#------------------------------------------------------------------------------ #$Date: 2009-05-03 21:56:13 +0300 (Sun, 03 May 2009) $ #$Revision: 691 $ #$URL: file:///home/coder/svn-repositories/cod/hkl/2/2219385.hkl $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2219385_Fobs loop_ _publ_author_name 'Wei, Jian' 'Liang, Guang' 'Gai, Yuhong' 'Lu, Jingmei' _publ_section_title ; (E,E)-2,5-Bis(4-tert-butylbenzylidene)cyclopentanone ; _journal_coeditor_code LH2667 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1755 _journal_volume 64 _journal_year 2008 _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 O' _chemical_formula_weight 372.53 _chemical_melting_point ? _chemical_name_common ? _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 94.243(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 20 _cell_length_a 41.246 _cell_length_b 6.2930 _cell_length_c 43.001 _cell_measurement_reflns_used 2156 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 40.814 _cell_measurement_theta_min 5.282 _cell_volume 11131(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1284 _diffrn_reflns_av_sigmaI/netI 0.1307 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_number 28046 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 1.90 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76060 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 4040 _exptl_crystal_size_max 0.497 _exptl_crystal_size_mid 0.411 _exptl_crystal_size_min 0.176 _refine_diff_density_max 0.199 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.052 _refine_ls_extinction_coef 0.00016(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 648 _refine_ls_number_reflns 10373 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.856 _refine_ls_R_factor_all 0.1631 _refine_ls_R_factor_gt 0.0683 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1461 _refine_ls_wR_factor_ref 0.1803 _reflns_number_gt 4318 _reflns_number_total 10373 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file lh2667Isup2.hkl _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 O1 O 0.29393(5) 0.4048(3) 0.07533(6) 0.0780(7) Uani 1 1 d . . . O2 O 0.39495(5) 0.5016(3) 0.17171(6) 0.0781(7) Uani 1 1 d . . . O3 O 0.5000 0.4826(5) 0.2500 0.150(2) Uani 1 2 d S . . C1 C 0.29711(7) 0.5803(5) 0.06428(7) 0.0541(8) Uani 1 1 d . . . C2 C 0.27036(7) 0.7186(5) 0.05130(7) 0.0518(8) Uani 1 1 d . . . C3 C 0.28460(7) 0.9189(5) 0.03993(7) 0.0564(8) Uani 1 1 d . . . H3A H 0.2770 1.0396 0.0514 0.068 Uiso 1 1 calc R . . H3B H 0.2782 0.9391 0.0180 0.068 Uiso 1 1 calc R . . C4 C 0.32163(7) 0.9001(5) 0.04504(7) 0.0609(9) Uani 1 1 d . . . H4A H 0.3314 0.9010 0.0252 0.073 Uiso 1 1 calc R . . H4B H 0.3305 1.0176 0.0576 0.073 Uiso 1 1 calc R . . C5 C 0.32819(7) 0.6937(4) 0.06157(7) 0.0498(8) Uani 1 1 d . . . C6 C 0.35604(7) 0.6012(5) 0.07231(7) 0.0560(8) Uani 1 1 d . . . H6 H 0.3533 0.4710 0.0820 0.067 Uiso 1 1 calc R . . C7 C 0.38955(7) 0.6671(5) 0.07152(7) 0.0504(8) Uani 1 1 d . . . C8 C 0.39985(8) 0.8547(5) 0.05871(8) 0.0693(10) Uani 1 1 d . . . H8 H 0.3844 0.9530 0.0512 0.083 Uiso 1 1 calc R . . C9 C 0.43234(8) 0.9011(5) 0.05671(7) 0.0662(10) Uani 1 1 d . . . H9 H 0.4380 1.0308 0.0483 0.079 Uiso 1 1 calc R . . C10 C 0.45680(7) 0.7603(5) 0.06689(7) 0.0501(8) Uani 1 1 d . . . C11 C 0.44633(8) 0.5780(5) 0.08082(8) 0.0676(10) Uani 1 1 d . . . H11 H 0.4618 0.4827 0.0893 0.081 Uiso 1 1 calc R . . C12 C 0.41393(8) 0.5305(5) 0.08281(8) 0.0669(10) Uani 1 1 d . . . H12 H 0.4083 0.4032 0.0920 0.080 Uiso 1 1 calc R . . C13 C 0.23963(7) 0.6558(5) 0.05233(7) 0.0569(9) Uani 1 1 d . . . H13 H 0.2373 0.5182 0.0597 0.068 Uiso 1 1 calc R . . C14 C 0.20898(7) 0.7645(5) 0.04394(7) 0.0521(8) Uani 1 1 d . . . C15 C 0.20580(8) 0.9549(5) 0.02837(8) 0.0651(9) Uani 1 1 d . . . H15 H 0.2242 1.0205 0.0216 0.078 Uiso 1 1 calc R . . C16 C 0.17589(8) 1.0512(5) 0.02251(8) 0.0691(10) Uani 1 1 d . . . H16 H 0.1746 1.1799 0.0119 0.083 Uiso 1 1 calc R . . C17 C 0.14765(7) 0.9602(5) 0.03214(7) 0.0516(8) Uani 1 1 d . . . C18 C 0.15075(8) 0.7686(5) 0.04666(8) 0.0693(10) Uani 1 1 d . . . H18 H 0.1322 0.7016 0.0530 0.083 Uiso 1 1 calc R . . C19 C 0.18059(8) 0.6705(5) 0.05234(8) 0.0683(10) Uani 1 1 d . . . H19 H 0.1816 0.5382 0.0620 0.082 Uiso 1 1 calc R . . C20 C 0.49193(7) 0.8047(5) 0.06146(7) 0.0586(9) Uani 1 1 d . . . C21 C 0.50018(8) 1.0402(6) 0.06386(8) 0.0873(12) Uani 1 1 d . . . H21A H 0.4866 1.1179 0.0487 0.121 Uiso 1 1 calc R . . H21B H 0.5226 1.0609 0.0600 0.121 Uiso 1 1 calc R . . H21C H 0.4965 1.0905 0.0844 0.121 Uiso 1 1 calc R . . C22 C 0.49753(8) 0.7297(6) 0.02807(7) 0.0924(13) Uani 1 1 d . . . H22A H 0.4935 0.5797 0.0264 0.129 Uiso 1 1 calc R . . H22B H 0.5196 0.7589 0.0237 0.129 Uiso 1 1 calc R . . H22C H 0.4830 0.8039 0.0134 0.129 Uiso 1 1 calc R . . C23 C 0.51543(7) 0.6833(5) 0.08448(8) 0.0813(11) Uani 1 1 d . . . H23A H 0.5115 0.7228 0.1054 0.112 Uiso 1 1 calc R . . H23B H 0.5374 0.7180 0.0806 0.112 Uiso 1 1 calc R . . H23C H 0.5121 0.5333 0.0818 0.112 Uiso 1 1 calc R . . C24 C 0.11478(7) 1.0750(5) 0.02828(7) 0.0600(9) Uani 1 1 d . . . C25 C 0.11316(9) 1.2364(6) 0.00167(8) 0.0994(13) Uani 1 1 d . . . H25A H 0.0917 1.2959 -0.0009 0.129 Uiso 1 1 calc R . . H25B H 0.1181 1.1670 -0.0173 0.129 Uiso 1 1 calc R . . H25C H 0.1286 1.3477 0.0065 0.129 Uiso 1 1 calc R . . C26 C 0.08709(8) 0.9174(6) 0.02227(10) 0.1145(16) Uani 1 1 d . . . H26A H 0.0856 0.8292 0.0403 0.132 Uiso 1 1 calc R . . H26B H 0.0912 0.8303 0.0046 0.132 Uiso 1 1 calc R . . H26C H 0.0671 0.9933 0.0180 0.132 Uiso 1 1 calc R . . C27 C 0.10989(8) 1.1952(5) 0.05843(8) 0.0823(11) Uani 1 1 d . . . H27A H 0.1092 1.0959 0.0753 0.113 Uiso 1 1 calc R . . H27B H 0.0898 1.2729 0.0562 0.113 Uiso 1 1 calc R . . H27C H 0.1276 1.2922 0.0628 0.113 Uiso 1 1 calc R . . C28 C 0.39418(8) 0.6813(5) 0.16108(7) 0.0569(9) Uani 1 1 d . . . C29 C 0.36451(8) 0.8006(5) 0.14964(7) 0.0530(8) Uani 1 1 d . . . C30 C 0.37431(7) 1.0141(5) 0.13873(7) 0.0610(9) Uani 1 1 d . . . H30A H 0.3645 1.1246 0.1507 0.073 Uiso 1 1 calc R . . H30B H 0.3673 1.0331 0.1169 0.073 Uiso 1 1 calc R . . C31 C 0.41147(7) 1.0257(5) 0.14342(7) 0.0598(9) Uani 1 1 d . . . H31A H 0.4208 1.0478 0.1236 0.072 Uiso 1 1 calc R . . H31B H 0.4180 1.1422 0.1572 0.072 Uiso 1 1 calc R . . C32 C 0.42270(8) 0.8190(5) 0.15740(7) 0.0525(8) Uani 1 1 d . . . C33 C 0.45271(8) 0.7498(5) 0.16590(7) 0.0591(9) Uani 1 1 d . . . H33 H 0.4536 0.6132 0.1742 0.071 Uiso 1 1 calc R . . C34 C 0.48430(8) 0.8524(5) 0.16440(7) 0.0572(9) Uani 1 1 d . . . C35 C 0.48909(8) 1.0564(5) 0.15346(8) 0.0651(9) Uani 1 1 d . . . H35 H 0.4712 1.1402 0.1474 0.078 Uiso 1 1 calc R . . C36 C 0.51997(9) 1.1379(5) 0.15140(8) 0.0693(10) Uani 1 1 d . . . H36 H 0.5221 1.2766 0.1444 0.083 Uiso 1 1 calc R . . C37 C 0.54771(8) 1.0213(6) 0.15933(7) 0.0596(9) Uani 1 1 d . . . C38 C 0.54279(8) 0.8225(6) 0.17108(8) 0.0700(10) Uani 1 1 d . . . H38 H 0.5608 0.7416 0.1778 0.084 Uiso 1 1 calc R . . C39 C 0.51227(8) 0.7368(5) 0.17340(7) 0.0656(9) Uani 1 1 d . . . H39 H 0.5103 0.5996 0.1811 0.079 Uiso 1 1 calc R . . C40 C 0.33520(8) 0.7134(5) 0.15129(7) 0.0575(9) Uani 1 1 d . . . H40 H 0.3354 0.5726 0.1579 0.069 Uiso 1 1 calc R . . C41 C 0.30296(8) 0.8035(5) 0.14442(7) 0.0542(8) Uani 1 1 d . . . C42 C 0.29618(8) 0.9955(5) 0.13020(7) 0.0650(9) Uani 1 1 d . . . H42 H 0.3131 1.0715 0.1223 0.078 Uiso 1 1 calc R . . C43 C 0.26539(8) 1.0797(5) 0.12713(7) 0.0621(9) Uani 1 1 d . . . H43 H 0.2621 1.2104 0.1173 0.075 Uiso 1 1 calc R . . C44 C 0.23909(7) 0.9745(5) 0.13833(6) 0.0487(8) Uani 1 1 d . . . C45 C 0.24561(8) 0.7785(5) 0.15148(8) 0.0692(10) Uani 1 1 d . . . H45 H 0.2286 0.7013 0.1589 0.083 Uiso 1 1 calc R . . C46 C 0.27610(8) 0.6926(5) 0.15411(8) 0.0697(10) Uani 1 1 d . . . H46 H 0.2791 0.5573 0.1625 0.084 Uiso 1 1 calc R . . C47 C 0.58159(8) 1.1126(6) 0.15588(8) 0.0694(10) Uani 1 1 d . . . C48 C 0.58196(9) 1.2481(8) 0.12684(10) 0.116(2) Uani 1 1 d . . . H48A H 0.5704 1.3778 0.1298 0.133 Uiso 1 1 calc R . . H48B H 0.5717 1.1721 0.1094 0.133 Uiso 1 1 calc R . . H48C H 0.6040 1.2803 0.1229 0.133 Uiso 1 1 calc R . . C49 C 0.60698(9) 0.9422(7) 0.15397(13) 0.115(2) Uani 1 1 d . . . H49A H 0.6092 0.8657 0.1733 0.132 Uiso 1 1 calc R . . H49B H 0.6274 1.0063 0.1500 0.132 Uiso 1 1 calc R . . H49C H 0.6005 0.8460 0.1373 0.132 Uiso 1 1 calc R . . C50 C 0.59097(9) 1.2498(6) 0.18397(10) 0.1174(16) Uani 1 1 d . . . H50A H 0.5930 1.1627 0.2023 0.136 Uiso 1 1 calc R . . H50B H 0.5745 1.3556 0.1861 0.136 Uiso 1 1 calc R . . H50C H 0.6114 1.3181 0.1813 0.136 Uiso 1 1 calc R . . C51 C 0.20573(7) 1.0771(5) 0.13858(7) 0.0539(8) Uani 1 1 d . . . C52 C 0.19933(8) 1.2366(5) 0.11190(8) 0.0842(11) Uani 1 1 d . . . H52A H 0.2155 1.3465 0.1136 0.116 Uiso 1 1 calc R . . H52B H 0.1782 1.2984 0.1131 0.116 Uiso 1 1 calc R . . H52C H 0.2003 1.1649 0.0923 0.116 Uiso 1 1 calc R . . C53 C 0.17837(8) 0.9136(6) 0.13635(9) 0.0906(12) Uani 1 1 d . . . H53A H 0.1798 0.8295 0.1179 0.126 Uiso 1 1 calc R . . H53B H 0.1578 0.9854 0.1354 0.126 Uiso 1 1 calc R . . H53C H 0.1803 0.8230 0.1543 0.126 Uiso 1 1 calc R . . C54 C 0.20421(8) 1.1991(5) 0.16945(8) 0.0819(11) Uani 1 1 d . . . H54A H 0.2071 1.1016 0.1866 0.113 Uiso 1 1 calc R . . H54B H 0.1835 1.2676 0.1699 0.113 Uiso 1 1 calc R . . H54C H 0.2211 1.3041 0.1711 0.113 Uiso 1 1 calc R . . C55 C 0.5000 0.6744(8) 0.2500 0.0757(15) Uani 1 2 d S . . C56 C 0.47090(8) 0.8110(5) 0.24588(7) 0.0558(8) Uani 1 1 d . . . C57 C 0.48172(6) 1.0344(4) 0.24519(7) 0.0578(9) Uani 1 1 d . . . H57A H 0.4701 1.1193 0.2596 0.069 Uiso 1 1 calc R . . H57B H 0.4776 1.0929 0.2244 0.069 Uiso 1 1 calc R . . C58 C 0.44126(8) 0.7242(5) 0.24475(7) 0.0621(9) Uani 1 1 d . . . H58 H 0.4408 0.5766 0.2457 0.075 Uiso 1 1 calc R . . C59 C 0.40947(8) 0.8272(5) 0.24219(7) 0.0541(8) Uani 1 1 d . . . C60 C 0.38304(8) 0.7181(5) 0.25263(8) 0.0692(10) Uani 1 1 d . . . H60 H 0.3861 0.5811 0.2604 0.083 Uiso 1 1 calc R . . C61 C 0.35248(8) 0.8073(5) 0.25171(8) 0.0694(10) Uani 1 1 d . . . H61 H 0.3356 0.7305 0.2595 0.083 Uiso 1 1 calc R . . C62 C 0.34621(7) 1.0063(5) 0.23968(7) 0.0508(8) Uani 1 1 d . . . C63 C 0.37253(8) 1.1119(5) 0.22831(7) 0.0576(9) Uani 1 1 d . . . H63 H 0.3692 1.2456 0.2194 0.069 Uiso 1 1 calc R . . C64 C 0.40330(8) 1.0253(5) 0.22976(7) 0.0570(9) Uani 1 1 d . . . H64 H 0.4202 1.1027 0.2222 0.068 Uiso 1 1 calc R . . C65 C 0.31284(8) 1.1083(5) 0.24011(7) 0.0554(8) Uani 1 1 d . . . C66 C 0.30633(8) 1.2711(6) 0.21395(8) 0.0984(13) Uani 1 1 d . . . H66A H 0.3220 1.3839 0.2164 0.128 Uiso 1 1 calc R . . H66B H 0.2848 1.3282 0.2148 0.128 Uiso 1 1 calc R . . H66C H 0.3081 1.2033 0.1942 0.128 Uiso 1 1 calc R . . C67 C 0.28577(8) 0.9443(6) 0.23752(10) 0.1012(14) Uani 1 1 d . . . H67A H 0.2864 0.8687 0.2182 0.132 Uiso 1 1 calc R . . H67B H 0.2652 1.0144 0.2381 0.132 Uiso 1 1 calc R . . H67C H 0.2886 0.8461 0.2546 0.132 Uiso 1 1 calc R . . C68 C 0.31128(8) 1.2240(6) 0.27122(8) 0.0887(12) Uani 1 1 d . . . H68A H 0.3141 1.1236 0.2880 0.123 Uiso 1 1 calc R . . H68B H 0.2905 1.2922 0.2719 0.123 Uiso 1 1 calc R . . H68C H 0.3282 1.3289 0.2733 0.123 Uiso 1 1 calc 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0684(16) 0.0598(15) 0.107(2) 0.0237(15) 0.0149(13) -0.0006(13) O2 0.0815(17) 0.0480(14) 0.106(2) 0.0113(14) 0.0130(14) 0.0022(13) O3 0.081(3) 0.036(2) 0.332(7) 0.000 0.016(3) 0.000 C1 0.059(2) 0.050(2) 0.055(2) 0.0025(17) 0.0105(16) 0.0021(18) C2 0.054(2) 0.053(2) 0.049(2) -0.0013(16) 0.0108(15) 0.0001(18) C3 0.054(2) 0.058(2) 0.058(2) 0.0071(16) 0.0104(16) -0.0018(17) C4 0.057(2) 0.062(2) 0.064(2) 0.0128(18) 0.0066(16) 0.0006(17) C5 0.051(2) 0.051(2) 0.0484(19) 0.0062(15) 0.0133(15) 0.0035(17) C6 0.064(2) 0.057(2) 0.048(2) 0.0040(16) 0.0105(16) 0.0030(18) C7 0.054(2) 0.053(2) 0.0443(19) 0.0060(15) 0.0059(15) 0.0046(17) C8 0.053(2) 0.069(2) 0.086(3) 0.022(2) 0.0015(18) 0.0052(19) C9 0.057(2) 0.066(2) 0.076(3) 0.0237(19) 0.0036(18) -0.0001(19) C10 0.052(2) 0.059(2) 0.0396(18) -0.0024(16) 0.0036(14) 0.0071(17) C11 0.056(2) 0.070(2) 0.077(3) 0.017(2) 0.0045(18) 0.0150(19) C12 0.059(2) 0.060(2) 0.082(3) 0.0227(19) 0.0071(19) 0.0062(19) C13 0.055(2) 0.055(2) 0.062(2) 0.0019(16) 0.0118(16) 0.0012(18) C14 0.054(2) 0.053(2) 0.049(2) 0.0050(16) 0.0067(15) -0.0008(17) C15 0.053(2) 0.070(2) 0.075(3) 0.0171(19) 0.0177(17) -0.0006(19) C16 0.063(2) 0.070(2) 0.075(3) 0.0223(19) 0.0118(19) 0.005(2) C17 0.054(2) 0.056(2) 0.0454(19) 0.0007(16) 0.0033(15) 0.0002(17) C18 0.055(2) 0.076(3) 0.077(3) 0.024(2) 0.0105(18) -0.0073(19) C19 0.055(2) 0.064(2) 0.086(3) 0.0267(19) 0.0052(19) -0.0021(19) C20 0.053(2) 0.075(2) 0.048(2) -0.0044(18) 0.0033(15) 0.0003(19) C21 0.068(3) 0.098(3) 0.097(3) -0.006(2) 0.012(2) -0.013(2) C22 0.072(3) 0.148(4) 0.060(3) -0.015(2) 0.0227(19) 0.001(2) C23 0.058(2) 0.114(3) 0.072(3) 0.010(2) 0.0023(18) 0.012(2) C24 0.058(2) 0.067(2) 0.055(2) 0.0030(18) -0.0008(16) 0.0061(18) C25 0.099(3) 0.126(3) 0.073(3) 0.031(2) 0.006(2) 0.041(3) C26 0.062(3) 0.101(3) 0.175(5) -0.027(3) -0.030(3) -0.005(2) C27 0.074(3) 0.100(3) 0.074(3) -0.008(2) 0.012(2) 0.014(2) C28 0.069(2) 0.049(2) 0.055(2) -0.0054(17) 0.0134(17) 0.0024(19) C29 0.064(2) 0.048(2) 0.048(2) -0.0042(15) 0.0161(16) 0.0015(18) C30 0.067(2) 0.059(2) 0.058(2) 0.0045(17) 0.0115(17) 0.0008(18) C31 0.062(2) 0.059(2) 0.059(2) 0.0041(17) 0.0093(16) -0.0003(18) C32 0.061(2) 0.046(2) 0.052(2) -0.0029(16) 0.0117(16) 0.0036(18) C33 0.073(2) 0.052(2) 0.054(2) -0.0035(16) 0.0167(17) 0.0012(19) C34 0.065(2) 0.058(2) 0.049(2) -0.0072(17) 0.0109(16) 0.0037(19) C35 0.060(2) 0.061(2) 0.075(3) -0.0022(19) 0.0121(18) 0.0040(19) C36 0.075(3) 0.061(2) 0.074(3) 0.0010(19) 0.015(2) -0.006(2) C37 0.065(2) 0.062(2) 0.052(2) -0.0049(17) 0.0042(17) -0.001(2) C38 0.058(2) 0.079(3) 0.072(3) 0.004(2) -0.0030(18) 0.005(2) C39 0.065(2) 0.061(2) 0.071(3) 0.0053(18) 0.0033(18) 0.006(2) C40 0.069(2) 0.049(2) 0.056(2) 0.0010(16) 0.0148(17) -0.0004(18) C41 0.064(2) 0.051(2) 0.049(2) 0.0044(16) 0.0099(16) -0.0018(18) C42 0.060(2) 0.069(2) 0.068(2) 0.0224(19) 0.0192(17) -0.0015(19) C43 0.069(2) 0.055(2) 0.064(2) 0.0155(17) 0.0135(18) -0.0048(19) C44 0.059(2) 0.051(2) 0.0366(18) 0.0015(15) 0.0027(14) -0.0042(17) C45 0.063(2) 0.063(2) 0.082(3) 0.021(2) 0.0137(19) -0.0110(19) C46 0.068(3) 0.050(2) 0.091(3) 0.0208(19) 0.004(2) -0.007(2) C47 0.055(2) 0.081(3) 0.071(3) -0.004(2) -0.0033(18) -0.008(2) C48 0.093(3) 0.177(6) 0.095(4) 0.087(4) -0.007(3) -0.069(4) C49 0.070(3) 0.120(4) 0.180(7) -0.020(4) 0.057(4) 0.003(3) C50 0.101(3) 0.139(4) 0.109(4) -0.020(3) -0.010(3) -0.046(3) C51 0.058(2) 0.058(2) 0.046(2) 0.0049(16) 0.0041(15) -0.0061(17) C52 0.083(3) 0.104(3) 0.065(3) 0.029(2) 0.0042(19) 0.017(2) C53 0.066(3) 0.096(3) 0.109(3) 0.005(2) -0.002(2) -0.017(2) C54 0.086(3) 0.093(3) 0.068(3) -0.005(2) 0.010(2) 0.014(2) C55 0.076(4) 0.038(3) 0.114(5) 0.000 0.017(3) 0.000 C56 0.065(2) 0.0397(19) 0.063(2) -0.0012(16) 0.0130(17) -0.0012(17) C57 0.063(2) 0.0414(19) 0.070(2) 0.0011(16) 0.0114(18) -0.0032(15) C58 0.073(3) 0.0409(19) 0.073(2) -0.0013(17) 0.0110(18) 0.0005(19) C59 0.070(2) 0.0397(19) 0.054(2) -0.0054(16) 0.0093(17) -0.0034(17) C60 0.075(3) 0.044(2) 0.090(3) 0.0126(18) 0.013(2) -0.006(2) C61 0.066(3) 0.059(2) 0.085(3) 0.015(2) 0.0184(19) -0.0039(19) C62 0.064(2) 0.047(2) 0.0414(19) -0.0054(15) 0.0048(15) -0.0034(17) C63 0.078(3) 0.047(2) 0.048(2) 0.0064(16) 0.0051(17) -0.0015(19) C64 0.068(2) 0.050(2) 0.055(2) 0.0035(16) 0.0155(17) -0.0060(18) C65 0.064(2) 0.057(2) 0.045(2) -0.0043(16) 0.0024(15) -0.0012(18) C66 0.101(3) 0.122(3) 0.071(3) 0.027(2) 0.004(2) 0.033(3) C67 0.069(3) 0.091(3) 0.142(4) -0.011(3) -0.006(2) -0.006(2) C68 0.085(3) 0.112(3) 0.070(3) -0.021(2) 0.011(2) 0.021(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _audit_creation_method SHELXL-97 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_3 _geom_angle_publ_flag O1 C1 C5 126.1(3) . . ? O1 C1 C2 125.7(3) . . ? C5 C1 C2 108.2(3) . . ? C13 C2 C1 119.8(3) . . ? C13 C2 C3 131.5(3) . . ? C1 C2 C3 108.7(3) . . ? C2 C3 C4 107.5(2) . . ? C2 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? C2 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C5 C4 C3 106.2(2) . . ? C5 C4 H4A 110.5 . . ? C3 C4 H4A 110.5 . . ? C5 C4 H4B 110.5 . . ? C3 C4 H4B 110.5 . . ? H4A C4 H4B 108.7 . . ? C6 C5 C1 119.3(3) . . ? C6 C5 C4 131.4(3) . . ? C1 C5 C4 109.2(3) . . ? C5 C6 C7 131.6(3) . . ? C5 C6 H6 114.2 . . ? C7 C6 H6 114.2 . . ? C12 C7 C8 115.7(3) . . ? C12 C7 C6 119.0(3) . . ? C8 C7 C6 125.2(3) . . ? C9 C8 C7 122.3(3) . . ? C9 C8 H8 118.9 . . ? C7 C8 H8 118.9 . . ? C8 C9 C10 122.1(3) . . ? C8 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C11 C10 C9 115.1(3) . . ? C11 C10 C20 123.8(3) . . ? C9 C10 C20 121.1(3) . . ? C12 C11 C10 122.9(3) . . ? C12 C11 H11 118.5 . . ? C10 C11 H11 118.5 . . ? C11 C12 C7 121.8(3) . . ? C11 C12 H12 119.1 . . ? C7 C12 H12 119.1 . . ? C2 C13 C14 131.5(3) . . ? C2 C13 H13 114.3 . . ? C14 C13 H13 114.3 . . ? C15 C14 C19 116.6(3) . . ? C15 C14 C13 125.4(3) . . ? C19 C14 C13 118.0(3) . . ? C14 C15 C16 121.6(3) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C17 121.5(3) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 116.8(3) . . ? C18 C17 C24 121.3(3) . . ? C16 C17 C24 121.8(3) . . ? C17 C18 C19 122.0(3) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C18 C19 C14 121.5(3) . . ? C18 C19 H19 119.3 . . ? C14 C19 H19 119.3 . . ? C10 C20 C21 112.4(3) . . ? C10 C20 C23 112.0(3) . . ? C21 C20 C23 108.2(3) . . ? C10 C20 C22 107.4(2) . . ? C21 C20 C22 108.2(3) . . ? C23 C20 C22 108.4(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C27 108.8(3) . . ? C26 C24 C25 108.4(3) . . ? C27 C24 C25 107.8(3) . . ? C26 C24 C17 111.0(3) . . ? C27 C24 C17 108.2(2) . . ? C25 C24 C17 112.5(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 C28 C32 125.8(3) . . ? O2 C28 C29 126.2(3) . . ? C32 C28 C29 108.1(3) . . ? C40 C29 C28 120.1(3) . . ? C40 C29 C30 131.0(3) . . ? C28 C29 C30 108.9(3) . . ? C29 C30 C31 107.1(2) . . ? C29 C30 H30A 110.3 . . ? C31 C30 H30A 110.3 . . ? C29 C30 H30B 110.3 . . ? C31 C30 H30B 110.3 . . ? H30A C30 H30B 108.6 . . ? C32 C31 C30 106.8(2) . . ? C32 C31 H31A 110.4 . . ? C30 C31 H31A 110.4 . . ? C32 C31 H31B 110.4 . . ? C30 C31 H31B 110.4 . . ? H31A C31 H31B 108.6 . . ? C33 C32 C28 120.5(3) . . ? C33 C32 C31 130.4(3) . . ? C28 C32 C31 109.1(3) . . ? C32 C33 C34 130.9(3) . . ? C32 C33 H33 114.5 . . ? C34 C33 H33 114.5 . . ? C35 C34 C39 116.2(3) . . ? C35 C34 C33 125.1(3) . . ? C39 C34 C33 118.7(3) . . ? C36 C35 C34 121.4(3) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C37 C36 C35 122.5(3) . . ? C37 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? C38 C37 C36 115.7(3) . . ? C38 C37 C47 122.7(3) . . ? C36 C37 C47 121.6(3) . . ? C37 C38 C39 123.0(3) . . ? C37 C38 H38 118.5 . . ? C39 C38 H38 118.5 . . ? C38 C39 C34 121.1(3) . . ? C38 C39 H39 119.4 . . ? C34 C39 H39 119.4 . . ? C29 C40 C41 130.3(3) . . ? C29 C40 H40 114.9 . . ? C41 C40 H40 114.9 . . ? C42 C41 C46 115.6(3) . . ? C42 C41 C40 125.9(3) . . ? C46 C41 C40 118.5(3) . . ? C43 C42 C41 122.6(3) . . ? C43 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? C42 C43 C44 121.6(3) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C45 C44 C43 115.9(3) . . ? C45 C44 C51 121.8(3) . . ? C43 C44 C51 122.1(3) . . ? C46 C45 C44 122.7(3) . . ? C46 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C45 C46 C41 121.5(3) . . ? C45 C46 H46 119.2 . . ? C41 C46 H46 119.2 . . ? C49 C47 C50 108.2(3) . . ? C49 C47 C48 107.9(4) . . ? C50 C47 C48 108.7(3) . . ? C49 C47 C37 112.5(3) . . ? C50 C47 C37 108.6(3) . . ? C48 C47 C37 110.9(3) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C44 C51 C53 112.3(3) . . ? C44 C51 C52 112.2(3) . . ? C53 C51 C52 108.0(3) . . ? C44 C51 C54 108.2(2) . . ? C53 C51 C54 108.3(3) . . ? C52 C51 C54 107.6(3) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O3 C55 C56 125.6(2) . 2_655 ? O3 C55 C56 125.6(2) . . ? C56 C55 C56 108.8(4) 2_655 . ? C58 C56 C55 120.0(3) . . ? C58 C56 C57 131.7(3) . . ? C55 C56 C57 108.2(3) . . ? C56 C57 C57 106.69(17) . 2_655 ? C56 C57 H57A 110.4 . . ? C57 C57 H57A 110.4 2_655 . ? C56 C57 H57B 110.4 . . ? C57 C57 H57B 110.4 2_655 . ? H57A C57 H57B 108.6 . . ? C56 C58 C59 129.4(3) . . ? C56 C58 H58 115.3 . . ? C59 C58 H58 115.3 . . ? C64 C59 C60 116.6(3) . . ? C64 C59 C58 124.9(3) . . ? C60 C59 C58 118.5(3) . . ? C61 C60 C59 121.8(3) . . ? C61 C60 H60 119.1 . . ? C59 C60 H60 119.1 . . ? C62 C61 C60 122.0(3) . . ? C62 C61 H61 119.0 . . ? C60 C61 H61 119.0 . . ? C61 C62 C63 116.0(3) . . ? C61 C62 C65 121.8(3) . . ? C63 C62 C65 122.2(3) . . ? C64 C63 C62 122.3(3) . . ? C64 C63 H63 118.8 . . ? C62 C63 H63 118.8 . . ? C59 C64 C63 121.3(3) . . ? C59 C64 H64 119.3 . . ? C63 C64 H64 119.3 . . ? C67 C65 C62 111.9(3) . . ? C67 C65 C68 108.0(3) . . ? C62 C65 C68 108.0(2) . . ? C67 C65 C66 108.2(3) . . ? C62 C65 C66 112.6(3) . . ? C68 C65 C66 107.9(3) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.213(3) . ? O2 C28 1.219(3) . ? O3 C55 1.207(5) . ? C1 C5 1.479(4) . ? C1 C2 1.482(4) . ? C2 C13 1.331(4) . ? C2 C3 1.489(4) . ? C3 C4 1.532(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.496(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.339(4) . ? C6 C7 1.446(4) . ? C6 H6 0.9300 . ? C7 C12 1.383(4) . ? C7 C8 1.383(4) . ? C8 C9 1.381(4) . ? C8 H8 0.9300 . ? C9 C10 1.389(4) . ? C9 H9 0.9300 . ? C10 C11 1.379(4) . ? C10 C20 1.511(4) . ? C11 C12 1.378(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.459(4) . ? C13 H13 0.9300 . ? C14 C15 1.374(4) . ? C14 C19 1.384(4) . ? C15 C16 1.381(4) . ? C15 H15 0.9300 . ? C16 C17 1.388(4) . ? C16 H16 0.9300 . ? C17 C18 1.359(4) . ? C17 C24 1.534(4) . ? C18 C19 1.383(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.523(4) . ? C20 C23 1.536(4) . ? C20 C22 1.545(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C26 1.520(4) . ? C24 C27 1.527(4) . ? C24 C25 1.528(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C32 1.479(4) . ? C28 C29 1.488(4) . ? C29 C40 1.334(4) . ? C29 C30 1.489(4) . ? C30 C31 1.532(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.492(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.337(4) . ? C33 C34 1.460(4) . ? C33 H33 0.9300 . ? C34 C35 1.387(4) . ? C34 C39 1.394(4) . ? C35 C36 1.382(4) . ? C35 H35 0.9300 . ? C36 C37 1.381(4) . ? C36 H36 0.9300 . ? C37 C38 1.370(4) . ? C37 C47 1.528(4) . ? C38 C39 1.380(4) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.456(4) . ? C40 H40 0.9300 . ? C41 C42 1.374(4) . ? C41 C46 1.399(4) . ? C42 C43 1.374(4) . ? C42 H42 0.9300 . ? C43 C44 1.387(4) . ? C43 H43 0.9300 . ? C44 C45 1.375(4) . ? C44 C51 1.521(4) . ? C45 C46 1.366(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C49 1.505(5) . ? C47 C50 1.512(4) . ? C47 C48 1.513(4) . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C53 1.524(4) . ? C51 C52 1.533(4) . ? C51 C54 1.539(4) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.476(4) 2_655 ? C55 C56 1.476(4) . ? C56 C58 1.337(4) . ? C56 C57 1.476(4) . ? C57 C57 1.534(5) 2_655 ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.460(4) . ? C58 H58 0.9300 . ? C59 C64 1.373(4) . ? C59 C60 1.391(4) . ? C60 C61 1.378(4) . ? C60 H60 0.9300 . ? C61 C62 1.372(4) . ? C61 H61 0.9300 . ? C62 C63 1.392(4) . ? C62 C65 1.520(4) . ? C63 C64 1.379(4) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 C67 1.518(4) . ? C65 C68 1.529(4) . ? C65 C66 1.530(4) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? 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 O1 C1 C2 C13 2.8(5) . . . . ? C5 C1 C2 C13 -177.0(3) . . . . ? O1 C1 C2 C3 -179.5(3) . . . . ? C5 C1 C2 C3 0.8(3) . . . . ? C13 C2 C3 C4 179.5(3) . . . . ? C1 C2 C3 C4 2.1(3) . . . . ? C2 C3 C4 C5 -4.1(3) . . . . ? O1 C1 C5 C6 -0.8(5) . . . . ? C2 C1 C5 C6 178.9(3) . . . . ? O1 C1 C5 C4 176.9(3) . . . . ? C2 C1 C5 C4 -3.4(3) . . . . ? C3 C4 C5 C6 -178.1(3) . . . . ? C3 C4 C5 C1 4.6(3) . . . . ? C1 C5 C6 C7 176.5(3) . . . . ? C4 C5 C6 C7 -0.5(6) . . . . ? C5 C6 C7 C12 -175.7(3) . . . . ? C5 C6 C7 C8 0.7(5) . . . . ? C12 C7 C8 C9 1.3(5) . . . . ? C6 C7 C8 C9 -175.2(3) . . . . ? C7 C8 C9 C10 1.3(5) . . . . ? C8 C9 C10 C11 -3.8(5) . . . . ? C8 C9 C10 C20 173.7(3) . . . . ? C9 C10 C11 C12 4.1(5) . . . . ? C20 C10 C11 C12 -173.4(3) . . . . ? C10 C11 C12 C7 -1.7(5) . . . . ? C8 C7 C12 C11 -1.1(5) . . . . ? C6 C7 C12 C11 175.6(3) . . . . ? C1 C2 C13 C14 174.1(3) . . . . ? C3 C2 C13 C14 -3.0(6) . . . . ? C2 C13 C14 C15 10.0(5) . . . . ? C2 C13 C14 C19 -169.6(3) . . . . ? C19 C14 C15 C16 2.4(5) . . . . ? C13 C14 C15 C16 -177.2(3) . . . . ? C14 C15 C16 C17 0.1(5) . . . . ? C15 C16 C17 C18 -2.2(5) . . . . ? C15 C16 C17 C24 174.6(3) . . . . ? C16 C17 C18 C19 1.5(5) . . . . ? C24 C17 C18 C19 -175.2(3) . . . . ? C17 C18 C19 C14 1.1(5) . . . . ? C15 C14 C19 C18 -3.0(5) . . . . ? C13 C14 C19 C18 176.6(3) . . . . ? C11 C10 C20 C21 -147.0(3) . . . . ? C9 C10 C20 C21 35.7(4) . . . . ? C11 C10 C20 C23 -24.8(4) . . . . ? C9 C10 C20 C23 157.9(3) . . . . ? C11 C10 C20 C22 94.1(4) . . . . ? C9 C10 C20 C22 -83.2(4) . . . . ? C18 C17 C24 C26 -36.4(4) . . . . ? C16 C17 C24 C26 147.1(3) . . . . ? C18 C17 C24 C27 83.0(4) . . . . ? C16 C17 C24 C27 -93.6(4) . . . . ? C18 C17 C24 C25 -158.0(3) . . . . ? C16 C17 C24 C25 25.4(4) . . . . ? O2 C28 C29 C40 1.9(5) . . . . ? C32 C28 C29 C40 -178.0(3) . . . . ? O2 C28 C29 C30 179.8(3) . . . . ? C32 C28 C29 C30 0.0(3) . . . . ? C40 C29 C30 C31 178.1(3) . . . . ? C28 C29 C30 C31 0.5(3) . . . . ? C29 C30 C31 C32 -0.7(3) . . . . ? O2 C28 C32 C33 0.3(5) . . . . ? C29 C28 C32 C33 -179.9(3) . . . . ? O2 C28 C32 C31 179.7(3) . . . . ? C29 C28 C32 C31 -0.4(3) . . . . ? C30 C31 C32 C33 -179.9(3) . . . . ? C30 C31 C32 C28 0.7(3) . . . . ? C28 C32 C33 C34 179.3(3) . . . . ? C31 C32 C33 C34 0.0(5) . . . . ? C32 C33 C34 C35 1.1(5) . . . . ? C32 C33 C34 C39 -176.3(3) . . . . ? C39 C34 C35 C36 0.7(5) . . . . ? C33 C34 C35 C36 -176.8(3) . . . . ? C34 C35 C36 C37 1.4(5) . . . . ? C35 C36 C37 C38 -3.4(5) . . . . ? C35 C36 C37 C47 178.0(3) . . . . ? C36 C37 C38 C39 3.5(5) . . . . ? C47 C37 C38 C39 -178.0(3) . . . . ? C37 C38 C39 C34 -1.5(5) . . . . ? C35 C34 C39 C38 -0.6(5) . . . . ? C33 C34 C39 C38 177.0(3) . . . . ? C28 C29 C40 C41 173.8(3) . . . . ? C30 C29 C40 C41 -3.6(6) . . . . ? C29 C40 C41 C42 10.0(5) . . . . ? C29 C40 C41 C46 -167.0(3) . . . . ? C46 C41 C42 C43 3.5(5) . . . . ? C40 C41 C42 C43 -173.6(3) . . . . ? C41 C42 C43 C44 0.0(5) . . . . ? C42 C43 C44 C45 -2.4(5) . . . . ? C42 C43 C44 C51 172.6(3) . . . . ? C43 C44 C45 C46 1.3(5) . . . . ? C51 C44 C45 C46 -173.7(3) . . . . ? C44 C45 C46 C41 2.2(5) . . . . ? C42 C41 C46 C45 -4.5(5) . . . . ? C40 C41 C46 C45 172.8(3) . . . . ? C38 C37 C47 C49 23.2(5) . . . . ? C36 C37 C47 C49 -158.4(4) . . . . ? C38 C37 C47 C50 -96.5(4) . . . . ? C36 C37 C47 C50 81.9(4) . . . . ? C38 C37 C47 C48 144.1(4) . . . . ? C36 C37 C47 C48 -37.5(5) . . . . ? C45 C44 C51 C53 -33.2(4) . . . . ? C43 C44 C51 C53 152.1(3) . . . . ? C45 C44 C51 C52 -155.1(3) . . . . ? C43 C44 C51 C52 30.2(4) . . . . ? C45 C44 C51 C54 86.3(4) . . . . ? C43 C44 C51 C54 -88.4(3) . . . . ? O3 C55 C56 C58 6.5(3) . . . . ? C56 C55 C56 C58 -173.5(3) 2_655 . . . ? O3 C55 C56 C57 -176.10(15) . . . . ? C56 C55 C56 C57 3.90(15) 2_655 . . . ? C58 C56 C57 C57 167.2(3) . . . 2_655 ? C55 C56 C57 C57 -9.8(4) . . . 2_655 ? C55 C56 C58 C59 177.1(3) . . . . ? C57 C56 C58 C59 0.4(6) . . . . ? C56 C58 C59 C64 24.2(5) . . . . ? C56 C58 C59 C60 -156.7(3) . . . . ? C64 C59 C60 C61 -2.5(5) . . . . ? C58 C59 C60 C61 178.3(3) . . . . ? C59 C60 C61 C62 1.8(5) . . . . ? C60 C61 C62 C63 0.3(5) . . . . ? C60 C61 C62 C65 -177.1(3) . . . . ? C61 C62 C63 C64 -1.7(4) . . . . ? C65 C62 C63 C64 175.7(3) . . . . ? C60 C59 C64 C63 1.1(5) . . . . ? C58 C59 C64 C63 -179.7(3) . . . . ? C62 C63 C64 C59 1.0(5) . . . . ? C61 C62 C65 C67 -31.6(4) . . . . ? C63 C62 C65 C67 151.2(3) . . . . ? C61 C62 C65 C68 87.2(4) . . . . ? C63 C62 C65 C68 -90.0(3) . . . . ? C61 C62 C65 C66 -153.7(3) . . . . ? C63 C62 C65 C66 29.0(4) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 2 0 0 12680.40 13930.46 114.85 o