.0629(1) 0.4143(4) 0.0265(10) Uani 1.00 d . . . C(4) C 0.4125(2) 0.0533(1) 0.3594(4) 0.030(1) Uani 1.00 d . . . C(5) C 0.4541(1) 0.0527(1) 0.4280(4) 0.0318(10) Uani 1.00 d . . . C(6) C 0.4523(1) 0.0606(1) 0.5518(4) 0.0306(10) Uani 1.00 d . . . C(7) C 0.4055(1) 0.0786(1) 0.7433(4) 0.0229(9) Uani 1.00 d . . . C(8) C 0.3603(1) 0.0726(1) 0.8029(3) 0.0205(8) Uani 1.00 d . . . C(9) C 0.3580(1) 0.0822(1) 0.9272(4) 0.0251(9) Uani 1.00 d . . . C(10) C 0.3986(2) 0.0951(1) 0.9915(4) 0.029(1) Uani 1.00 d . . . C(11) C 0.4423(1) 0.0995(1) 0.9357(4) 0.0308(10) Uani 1.00 d . . . C(12) C 0.4457(1) 0.0916(1) 0.8112(4) 0.0279(10) Uani 1.00 d . . . C(13) C 0.3194(1) 0.0823(1) 0.6054(3) 0.0190(8) Uani 1.00 d . . . C(14) C 0.2845(1) 0.1121(1) 0.5674(3) 0.0192(9) Uani 1.00 d . . . C(15) C 0.2433(1) 0.1265(1) 0.6470(3) 0.0222(9) Uani 1.00 d . . . C(16) C 0.2514(1) 0.1420(1) 0.7666(4) 0.0242(10) Uani 1.00 d . . . C(17) C 0.2137(1) 0.1564(1) 0.8401(4) 0.030(1) Uani 1.00 d . . . C(18) C 0.1667(2) 0.1554(1) 0.7959(4) 0.0302(10) Uani 1.00 d . . . C(19) C 0.1578(1) 0.1405(1) 0.6786(4) 0.0267(10) Uani 1.00 d . . . C(20) C 0.1961(1) 0.1261(1) 0.6053(4) 0.0248(9) Uani 1.00 d . . . C(21) C 0.0828(2) 0.1676(2) 0.8375(5) 0.054(1) Uani 1.00 d . . . C(22) C 0.2827(1) 0.1344(1) 0.4436(3) 0.0208(9) Uani 1.00 d . . . C(23) C 0.2613(1) 0.1104(1) 0.3450(4) 0.029(1) Uani 1.00 d . . . C(24) C 0.2578(2) 0.1317(2) 0.2334(4) 0.031(1) Uani 1.00 d . . . C(25) C 0.2755(1) 0.1774(1) 0.2151(3) 0.0263(9) Uani 1.00 d . . . C(26) C 0.2964(2) 0.2020(1) 0.3094(4) 0.030(1) Uani 1.00 d . . . C(27) C 0.2998(1) 0.1802(1) 0.4236(4) 0.0267(10) Uani 1.00 d . . . C(28) C 0.2867(2) 0.2433(2) 0.0778(4) 0.047(1) Uani 1.00 d . . . C(29) C 0.3185(1) 0.0591(1) 0.7279(3) 0.0181(8) Uani 1.00 d . . . C(30) C 0.2837(1) 0.0277(1) 0.7620(3) 0.0184(9) Uani 1.00 d . . . C(31) C 0.2445(1) 0.0121(1) 0.6776(3) 0.0197(8) Uani 1.00 d . . . C(32) C 0.2545(1) -0.0040(1) 0.5603(4) 0.0230(9) Uani 1.00 d . . . C(33) C 0.2186(1) -0.0200(2) 0.4842(4) 0.031(1) Uani 1.00 d . . . C(34) C 0.1705(1) -0.0205(1) 0.5229(4) 0.0277(9) Uani 1.00 d . . . C(35) C 0.1594(1) -0.0052(1) 0.6388(4) 0.029(1) Uani 1.00 d . . . C(36) C 0.1967(1) 0.0112(1) 0.7143(4) 0.0267(10) Uani 1.00 d . . . C(37) C 0.0896(2) -0.0442(2) 0.4786(5) 0.045(1) Uani 1.00 d . . . C(38) C 0.2824(1) 0.0068(1) 0.8867(4) 0.0207(9) Uani 1.00 d . . . C(39) C 0.2530(1) 0.0266(1) 0.9772(4) 0.0225(9) Uani 1.00 d . . . C(40) C 0.2542(1) 0.0090(1) 1.0945(4) 0.028(1) Uani 1.00 d . . . C(41) C 0.2845(1) -0.0287(1) 1.1238(4) 0.0262(9) Uani 1.00 d . . . C(42) C 0.3128(1) -0.0495(1) 1.0358(4) 0.0256(10) Uani 1.00 d . . . C(43) C 0.3112(1) -0.0319(1) 0.9174(3) 0.0226(9) Uani 1.00 d . . . C(44) C 0.3186(2) -0.0746(2) 1.2840(4) 0.051(1) Uani 1.00 d . . . C(45) C 0.2301(2) -0.1156(2) 0.7284(4) 0.0370(10) Uani 1.00 d . . . C(46) C 0.1049(3) 0.0790(3) 0.131(1) 0.122(2) Uani 1.00 d . . . H(1) H 0.3399 0.0635 0.3659 0.0322 Uiso 1.00 calc . . . H(2) H 0.4141 0.0469 0.2747 0.0363 Uiso 1.00 calc . . . H(3) H 0.4844 0.0468 0.3899 0.0388 Uiso 1.00 calc . . . H(4) H 0.4813 0.0597 0.5983 0.0364 Uiso 1.00 calc . . . H(5) H 0.3278 0.0802 0.9677 0.0306 Uiso 1.00 calc . . . H(6) H 0.3963 0.1003 1.0761 0.0351 Uiso 1.00 calc . . . H(7) H 0.4700 0.1081 0.9809 0.0376 Uiso 1.00 calc . . . H(8) H 0.4761 0.0956 0.7719 0.0335 Uiso 1.00 calc . . . H(9) H 0.2832 0.1426 0.7979 0.0297 Uiso 1.00 calc . . . H(10) H 0.2202 0.1671 0.9206 0.0350 Uiso 1.00 calc . . . H(11) H 0.1256 0.1399 0.6477 0.0324 Uiso 1.00 calc . . . H(12) H 0.1898 0.1160 0.5243 0.0304 Uiso 1.00 calc . . . H(13) H 0.0621 0.1784 0.8999 0.0616 Uiso 1.00 calc . . . H(14) H 0.0780 0.1855 0.7659 0.0616 Uiso 1.00 calc . . . H(15) H 0.0751 0.1340 0.8207 0.0616 Uiso 1.00 calc . . . H(16) H 0.2492 0.0786 0.3567 0.0348 Uiso 1.00 calc . . . H(17) H 0.2433 0.1147 0.1677 0.0379 Uiso 1.00 calc . . . H(18) H 0.3077 0.2341 0.2974 0.0366 Uiso 1.00 calc . . . H(19) H 0.3147 0.1972 0.4887 0.0329 Uiso 1.00 calc . . . H(20) H 0.3201 0.2451 0.0946 0.0558 Uiso 1.00 calc . . . H(21) H 0.2812 0.2513 -0.0054 0.0558 Uiso 1.00 calc . . . H(22) H 0.2695 0.2649 0.1282 0.0558 Uiso 1.00 calc . . . H(23) H 0.2868 -0.0038 0.5322 0.0296 Uiso 1.00 calc . . . H(24) H 0.2265 -0.0315 0.4049 0.0358 Uiso 1.00 calc . . . H(25) H 0.1269 -0.0055 0.6674 0.0355 Uiso 1.00 calc . . . H(26) H 0.1891 0.0208 0.7945 0.0329 Uiso 1.00 calc . . . H(27) H 0.0773 -0.0136 0.5063 0.0544 Uiso 1.00 calc . . . H(28) H 0.0705 -0.0550 0.4129 0.0544 Uiso 1.00 calc . . . H(29) H 0.0883 -0.0665 0.5433 0.0544 Uiso 1.00 calc . . . H(30) H 0.2317 0.0527 0.9584 0.0276 Uiso 1.00 calc . . . H(31) H 0.2340 0.0224 1.1557 0.0347 Uiso 1.00 calc . . . H(32) H 0.3337 -0.0755 1.0556 0.0318 Uiso 1.00 calc . . . H(33) H 0.3301 -0.0470 0.8564 0.0289 Uiso 1.00 calc . . . H(34) H 0.3137 -0.0808 1.3682 0.0622 Uiso 1.00 calc . . . H(35) H 0.3162 -0.1038 1.2398 0.0622 Uiso 1.00 calc . . . H(36) H 0.3493 -0.0606 1.2721 0.0622 Uiso 1.00 calc . . . H(37) H 0.2275 -0.0819 0.7193 0.0436 Uiso 1.00 calc . . . H(38) H 0.1162 0.1226 0.1474 0.2193 Uiso 0.60 calc P . . H(39) H 0.1297 0.1036 0.1359 0.1411 Uiso 0.40 calc P . . 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) 0.0374(7) 0.0846(10) 0.111(1) 0.0123(7) -0.0033(8) -0.0483(9) Cl(2) 0.0432(6) 0.0535(7) 0.0477(7) -0.0033(6) -0.0087(6) -0.0102(6) Cl(3) 0.0822(10) 0.0834(10) 0.0379(7) -0.0302(8) -0.0091(7) 0.0168(8) Cl(4) 0.121(2) 0.250(3) 0.147(2) 0.090(2) 0.061(1) 0.104(2) Cl(5) 0.142(2) 0.139(2) 0.120(2) 0.062(1) 0.037(1) -0.003(2) Cl(6) 0.059(2) 0.377(5) 0.193(3) -0.019(2) 0.037(2) -0.212(3) Cl(7) 0.170(4) 0.238(4) 0.181(6) 0.158(3) 0.083(4) 0.068(5) O(1) 0.035(1) 0.069(2) 0.029(2) 0.021(1) 0.005(1) -0.008(2) O(2) 0.053(2) 0.033(1) 0.020(1) 0.002(1) -0.002(1) 0.007(1) O(3) 0.029(1) 0.050(2) 0.034(2) -0.013(1) -0.009(1) -0.008(2) O(4) 0.035(2) 0.058(2) 0.017(1) 0.009(1) 0.001(1) 0.010(1) C(1) 0.026(2) 0.013(2) 0.027(2) 0.000(2) 0.004(1) 0.006(2) C(2) 0.025(2) 0.014(2) 0.023(2) 0.001(2) 0.004(1) 0.006(2) C(3) 0.035(2) 0.024(2) 0.021(2) -0.001(2) 0.000(2) 0.006(2) C(4) 0.040(2) 0.024(2) 0.025(2) 0.004(2) 0.009(2) 0.006(2) C(5) 0.030(2) 0.027(2) 0.038(2) 0.006(2) 0.016(2) 0.008(2) C(6) 0.021(2) 0.031(2) 0.039(2) 0.001(2) 0.004(2) 0.008(2) C(7) 0.024(2) 0.020(2) 0.025(2) -0.004(2) 0.000(1) 0.009(2) C(8) 0.023(2) 0.016(2) 0.022(2) 0.000(2) -0.004(1) 0.007(2) C(9) 0.030(2) 0.023(2) 0.022(2) -0.004(2) 0.000(2) 0.004(2) C(10) 0.034(2) 0.031(2) 0.021(2) -0.005(2) -0.005(1) 0.003(2) C(11) 0.028(2) 0.029(2) 0.035(2) -0.006(2) -0.012(2) 0.003(2) C(12) 0.022(2) 0.027(2) 0.035(2) -0.003(2) -0.004(2) 0.009(2) C(13) 0.022(2) 0.019(2) 0.016(2) -0.008(1) 0.001(1) -0.001(1) C(14) 0.025(2) 0.016(2) 0.017(2) -0.005(1) -0.002(1) -0.002(1) C(15) 0.027(2) 0.020(2) 0.019(2) 0.002(2) -0.002(1) 0.004(2) C(16) 0.028(2) 0.022(2) 0.023(2) 0.003(2) -0.006(2) -0.003(2) C(17) 0.039(2) 0.033(2) 0.017(2) 0.006(2) 0.000(2) -0.007(2) C(18) 0.036(2) 0.031(2) 0.024(2) 0.010(2) 0.005(1) 0.000(2) C(19) 0.025(2) 0.030(2) 0.025(2) 0.005(2) -0.003(2) -0.001(2) C(20) 0.027(2) 0.026(2) 0.022(2) 0.005(2) -0.004(1) 0.000(2) C(21) 0.035(2) 0.084(4) 0.042(3) 0.026(3) 0.005(2) 0.001(3) C(22) 0.022(2) 0.025(2) 0.016(2) 0.006(1) 0.000(2) 0.001(1) C(23) 0.039(2) 0.022(2) 0.024(2) -0.010(2) -0.008(2) 0.005(2) C(24) 0.040(2) 0.034(2) 0.020(2) -0.006(2) -0.006(2) 0.001(2) C(25) 0.031(2) 0.029(2) 0.019(2) 0.005(2) 0.000(2) 0.006(1) C(26) 0.044(2) 0.018(2) 0.028(2) -0.005(2) 0.002(2) 0.004(2) C(27) 0.033(2) 0.024(2) 0.023(2) 0.002(2) -0.001(2) -0.003(2) C(28) 0.077(3) 0.036(2) 0.030(3) 0.000(2) -0.004(3) 0.015(2) C(29) 0.019(2) 0.017(2) 0.019(2) 0.002(1) 0.000(1) 0.002(1) C(30) 0.017(2) 0.020(2) 0.018(2) 0.004(1) 0.001(1) 0.001(1) C(31) 0.022(2) 0.017(2) 0.021(2) -0.004(2) -0.001(1) -0.001(2) C(32) 0.023(2) 0.023(2) 0.022(2) -0.003(2) 0.002(2) -0.002(2) C(33) 0.031(2) 0.038(2) 0.022(2) -0.009(2) 0.001(2) -0.010(2) C(34) 0.029(2) 0.028(2) 0.026(2) -0.005(2) -0.004(1) -0.001(2) C(35) 0.021(2) 0.034(2) 0.031(2) 0.002(2) 0.000(2) -0.007(2) C(36) 0.025(2) 0.034(2) 0.022(2) -0.002(2) 0.002(2) -0.006(2) C(37) 0.029(2) 0.058(3) 0.048(3) -0.001(2) -0.009(2) -0.007(3) C(38) 0.019(2) 0.023(2) 0.020(2) -0.002(1) 0.002(2) 0.003(1) C(39) 0.022(2) 0.023(2) 0.022(2) 0.005(2) 0.000(2) 0.000(2) C(40) 0.028(2) 0.033(2) 0.021(2) 0.002(2) 0.006(2) 0.000(2) C(41) 0.025(2) 0.038(2) 0.016(1) -0.002(2) 0.001(2) 0.002(2) C(42) 0.025(2) 0.031(2) 0.020(2) 0.008(2) 0.000(2) 0.004(2) C(43) 0.022(2) 0.026(2) 0.019(2) 0.002(1) 0.004(2) 0.001(2) C(44) 0.049(3) 0.074(3) 0.030(3) 0.022(2) 0.001(2) 0.022(2) C(45) 0.039(2) 0.034(2) 0.039(2) 0.002(2) -0.001(2) 0.000(2) C(46) 0.086(3) 0.126(6) 0.155(3) -0.021(3) -0.023(4) 0.006(5) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl(1) C(45) 1.738(6) . . yes Cl(2) C(45) 1.761(6) . . yes Cl(3) C(45) 1.765(6) . . yes Cl(4) C(46) 1.67(1) . . yes Cl(5) C(46) 1.75(1) . . yes Cl(6) Cl(7) 1.609 . . yes Cl(6) C(46) 1.797(9) . . yes Cl(7) C(46) 1.46(1) . . yes O(1) C(18) 1.370(6) . . yes O(1) C(21) 1.430(7) . . yes O(2) C(25) 1.379(6) . . yes O(2) C(28) 1.422(7) . . yes O(3) C(34) 1.372(6) . . yes O(3) C(37) 1.419(7) . . yes O(4) C(41) 1.373(6) . . yes O(4) C(44) 1.397(7) . . yes C(1) C(2) 1.411(7) . . yes C(1) C(6) 1.405(7) . . yes C(1) C(7) 1.491(7) . . yes C(2) C(3) 1.407(7) . . yes C(2) C(13) 1.497(7) . . yes C(3) C(4) 1.383(7) . . yes C(4) C(5) 1.379(7) . . yes C(5) C(6) 1.382(8) . . yes C(7) C(8) 1.423(7) . . yes C(7) C(12) 1.390(7) . . yes C(8) C(9) 1.395(7) . . yes C(8) C(29) 1.471(6) . . yes C(9) C(10) 1.378(7) . . yes C(10) C(11) 1.363(7) . . yes C(11) C(12) 1.390(7) . . yes C(13) C(14) 1.338(6) . . yes C(13) C(29) 1.493(7) . . yes C(14) C(15) 1.495(7) . . yes C(14) C(22) 1.496(7) . . yes C(15) C(16) 1.403(7) . . yes C(15) C(20) 1.388(7) . . yes C(16) C(17) 1.381(7) . . yes C(17) C(18) 1.393(7) . . yes C(18) C(19) 1.378(7) . . yes C(19) C(20) 1.392(7) . . yes C(22) C(23) 1.405(7) . . yes C(22) C(27) 1.375(7) . . yes C(23) C(24) 1.365(7) . . yes C(24) C(25) 1.373(7) . . yes C(25) C(26) 1.370(7) . . yes C(26) C(27) 1.397(7) . . yes C(29) C(30) 1.353(6) . . yes C(30) C(31) 1.496(6) . . yes C(30) C(38) 1.490(7) . . yes C(31) C(32) 1.393(7) . . yes C(31) C(36) 1.385(7) . . yes C(32) C(33) 1.374(7) . . yes C(33) C(34) 1.402(7) . . yes C(34) C(35) 1.379(8) . . yes C(35) C(36) 1.403(7) . . yes C(38) C(39) 1.400(7) . . yes C(38) C(43) 1.380(6) . . yes C(39) C(40) 1.381(7) . . yes C(40) C(41) 1.380(7) . . yes C(41) C(42) 1.374(7) . . yes C(42) C(43) 1.392(7) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(7) Cl(6) C(46) 50.5(3) . . . yes Cl(6) Cl(7) C(46) 71.5(4) . . . yes C(18) O(1) C(21) 117.6(4) . . . yes C(25) O(2) C(28) 117.3(4) . . . yes C(34) O(3) C(37) 117.6(4) . . . yes C(41) O(4) C(44) 117.7(4) . . . yes C(2) C(1) C(6) 119.4(5) . . . yes C(2) C(1) C(7) 119.4(4) . . . yes C(6) C(1) C(7) 121.3(5) . . . yes C(1) C(2) C(3) 118.5(5) . . . yes C(1) C(2) C(13) 117.4(4) . . . yes C(3) C(2) C(13) 124.1(4) . . . yes C(2) C(3) C(4) 121.2(5) . . . yes C(3) C(4) C(5) 120.0(5) . . . yes C(4) C(5) C(6) 120.5(5) . . . yes C(1) C(6) C(5) 120.6(5) . . . yes C(1) C(7) C(8) 118.7(4) . . . yes C(1) C(7) C(12) 122.1(5) . . . yes C(8) C(7) C(12) 119.2(5) . . . yes C(7) C(8) C(9) 118.1(4) . . . yes C(7) C(8) C(29) 117.7(4) . . . yes C(9) C(8) C(29) 124.1(5) . . . yes C(8) C(9) C(10) 121.0(5) . . . yes C(9) C(10) C(11) 121.2(5) . . . yes C(10) C(11) C(12) 119.5(5) . . . yes C(7) C(12) C(11) 121.0(5) . . . yes C(2) C(13) C(14) 125.5(4) . . . yes C(2) C(13) C(29) 111.8(4) . . . yes C(14) C(13) C(29) 122.4(4) . . . yes C(13) C(14) C(15) 122.3(4) . . . yes C(13) C(14) C(22) 124.3(4) . . . yes C(15) C(14) C(22) 113.4(4) . . . yes C(14) C(15) C(16) 120.6(4) . . . yes C(14) C(15) C(20) 121.7(4) . . . yes C(16) C(15) C(20) 117.6(5) . . . yes C(15) C(16) C(17) 121.1(5) . . . yes C(16) C(17) C(18) 119.9(5) . . . yes O(1) C(18) C(17) 115.3(5) . . . yes O(1) C(18) C(19) 124.6(5) . . . yes C(17) C(18) C(19) 120.1(5) . . . yes C(18) C(19) C(20) 119.5(5) . . . yes C(15) C(20) C(19) 121.8(5) . . . yes C(14) C(22) C(23) 121.5(4) . . . yes C(14) C(22) C(27) 121.1(4) . . . yes C(23) C(22) C(27) 117.3(4) . . . yes C(22) C(23) C(24) 121.4(4) . . . yes C(23) C(24) C(25) 120.3(5) . . . yes O(2) C(25) C(24) 115.7(4) . . . yes O(2) C(25) C(26) 124.4(4) . . . yes C(24) C(25) C(26) 119.9(5) . . . yes C(25) C(26) C(27) 119.7(4) . . . yes C(22) C(27) C(26) 121.3(5) . . . yes C(8) C(29) C(13) 112.7(4) . . . yes C(8) C(29) C(30) 124.7(4) . . . yes C(13) C(29) C(30) 122.6(4) . . . yes C(29) C(30) C(31) 122.2(4) . . . yes C(29) C(30) C(38) 121.6(4) . . . yes C(31) C(30) C(38) 116.2(4) . . . yes C(30) C(31) C(32) 121.5(4) . . . yes C(30) C(31) C(36) 121.3(4) . . . yes C(32) C(31) C(36) 117.1(4) . . . yes C(31) C(32) C(33) 121.6(4) . . . yes C(32) C(33) C(34) 120.4(5) . . . yes O(3) C(34) C(33) 115.2(5) . . . yes O(3) C(34) C(35) 125.3(5) . . . yes C(33) C(34) C(35) 119.5(5) . . . yes C(34) C(35) C(36) 118.9(5) . . . yes C(31) C(36) C(35) 122.5(5) . . . yes C(30) C(38) C(39) 121.1(4) . . . yes C(30) C(38) C(43) 120.9(4) . . . yes C(39) C(38) C(43) 118.0(4) . . . yes C(38) C(39) C(40) 120.7(4) . . . yes C(39) C(40) C(41) 120.1(5) . . . yes O(4) C(41) C(40) 114.9(4) . . . yes O(4) C(41) C(42) 125.0(5) . . . yes C(40) C(41) C(42) 120.1(5) . . . yes C(41) C(42) C(43) 119.7(4) . . . yes C(38) C(43) C(42) 121.4(4) . . . yes Cl(1) C(45) Cl(2) 111.8(3) . . . yes Cl(1) C(45) Cl(3) 111.8(3) . . . yes Cl(2) C(45) Cl(3) 109.5(3) . . . yes Cl(4) C(46) Cl(5) 110.8(6) . . . yes Cl(4) C(46) Cl(6) 106.3(6) . . . yes Cl(4) C(46) Cl(7) 123.7(9) . . . yes Cl(5) C(46) Cl(6) 108.6(6) . . . yes Cl(5) C(46) Cl(7) 125.5(9) . . . yes Cl(6) C(46) Cl(7) 58.1(3) . . . yes #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl(4) C(46) Cl(6) Cl(7) -120.0(8) . . . . yes Cl(4) C(46) Cl(7) Cl(6) 88.9(7) . . . . yes Cl(5) C(46) Cl(6) Cl(7) 120.8(9) . . . . yes Cl(5) C(46) Cl(7) Cl(6) -91.0(7) . . . . yes O(1) C(18) C(17) C(16) 180.0(5) . . . . yes O(1) C(18) C(19) C(20) 180.0(5) . . . . yes O(2) C(25) C(24) C(23) 179.8(5) . . . . yes O(2) C(25) C(26) C(27) -180.0(5) . . . . yes O(3) C(34) C(33) C(32) -178.9(5) . . . . yes O(3) C(34) C(35) C(36) 179.0(5) . . . . yes O(4) C(41) C(40) C(39) 179.0(5) . . . . yes O(4) C(41) C(42) C(43) -179.8(5) . . . . yes C(1) C(2) C(3) C(4) -2.0(7) . . . . yes C(1) C(2) C(13) C(14) 137.5(5) . . . . yes C(1) C(2) C(13) C(29) -36.0(5) . . . . yes C(1) C(6) C(5) C(4) -1.2(8) . . . . yes C(1) C(7) C(8) C(9) -177.8(4) . . . . yes C(1) C(7) C(8) C(29) -1.1(6) . . . . yes C(1) C(7) C(12) C(11) 179.7(5) . . . . yes C(2) C(1) C(6) C(5) -0.7(7) . . . . yes C(2) C(1) C(7) C(8) 20.7(6) . . . . yes C(2) C(1) C(7) C(12) -160.0(4) . . . . yes C(2) C(3) C(4) C(5) 0.1(7) . . . . yes C(2) C(13) C(14) C(15) -169.6(4) . . . . yes C(2) C(13) C(14) C(22) 10.0(7) . . . . yes C(2) C(13) C(29) C(8) 54.4(5) . . . . yes C(2) C(13) C(29) C(30) -122.9(5) . . . . yes C(3) C(2) C(1) C(6) 2.3(7) . . . . yes C(3) C(2) C(1) C(7) -178.2(4) . . . . yes C(3) C(2) C(13) C(14) -45.4(7) . . . . yes C(3) C(2) C(13) C(29) 141.2(5) . . . . yes C(3) C(4) C(5) C(6) 1.5(8) . . . . yes C(4) C(3) C(2) C(13) -179.1(4) . . . . yes C(5) C(6) C(1) C(7) 179.7(5) . . . . yes C(6) C(1) C(2) C(13) 179.5(4) . . . . yes C(6) C(1) C(7) C(8) -159.8(4) . . . . yes C(6) C(1) C(7) C(12) 19.6(7) . . . . yes C(7) C(1) C(2) C(13) -0.9(6) . . . . yes C(7) C(8) C(9) C(10) -2.8(7) . . . . yes C(7) C(8) C(29) C(13) -36.2(6) . . . . yes C(7) C(8) C(29) C(30) 141.0(5) . . . . yes C(7) C(12) C(11) C(10) -1.1(8) . . . . yes C(8) C(7) C(12) C(11) -1.0(7) . . . . yes C(8) C(9) C(10) C(11) 0.8(8) . . . . yes C(8) C(29) C(13) C(14) -119.3(5) . . . . yes C(8) C(29) C(30) C(31) -174.4(4) . . . . yes C(8) C(29) C(30) C(38) 5.8(7) . . . . yes C(9) C(8) C(7) C(12) 2.8(7) . . . . yes C(9) C(8) C(29) C(13) 140.4(5) . . . . yes C(9) C(8) C(29) C(30) -42.4(7) . . . . yes C(9) C(10) C(11) C(12) 1.2(8) . . . . yes C(10) C(9) C(8) C(29) -179.3(4) . . . . yes C(12) C(7) C(8) C(29) 179.6(4) . . . . yes C(13) C(14) C(15) C(16) 47.6(6) . . . . yes C(13) C(14) C(15) C(20) -134.0(5) . . . . yes C(13) C(14) C(22) C(23) 86.8(6) . . . . yes C(13) C(14) C(22) C(27) -96.6(6) . . . . yes C(13) C(29) C(30) C(31) 2.6(7) . . . . yes C(13) C(29) C(30) C(38) -177.2(4) . . . . yes C(14) C(13) C(29) C(30) 63.4(6) . . . . yes C(14) C(15) C(16) C(17) 178.6(4) . . . . yes C(14) C(15) C(20) C(19) -178.7(4) . . . . yes C(14) C(22) C(23) C(24) 177.1(5) . . . . yes C(14) C(22) C(27) C(26) -177.3(5) . . . . yes C(15) C(14) C(13) C(29) 3.2(7) . . . . yes C(15) C(14) C(22) C(23) -93.5(5) . . . . yes C(15) C(14) C(22) C(27) 83.0(6) . . . . yes C(15) C(16) C(17) C(18) 0.2(8) . . . . yes C(15) C(20) C(19) C(18) -0.1(8) . . . . yes C(16) C(15) C(14) C(22) -132.1(5) . . . . yes C(16) C(15) C(20) C(19) -0.2(7) . . . . yes C(16) C(17) C(18) C(19) -0.4(8) . . . . yes C(17) C(16) C(15) C(20) 0.1(7) . . . . yes C(17) C(18) O(1) C(21) -176.7(5) . . . . yes C(17) C(18) C(19) C(20) 0.4(8) . . . . yes C(19) C(18) O(1) C(21) 3.7(8) . . . . yes C(20) C(15) C(14) C(22) 46.4(6) . . . . yes C(22) C(14) C(13) C(29) -177.2(4) . . . . yes C(22) C(23) C(24) C(25) 0.1(8) . . . . yes C(22) C(27) C(26) C(25) 0.1(8) . . . . yes C(23) C(22) C(27) C(26) -0.6(8) . . . . yes C(23) C(24) C(25) C(26) -0.6(8) . . . . yes C(24) C(23) C(22) C(27) 0.5(8) . . . . yes C(24) C(25) O(2) C(28) 177.8(5) . . . . yes C(24) C(25) C(26) C(27) 0.5(8) . . . . yes C(26) C(25) O(2) C(28) -1.8(7) . . . . yes C(29) C(30) C(31) C(32) 49.0(7) . . . . yes C(29) C(30) C(31) C(36) -133.3(5) . . . . yes C(29) C(30) C(38) C(39) 97.0(6) . . . . yes C(29) C(30) C(38) C(43) -81.2(6) . . . . yes C(30) C(31) C(32) C(33) 177.6(5) . . . . yes C(30) C(31) C(36) C(35) -177.2(5) . . . . yes C(30) C(38) C(39) C(40) -175.9(4) . . . . yes C(30) C(38) C(43) C(42) 175.2(4) . . . . yes C(31) C(30) C(38) C(39) -82.8(5) . . . . yes C(31) C(30) C(38) C(43) 99.0(5) . . . . yes C(31) C(32) C(33) C(34) 0.3(8) . . . . yes C(31) C(36) C(35) C(34) -1.0(8) . . . . yes C(32) C(31) C(30) C(38) -131.2(5) . . . . yes C(32) C(31) C(36) C(35) 0.5(7) . . . . yes C(32) C(33) C(34) C(35) -0.8(8) . . . . yes C(33) C(32) C(31) C(36) -0.2(7) . . . . yes C(33) C(34) O(3) C(37) 173.3(5) . . . . yes C(33) C(34) C(35) C(36) 1.1(8) . . . . yes C(35) C(34) O(3) C(37) -4.6(7) . . . . yes C(36) C(31) C(30) C(38) 46.5(6) . . . . yes C(38) C(39) C(40) C(41) -0.2(8) . . . . yes C(38) C(43) C(42) C(41) 1.6(7) . . . . yes C(39) C(38) C(43) C(42) -3.2(7) . . . . yes C(39) C(40) C(41) C(42) -1.4(8) . . . . yes C(40) C(39) C(38) C(43) 2.4(7) . . . . yes C(40) C(41) O(4) C(44) -169.2(5) . . . . yes C(40) C(41) C(42) C(43) 0.7(7) . . . . yes C(42) C(41) O(4) C(44) 11.3(8) . . . . yes C(42) C(41) O(4) C(44) 11.3(8) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(2) C(20) 3.439(5) . 3_556 ? Cl(2) C(28) 3.560(6) . 8_545 ? Cl(3) O(1) 2.957(4) . 3_557 ? Cl(3) Cl(7) 3.250(2) . 3_556 ? Cl(4) O(1) 3.357(5) . 1_554 ? Cl(5) O(3) 3.170(5) . . ? Cl(7) C(35) 3.207(5) . 4_556 ? Cl(7) C(36) 3.506(5) . 4_556 ? O(2) C(17) 3.429(6) . 1_554 ? O(3) C(21) 3.396(8) . 3_556 ? O(3) C(19) 3.568(6) . 3_556 ? O(4) C(33) 3.257(6) . 1_556 ? O(4) C(21) 3.507(8) . 3_557 ? C(1) C(12) 3.561(6) . 8_546 ? C(1) C(11) 3.590(7) . 8_546 ? C(6) C(11) 3.585(7) . 8_546 ? C(6) C(43) 3.598(7) . 7_556 ? C(10) C(44) 3.519(8) . 7_557 ? C(21) C(40) 3.577(8) . 4_557 ? C(21) C(41) 3.597(8) . 4_557 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_COMPOUND_2 _database_code_depnum_ccdc_archive 'CCDC 237043' _audit_creation_date 'Tue Jun 3 13:29:25 2003' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C44 H38 O4 ' _chemical_formula_moiety 'C44 H38 O4 ' _chemical_formula_weight 630.78 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21/b 21/c 21/a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-y,1/2+z -x,-y,-z 1/2-x,1/2+y,z x,1/2-y,1/2+z 1/2+x,y,1/2-z _cell_length_a 10.1566(7) _cell_length_b 18.671(1) _cell_length_c 35.302(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6694.5(8) _cell_formula_units_Z 8 _cell_measurement_reflns_used 16997 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.996 _exptl_absorpt_correction_T_max 0.996 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.62 _diffrn_reflns_number 352 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9652 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9652 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7406 _reflns_number_gt 4939 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0514 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4939 _refine_ls_number_parameters 433 _refine_ls_goodness_of_fit_ref 1.263 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_shift/su_max 0.0044 _refine_diff_density_max 0.25 _refine_diff_density_min -0.19 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 1.4153(1) 0.10140(7) 0.26403(4) 0.0337(4) Uani 1.00 d . . . O(2) O 1.5026(1) 0.44726(7) 0.06588(4) 0.0352(4) Uani 1.00 d . . . O(3) O 1.0106(1) 0.62309(7) 0.02736(4) 0.0346(4) Uani 1.00 d . . . O(4) O 1.0135(2) 0.39452(8) 0.28403(4) 0.0455(4) Uani 1.00 d . . . C(1) C 0.9004(2) 0.19865(8) 0.07536(5) 0.0198(4) Uani 1.00 d . . . C(2) C 1.0392(2) 0.19408(8) 0.07650(5) 0.0201(4) Uani 1.00 d . . . C(3) C 1.1090(2) 0.19117(9) 0.04227(5) 0.0238(4) Uani 1.00 d . . . C(4) C 1.0440(2) 0.19242(9) 0.00787(5) 0.0276(5) Uani 1.00 d . . . C(5) C 0.9078(2) 0.19773(10) 0.00681(5) 0.0297(5) Uani 1.00 d . . . C(6) C 0.8372(2) 0.20061(9) 0.04034(5) 0.0256(4) Uani 1.00 d . . . C(7) C 0.8216(1) 0.20228(9) 0.11117(5) 0.0199(4) Uani 1.00 d . . . C(8) C 0.8033(1) 0.26813(8) 0.12983(5) 0.0195(4) Uani 1.00 d . . . C(9) C 0.7289(2) 0.26965(9) 0.16326(5) 0.0242(4) Uani 1.00 d . . . C(10) C 0.6734(2) 0.20787(10) 0.17781(5) 0.0274(5) Uani 1.00 d . . . C(11) C 0.6892(2) 0.14354(10) 0.15893(6) 0.0303(5) Uani 1.00 d . . . C(12) C 0.7633(2) 0.14053(9) 0.12597(5) 0.0271(4) Uani 1.00 d . . . C(13) C 1.1061(2) 0.18374(9) 0.11309(5) 0.0213(4) Uani 1.00 d . . . C(14) C 1.2189(1) 0.21306(9) 0.12616(5) 0.0197(4) Uani 1.00 d . . . C(15) C 1.2745(1) 0.18501(9) 0.16223(5) 0.0200(4) Uani 1.00 d . . . C(16) C 1.2817(2) 0.11138(9) 0.16926(5) 0.0217(4) Uani 1.00 d . . . C(17) C 1.3303(2) 0.08500(9) 0.20329(5) 0.0241(4) Uani 1.00 d . . . C(18) C 1.3704(2) 0.13230(10) 0.23142(5) 0.0238(4) Uani 1.00 d . . . C(19) C 1.3640(2) 0.20570(9) 0.22516(5) 0.0235(4) Uani 1.00 d . . . C(20) C 1.3188(2) 0.23117(9) 0.19057(5) 0.0230(4) Uani 1.00 d . . . C(21) C 1.4854(2) 0.1467(1) 0.28948(5) 0.0339(5) Uani 1.00 d . . . C(22) C 1.2890(2) 0.27424(9) 0.10845(4) 0.0197(4) Uani 1.00 d . . . C(23) C 1.2229(2) 0.33475(9) 0.09575(5) 0.0214(4) Uani 1.00 d . . . C(24) C 1.2892(2) 0.39409(9) 0.08157(5) 0.0233(4) Uani 1.00 d . . . C(25) C 1.4262(2) 0.39267(9) 0.07960(5) 0.0235(4) Uani 1.00 d . . . C(26) C 1.4939(2) 0.33257(10) 0.09209(5) 0.0257(4) Uani 1.00 d . . . C(27) C 1.4274(2) 0.27443(9) 0.10639(5) 0.0235(4) Uani 1.00 d . . . C(28) C 1.4388(2) 0.5104(1) 0.05327(7) 0.0470(7) Uani 1.00 d . . . C(29) C 0.8479(2) 0.33482(9) 0.11146(5) 0.0203(4) Uani 1.00 d . . . C(30) C 0.8886(1) 0.39624(8) 0.12768(5) 0.0205(4) Uani 1.00 d . . . C(31) C 0.9099(2) 0.46000(8) 0.10305(5) 0.0204(4) Uani 1.00 d . . . C(32) C 0.8320(2) 0.47271(9) 0.07136(5) 0.0234(4) Uani 1.00 d . . . C(33) C 0.8610(2) 0.52679(9) 0.04563(5) 0.0252(4) Uani 1.00 d . . . C(34) C 0.9703(2) 0.57019(9) 0.05172(5) 0.0252(4) Uani 1.00 d . . . C(35) C 1.0451(2) 0.56136(9) 0.08424(5) 0.0269(5) Uani 1.00 d . . . C(36) C 1.0149(2) 0.50718(9) 0.10959(5) 0.0246(4) Uani 1.00 d . . . C(37) C 0.9532(2) 0.62391(10) -0.00933(5) 0.0335(5) Uani 1.00 d . . . C(38) C 0.9224(2) 0.40056(9) 0.16870(5) 0.0221(4) Uani 1.00 d . . . C(39) C 1.0171(2) 0.35452(10) 0.18402(5) 0.0271(5) Uani 1.00 d . . . C(40) C 1.0465(2) 0.3547(1) 0.22221(5) 0.0322(5) Uani 1.00 d . . . C(41) C 0.9805(2) 0.40074(10) 0.24643(5) 0.0311(5) Uani 1.00 d . . . C(42) C 0.8880(2) 0.44793(10) 0.23207(5) 0.0342(5) Uani 1.00 d . . . C(43) C 0.8605(2) 0.44771(9) 0.19326(5) 0.0289(5) Uani 1.00 d . . . C(44) C 0.9464(3) 0.4388(1) 0.31027(6) 0.0630(8) Uani 1.00 d . . . H(1) H 1.2037 0.1886 0.0429 0.0295 Uiso 1.00 calc . . . H(2) H 1.0933 0.1890 -0.0152 0.0355 Uiso 1.00 calc . . . H(3) H 0.8622 0.1994 -0.0168 0.0377 Uiso 1.00 calc . . . H(4) H 0.7425 0.2043 0.0396 0.0325 Uiso 1.00 calc . . . H(5) H 0.7174 0.3144 0.1767 0.0317 Uiso 1.00 calc . . . H(6) H 0.6248 0.2095 0.2011 0.0349 Uiso 1.00 calc . . . H(7) H 0.6481 0.1011 0.1690 0.0382 Uiso 1.00 calc . . . H(8) H 0.7748 0.0960 0.1132 0.0339 Uiso 1.00 calc . . . H(9) H 1.0631 0.1511 0.1301 0.0277 Uiso 1.00 calc . . . H(10) H 1.2519 0.0780 0.1504 0.0282 Uiso 1.00 calc . . . H(11) H 1.3365 0.0346 0.2072 0.0304 Uiso 1.00 calc . . . H(12) H 1.3915 0.2385 0.2444 0.0294 Uiso 1.00 calc . . . H(13) H 1.3181 0.2816 0.1860 0.0299 Uiso 1.00 calc . . . H(14) H 1.5131 0.1209 0.3112 0.0431 Uiso 1.00 calc . . . H(15) H 1.5615 0.1662 0.2771 0.0431 Uiso 1.00 calc . . . H(16) H 1.4306 0.1856 0.2972 0.0431 Uiso 1.00 calc . . . H(17) H 1.1282 0.3351 0.0965 0.0267 Uiso 1.00 calc . . . H(18) H 1.2421 0.4362 0.0732 0.0295 Uiso 1.00 calc . . . H(19) H 1.5884 0.3316 0.0904 0.0325 Uiso 1.00 calc . . . H(20) H 1.4754 0.2337 0.1152 0.0300 Uiso 1.00 calc . . . H(21) H 1.5007 0.5443 0.0444 0.0600 Uiso 1.00 calc . . . H(22) H 1.3792 0.4989 0.0329 0.0600 Uiso 1.00 calc . . . H(23) H 1.3884 0.5311 0.0733 0.0600 Uiso 1.00 calc . . . H(24) H 0.8485 0.3344 0.0841 0.0264 Uiso 1.00 calc . . . H(25) H 0.7564 0.4428 0.0673 0.0298 Uiso 1.00 calc . . . H(26) H 0.8062 0.5344 0.0237 0.0322 Uiso 1.00 calc . . . H(27) H 1.1175 0.5931 0.0893 0.0346 Uiso 1.00 calc . . . H(28) H 1.0666 0.5015 0.1324 0.0316 Uiso 1.00 calc . . . H(29) H 0.8597 0.6301 -0.0076 0.0427 Uiso 1.00 calc . . . H(30) H 0.9880 0.6628 -0.0240 0.0427 Uiso 1.00 calc . . . H(31) H 0.9706 0.5803 -0.0224 0.0427 Uiso 1.00 calc . . . H(32) H 1.0627 0.3217 0.1676 0.0335 Uiso 1.00 calc . . . H(33) H 1.1130 0.3233 0.2324 0.0396 Uiso 1.00 calc . . . H(34) H 0.8432 0.4805 0.2488 0.0420 Uiso 1.00 calc . . . H(35) H 0.7981 0.4816 0.1834 0.0363 Uiso 1.00 calc . . . H(36) H 0.9756 0.4305 0.3353 0.0790 Uiso 1.00 calc . . . H(37) H 0.9573 0.4880 0.3041 0.0790 Uiso 1.00 calc . . . H(38) H 0.8526 0.4284 0.3093 0.0790 Uiso 1.00 calc . . . 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 O(1) 0.0400(7) 0.0384(7) 0.0228(7) 0.0028(6) -0.0112(6) 0.0045(6) O(2) 0.0283(7) 0.0283(7) 0.0491(9) -0.0062(6) 0.0017(6) 0.0108(6) O(3) 0.0441(8) 0.0275(7) 0.0321(7) -0.0087(6) -0.0030(6) 0.0120(6) O(4) 0.0653(10) 0.0475(9) 0.0237(7) 0.0066(8) -0.0028(7) -0.0003(6) C(1) 0.0252(8) 0.0141(7) 0.0200(8) -0.0026(7) -0.0036(7) -0.0015(6) C(2) 0.0242(8) 0.0152(7) 0.0208(8) -0.0020(6) -0.0038(7) 0.0012(6) C(3) 0.0269(8) 0.0219(8) 0.0226(9) -0.0017(7) -0.0012(7) 0.0013(7) C(4) 0.0379(10) 0.0262(9) 0.0188(9) -0.0034(8) 0.0008(8) -0.0005(7) C(5) 0.038(1) 0.0300(10) 0.0209(9) -0.0023(8) -0.0106(8) -0.0016(8) C(6) 0.0270(9) 0.0247(9) 0.0249(9) -0.0004(7) -0.0071(7) -0.0026(7) C(7) 0.0170(7) 0.0213(8) 0.0214(8) -0.0014(6) -0.0060(7) 0.0010(7) C(8) 0.0157(7) 0.0203(8) 0.0224(8) -0.0013(6) -0.0030(6) 0.0015(7) C(9) 0.0197(8) 0.0243(9) 0.0284(9) 0.0013(7) 0.0007(7) 0.0009(7) C(10) 0.0200(8) 0.035(1) 0.0276(9) -0.0022(7) 0.0020(7) 0.0058(8) C(11) 0.0279(9) 0.0284(10) 0.035(1) -0.0084(8) -0.0031(8) 0.0088(8) C(12) 0.0307(9) 0.0211(9) 0.0297(9) -0.0050(7) -0.0046(8) 0.0005(8) C(13) 0.0214(8) 0.0231(9) 0.0194(8) -0.0016(7) -0.0002(7) 0.0025(7) C(14) 0.0185(8) 0.0236(8) 0.0172(8) 0.0033(6) 0.0006(7) -0.0002(7) C(15) 0.0155(7) 0.0267(9) 0.0178(8) 0.0010(7) 0.0019(6) 0.0016(7) C(16) 0.0197(8) 0.0267(9) 0.0188(8) 0.0011(7) 0.0003(6) -0.0025(7) C(17) 0.0236(8) 0.0248(9) 0.0239(9) 0.0016(7) -0.0002(7) 0.0024(7) C(18) 0.0201(8) 0.0348(10) 0.0164(8) 0.0019(7) -0.0011(7) 0.0043(7) C(19) 0.0213(8) 0.0303(9) 0.0189(8) -0.0012(7) -0.0020(7) -0.0022(7) C(20) 0.0210(8) 0.0246(9) 0.0235(9) -0.0014(7) -0.0009(7) 0.0015(7) C(21) 0.0293(9) 0.050(1) 0.0220(9) 0.0047(9) -0.0092(8) 0.0000(9) C(22) 0.0196(8) 0.0241(8) 0.0154(7) -0.0005(7) -0.0016(6) -0.0005(7) C(23) 0.0171(8) 0.0262(9) 0.0210(8) 0.0002(7) -0.0009(7) -0.0007(7) C(24) 0.0250(8) 0.0217(8) 0.0233(9) 0.0025(7) -0.0014(7) 0.0007(7) C(25) 0.0248(8) 0.0253(9) 0.0204(8) -0.0046(7) 0.0005(7) -0.0001(7) C(26) 0.0172(8) 0.036(1) 0.0242(9) -0.0007(7) -0.0007(7) 0.0018(8) C(27) 0.0214(8) 0.0270(9) 0.0222(9) 0.0029(7) -0.0025(7) 0.0032(7) C(28) 0.046(1) 0.025(1) 0.070(2) -0.0037(9) 0.010(1) 0.013(1) C(29) 0.0194(8) 0.0214(8) 0.0200(8) 0.0012(7) 0.0024(7) 0.0007(7) C(30) 0.0172(7) 0.0202(8) 0.0242(9) 0.0016(6) 0.0036(7) 0.0010(7) C(31) 0.0209(8) 0.0171(8) 0.0232(9) 0.0026(7) 0.0029(7) -0.0015(7) C(32) 0.0197(8) 0.0205(8) 0.0298(9) 0.0000(7) 0.0000(7) -0.0009(7) C(33) 0.0248(9) 0.0231(9) 0.0277(9) 0.0033(7) -0.0026(8) 0.0020(7) C(34) 0.0301(9) 0.0177(8) 0.0278(9) 0.0016(7) 0.0044(8) 0.0038(7) C(35) 0.0275(9) 0.0214(9) 0.032(1) -0.0058(7) -0.0019(8) 0.0010(7) C(36) 0.0262(8) 0.0213(9) 0.0263(9) -0.0008(7) -0.0023(7) -0.0006(7) C(37) 0.044(1) 0.030(1) 0.0270(10) 0.0059(9) 0.0072(9) 0.0045(8) C(38) 0.0235(8) 0.0196(8) 0.0232(9) -0.0030(7) 0.0027(7) 0.0004(7) C(39) 0.0262(9) 0.0269(9) 0.0281(9) 0.0022(7) 0.0025(7) -0.0004(8) C(40) 0.0317(10) 0.035(1) 0.030(1) 0.0023(8) -0.0028(8) 0.0034(8) C(41) 0.041(1) 0.0296(9) 0.0225(9) -0.0049(9) -0.0010(8) 0.0019(8) C(42) 0.048(1) 0.0255(9) 0.029(1) 0.0021(9) 0.0087(9) -0.0049(8) C(43) 0.0367(10) 0.0209(9) 0.0290(10) 0.0025(8) 0.0035(8) 0.0020(8) C(44) 0.118(2) 0.049(1) 0.023(1) 0.013(1) 0.004(1) -0.0033(10) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(18) 1.366(2) . . yes O(1) C(21) 1.425(2) . . yes O(2) C(25) 1.370(2) . . yes O(2) C(28) 1.417(2) . . yes O(3) C(34) 1.372(2) . . yes O(3) C(37) 1.420(2) . . yes O(4) C(41) 1.374(2) . . yes O(4) C(44) 1.416(3) . . yes C(1) C(2) 1.413(2) . . yes C(1) C(6) 1.394(2) . . yes C(1) C(7) 1.498(2) . . yes C(2) C(3) 1.402(2) . . yes C(2) C(13) 1.472(2) . . yes C(3) C(4) 1.382(2) . . yes C(4) C(5) 1.387(3) . . yes C(5) C(6) 1.385(3) . . yes C(7) C(8) 1.407(2) . . yes C(7) C(12) 1.397(2) . . yes C(8) C(9) 1.402(2) . . yes C(8) C(29) 1.475(2) . . yes C(9) C(10) 1.383(2) . . yes C(10) C(11) 1.383(3) . . yes C(11) C(12) 1.387(3) . . yes C(13) C(14) 1.351(2) . . yes C(14) C(15) 1.488(2) . . yes C(14) C(22) 1.484(2) . . yes C(15) C(16) 1.399(2) . . yes C(15) C(20) 1.395(2) . . yes C(16) C(17) 1.389(2) . . yes C(17) C(18) 1.390(2) . . yes C(18) C(19) 1.390(2) . . yes C(19) C(20) 1.389(2) . . yes C(22) C(23) 1.388(2) . . yes C(22) C(27) 1.408(2) . . yes C(23) C(24) 1.390(2) . . yes C(24) C(25) 1.394(2) . . yes C(25) C(26) 1.388(2) . . yes C(26) C(27) 1.375(2) . . yes C(29) C(30) 1.347(2) . . yes C(30) C(31) 1.490(2) . . yes C(30) C(38) 1.490(2) . . yes C(31) C(32) 1.391(2) . . yes C(31) C(36) 1.402(2) . . yes C(32) C(33) 1.390(2) . . yes C(33) C(34) 1.391(2) . . yes C(34) C(35) 1.387(3) . . yes C(35) C(36) 1.385(2) . . yes C(38) C(39) 1.399(2) . . yes C(38) C(43) 1.386(2) . . yes C(39) C(40) 1.381(3) . . yes C(40) C(41) 1.385(3) . . yes C(41) C(42) 1.385(3) . . yes C(42) C(43) 1.398(3) . . yes #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(18) O(1) C(21) 116.6(1) . . . yes C(25) O(2) C(28) 118.1(1) . . . yes C(34) O(3) C(37) 117.2(1) . . . yes C(41) O(4) C(44) 117.7(2) . . . yes C(2) C(1) C(6) 119.1(2) . . . yes C(2) C(1) C(7) 120.8(1) . . . yes C(6) C(1) C(7) 120.1(1) . . . yes C(1) C(2) C(3) 118.8(1) . . . yes C(1) C(2) C(13) 119.6(1) . . . yes C(3) C(2) C(13) 121.2(1) . . . yes C(2) C(3) C(4) 121.0(2) . . . yes C(3) C(4) C(5) 120.1(2) . . . yes C(4) C(5) C(6) 119.7(2) . . . yes C(1) C(6) C(5) 121.2(2) . . . yes C(1) C(7) C(8) 120.3(1) . . . yes C(1) C(7) C(12) 120.3(1) . . . yes C(8) C(7) C(12) 119.4(2) . . . yes C(7) C(8) C(9) 118.9(1) . . . yes C(7) C(8) C(29) 119.4(1) . . . yes C(9) C(8) C(29) 121.2(1) . . . yes C(8) C(9) C(10) 121.0(2) . . . yes C(9) C(10) C(11) 119.9(2) . . . yes C(10) C(11) C(12) 120.2(2) . . . yes C(7) C(12) C(11) 120.7(2) . . . yes C(2) C(13) C(14) 129.6(1) . . . yes C(13) C(14) C(15) 118.1(1) . . . yes C(13) C(14) C(22) 125.1(1) . . . yes C(15) C(14) C(22) 116.7(1) . . . yes C(14) C(15) C(16) 121.2(1) . . . yes C(14) C(15) C(20) 121.2(1) . . . yes C(16) C(15) C(20) 117.6(1) . . . yes C(15) C(16) C(17) 121.4(2) . . . yes C(16) C(17) C(18) 119.8(2) . . . yes O(1) C(18) C(17) 115.6(2) . . . yes O(1) C(18) C(19) 124.5(2) . . . yes C(17) C(18) C(19) 120.0(2) . . . yes C(18) C(19) C(20) 119.5(2) . . . yes C(15) C(20) C(19) 121.7(2) . . . yes C(14) C(22) C(23) 122.0(1) . . . yes C(14) C(22) C(27) 120.2(1) . . . yes C(23) C(22) C(27) 117.7(1) . . . yes C(22) C(23) C(24) 122.0(1) . . . yes C(23) C(24) C(25) 119.1(1) . . . yes O(2) C(25) C(24) 124.7(2) . . . yes O(2) C(25) C(26) 115.7(1) . . . yes C(24) C(25) C(26) 119.6(2) . . . yes C(25) C(26) C(27) 120.8(1) . . . yes C(22) C(27) C(26) 120.8(2) . . . yes C(8) C(29) C(30) 128.7(2) . . . yes C(29) C(30) C(31) 118.5(1) . . . yes C(29) C(30) C(38) 122.0(1) . . . yes C(31) C(30) C(38) 119.3(1) . . . yes C(30) C(31) C(32) 121.5(1) . . . yes C(30) C(31) C(36) 121.1(1) . . . yes C(32) C(31) C(36) 117.3(1) . . . yes C(31) C(32) C(33) 121.9(2) . . . yes C(32) C(33) C(34) 119.4(2) . . . yes O(3) C(34) C(33) 124.1(2) . . . yes O(3) C(34) C(35) 116.2(2) . . . yes C(33) C(34) C(35) 119.7(2) . . . yes C(34) C(35) C(36) 120.0(2) . . . yes C(31) C(36) C(35) 121.4(2) . . . yes C(30) C(38) C(39) 120.1(2) . . . yes C(30) C(38) C(43) 122.5(2) . . . yes C(39) C(38) C(43) 117.4(2) . . . yes C(38) C(39) C(40) 121.6(2) . . . yes C(39) C(40) C(41) 120.0(2) . . . yes O(4) C(41) C(40) 115.2(2) . . . yes O(4) C(41) C(42) 125.0(2) . . . yes C(40) C(41) C(42) 119.8(2) . . . yes C(41) C(42) C(43) 119.5(2) . . . yes C(38) C(43) C(42) 121.6(2) . . . yes #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(18) C(17) C(16) 179.3(1) . . . . yes O(1) C(18) C(19) C(20) 178.8(2) . . . . yes O(2) C(25) C(24) C(23) 179.3(2) . . . . yes O(2) C(25) C(26) C(27) -179.9(2) . . . . yes O(3) C(34) C(33) C(32) 177.3(2) . . . . yes O(3) C(34) C(35) C(36) -177.2(2) . . . . yes O(4) C(41) C(40) C(39) 177.5(2) . . . . yes O(4) C(41) C(42) C(43) -178.2(2) . . . . yes C(1) C(2) C(3) C(4) -0.3(2) . . . . yes C(1) C(2) C(13) C(14) -140.5(2) . . . . yes C(1) C(6) C(5) C(4) 0.3(3) . . . . yes C(1) C(7) C(8) C(9) 180.0(1) . . . . yes C(1) C(7) C(8) C(29) 7.7(2) . . . . yes C(1) C(7) C(12) C(11) -179.5(2) . . . . yes C(2) C(1) C(6) C(5) 0.4(3) . . . . yes C(2) C(1) C(7) C(8) 83.2(2) . . . . yes C(2) C(1) C(7) C(12) -98.0(2) . . . . yes C(2) C(3) C(4) C(5) 1.0(3) . . . . yes C(2) C(13) C(14) C(15) -171.3(2) . . . . yes C(2) C(13) C(14) C(22) 12.3(3) . . . . yes C(3) C(2) C(1) C(6) -0.4(2) . . . . yes C(3) C(2) C(1) C(7) -179.7(1) . . . . yes C(3) C(2) C(13) C(14) 47.0(3) . . . . yes C(3) C(4) C(5) C(6) -1.0(3) . . . . yes C(4) C(3) C(2) C(13) 172.3(2) . . . . yes C(5) C(6) C(1) C(7) 179.7(2) . . . . yes C(6) C(1) C(2) C(13) -173.1(1) . . . . yes C(6) C(1) C(7) C(8) -96.1(2) . . . . yes C(6) C(1) C(7) C(12) 82.8(2) . . . . yes C(7) C(1) C(2) C(13) 7.7(2) . . . . yes C(7) C(8) C(9) C(10) -0.3(2) . . . . yes C(7) C(8) C(29) C(30) -151.2(2) . . . . yes C(7) C(12) C(11) C(10) -0.7(3) . . . . yes C(8) C(7) C(12) C(11) -0.6(2) . . . . yes C(8) C(9) C(10) C(11) -1.0(3) . . . . yes C(8) C(29) C(30) C(31) -171.1(1) . . . . yes C(8) C(29) C(30) C(38) 13.7(3) . . . . yes C(9) C(8) C(7) C(12) 1.2(2) . . . . yes C(9) C(8) C(29) C(30) 36.7(2) . . . . yes C(9) C(10) C(11) C(12) 1.6(3) . . . . yes C(10) C(9) C(8) C(29) 171.8(2) . . . . yes C(12) C(7) C(8) C(29) -171.1(1) . . . . yes C(13) C(14) C(15) C(16) 44.6(2) . . . . yes C(13) C(14) C(15) C(20) -134.1(2) . . . . yes C(13) C(14) C(22) C(23) 44.4(2) . . . . yes C(13) C(14) C(22) C(27) -139.9(2) . . . . yes C(14) C(15) C(16) C(17) -178.3(1) . . . . yes C(14) C(15) C(20) C(19) 176.4(1) . . . . yes C(14) C(22) C(23) C(24) 175.5(2) . . . . yes C(14) C(22) C(27) C(26) -176.2(2) . . . . yes C(15) C(14) C(22) C(23) -132.1(2) . . . . yes C(15) C(14) C(22) C(27) 43.6(2) . . . . yes C(15) C(16) C(17) C(18) 1.3(2) . . . . yes C(15) C(20) C(19) C(18) 2.5(2) . . . . yes C(16) C(15) C(14) C(22) -138.6(2) . . . . yes C(16) C(15) C(20) C(19) -2.4(2) . . . . yes C(16) C(17) C(18) C(19) -1.2(2) . . . . yes C(17) C(16) C(15) C(20) 0.5(2) . . . . yes C(17) C(18) O(1) C(21) 165.5(1) . . . . yes C(17) C(18) C(19) C(20) -0.7(2) . . . . yes C(19) C(18) O(1) C(21) -13.9(2) . . . . yes C(20) C(15) C(14) C(22) 42.7(2) . . . . yes C(22) C(23) C(24) C(25) 0.7(3) . . . . yes C(22) C(27) C(26) C(25) 0.5(3) . . . . yes C(23) C(22) C(27) C(26) -0.3(3) . . . . yes C(23) C(24) C(25) C(26) -0.6(3) . . . . yes C(24) C(23) C(22) C(27) -0.3(2) . . . . yes C(24) C(25) O(2) C(28) 1.1(3) . . . . yes C(24) C(25) C(26) C(27) 0.0(3) . . . . yes C(26) C(25) O(2) C(28) -179.0(2) . . . . yes C(29) C(30) C(31) C(32) 34.1(2) . . . . yes C(29) C(30) C(31) C(36) -141.9(2) . . . . yes C(29) C(30) C(38) C(39) 55.7(2) . . . . yes C(29) C(30) C(38) C(43) -122.3(2) . . . . yes C(30) C(31) C(32) C(33) -171.9(2) . . . . yes C(30) C(31) C(36) C(35) 172.0(2) . . . . yes C(30) C(38) C(39) C(40) -176.9(2) . . . . yes C(30) C(38) C(43) C(42) 176.0(2) . . . . yes C(31) C(30) C(38) C(39) -119.5(2) . . . . yes C(31) C(30) C(38) C(43) 62.5(2) . . . . yes C(31) C(32) C(33) C(34) -0.7(3) . . . . yes C(31) C(36) C(35) C(34) 0.5(3) . . . . yes C(32) C(31) C(30) C(38) -150.6(2) . . . . yes C(32) C(31) C(36) C(35) -4.1(2) . . . . yes C(32) C(33) C(34) C(35) -3.1(3) . . . . yes C(33) C(32) C(31) C(36) 4.2(2) . . . . yes C(33) C(34) O(3) C(37) -12.8(2) . . . . yes C(33) C(34) C(35) C(36) 3.2(3) . . . . yes C(35) C(34) O(3) C(37) 167.6(2) . . . . yes C(36) C(31) C(30) C(38) 33.5(2) . . . . yes C(38) C(39) C(40) C(41) 0.8(3) . . . . yes C(38) C(43) C(42) C(41) 0.9(3) . . . . yes C(39) C(38) C(43) C(42) -2.1(3) . . . . yes C(39) C(40) C(41) C(42) -1.9(3) . . . . yes C(40) C(39) C(38) C(43) 1.2(3) . . . . yes C(40) C(41) O(4) C(44) -178.2(2) . . . . yes C(40) C(41) C(42) C(43) 1.1(3) . . . . yes C(42) C(41) O(4) C(44) 1.2(3) . . . . yes C(42) C(41) O(4) C(44) 1.2(3) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(2) C(32) 3.385(2) . 1_655 ? C(2) C(28) 3.533(3) . 6_745 ? C(3) C(28) 3.432(3) . 6_745 ? C(4) C(37) 3.430(3) . 5_765 ? C(4) C(26) 3.596(3) . 2_455 ? C(5) C(25) 3.491(2) . 2_455 ? C(10) C(19) 3.560(2) . 1_455 ? C(10) C(21) 3.561(3) . 8_455 ? C(11) C(21) 3.517(3) . 8_455 ? C(15) C(21) 3.469(2) . 8_455 ? C(16) C(21) 3.407(2) . 8_455 ? C(16) C(36) 3.534(2) . 6_745 ? C(24) C(37) 3.560(3) . 5_765 ? C(32) C(37) 3.580(3) . 5_765 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------