data_I 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 loop_ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 O' _chemical_formula_weight 372.53 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_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' _cell_length_a 41.246(7) _cell_length_b 6.2930(10) _cell_length_c 43.001(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.243(4) _cell_angle_gamma 90.00 _cell_volume 11131(3) _cell_formula_units_Z 20 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2156 _cell_measurement_theta_min 5.282 _cell_measurement_theta_max 40.814 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.497 _exptl_crystal_size_mid 0.411 _exptl_crystal_size_min 0.176 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4040 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.76060 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28046 _diffrn_reflns_av_R_equivalents 0.1284 _diffrn_reflns_av_sigmaI/netI 0.1307 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10373 _reflns_number_gt 4318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _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_number_reflns 10373 _refine_ls_number_parameters 648 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1631 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1461 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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_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_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) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.199 _refine_diff_density_min -0.182 _refine_diff_density_rms 0.052