# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chunju Li' _publ_contact_author_email cjli@shu.edu.cn loop_ _publ_author_name 'Xiaoyan Shu' 'Jiazeng Fan' 'Jian Li' 'Xiaoyang Wang' 'Wei Chen' 'Xueshun Jia' 'Chunju Li' data_mo11011b _database_code_depnum_ccdc_archive 'CCDC 852484' #TrackingRef 'DClBu-EtP5A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H78 Cl2 O10' _chemical_formula_weight 1018.11 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 42.526(8) _cell_length_b 15.758(3) _cell_length_c 16.686(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11181(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9211 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4368 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9582 _exptl_absorpt_correction_T_max 0.9664 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49628 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10399 _reflns_number_gt 7669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^2^+70.1299P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10399 _refine_ls_number_parameters 650 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1516 _refine_ls_R_factor_gt 0.1193 _refine_ls_wR_factor_ref 0.3259 _refine_ls_wR_factor_gt 0.2971 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.11790(10) 0.4522(3) 0.4668(2) 0.0414(10) Uani 1 1 d . . . O2 O 0.05513(10) 0.7140(3) 0.3132(2) 0.0432(10) Uani 1 1 d . . . O3 O 0.21910(9) 0.5677(3) 0.5881(2) 0.0385(9) Uani 1 1 d . . . O4 O 0.17837(11) 0.6917(3) 0.2962(2) 0.0466(11) Uani 1 1 d . . . O5 O 0.19093(9) 0.7876(2) 0.7922(2) 0.0367(9) Uani 1 1 d . . . O6 O 0.23095(10) 0.8862(3) 0.4904(2) 0.0400(10) Uani 1 1 d . . . O7 O 0.07048(8) 0.8048(3) 0.7959(2) 0.0347(9) Uani 1 1 d . . . O8 O 0.13991(9) 1.0383(3) 0.6229(3) 0.0424(10) Uani 1 1 d . . . O9 O 0.03597(10) 0.9359(3) 0.5197(2) 0.0400(10) Uani 1 1 d . . . O10 O 0.02550(10) 0.5977(3) 0.6048(3) 0.0447(10) Uani 1 1 d . . . C1 C 0.05622(12) 0.6080(4) 0.4129(3) 0.0316(12) Uani 1 1 d . . . C2 C 0.07185(13) 0.5424(3) 0.4518(3) 0.0340(12) Uani 1 1 d . . . H2 H 0.0614 0.5128 0.4936 0.041 Uiso 1 1 calc R . . C3 C 0.10211(13) 0.5191(4) 0.4315(3) 0.0338(12) Uani 1 1 d . . . C4 C 0.11807(13) 0.5606(3) 0.3690(3) 0.0315(12) Uani 1 1 d . . . C5 C 0.10196(14) 0.6264(3) 0.3297(3) 0.0348(13) Uani 1 1 d . . . H5 H 0.1122 0.6556 0.2872 0.042 Uiso 1 1 calc R . . C6 C 0.07184(13) 0.6499(4) 0.3506(3) 0.0328(12) Uani 1 1 d . . . C7 C 0.10819(16) 0.4281(4) 0.5453(4) 0.0453(15) Uani 1 1 d . . . H7A H 0.0860 0.4089 0.5442 0.054 Uiso 1 1 calc R . . H7B H 0.1098 0.4773 0.5820 0.054 Uiso 1 1 calc R . . C8 C 0.12883(18) 0.3582(5) 0.5738(4) 0.0563(19) Uani 1 1 d . . . H8A H 0.1248 0.3070 0.5421 0.085 Uiso 1 1 calc R . . H8B H 0.1244 0.3466 0.6304 0.085 Uiso 1 1 calc R . . H8C H 0.1509 0.3748 0.5676 0.085 Uiso 1 1 calc R . . C9 C 0.06900(16) 0.7532(5) 0.2448(4) 0.0512(17) Uani 1 1 d . . . H9A H 0.0745 0.7098 0.2043 0.061 Uiso 1 1 calc R . . H9B H 0.0884 0.7838 0.2603 0.061 Uiso 1 1 calc R . . C10 C 0.04529(19) 0.8140(5) 0.2111(5) 0.070(2) Uani 1 1 d . . . H10A H 0.0249 0.7854 0.2057 0.106 Uiso 1 1 calc R . . H10B H 0.0523 0.8338 0.1584 0.106 Uiso 1 1 calc R . . H10C H 0.0431 0.8627 0.2472 0.106 Uiso 1 1 calc R . . C11 C 0.15118(13) 0.5375(4) 0.3462(3) 0.0354(13) Uani 1 1 d . . . H11A H 0.1544 0.5503 0.2886 0.042 Uiso 1 1 calc R . . H11B H 0.1541 0.4757 0.3536 0.042 Uiso 1 1 calc R . . C12 C 0.17622(13) 0.5854(3) 0.3958(3) 0.0312(12) Uani 1 1 d . . . C13 C 0.18604(13) 0.5532(4) 0.4685(3) 0.0340(12) Uani 1 1 d . . . H13 H 0.1774 0.5014 0.4874 0.041 Uiso 1 1 calc R . . C14 C 0.20850(12) 0.5955(4) 0.5150(3) 0.0325(12) Uani 1 1 d . . . C15 C 0.22173(12) 0.6708(4) 0.4874(3) 0.0322(12) Uani 1 1 d . . . C16 C 0.21190(14) 0.7022(4) 0.4139(4) 0.0395(14) Uani 1 1 d . . . H16 H 0.2209 0.7532 0.3941 0.047 Uiso 1 1 calc R . . C17 C 0.18917(14) 0.6607(4) 0.3685(3) 0.0349(13) Uani 1 1 d . . . C18 C 0.20645(13) 0.4893(4) 0.6185(3) 0.0385(13) Uani 1 1 d . . . H18A H 0.2118 0.4419 0.5821 0.046 Uiso 1 1 calc R . . H18B H 0.1833 0.4931 0.6227 0.046 Uiso 1 1 calc R . . C19 C 0.22057(15) 0.4751(4) 0.6990(3) 0.0443(15) Uani 1 1 d . . . H19A H 0.2435 0.4708 0.6939 0.066 Uiso 1 1 calc R . . H19B H 0.2123 0.4223 0.7218 0.066 Uiso 1 1 calc R . . H19C H 0.2152 0.5226 0.7343 0.066 Uiso 1 1 calc R . . C20 C 0.1935(2) 0.7674(4) 0.2665(4) 0.065(2) Uani 1 1 d . . . H20A H 0.1895 0.8154 0.3034 0.078 Uiso 1 1 calc R . . H20B H 0.2165 0.7583 0.2632 0.078 Uiso 1 1 calc R . . C21 C 0.1811(2) 0.7863(5) 0.1885(5) 0.074(3) Uani 1 1 d . . . H21A H 0.1854 0.7388 0.1522 0.111 Uiso 1 1 calc R . . H21B H 0.1911 0.8378 0.1677 0.111 Uiso 1 1 calc R . . H21C H 0.1584 0.7952 0.1923 0.111 Uiso 1 1 calc R . . C22 C 0.24520(13) 0.7198(4) 0.5380(4) 0.0395(14) Uani 1 1 d . . . H22A H 0.2576 0.6797 0.5710 0.047 Uiso 1 1 calc R . . H22B H 0.2599 0.7507 0.5025 0.047 Uiso 1 1 calc R . . C23 C 0.22845(12) 0.7821(3) 0.5918(3) 0.0294(11) Uani 1 1 d . . . C24 C 0.21881(12) 0.7570(4) 0.6676(3) 0.0311(12) Uani 1 1 d . . . H24 H 0.2243 0.7020 0.6862 0.037 Uiso 1 1 calc R . . C25 C 0.20127(11) 0.8105(4) 0.7172(3) 0.0281(11) Uani 1 1 d . . . C26 C 0.19285(12) 0.8907(3) 0.6902(3) 0.0282(11) Uani 1 1 d . . . C27 C 0.20270(12) 0.9168(4) 0.6149(3) 0.0323(12) Uani 1 1 d . . . H27 H 0.1975 0.9722 0.5966 0.039 Uiso 1 1 calc R . . C28 C 0.22014(12) 0.8630(4) 0.5657(3) 0.0302(12) Uani 1 1 d . . . C29 C 0.19967(13) 0.7057(4) 0.8213(3) 0.0351(13) Uani 1 1 d . . . H29A H 0.2228 0.7019 0.8265 0.042 Uiso 1 1 calc R . . H29B H 0.1925 0.6612 0.7835 0.042 Uiso 1 1 calc R . . C30 C 0.18443(15) 0.6936(4) 0.9013(4) 0.0414(14) Uani 1 1 d . . . H30A H 0.1910 0.7391 0.9376 0.062 Uiso 1 1 calc R . . H30B H 0.1907 0.6386 0.9236 0.062 Uiso 1 1 calc R . . H30C H 0.1615 0.6950 0.8951 0.062 Uiso 1 1 calc R . . C31 C 0.22213(14) 0.9676(4) 0.4606(3) 0.0394(14) Uani 1 1 d . . . H31A H 0.2293 1.0126 0.4977 0.047 Uiso 1 1 calc R . . H31B H 0.1990 0.9713 0.4554 0.047 Uiso 1 1 calc R . . C32 C 0.23744(15) 0.9786(5) 0.3797(4) 0.0465(16) Uani 1 1 d . . . H32A H 0.2603 0.9727 0.3852 0.070 Uiso 1 1 calc R . . H32B H 0.2325 1.0350 0.3585 0.070 Uiso 1 1 calc R . . H32C H 0.2295 0.9352 0.3428 0.070 Uiso 1 1 calc R . . C33 C 0.17223(13) 0.9483(4) 0.7419(3) 0.0343(12) Uani 1 1 d . . . H33A H 0.1766 0.9366 0.7992 0.041 Uiso 1 1 calc R . . H33B H 0.1778 1.0082 0.7313 0.041 Uiso 1 1 calc R . . C34 C 0.13750(12) 0.9358(3) 0.7261(3) 0.0264(11) Uani 1 1 d . . . C35 C 0.12021(12) 0.8768(3) 0.7703(3) 0.0286(11) Uani 1 1 d . . . H35 H 0.1304 0.8446 0.8108 0.034 Uiso 1 1 calc R . . C36 C 0.08871(13) 0.8643(3) 0.7566(3) 0.0303(11) Uani 1 1 d . . . C37 C 0.07269(12) 0.9122(3) 0.6994(3) 0.0303(11) Uani 1 1 d . . . C38 C 0.08989(13) 0.9711(4) 0.6552(3) 0.0343(12) Uani 1 1 d . . . H38 H 0.0794 1.0044 0.6159 0.041 Uiso 1 1 calc R . . C39 C 0.12186(12) 0.9824(3) 0.6672(3) 0.0307(12) Uani 1 1 d . . . C40 C 0.08464(14) 0.7558(4) 0.8583(4) 0.0423(14) Uani 1 1 d . . . H40A H 0.0936 0.7936 0.8998 0.051 Uiso 1 1 calc R . . H40B H 0.1017 0.7201 0.8363 0.051 Uiso 1 1 calc R . . C41 C 0.05927(16) 0.7013(5) 0.8934(5) 0.060(2) Uani 1 1 d . . . H41A H 0.0420 0.7373 0.9121 0.090 Uiso 1 1 calc R . . H41B H 0.0678 0.6690 0.9387 0.090 Uiso 1 1 calc R . . H41C H 0.0515 0.6620 0.8525 0.090 Uiso 1 1 calc R . . C42 C 0.12541(15) 1.0775(4) 0.5558(4) 0.0452(15) Uani 1 1 d . . . H42A H 0.1095 1.1192 0.5741 0.054 Uiso 1 1 calc R . . H42B H 0.1147 1.0342 0.5226 0.054 Uiso 1 1 calc R . . C43 C 0.15054(17) 1.1216(5) 0.5072(4) 0.0550(18) Uani 1 1 d . . . H43A H 0.1600 1.1670 0.5392 0.083 Uiso 1 1 calc R . . H43B H 0.1411 1.1457 0.4587 0.083 Uiso 1 1 calc R . . H43C H 0.1668 1.0805 0.4921 0.083 Uiso 1 1 calc R . . C44 C 0.03805(13) 0.8990(4) 0.6832(3) 0.0374(13) Uani 1 1 d . . . H44A H 0.0274 0.8822 0.7335 0.045 Uiso 1 1 calc R . . H44B H 0.0286 0.9530 0.6647 0.045 Uiso 1 1 calc R . . C45 C 0.03292(11) 0.8316(4) 0.6207(3) 0.0311(12) Uani 1 1 d . . . C46 C 0.03023(12) 0.7467(4) 0.6424(3) 0.0319(12) Uani 1 1 d . . . H46 H 0.0302 0.7321 0.6977 0.038 Uiso 1 1 calc R . . C47 C 0.02751(12) 0.6827(4) 0.5853(3) 0.0339(12) Uani 1 1 d . . . C48 C 0.02526(11) 0.7027(4) 0.5037(3) 0.0315(12) Uani 1 1 d . . . C49 C 0.02780(12) 0.7882(4) 0.4817(3) 0.0350(13) Uani 1 1 d . . . H49 H 0.0267 0.8032 0.4267 0.042 Uiso 1 1 calc R . . C50 C 0.03195(11) 0.8516(4) 0.5389(3) 0.0300(12) Uani 1 1 d . . . C51 C 0.03546(15) 0.9587(4) 0.4366(4) 0.0433(15) Uani 1 1 d . . . H51A H 0.0143 0.9487 0.4137 0.052 Uiso 1 1 calc R . . H51B H 0.0509 0.9244 0.4063 0.052 Uiso 1 1 calc R . . C52 C 0.04373(16) 1.0513(4) 0.4319(4) 0.0529(17) Uani 1 1 d . . . H52A H 0.0311 1.0831 0.4707 0.079 Uiso 1 1 calc R . . H52B H 0.0394 1.0723 0.3777 0.079 Uiso 1 1 calc R . . H52C H 0.0661 1.0588 0.4442 0.079 Uiso 1 1 calc R . . C53 C 0.03751(19) 0.5732(5) 0.6814(4) 0.059(2) Uani 1 1 d . . . H53A H 0.0245 0.5984 0.7245 0.071 Uiso 1 1 calc R . . H53B H 0.0594 0.5938 0.6878 0.071 Uiso 1 1 calc R . . C54 C 0.0367(2) 0.4787(4) 0.6869(5) 0.062(2) Uani 1 1 d . . . H54A H 0.0148 0.4591 0.6837 0.093 Uiso 1 1 calc R . . H54B H 0.0459 0.4607 0.7381 0.093 Uiso 1 1 calc R . . H54C H 0.0488 0.4542 0.6426 0.093 Uiso 1 1 calc R . . C55 C 0.02367(13) 0.6353(4) 0.4402(4) 0.0385(13) Uani 1 1 d . . . H55A H 0.0117 0.6573 0.3937 0.046 Uiso 1 1 calc R . . H55B H 0.0123 0.5855 0.4616 0.046 Uiso 1 1 calc R . . C56 C 0.1160(5) 0.3036(9) 0.1135(9) 0.237(12) Uani 1 1 d D . . H56A H 0.1058 0.2574 0.1443 0.284 Uiso 1 1 calc R . . H56B H 0.0990 0.3327 0.0836 0.284 Uiso 1 1 calc R . . C57 C 0.1345(3) 0.2652(7) 0.0576(8) 0.148(6) Uani 1 1 d D . . H57A H 0.1522 0.2376 0.0860 0.177 Uiso 1 1 calc R . . H57B H 0.1436 0.3101 0.0231 0.177 Uiso 1 1 calc R . . C58 C 0.1204(3) 0.2042(6) 0.0073(6) 0.106(4) Uani 1 1 d D . . H58A H 0.1118 0.1580 0.0411 0.127 Uiso 1 1 calc R . . H58B H 0.1025 0.2310 -0.0209 0.127 Uiso 1 1 calc R . . C59 C 0.1403(4) 0.1689(11) -0.0491(10) 0.210(9) Uani 1 1 d D . . H59A H 0.1582 0.1440 -0.0195 0.252 Uiso 1 1 calc R . . H59B H 0.1489 0.2164 -0.0813 0.252 Uiso 1 1 calc R . . Cl1 Cl 0.13039(5) 0.37871(15) 0.18608(14) 0.0767(6) Uani 1 1 d D . . Cl2 Cl 0.12714(6) 0.09096(16) -0.11756(15) 0.0849(7) Uani 1 1 d D . . 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 0.048(2) 0.038(2) 0.039(2) 0.0125(18) 0.0081(19) 0.0081(19) O2 0.044(2) 0.049(3) 0.036(2) 0.0098(19) -0.0016(18) 0.007(2) O3 0.037(2) 0.047(2) 0.032(2) 0.0051(18) -0.0009(17) -0.0019(18) O4 0.070(3) 0.041(2) 0.029(2) 0.0064(18) 0.001(2) -0.005(2) O5 0.043(2) 0.036(2) 0.031(2) 0.0057(17) 0.0041(17) 0.0028(18) O6 0.044(2) 0.046(2) 0.030(2) 0.0022(18) 0.0053(18) -0.0046(19) O7 0.0268(19) 0.045(2) 0.032(2) 0.0102(17) -0.0022(16) -0.0040(17) O8 0.035(2) 0.045(2) 0.047(2) 0.020(2) -0.0089(19) -0.0097(18) O9 0.044(2) 0.040(2) 0.037(2) 0.0076(18) 0.0004(18) 0.0054(18) O10 0.052(3) 0.039(2) 0.043(2) 0.0062(19) -0.006(2) -0.007(2) C1 0.030(3) 0.038(3) 0.027(3) -0.004(2) -0.008(2) -0.002(2) C2 0.040(3) 0.032(3) 0.030(3) 0.005(2) 0.002(2) -0.005(2) C3 0.040(3) 0.033(3) 0.029(3) 0.001(2) 0.001(2) -0.001(2) C4 0.037(3) 0.031(3) 0.027(3) -0.002(2) -0.002(2) -0.001(2) C5 0.050(3) 0.031(3) 0.023(3) 0.002(2) 0.002(2) -0.007(3) C6 0.039(3) 0.033(3) 0.027(3) -0.001(2) -0.010(2) 0.001(2) C7 0.057(4) 0.047(4) 0.032(3) 0.007(3) 0.003(3) 0.008(3) C8 0.068(5) 0.051(4) 0.050(4) 0.020(3) 0.013(3) 0.016(4) C9 0.052(4) 0.060(4) 0.042(3) 0.021(3) -0.001(3) 0.005(3) C10 0.067(5) 0.075(5) 0.070(5) 0.031(4) 0.004(4) 0.013(4) C11 0.040(3) 0.042(3) 0.025(3) -0.004(2) 0.001(2) -0.001(3) C12 0.035(3) 0.031(3) 0.027(3) -0.003(2) 0.008(2) 0.002(2) C13 0.033(3) 0.036(3) 0.033(3) 0.003(2) 0.009(2) 0.005(2) C14 0.029(3) 0.039(3) 0.030(3) -0.001(2) 0.007(2) 0.003(2) C15 0.027(3) 0.040(3) 0.030(3) -0.001(2) 0.012(2) 0.000(2) C16 0.038(3) 0.041(3) 0.039(3) -0.001(3) 0.008(3) -0.005(3) C17 0.040(3) 0.035(3) 0.030(3) 0.000(2) 0.006(2) 0.005(2) C18 0.034(3) 0.044(3) 0.037(3) 0.005(3) 0.008(2) 0.001(3) C19 0.042(3) 0.057(4) 0.033(3) 0.005(3) 0.002(3) 0.009(3) C20 0.107(7) 0.041(4) 0.046(4) 0.006(3) -0.008(4) -0.018(4) C21 0.114(7) 0.056(5) 0.053(4) 0.011(4) -0.011(5) -0.016(5) C22 0.026(3) 0.051(4) 0.042(3) -0.002(3) 0.012(2) -0.001(3) C23 0.021(2) 0.038(3) 0.028(3) -0.007(2) 0.003(2) -0.003(2) C24 0.020(2) 0.036(3) 0.037(3) 0.000(2) 0.005(2) -0.002(2) C25 0.016(2) 0.042(3) 0.026(3) -0.004(2) 0.000(2) -0.001(2) C26 0.023(2) 0.030(3) 0.031(3) -0.002(2) -0.002(2) -0.008(2) C27 0.027(3) 0.037(3) 0.033(3) 0.000(2) -0.004(2) -0.007(2) C28 0.026(3) 0.037(3) 0.027(3) 0.000(2) 0.003(2) -0.008(2) C29 0.033(3) 0.036(3) 0.035(3) 0.001(2) 0.002(2) 0.004(2) C30 0.048(4) 0.037(3) 0.040(3) 0.004(3) 0.005(3) -0.001(3) C31 0.037(3) 0.045(3) 0.036(3) 0.008(3) 0.006(3) -0.005(3) C32 0.041(3) 0.061(4) 0.038(3) 0.009(3) -0.007(3) -0.008(3) C33 0.033(3) 0.032(3) 0.038(3) -0.004(2) -0.006(2) -0.004(2) C34 0.024(3) 0.032(3) 0.023(2) -0.004(2) 0.003(2) 0.001(2) C35 0.028(3) 0.032(3) 0.026(3) -0.003(2) 0.000(2) 0.005(2) C36 0.032(3) 0.034(3) 0.025(3) -0.003(2) 0.004(2) 0.000(2) C37 0.029(3) 0.035(3) 0.027(3) -0.003(2) 0.002(2) 0.004(2) C38 0.034(3) 0.035(3) 0.034(3) 0.006(2) -0.005(2) 0.007(2) C39 0.033(3) 0.030(3) 0.030(3) 0.002(2) 0.002(2) -0.004(2) C40 0.033(3) 0.050(4) 0.043(3) 0.013(3) -0.004(3) -0.002(3) C41 0.045(4) 0.067(5) 0.068(5) 0.032(4) 0.002(3) -0.005(3) C42 0.040(3) 0.052(4) 0.043(3) 0.018(3) -0.004(3) -0.006(3) C43 0.059(4) 0.055(4) 0.051(4) 0.020(3) 0.004(3) -0.004(3) C44 0.032(3) 0.044(3) 0.036(3) 0.000(3) 0.006(2) 0.008(3) C45 0.016(2) 0.047(3) 0.031(3) 0.002(2) 0.002(2) 0.004(2) C46 0.024(3) 0.040(3) 0.032(3) 0.005(2) -0.001(2) 0.000(2) C47 0.023(3) 0.041(3) 0.038(3) 0.005(3) -0.007(2) 0.000(2) C48 0.015(2) 0.044(3) 0.035(3) 0.004(2) 0.001(2) 0.001(2) C49 0.025(3) 0.046(3) 0.033(3) 0.004(3) -0.005(2) 0.004(2) C50 0.017(2) 0.041(3) 0.032(3) 0.004(2) -0.002(2) 0.004(2) C51 0.039(3) 0.052(4) 0.040(3) 0.011(3) 0.000(3) 0.007(3) C52 0.045(4) 0.057(4) 0.056(4) 0.021(3) 0.004(3) 0.004(3) C53 0.064(5) 0.058(4) 0.056(4) 0.022(4) -0.018(4) -0.012(4) C54 0.080(5) 0.050(4) 0.055(4) 0.019(4) 0.000(4) -0.008(4) C55 0.030(3) 0.048(4) 0.038(3) 0.003(3) -0.008(2) -0.005(3) C56 0.43(4) 0.114(14) 0.166(18) 0.023(13) 0.07(2) -0.049(19) C57 0.25(2) 0.073(8) 0.118(11) 0.002(8) 0.011(12) -0.021(10) C58 0.154(11) 0.061(6) 0.102(8) 0.018(6) 0.031(8) 0.011(7) C59 0.25(2) 0.159(16) 0.22(2) -0.076(16) 0.035(18) -0.050(16) Cl1 0.0724(13) 0.0805(15) 0.0772(14) 0.0071(11) -0.0178(11) -0.0137(11) Cl2 0.0961(17) 0.0789(15) 0.0796(15) -0.0082(12) 0.0009(13) 0.0056(13) _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 C3 1.382(7) . ? O1 C7 1.424(7) . ? O2 C6 1.383(7) . ? O2 C9 1.427(7) . ? O3 C14 1.373(7) . ? O3 C18 1.438(7) . ? O4 C17 1.380(7) . ? O4 C20 1.442(8) . ? O5 C25 1.375(6) . ? O5 C29 1.428(7) . ? O6 C28 1.386(6) . ? O6 C31 1.426(7) . ? O7 C36 1.382(6) . ? O7 C40 1.428(7) . ? O8 C39 1.383(6) . ? O8 C42 1.420(7) . ? O9 C50 1.377(7) . ? O9 C51 1.433(7) . ? O10 C47 1.380(7) . ? O10 C53 1.431(8) . ? C1 C2 1.390(8) . ? C1 C6 1.398(8) . ? C1 C55 1.520(8) . ? C2 C3 1.380(8) . ? C2 H2 0.9500 . ? C3 C4 1.405(8) . ? C4 C5 1.406(8) . ? C4 C11 1.503(8) . ? C5 C6 1.379(8) . ? C5 H5 0.9500 . ? C7 C8 1.487(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.500(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.546(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.380(8) . ? C12 C17 1.385(8) . ? C13 C14 1.400(8) . ? C13 H13 0.9500 . ? C14 C15 1.391(8) . ? C15 C16 1.387(8) . ? C15 C22 1.518(8) . ? C16 C17 1.391(8) . ? C16 H16 0.9500 . ? C18 C19 1.488(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.436(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.510(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.387(7) . ? C23 C28 1.393(8) . ? C24 C25 1.397(7) . ? C24 H24 0.9500 . ? C25 C26 1.388(8) . ? C26 C27 1.387(7) . ? C26 C33 1.530(8) . ? C27 C28 1.394(8) . ? C27 H27 0.9500 . ? C29 C30 1.497(8) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.508(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.513(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.395(7) . ? C34 C35 1.397(7) . ? C35 C36 1.373(7) . ? C35 H35 0.9500 . ? C36 C37 1.394(7) . ? C37 C38 1.393(8) . ? C37 C44 1.512(8) . ? C38 C39 1.386(8) . ? C38 H38 0.9500 . ? C40 C41 1.499(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.511(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.505(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.391(8) . ? C45 C50 1.402(7) . ? C46 C47 1.394(8) . ? C46 H46 0.9500 . ? C47 C48 1.400(8) . ? C48 C49 1.400(8) . ? C48 C55 1.501(8) . ? C49 C50 1.393(8) . ? C49 H49 0.9500 . ? C51 C52 1.502(9) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.493(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.363(9) . ? C56 Cl1 1.801(12) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.410(9) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.381(9) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 Cl2 1.768(11) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? 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 C3 O1 C7 117.0(4) . . ? C6 O2 C9 117.7(5) . . ? C14 O3 C18 117.7(4) . . ? C17 O4 C20 116.4(5) . . ? C25 O5 C29 117.6(4) . . ? C28 O6 C31 117.8(4) . . ? C36 O7 C40 118.4(4) . . ? C39 O8 C42 117.2(4) . . ? C50 O9 C51 117.7(5) . . ? C47 O10 C53 116.8(5) . . ? C2 C1 C6 118.1(5) . . ? C2 C1 C55 120.4(5) . . ? C6 C1 C55 121.5(5) . . ? C3 C2 C1 122.0(5) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 O1 123.5(5) . . ? C2 C3 C4 120.6(5) . . ? O1 C3 C4 115.9(5) . . ? C3 C4 C5 117.0(5) . . ? C3 C4 C11 121.9(5) . . ? C5 C4 C11 121.1(5) . . ? C6 C5 C4 122.2(5) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 O2 124.0(5) . . ? C5 C6 C1 120.2(5) . . ? O2 C6 C1 115.8(5) . . ? O1 C7 C8 108.7(5) . . ? O1 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O1 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C10 107.4(6) . . ? O2 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? O2 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 C12 113.0(4) . . ? C4 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C4 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C17 118.9(5) . . ? C13 C12 C11 120.0(5) . . ? C17 C12 C11 121.1(5) . . ? C12 C13 C14 121.3(5) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? O3 C14 C15 115.7(5) . . ? O3 C14 C13 124.4(5) . . ? C15 C14 C13 119.9(5) . . ? C16 C15 C14 118.3(5) . . ? C16 C15 C22 120.5(5) . . ? C14 C15 C22 121.1(5) . . ? C15 C16 C17 121.6(6) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? O4 C17 C12 117.3(5) . . ? O4 C17 C16 122.7(5) . . ? C12 C17 C16 120.0(5) . . ? O3 C18 C19 107.2(5) . . ? O3 C18 H18A 110.3 . . ? C19 C18 H18A 110.3 . . ? O3 C18 H18B 110.3 . . ? C19 C18 H18B 110.3 . . ? H18A C18 H18B 108.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 O4 108.6(6) . . ? C21 C20 H20A 110.0 . . ? O4 C20 H20A 110.0 . . ? C21 C20 H20B 110.0 . . ? O4 C20 H20B 110.0 . . ? H20A C20 H20B 108.3 . . ? 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 . . ? C23 C22 C15 110.6(4) . . ? C23 C22 H22A 109.5 . . ? C15 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C28 118.2(5) . . ? C24 C23 C22 119.7(5) . . ? C28 C23 C22 121.9(5) . . ? C23 C24 C25 121.7(5) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? O5 C25 C26 116.8(5) . . ? O5 C25 C24 123.5(5) . . ? C26 C25 C24 119.6(5) . . ? C27 C26 C25 119.1(5) . . ? C27 C26 C33 120.5(5) . . ? C25 C26 C33 120.3(5) . . ? C26 C27 C28 120.9(5) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? O6 C28 C23 116.1(5) . . ? O6 C28 C27 123.4(5) . . ? C23 C28 C27 120.5(5) . . ? O5 C29 C30 107.8(5) . . ? O5 C29 H29A 110.1 . . ? C30 C29 H29A 110.1 . . ? O5 C29 H29B 110.1 . . ? C30 C29 H29B 110.1 . . ? H29A C29 H29B 108.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O6 C31 C32 107.6(5) . . ? O6 C31 H31A 110.2 . . ? C32 C31 H31A 110.2 . . ? O6 C31 H31B 110.2 . . ? C32 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C26 112.5(4) . . ? C34 C33 H33A 109.1 . . ? C26 C33 H33A 109.1 . . ? C34 C33 H33B 109.1 . . ? C26 C33 H33B 109.1 . . ? H33A C33 H33B 107.8 . . ? C39 C34 C35 118.1(5) . . ? C39 C34 C33 121.3(5) . . ? C35 C34 C33 120.5(5) . . ? C36 C35 C34 121.4(5) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 O7 124.4(5) . . ? C35 C36 C37 120.9(5) . . ? O7 C36 C37 114.7(5) . . ? C38 C37 C36 117.8(5) . . ? C38 C37 C44 120.5(5) . . ? C36 C37 C44 121.6(5) . . ? C39 C38 C37 121.6(5) . . ? C39 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? O8 C39 C38 123.3(5) . . ? O8 C39 C34 116.5(5) . . ? C38 C39 C34 120.1(5) . . ? O7 C40 C41 106.9(5) . . ? O7 C40 H40A 110.3 . . ? C41 C40 H40A 110.3 . . ? O7 C40 H40B 110.3 . . ? C41 C40 H40B 110.3 . . ? H40A C40 H40B 108.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O8 C42 C43 108.5(5) . . ? O8 C42 H42A 110.0 . . ? C43 C42 H42A 110.0 . . ? O8 C42 H42B 110.0 . . ? C43 C42 H42B 110.0 . . ? H42A C42 H42B 108.4 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C37 111.2(4) . . ? C45 C44 H44A 109.4 . . ? C37 C44 H44A 109.4 . . ? C45 C44 H44B 109.4 . . ? C37 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C46 C45 C50 117.9(5) . . ? C46 C45 C44 120.6(5) . . ? C50 C45 C44 121.4(5) . . ? C45 C46 C47 121.7(5) . . ? C45 C46 H46 119.2 . . ? C47 C46 H46 119.2 . . ? O10 C47 C46 123.2(5) . . ? O10 C47 C48 116.3(5) . . ? C46 C47 C48 120.5(5) . . ? C47 C48 C49 117.8(5) . . ? C47 C48 C55 122.0(5) . . ? C49 C48 C55 119.9(5) . . ? C50 C49 C48 121.4(5) . . ? C50 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? O9 C50 C49 123.3(5) . . ? O9 C50 C45 116.1(5) . . ? C49 C50 C45 120.6(5) . . ? O9 C51 C52 106.9(5) . . ? O9 C51 H51A 110.3 . . ? C52 C51 H51A 110.3 . . ? O9 C51 H51B 110.3 . . ? C52 C51 H51B 110.3 . . ? H51A C51 H51B 108.6 . . ? 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 . . ? O10 C53 C54 108.4(6) . . ? O10 C53 H53A 110.0 . . ? C54 C53 H53A 110.0 . . ? O10 C53 H53B 110.0 . . ? C54 C53 H53B 110.0 . . ? H53A C53 H53B 108.4 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C48 C55 C1 111.8(4) . . ? C48 C55 H55A 109.3 . . ? C1 C55 H55A 109.3 . . ? C48 C55 H55B 109.3 . . ? C1 C55 H55B 109.3 . . ? H55A C55 H55B 107.9 . . ? C57 C56 Cl1 123.7(13) . . ? C57 C56 H56A 106.4 . . ? Cl1 C56 H56A 106.4 . . ? C57 C56 H56B 106.4 . . ? Cl1 C56 H56B 106.4 . . ? H56A C56 H56B 106.5 . . ? C56 C57 C58 117.7(10) . . ? C56 C57 H57A 107.9 . . ? C58 C57 H57A 107.9 . . ? C56 C57 H57B 107.9 . . ? C58 C57 H57B 107.9 . . ? H57A C57 H57B 107.2 . . ? C59 C58 C57 114.8(9) . . ? C59 C58 H58A 108.6 . . ? C57 C58 H58A 108.6 . . ? C59 C58 H58B 108.6 . . ? C57 C58 H58B 108.6 . . ? H58A C58 H58B 107.5 . . ? C58 C59 Cl2 121.7(11) . . ? C58 C59 H59A 106.9 . . ? Cl2 C59 H59A 106.9 . . ? C58 C59 H59B 106.9 . . ? Cl2 C59 H59B 106.9 . . ? H59A C59 H59B 106.7 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.073 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.094 data_mo_11012a_0m _database_code_depnum_ccdc_archive 'CCDC 863689' #TrackingRef 'DClBu-OctP5A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59.50 H99 Cl O5' _chemical_formula_weight 929.84 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.897(4) _cell_length_b 21.540(4) _cell_length_c 25.200(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.280(4) _cell_angle_gamma 90.00 _cell_volume 11761(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9941 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.93 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4104 _exptl_absorpt_coefficient_mu 0.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9632 _exptl_absorpt_correction_T_max 0.9683 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55903 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20013 _reflns_number_gt 11160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^2^+20.0282P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20013 _refine_ls_number_parameters 1171 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.2188 _refine_ls_R_factor_gt 0.1394 _refine_ls_wR_factor_ref 0.3894 _refine_ls_wR_factor_gt 0.3347 _refine_ls_goodness_of_fit_ref 1.508 _refine_ls_restrained_S_all 1.537 _refine_ls_shift/su_max 0.230 _refine_ls_shift/su_mean 0.006 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 -0.11086(18) 0.48905(18) 0.64211(16) 0.0420(10) Uani 1 1 d . . . O2 O 0.02794(17) 0.39623(17) 0.49267(14) 0.0362(9) Uani 1 1 d . . . O3 O 0.02805(18) 0.45190(17) 0.82652(15) 0.0399(10) Uani 1 1 d . . . O4 O 0.13303(18) 0.51956(19) 0.64823(15) 0.0436(10) Uani 1 1 d . . . O5 O 0.02581(18) 0.22792(18) 0.82585(17) 0.0449(10) Uani 1 1 d . . . O6 O 0.23684(19) 0.34831(19) 0.78310(18) 0.0515(11) Uani 1 1 d . . . O7 O -0.08564(17) 0.11736(18) 0.65800(16) 0.0423(10) Uani 1 1 d . . . O8 O 0.16851(18) 0.14429(19) 0.68749(16) 0.0454(10) Uani 1 1 d . . . O9 O -0.17155(17) 0.28367(17) 0.53861(16) 0.0417(10) Uani 1 1 d . . . O10 O 0.04506(18) 0.16833(17) 0.50310(17) 0.0453(10) Uani 1 1 d . . . C1 C -0.0791(2) 0.4662(2) 0.6030(2) 0.0307(12) Uani 1 1 d . . . C2 C -0.0191(2) 0.4899(2) 0.6030(2) 0.0304(12) Uani 1 1 d . . . C3 C 0.0164(3) 0.4667(2) 0.5661(2) 0.0321(12) Uani 1 1 d . . . H3 H 0.0570 0.4823 0.5662 0.038 Uiso 1 1 calc R . . C4 C -0.0057(2) 0.4218(2) 0.5294(2) 0.0286(12) Uani 1 1 d . . . C5 C -0.0668(3) 0.3999(2) 0.5273(2) 0.0311(12) Uani 1 1 d . . . C6 C -0.1020(3) 0.4230(2) 0.5647(2) 0.0331(13) Uani 1 1 d . . . H6 H -0.1432 0.4086 0.5639 0.040 Uiso 1 1 calc R . . C7 C 0.0067(3) 0.5391(2) 0.6429(2) 0.0367(13) Uani 1 1 d . . . H7A H -0.0278 0.5629 0.6544 0.044 Uiso 1 1 calc R . . H7B H 0.0323 0.5683 0.6253 0.044 Uiso 1 1 calc R . . C8 C 0.0454(2) 0.5113(2) 0.6917(2) 0.0302(12) Uani 1 1 d . . . C9 C 0.1083(2) 0.4991(2) 0.6927(2) 0.0304(12) Uani 1 1 d . . . C10 C 0.1416(3) 0.4708(2) 0.7370(2) 0.0367(13) Uani 1 1 d . . . H10 H 0.1843 0.4625 0.7371 0.044 Uiso 1 1 calc R . . C11 C 0.1145(3) 0.4542(2) 0.7811(2) 0.0317(12) Uani 1 1 d . . . C12 C 0.0518(2) 0.4671(2) 0.7808(2) 0.0293(12) Uani 1 1 d . . . C13 C 0.0187(3) 0.4945(2) 0.7361(2) 0.0331(13) Uani 1 1 d . . . H13 H -0.0241 0.5022 0.7358 0.040 Uiso 1 1 calc R . . C14 C 0.1513(3) 0.4191(3) 0.8280(2) 0.0411(14) Uani 1 1 d . . . H14A H 0.1956 0.4299 0.8308 0.049 Uiso 1 1 calc R . . H14B H 0.1366 0.4310 0.8620 0.049 Uiso 1 1 calc R . . C15 C 0.1428(3) 0.3502(2) 0.8189(2) 0.0338(13) Uani 1 1 d . . . C16 C 0.1851(3) 0.3163(2) 0.7939(2) 0.0338(13) Uani 1 1 d . . . C17 C 0.1756(3) 0.2539(3) 0.7823(2) 0.0371(13) Uani 1 1 d . . . H17 H 0.2060 0.2311 0.7672 0.044 Uiso 1 1 calc R . . C18 C 0.1219(2) 0.2241(2) 0.7926(2) 0.0316(12) Uani 1 1 d . . . C19 C 0.0788(2) 0.2586(2) 0.8166(2) 0.0308(12) Uani 1 1 d . . . C20 C 0.0903(3) 0.3197(3) 0.8301(2) 0.0349(13) Uani 1 1 d . . . H20 H 0.0615 0.3418 0.8477 0.042 Uiso 1 1 calc R . . C21 C 0.1104(3) 0.1558(3) 0.7787(2) 0.0416(15) Uani 1 1 d . . . H21A H 0.1507 0.1343 0.7815 0.050 Uiso 1 1 calc R . . H21B H 0.0873 0.1371 0.8058 0.050 Uiso 1 1 calc R . . C22 C 0.0755(2) 0.1439(2) 0.7243(2) 0.0330(13) Uani 1 1 d . . . C23 C 0.1043(2) 0.1373(2) 0.6789(2) 0.0325(13) Uani 1 1 d . . . C24 C 0.0713(3) 0.1235(2) 0.6285(2) 0.0388(14) Uani 1 1 d . . . H24 H 0.0927 0.1184 0.5986 0.047 Uiso 1 1 calc R . . C25 C 0.0072(3) 0.1172(2) 0.6219(2) 0.0345(13) Uani 1 1 d . . . C26 C -0.0221(2) 0.1242(2) 0.6663(2) 0.0316(12) Uani 1 1 d . . . C27 C 0.0111(3) 0.1380(2) 0.7170(2) 0.0400(14) Uani 1 1 d . . . H27 H -0.0105 0.1435 0.7468 0.048 Uiso 1 1 calc R . . C28 C -0.0282(3) 0.1047(3) 0.5667(2) 0.0449(15) Uani 1 1 d . . . H28A H -0.0650 0.0790 0.5698 0.054 Uiso 1 1 calc R . . H28B H -0.0018 0.0820 0.5446 0.054 Uiso 1 1 calc R . . C29 C -0.0480(3) 0.1670(2) 0.5404(2) 0.0323(13) Uani 1 1 d . . . C30 C -0.0077(2) 0.1991(2) 0.5116(2) 0.0328(13) Uani 1 1 d . . . C31 C -0.0235(3) 0.2584(2) 0.4925(2) 0.0325(13) Uani 1 1 d . . . H31 H 0.0035 0.2801 0.4727 0.039 Uiso 1 1 calc R . . C32 C -0.0781(2) 0.2867(2) 0.5022(2) 0.0295(12) Uani 1 1 d . . . C33 C -0.1174(2) 0.2537(2) 0.5301(2) 0.0320(12) Uani 1 1 d . . . C34 C -0.1027(3) 0.1941(2) 0.5485(2) 0.0330(13) Uani 1 1 d . . . H34 H -0.1306 0.1719 0.5670 0.040 Uiso 1 1 calc R . . C35 C -0.0924(3) 0.3532(2) 0.4848(2) 0.0383(14) Uani 1 1 d . . . H35A H -0.1377 0.3585 0.4766 0.046 Uiso 1 1 calc R . . H35B H -0.0746 0.3616 0.4515 0.046 Uiso 1 1 calc R . . C36 C -0.1677(3) 0.4601(3) 0.6489(2) 0.0395(14) Uani 1 1 d . . . H36A H -0.1625 0.4145 0.6504 0.047 Uiso 1 1 calc R . . H36B H -0.1997 0.4703 0.6183 0.047 Uiso 1 1 calc R . . C37 C -0.1870(3) 0.4830(3) 0.6999(3) 0.0507(17) Uani 1 1 d . . . H37A H -0.1929 0.5286 0.6975 0.061 Uiso 1 1 calc R . . H37B H -0.1535 0.4747 0.7298 0.061 Uiso 1 1 calc R . . C38 C -0.2452(3) 0.4538(3) 0.7125(3) 0.0589(19) Uani 1 1 d . . . H38A H -0.2387 0.4084 0.7155 0.071 Uiso 1 1 calc R . . H38B H -0.2782 0.4612 0.6819 0.071 Uiso 1 1 calc R . . C39 C -0.2674(3) 0.4765(4) 0.7628(3) 0.070(2) Uani 1 1 d . . . H39A H -0.2336 0.4705 0.7930 0.084 Uiso 1 1 calc R . . H39B H -0.2748 0.5217 0.7591 0.084 Uiso 1 1 calc R . . C40 C -0.3237(4) 0.4474(4) 0.7777(4) 0.091(3) Uani 1 1 d . . . H40A H -0.3569 0.4514 0.7468 0.109 Uiso 1 1 calc R . . H40B H -0.3155 0.4025 0.7834 0.109 Uiso 1 1 calc R . . C41 C -0.3473(4) 0.4721(5) 0.8257(4) 0.095(3) Uani 1 1 d . . . H41A H -0.3144 0.4672 0.8567 0.114 Uiso 1 1 calc R . . H41B H -0.3544 0.5172 0.8203 0.114 Uiso 1 1 calc R . . C42 C -0.4038(7) 0.4449(7) 0.8400(6) 0.170(7) Uani 1 1 d . . . H42A H -0.3985 0.3993 0.8428 0.204 Uiso 1 1 calc R . . H42B H -0.4381 0.4533 0.8108 0.204 Uiso 1 1 calc R . . C43 C -0.4215(9) 0.4689(9) 0.8920(8) 0.240(10) Uani 1 1 d . . . H43A H -0.3869 0.4921 0.9116 0.359 Uiso 1 1 calc R . . H43B H -0.4318 0.4339 0.9139 0.359 Uiso 1 1 calc R . . H43C H -0.4574 0.4964 0.8843 0.359 Uiso 1 1 calc R . . C44 C 0.0914(2) 0.4149(3) 0.4962(2) 0.0341(13) Uani 1 1 d . . . H44A H 0.1138 0.4045 0.5320 0.041 Uiso 1 1 calc R . . H44B H 0.0939 0.4604 0.4910 0.041 Uiso 1 1 calc R . . C45 C 0.1202(3) 0.3817(3) 0.4535(2) 0.0378(13) Uani 1 1 d . . . H45A H 0.0968 0.3918 0.4180 0.045 Uiso 1 1 calc R . . H45B H 0.1170 0.3363 0.4590 0.045 Uiso 1 1 calc R . . C46 C 0.1871(3) 0.3983(3) 0.4534(2) 0.0442(15) Uani 1 1 d . . . H46A H 0.2115 0.3829 0.4870 0.053 Uiso 1 1 calc R . . H46B H 0.1911 0.4441 0.4530 0.053 Uiso 1 1 calc R . . C47 C 0.2137(3) 0.3718(3) 0.4063(3) 0.0489(16) Uani 1 1 d . . . H47A H 0.2108 0.3260 0.4080 0.059 Uiso 1 1 calc R . . H47B H 0.1873 0.3853 0.3731 0.059 Uiso 1 1 calc R . . C48 C 0.2794(3) 0.3885(4) 0.4015(3) 0.0543(18) Uani 1 1 d . . . H48A H 0.3062 0.3738 0.4340 0.065 Uiso 1 1 calc R . . H48B H 0.2827 0.4343 0.4006 0.065 Uiso 1 1 calc R . . C49 C 0.3038(3) 0.3626(4) 0.3530(3) 0.0610(19) Uani 1 1 d . . . H49A H 0.3005 0.3168 0.3540 0.073 Uiso 1 1 calc R . . H49B H 0.2767 0.3771 0.3205 0.073 Uiso 1 1 calc R . . C50 C 0.3689(3) 0.3790(5) 0.3474(4) 0.085(3) Uani 1 1 d . . . H50A H 0.3961 0.3650 0.3800 0.102 Uiso 1 1 calc R . . H50B H 0.3723 0.4248 0.3457 0.102 Uiso 1 1 calc R . . C51 C 0.3922(4) 0.3515(5) 0.2989(4) 0.103(3) Uani 1 1 d . . . H51A H 0.3868 0.3063 0.2990 0.155 Uiso 1 1 calc R . . H51B H 0.4361 0.3613 0.3002 0.155 Uiso 1 1 calc R . . H51C H 0.3689 0.3689 0.2662 0.155 Uiso 1 1 calc R . . C52 C -0.0369(3) 0.4606(3) 0.8270(2) 0.0374(13) Uani 1 1 d . . . H52A H -0.0606 0.4321 0.8009 0.045 Uiso 1 1 calc R . . H52B H -0.0486 0.5038 0.8167 0.045 Uiso 1 1 calc R . . C53 C -0.0512(3) 0.4473(3) 0.8824(2) 0.0405(14) Uani 1 1 d . . . H53A H -0.0388 0.4042 0.8923 0.049 Uiso 1 1 calc R . . H53B H -0.0265 0.4755 0.9082 0.049 Uiso 1 1 calc R . . C54 C -0.1181(3) 0.4555(3) 0.8871(3) 0.0481(16) Uani 1 1 d . . . H54A H -0.1421 0.4231 0.8653 0.058 Uiso 1 1 calc R . . H54B H -0.1319 0.4963 0.8718 0.058 Uiso 1 1 calc R . . C55 C -0.1328(3) 0.4518(3) 0.9440(3) 0.0578(19) Uani 1 1 d . . . H55A H -0.1198 0.4106 0.9591 0.069 Uiso 1 1 calc R . . H55B H -0.1082 0.4836 0.9660 0.069 Uiso 1 1 calc R . . C56 C -0.1996(3) 0.4611(3) 0.9489(3) 0.063(2) Uani 1 1 d . . . H56A H -0.2240 0.4285 0.9277 0.076 Uiso 1 1 calc R . . H56B H -0.2129 0.5017 0.9327 0.076 Uiso 1 1 calc R . . C57 C -0.2148(4) 0.4595(4) 1.0061(3) 0.081(3) Uani 1 1 d . . . H57A H -0.2022 0.4187 1.0222 0.098 Uiso 1 1 calc R . . H57B H -0.1903 0.4918 1.0274 0.098 Uiso 1 1 calc R . . C58 C -0.2824(4) 0.4697(5) 1.0099(4) 0.096(3) Uani 1 1 d . . . H58A H -0.2951 0.5108 0.9944 0.115 Uiso 1 1 calc R . . H58B H -0.3071 0.4377 0.9884 0.115 Uiso 1 1 calc R . . C59 C -0.2962(5) 0.4671(6) 1.0659(5) 0.129(4) Uani 1 1 d . . . H59A H -0.2847 0.4262 1.0812 0.193 Uiso 1 1 calc R . . H59B H -0.3404 0.4741 1.0660 0.193 Uiso 1 1 calc R . . H59C H -0.2725 0.4993 1.0873 0.193 Uiso 1 1 calc R . . C60 C 0.1931(3) 0.4996(3) 0.6409(2) 0.0407(14) Uani 1 1 d . . . H60A H 0.1939 0.4539 0.6371 0.049 Uiso 1 1 calc R . . H60B H 0.2233 0.5116 0.6723 0.049 Uiso 1 1 calc R . . C61 C 0.2092(3) 0.5303(3) 0.5906(2) 0.0459(15) Uani 1 1 d . . . H61A H 0.1767 0.5206 0.5603 0.055 Uiso 1 1 calc R . . H61B H 0.2099 0.5759 0.5958 0.055 Uiso 1 1 calc R . . C62 C 0.2697(3) 0.5102(3) 0.5767(3) 0.0540(17) Uani 1 1 d . . . H62A H 0.2685 0.4649 0.5701 0.065 Uiso 1 1 calc R . . H62B H 0.3020 0.5183 0.6077 0.065 Uiso 1 1 calc R . . C63 C 0.2874(3) 0.5430(3) 0.5274(3) 0.0533(17) Uani 1 1 d . . . H63A H 0.2543 0.5360 0.4968 0.064 Uiso 1 1 calc R . . H63B H 0.2897 0.5882 0.5345 0.064 Uiso 1 1 calc R . . C64 C 0.3477(3) 0.5219(3) 0.5118(3) 0.0598(19) Uani 1 1 d . . . H64A H 0.3465 0.4762 0.5079 0.072 Uiso 1 1 calc R . . H64B H 0.3810 0.5320 0.5415 0.072 Uiso 1 1 calc R . . C65 C 0.3641(3) 0.5499(3) 0.4607(3) 0.0625(19) Uani 1 1 d . . . H65A H 0.3672 0.5955 0.4651 0.075 Uiso 1 1 calc R . . H65B H 0.3303 0.5412 0.4311 0.075 Uiso 1 1 calc R . . C66 C 0.4239(4) 0.5259(4) 0.4448(4) 0.087(3) Uani 1 1 d . . . H66A H 0.4582 0.5368 0.4733 0.104 Uiso 1 1 calc R . . H66B H 0.4218 0.4801 0.4424 0.104 Uiso 1 1 calc R . . C67 C 0.4381(5) 0.5514(5) 0.3921(4) 0.113(4) Uani 1 1 d . . . H67A H 0.4095 0.5334 0.3626 0.170 Uiso 1 1 calc R . . H67B H 0.4806 0.5405 0.3876 0.170 Uiso 1 1 calc R . . H67C H 0.4336 0.5966 0.3918 0.170 Uiso 1 1 calc R . . C68 C -0.0219(3) 0.2654(3) 0.8429(2) 0.0420(14) Uani 1 1 d . . . H68A H -0.0318 0.3004 0.8177 0.050 Uiso 1 1 calc R . . H68B H -0.0074 0.2829 0.8789 0.050 Uiso 1 1 calc R . . C69 C -0.0788(3) 0.2268(3) 0.8450(3) 0.0459(15) Uani 1 1 d . . . H69A H -0.0688 0.1918 0.8702 0.055 Uiso 1 1 calc R . . H69B H -0.0934 0.2095 0.8090 0.055 Uiso 1 1 calc R . . C70 C -0.1292(3) 0.2668(3) 0.8634(3) 0.0522(17) Uani 1 1 d . . . H70A H -0.1128 0.2859 0.8982 0.063 Uiso 1 1 calc R . . H70B H -0.1395 0.3008 0.8371 0.063 Uiso 1 1 calc R . . C71 C -0.1880(3) 0.2317(3) 0.8695(3) 0.0601(19) Uani 1 1 d . . . H71A H -0.2069 0.2162 0.8338 0.072 Uiso 1 1 calc R . . H71B H -0.1773 0.1951 0.8928 0.072 Uiso 1 1 calc R . . C72 C -0.2350(4) 0.2710(4) 0.8931(3) 0.074(2) Uani 1 1 d . . . H72A H -0.2150 0.2892 0.9274 0.089 Uiso 1 1 calc R . . H72B H -0.2481 0.3057 0.8683 0.089 Uiso 1 1 calc R . . C73 C -0.2914(4) 0.2349(5) 0.9033(4) 0.102(3) Uani 1 1 d . . . H73A H -0.2780 0.1998 0.9276 0.122 Uiso 1 1 calc R . . H73B H -0.3115 0.2172 0.8689 0.122 Uiso 1 1 calc R . . C74 C -0.3387(5) 0.2734(6) 0.9278(5) 0.136(5) Uani 1 1 d . . . H74A H -0.3527 0.3081 0.9033 0.163 Uiso 1 1 calc R . . H74B H -0.3186 0.2915 0.9621 0.163 Uiso 1 1 calc R . . C75 C -0.3954(5) 0.2356(8) 0.9385(6) 0.190(7) Uani 1 1 d . . . H75A H -0.4171 0.2197 0.9045 0.285 Uiso 1 1 calc R . . H75B H -0.4233 0.2623 0.9555 0.285 Uiso 1 1 calc R . . H75C H -0.3820 0.2008 0.9624 0.285 Uiso 1 1 calc R . . C76 C 0.2757(3) 0.3211(3) 0.7494(3) 0.063(2) Uani 1 1 d . . . H76A H 0.2513 0.3073 0.7153 0.075 Uiso 1 1 calc R . . H76B H 0.2975 0.2847 0.7672 0.075 Uiso 1 1 calc R . . C77 C 0.3212(4) 0.3705(4) 0.7392(4) 0.097(3) Uani 1 1 d . . . H77A H 0.2979 0.4063 0.7220 0.117 Uiso 1 1 calc R . . H77B H 0.3429 0.3848 0.7742 0.117 Uiso 1 1 calc R . . C78 C 0.3676(5) 0.3523(6) 0.7058(5) 0.126(4) Uani 1 1 d . . . H78A H 0.3875 0.3133 0.7200 0.151 Uiso 1 1 calc R . . H78B H 0.3998 0.3848 0.7081 0.151 Uiso 1 1 calc R . . C79 C 0.3416(5) 0.3431(5) 0.6490(5) 0.111(4) Uani 1 1 d . . . H79A H 0.3117 0.3768 0.6376 0.133 Uiso 1 1 calc R . . H79B H 0.3189 0.3032 0.6452 0.133 Uiso 1 1 calc R . . C80 C 0.3925(6) 0.3428(6) 0.6115(6) 0.134(5) Uani 1 1 d . . . H80A H 0.4125 0.3841 0.6139 0.161 Uiso 1 1 calc R . . H80B H 0.4243 0.3121 0.6260 0.161 Uiso 1 1 calc R . . C81 C 0.3739(6) 0.3290(7) 0.5559(5) 0.143(5) Uani 1 1 d D . . H81A H 0.3361 0.3533 0.5438 0.172 Uiso 1 1 calc R . . H81B H 0.3622 0.2846 0.5533 0.172 Uiso 1 1 calc R . . C82 C 0.4188(7) 0.3406(9) 0.5156(7) 0.209(9) Uani 1 1 d D . . H82A H 0.3953 0.3359 0.4792 0.250 Uiso 1 1 calc R . . H82B H 0.4321 0.3844 0.5194 0.250 Uiso 1 1 calc R . . C83 C 0.4665(7) 0.3078(8) 0.5178(7) 0.202(8) Uani 1 1 d D . . H83A H 0.4914 0.3223 0.4910 0.304 Uiso 1 1 calc R . . H83B H 0.4547 0.2644 0.5105 0.304 Uiso 1 1 calc R . . H83C H 0.4905 0.3110 0.5536 0.304 Uiso 1 1 calc R . . C84 C -0.1188(3) 0.1257(3) 0.7024(2) 0.0422(14) Uani 1 1 d . . . H84A H -0.1157 0.1695 0.7144 0.051 Uiso 1 1 calc R . . H84B H -0.1009 0.0990 0.7326 0.051 Uiso 1 1 calc R . . C85 C -0.1856(3) 0.1087(3) 0.6850(3) 0.0495(16) Uani 1 1 d . . . H85A H -0.2026 0.1346 0.6539 0.059 Uiso 1 1 calc R . . H85B H -0.1882 0.0647 0.6734 0.059 Uiso 1 1 calc R . . C86 C -0.2237(3) 0.1178(4) 0.7294(3) 0.062(2) Uani 1 1 d . . . H86A H -0.2277 0.1628 0.7361 0.074 Uiso 1 1 calc R . . H86B H -0.2021 0.0987 0.7626 0.074 Uiso 1 1 calc R . . C87 C -0.2885(4) 0.0891(5) 0.7163(4) 0.092(3) Uani 1 1 d . . . H87A H -0.3103 0.1091 0.6835 0.110 Uiso 1 1 calc R . . H87B H -0.2842 0.0444 0.7083 0.110 Uiso 1 1 calc R . . C88 C -0.3272(4) 0.0956(6) 0.7604(5) 0.135(5) Uani 1 1 d . . . H88A H -0.3358 0.1402 0.7655 0.162 Uiso 1 1 calc R . . H88B H -0.3036 0.0799 0.7942 0.162 Uiso 1 1 calc R . . C89 C -0.3904(5) 0.0594(7) 0.7489(7) 0.192(8) Uani 1 1 d D . . H89A H -0.4150 0.0766 0.7161 0.230 Uiso 1 1 calc R . . H89B H -0.3819 0.0152 0.7419 0.230 Uiso 1 1 calc R . . C90 C -0.4270(7) 0.0635(11) 0.7940(9) 0.36(2) Uani 1 1 d D . . H90A H -0.4028 0.0468 0.8271 0.431 Uiso 1 1 calc R . . H90B H -0.4373 0.1073 0.8004 0.431 Uiso 1 1 calc R . . C91 C -0.4829(10) 0.0279(11) 0.7804(14) 0.85(7) Uani 1 1 d D . . H91A H -0.5074 0.0299 0.8100 1.270 Uiso 1 1 calc R . . H91B H -0.4724 -0.0155 0.7740 1.270 Uiso 1 1 calc R . . H91C H -0.5069 0.0450 0.7479 1.270 Uiso 1 1 calc R . . C92 C 0.2005(3) 0.1407(3) 0.6422(3) 0.0451(15) Uani 1 1 d . . . H92A H 0.1845 0.1726 0.6155 0.054 Uiso 1 1 calc R . . H92B H 0.1939 0.0994 0.6251 0.054 Uiso 1 1 calc R . . C93 C 0.2681(3) 0.1509(3) 0.6598(3) 0.0484(16) Uani 1 1 d . . . H93A H 0.2834 0.1199 0.6875 0.058 Uiso 1 1 calc R . . H93B H 0.2745 0.1926 0.6760 0.058 Uiso 1 1 calc R . . C94 C 0.3045(3) 0.1455(4) 0.6135(3) 0.0578(18) Uani 1 1 d . . . H94A H 0.2908 0.1784 0.5871 0.069 Uiso 1 1 calc R . . H94B H 0.2952 0.1050 0.5956 0.069 Uiso 1 1 calc R . . C95 C 0.3738(3) 0.1508(4) 0.6299(3) 0.065(2) Uani 1 1 d . . . H95A H 0.3873 0.1199 0.6582 0.078 Uiso 1 1 calc R . . H95B H 0.3836 0.1926 0.6452 0.078 Uiso 1 1 calc R . . C96 C 0.4097(4) 0.1404(5) 0.5828(4) 0.090(3) Uani 1 1 d . . . H96A H 0.3987 0.0992 0.5666 0.109 Uiso 1 1 calc R . . H96B H 0.3974 0.1723 0.5550 0.109 Uiso 1 1 calc R . . C97 C 0.4785(4) 0.1435(5) 0.5997(5) 0.110(4) Uani 1 1 d D . . H97A H 0.4906 0.1213 0.6340 0.132 Uiso 1 1 calc R . . H97B H 0.4927 0.1871 0.6039 0.132 Uiso 1 1 calc R . . C98 C 0.5121(6) 0.1039(15) 0.5429(8) 0.34(2) Uani 1 1 d D . . H98A H 0.5212 0.0592 0.5487 0.411 Uiso 1 1 calc R . . H98B H 0.4891 0.1118 0.5068 0.411 Uiso 1 1 calc R . . C99 C 0.5617(10) 0.1421(9) 0.5567(9) 0.37(2) Uani 1 1 d D . . H99A H 0.5921 0.1350 0.5325 0.555 Uiso 1 1 calc R . . H99B H 0.5804 0.1332 0.5937 0.555 Uiso 1 1 calc R . . H99C H 0.5480 0.1855 0.5540 0.555 Uiso 1 1 calc R . . C100 C -0.2098(3) 0.2528(3) 0.5713(3) 0.0574(19) Uani 1 1 d . . . H10A H -0.1849 0.2408 0.6058 0.069 Uiso 1 1 calc R . . H10B H -0.2267 0.2144 0.5532 0.069 Uiso 1 1 calc R . . C101 C -0.2612(4) 0.2939(3) 0.5818(4) 0.079(3) Uani 1 1 d . . . H10C H -0.2899 0.3004 0.5481 0.094 Uiso 1 1 calc R . . H10D H -0.2447 0.3348 0.5948 0.094 Uiso 1 1 calc R . . C102 C -0.2963(6) 0.2635(5) 0.6247(6) 0.157(6) Uani 1 1 d . . . H10E H -0.3133 0.2234 0.6100 0.188 Uiso 1 1 calc R . . H10F H -0.2656 0.2539 0.6564 0.188 Uiso 1 1 calc R . . C103 C -0.3425(5) 0.2949(5) 0.6418(4) 0.114(4) Uani 1 1 d . . . H10G H -0.3743 0.3026 0.6104 0.137 Uiso 1 1 calc R . . H10H H -0.3261 0.3359 0.6547 0.137 Uiso 1 1 calc R . . C104 C -0.3751(5) 0.2664(6) 0.6863(5) 0.127(4) Uani 1 1 d . . . H10I H -0.3876 0.2237 0.6751 0.152 Uiso 1 1 calc R . . H10J H -0.3442 0.2629 0.7190 0.152 Uiso 1 1 calc R . . C105 C -0.4298(7) 0.2984(8) 0.7014(6) 0.171(6) Uani 1 1 d D . . H10K H -0.4575 0.3082 0.6678 0.205 Uiso 1 1 calc R . . H10L H -0.4156 0.3384 0.7181 0.205 Uiso 1 1 calc R . . C106 C -0.4692(7) 0.2660(11) 0.7395(6) 0.252(12) Uani 1 1 d D . . H10Q H -0.5040 0.2932 0.7456 0.302 Uiso 1 1 calc R . . H10R H -0.4865 0.2268 0.7231 0.302 Uiso 1 1 calc R . . C108 C 0.0931(3) 0.2033(3) 0.4843(2) 0.0417(14) Uani 1 1 d . . . H10M H 0.1066 0.2373 0.5098 0.050 Uiso 1 1 calc R . . H10N H 0.0777 0.2220 0.4490 0.050 Uiso 1 1 calc R . . C109 C 0.1462(3) 0.1613(3) 0.4794(2) 0.0451(15) Uani 1 1 d . . . H10O H 0.1323 0.1273 0.4541 0.054 Uiso 1 1 calc R . . H10P H 0.1611 0.1427 0.5148 0.054 Uiso 1 1 calc R . . C110 C 0.1986(3) 0.1958(3) 0.4595(3) 0.0500(16) Uani 1 1 d . . . H11A H 0.2142 0.2277 0.4863 0.060 Uiso 1 1 calc R . . H11B H 0.1824 0.2175 0.4258 0.060 Uiso 1 1 calc R . . C111 C 0.2519(3) 0.1546(4) 0.4494(3) 0.0576(18) Uani 1 1 d . . . H11C H 0.2696 0.1346 0.4836 0.069 Uiso 1 1 calc R . . H11D H 0.2360 0.1214 0.4240 0.069 Uiso 1 1 calc R . . C112 C 0.3027(3) 0.1893(4) 0.4270(3) 0.070(2) Uani 1 1 d . . . H11E H 0.2847 0.2111 0.3939 0.084 Uiso 1 1 calc R . . H11F H 0.3200 0.2211 0.4533 0.084 Uiso 1 1 calc R . . C113 C 0.3543(4) 0.1477(5) 0.4145(4) 0.089(3) Uani 1 1 d . . . H11G H 0.3368 0.1150 0.3892 0.106 Uiso 1 1 calc R . . H11H H 0.3734 0.1270 0.4479 0.106 Uiso 1 1 calc R . . C114 C 0.4047(5) 0.1828(6) 0.3899(5) 0.130(4) Uani 1 1 d . . . H11I H 0.3857 0.2033 0.3564 0.156 Uiso 1 1 calc R . . H11J H 0.4221 0.2156 0.4152 0.156 Uiso 1 1 calc R . . C115 C 0.4562(5) 0.1414(8) 0.3776(6) 0.177(7) Uani 1 1 d . . . H11K H 0.4761 0.1219 0.4108 0.265 Uiso 1 1 calc R . . H11L H 0.4866 0.1661 0.3619 0.265 Uiso 1 1 calc R . . H11M H 0.4394 0.1091 0.3522 0.265 Uiso 1 1 calc R . . C117 C -0.0065(4) 0.3188(5) 0.6801(5) 0.138(6) Uani 1 1 d D . . H11N H 0.0090 0.3027 0.7163 0.166 Uiso 1 1 calc R . . H11O H -0.0103 0.3644 0.6835 0.166 Uiso 1 1 calc R . . C118 C 0.0420(6) 0.3070(5) 0.6459(4) 0.147(6) Uani 1 1 d D . . H11P H 0.0466 0.2613 0.6442 0.176 Uiso 1 1 calc R . . H11Q H 0.0248 0.3207 0.6093 0.176 Uiso 1 1 calc R . . Cl1 Cl -0.11549(16) 0.30982(11) 0.71122(10) 0.1139(10) Uani 1 1 d D . . Cl2 Cl 0.15863(15) 0.31047(10) 0.61278(10) 0.1125(10) Uani 1 1 d D . . C107 C -0.4351(12) 0.2545(15) 0.7845(8) 0.389(19) Uiso 1 1 d D . . H10S H -0.4603 0.2357 0.8093 0.584 Uiso 1 1 calc R . . H10T H -0.4170 0.2932 0.7998 0.584 Uiso 1 1 calc R . . H10U H -0.4021 0.2257 0.7785 0.584 Uiso 1 1 calc R . . C116 C -0.0661(5) 0.2952(6) 0.6656(5) 0.143(5) Uiso 1 1 d D . . H11R H -0.0633 0.2497 0.6608 0.171 Uiso 1 1 calc R . . H11S H -0.0838 0.3132 0.6306 0.171 Uiso 1 1 calc R . . C119 C 0.0979(6) 0.3298(8) 0.6556(7) 0.186(8) Uiso 1 1 d D . . H11T H 0.1147 0.3179 0.6928 0.223 Uiso 1 1 calc R . . H11U H 0.0937 0.3756 0.6553 0.223 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 0.043(2) 0.041(2) 0.048(2) -0.0104(18) 0.027(2) -0.0092(19) O2 0.040(2) 0.035(2) 0.037(2) -0.0056(17) 0.0193(18) -0.0005(18) O3 0.047(2) 0.040(2) 0.037(2) 0.0051(17) 0.0209(19) 0.0013(19) O4 0.039(2) 0.052(3) 0.042(2) 0.0135(19) 0.0153(19) 0.0046(19) O5 0.039(2) 0.038(2) 0.061(3) 0.007(2) 0.020(2) -0.0043(19) O6 0.042(3) 0.047(3) 0.069(3) -0.001(2) 0.021(2) -0.016(2) O7 0.031(2) 0.045(2) 0.052(2) 0.0068(19) 0.0078(19) -0.0032(18) O8 0.033(2) 0.053(3) 0.051(3) 0.009(2) 0.008(2) 0.0005(19) O9 0.035(2) 0.038(2) 0.056(3) 0.0079(19) 0.020(2) 0.0087(18) O10 0.042(2) 0.034(2) 0.065(3) 0.0000(19) 0.024(2) 0.0094(19) C1 0.034(3) 0.028(3) 0.034(3) 0.005(2) 0.016(2) 0.002(2) C2 0.035(3) 0.027(3) 0.030(3) 0.007(2) 0.010(2) 0.005(2) C3 0.037(3) 0.026(3) 0.035(3) 0.006(2) 0.010(2) 0.003(2) C4 0.035(3) 0.024(3) 0.029(3) 0.005(2) 0.014(2) 0.006(2) C5 0.039(3) 0.025(3) 0.029(3) 0.007(2) 0.005(2) 0.004(2) C6 0.040(3) 0.027(3) 0.033(3) 0.005(2) 0.008(3) 0.000(2) C7 0.041(3) 0.032(3) 0.039(3) 0.003(2) 0.011(3) 0.007(3) C8 0.034(3) 0.023(3) 0.034(3) -0.004(2) 0.007(2) -0.010(2) C9 0.035(3) 0.026(3) 0.034(3) -0.001(2) 0.016(2) -0.006(2) C10 0.041(3) 0.027(3) 0.043(3) -0.002(2) 0.009(3) 0.001(3) C11 0.039(3) 0.025(3) 0.032(3) -0.002(2) 0.008(2) -0.007(2) C12 0.038(3) 0.025(3) 0.028(3) 0.000(2) 0.015(2) -0.005(2) C13 0.037(3) 0.028(3) 0.037(3) -0.005(2) 0.011(3) -0.003(2) C14 0.042(4) 0.042(3) 0.036(3) 0.001(3) -0.001(3) -0.002(3) C15 0.037(3) 0.033(3) 0.031(3) 0.003(2) 0.002(2) -0.003(3) C16 0.033(3) 0.034(3) 0.036(3) 0.004(2) 0.007(3) -0.009(3) C17 0.031(3) 0.041(3) 0.039(3) 0.006(3) 0.007(3) -0.001(3) C18 0.028(3) 0.032(3) 0.034(3) 0.008(2) 0.002(2) 0.001(2) C19 0.025(3) 0.038(3) 0.029(3) 0.005(2) 0.002(2) -0.006(2) C20 0.036(3) 0.037(3) 0.031(3) 0.002(2) 0.003(2) -0.002(3) C21 0.037(3) 0.033(3) 0.054(4) 0.015(3) 0.002(3) 0.006(3) C22 0.032(3) 0.022(3) 0.045(3) 0.011(2) 0.004(3) 0.001(2) C23 0.022(3) 0.029(3) 0.046(3) 0.006(2) 0.004(3) 0.002(2) C24 0.045(4) 0.024(3) 0.050(4) 0.004(2) 0.016(3) 0.003(3) C25 0.036(3) 0.017(3) 0.051(3) 0.006(2) 0.007(3) 0.004(2) C26 0.026(3) 0.021(3) 0.047(3) 0.007(2) 0.002(3) 0.000(2) C27 0.050(4) 0.022(3) 0.051(4) 0.011(2) 0.018(3) 0.002(3) C28 0.049(4) 0.032(3) 0.052(4) 0.003(3) 0.003(3) -0.001(3) C29 0.034(3) 0.020(3) 0.042(3) -0.004(2) 0.003(3) 0.002(2) C30 0.027(3) 0.032(3) 0.040(3) 0.000(2) 0.006(2) 0.004(2) C31 0.037(3) 0.035(3) 0.026(3) -0.002(2) 0.005(2) -0.003(3) C32 0.032(3) 0.028(3) 0.027(3) 0.000(2) 0.002(2) 0.002(2) C33 0.031(3) 0.032(3) 0.035(3) 0.003(2) 0.009(2) 0.007(2) C34 0.032(3) 0.033(3) 0.034(3) 0.000(2) 0.003(2) -0.001(2) C35 0.046(4) 0.036(3) 0.031(3) 0.002(2) -0.001(3) 0.003(3) C36 0.040(3) 0.035(3) 0.049(3) -0.007(3) 0.023(3) -0.008(3) C37 0.047(4) 0.053(4) 0.057(4) -0.017(3) 0.026(3) -0.006(3) C38 0.059(4) 0.062(4) 0.065(4) -0.014(4) 0.037(4) -0.014(4) C39 0.052(5) 0.096(6) 0.070(5) -0.015(4) 0.038(4) -0.006(4) C40 0.082(6) 0.098(7) 0.108(7) -0.023(6) 0.062(6) -0.022(5) C41 0.071(6) 0.129(8) 0.099(7) -0.007(6) 0.059(5) -0.011(6) C42 0.177(13) 0.172(13) 0.200(14) -0.044(11) 0.162(12) -0.070(11) C43 0.25(2) 0.24(2) 0.27(2) -0.056(17) 0.178(19) -0.090(17) C44 0.031(3) 0.043(3) 0.032(3) 0.001(2) 0.015(2) 0.002(3) C45 0.034(3) 0.044(3) 0.039(3) -0.003(3) 0.019(3) 0.001(3) C46 0.034(3) 0.062(4) 0.039(3) 0.001(3) 0.013(3) 0.000(3) C47 0.039(4) 0.060(4) 0.052(4) -0.010(3) 0.025(3) -0.007(3) C48 0.037(4) 0.078(5) 0.051(4) -0.007(3) 0.018(3) -0.004(3) C49 0.040(4) 0.082(5) 0.068(5) -0.012(4) 0.030(4) -0.005(4) C50 0.049(5) 0.127(8) 0.086(6) -0.021(5) 0.035(4) -0.014(5) C51 0.072(6) 0.143(9) 0.105(7) -0.021(7) 0.048(6) -0.013(6) C52 0.039(3) 0.036(3) 0.042(3) 0.001(3) 0.024(3) 0.002(3) C53 0.043(4) 0.042(3) 0.042(3) 0.008(3) 0.024(3) 0.001(3) C54 0.054(4) 0.039(3) 0.055(4) 0.010(3) 0.021(3) 0.001(3) C55 0.048(4) 0.068(5) 0.063(4) 0.024(4) 0.029(3) 0.013(3) C56 0.060(5) 0.062(5) 0.074(5) 0.026(4) 0.030(4) 0.015(4) C57 0.070(5) 0.092(6) 0.093(6) 0.035(5) 0.048(5) 0.021(5) C58 0.070(6) 0.116(8) 0.112(8) 0.014(6) 0.051(6) 0.008(5) C59 0.103(8) 0.170(12) 0.125(9) 0.014(8) 0.061(7) 0.022(8) C60 0.037(3) 0.045(3) 0.044(3) 0.005(3) 0.018(3) 0.002(3) C61 0.037(3) 0.055(4) 0.050(4) 0.004(3) 0.022(3) -0.005(3) C62 0.046(4) 0.061(4) 0.060(4) 0.008(3) 0.024(3) 0.002(3) C63 0.050(4) 0.054(4) 0.058(4) 0.005(3) 0.016(3) -0.004(3) C64 0.053(4) 0.067(5) 0.064(4) 0.008(4) 0.024(4) -0.002(4) C65 0.056(5) 0.061(5) 0.075(5) 0.006(4) 0.025(4) -0.005(4) C66 0.071(6) 0.093(7) 0.103(7) 0.018(5) 0.038(5) 0.012(5) C67 0.107(8) 0.122(9) 0.126(9) 0.003(7) 0.070(7) -0.002(7) C68 0.039(3) 0.043(3) 0.045(3) 0.009(3) 0.009(3) 0.000(3) C69 0.039(4) 0.049(4) 0.051(4) 0.012(3) 0.013(3) -0.003(3) C70 0.048(4) 0.056(4) 0.057(4) 0.014(3) 0.022(3) 0.003(3) C71 0.048(4) 0.063(5) 0.071(5) 0.018(4) 0.017(4) 0.002(4) C72 0.061(5) 0.081(6) 0.088(6) 0.020(5) 0.034(4) 0.012(4) C73 0.052(5) 0.125(8) 0.138(9) 0.037(7) 0.050(6) 0.019(5) C74 0.089(8) 0.185(13) 0.147(10) 0.051(9) 0.064(8) 0.040(8) C75 0.077(8) 0.28(2) 0.235(17) 0.073(15) 0.088(10) 0.020(10) C76 0.054(4) 0.062(5) 0.078(5) 0.005(4) 0.029(4) -0.010(4) C77 0.073(6) 0.103(7) 0.130(8) 0.012(6) 0.062(6) -0.019(5) C78 0.101(9) 0.138(10) 0.144(11) 0.028(9) 0.035(8) -0.026(8) C79 0.120(9) 0.101(8) 0.113(9) -0.017(7) 0.022(7) 0.029(7) C80 0.109(9) 0.143(11) 0.153(12) 0.055(10) 0.029(9) -0.017(8) C81 0.160(13) 0.158(12) 0.126(11) 0.029(9) 0.071(10) 0.046(10) C82 0.123(12) 0.31(2) 0.219(18) 0.075(17) 0.101(13) 0.082(14) C83 0.162(15) 0.26(2) 0.197(17) -0.097(16) 0.056(13) 0.014(15) C84 0.038(3) 0.043(3) 0.048(4) 0.011(3) 0.013(3) 0.004(3) C85 0.036(4) 0.049(4) 0.066(4) 0.025(3) 0.013(3) 0.007(3) C86 0.042(4) 0.071(5) 0.076(5) 0.030(4) 0.021(4) 0.019(4) C87 0.055(5) 0.106(7) 0.124(8) 0.045(6) 0.042(5) 0.018(5) C88 0.069(6) 0.194(12) 0.158(10) 0.102(9) 0.073(7) 0.056(7) C89 0.087(8) 0.198(14) 0.32(2) 0.124(14) 0.127(12) 0.045(9) C90 0.158(16) 0.43(4) 0.55(4) 0.28(3) 0.27(2) 0.13(2) C91 0.53(5) 0.57(6) 1.66(16) 0.80(9) 0.88(9) 0.43(5) C92 0.039(4) 0.044(4) 0.055(4) 0.004(3) 0.015(3) 0.003(3) C93 0.036(4) 0.055(4) 0.056(4) 0.005(3) 0.012(3) -0.005(3) C94 0.049(4) 0.068(5) 0.058(4) 0.001(4) 0.016(3) 0.000(4) C95 0.054(5) 0.075(5) 0.069(5) -0.006(4) 0.021(4) -0.002(4) C96 0.082(7) 0.110(7) 0.085(6) -0.011(5) 0.032(5) -0.005(5) C97 0.067(6) 0.142(10) 0.131(9) -0.022(7) 0.046(6) -0.012(6) C98 0.059(8) 0.81(7) 0.162(17) 0.11(3) 0.041(9) -0.043(19) C99 0.77(7) 0.154(18) 0.20(2) -0.040(16) 0.14(4) 0.11(3) C100 0.056(4) 0.045(4) 0.081(5) 0.005(3) 0.042(4) 0.000(3) C101 0.056(5) 0.055(5) 0.140(8) -0.002(5) 0.066(5) 0.003(4) C102 0.137(10) 0.075(7) 0.300(18) 0.015(9) 0.171(12) 0.001(7) C103 0.125(9) 0.118(9) 0.111(8) -0.005(7) 0.058(7) -0.043(7) C104 0.084(7) 0.131(9) 0.182(12) 0.055(9) 0.076(8) 0.013(7) C105 0.159(14) 0.213(17) 0.156(13) 0.002(12) 0.074(11) -0.026(12) C106 0.156(15) 0.48(4) 0.137(13) 0.105(19) 0.075(12) 0.095(19) C108 0.039(4) 0.041(3) 0.047(3) -0.005(3) 0.015(3) 0.005(3) C109 0.042(4) 0.049(4) 0.046(4) -0.006(3) 0.014(3) 0.014(3) C110 0.041(4) 0.064(4) 0.048(4) -0.015(3) 0.015(3) 0.007(3) C111 0.047(4) 0.082(5) 0.047(4) -0.013(4) 0.018(3) 0.012(4) C112 0.049(4) 0.103(6) 0.063(5) -0.014(4) 0.025(4) 0.003(4) C113 0.059(5) 0.132(8) 0.083(6) -0.012(6) 0.037(5) 0.015(5) C114 0.075(7) 0.191(13) 0.138(10) -0.021(9) 0.060(7) 0.007(8) C115 0.087(8) 0.28(2) 0.180(14) -0.017(13) 0.078(9) 0.037(10) C117 0.129(10) 0.091(8) 0.169(12) 0.094(8) -0.059(9) -0.027(7) C118 0.28(2) 0.065(6) 0.108(9) 0.061(6) 0.066(11) 0.052(10) Cl1 0.197(3) 0.0658(14) 0.0719(15) 0.0127(11) -0.0038(17) 0.0286(17) Cl2 0.175(3) 0.0586(13) 0.0896(17) 0.0090(12) -0.0304(17) 0.0059(15) _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 1.377(6) . ? O1 C36 1.424(6) . ? O2 C4 1.378(6) . ? O2 C44 1.436(6) . ? O3 C12 1.370(6) . ? O3 C52 1.435(6) . ? O4 C9 1.385(6) . ? O4 C60 1.420(7) . ? O5 C19 1.384(6) . ? O5 C68 1.435(7) . ? O6 C16 1.385(6) . ? O6 C76 1.413(8) . ? O7 C26 1.384(6) . ? O7 C84 1.429(7) . ? O8 C23 1.400(6) . ? O8 C92 1.425(7) . ? O9 C33 1.393(6) . ? O9 C100 1.422(7) . ? O10 C30 1.375(6) . ? O10 C108 1.430(7) . ? C1 C6 1.381(7) . ? C1 C2 1.408(7) . ? C2 C3 1.388(7) . ? C2 C7 1.514(7) . ? C3 C4 1.377(7) . ? C3 H3 0.9500 . ? C4 C5 1.413(7) . ? C5 C6 1.392(7) . ? C5 C35 1.518(7) . ? C6 H6 0.9500 . ? C7 C8 1.514(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.383(7) . ? C8 C9 1.399(7) . ? C9 C10 1.385(8) . ? C10 C11 1.380(7) . ? C10 H10 0.9500 . ? C11 C12 1.400(7) . ? C11 C14 1.532(7) . ? C12 C13 1.381(7) . ? C13 H13 0.9500 . ? C14 C15 1.509(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.387(7) . ? C15 C16 1.398(8) . ? C16 C17 1.385(8) . ? C17 C18 1.397(7) . ? C17 H17 0.9500 . ? C18 C19 1.405(7) . ? C18 C21 1.525(8) . ? C19 C20 1.375(7) . ? C20 H20 0.9500 . ? C21 C22 1.494(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.389(8) . ? C22 C27 1.402(8) . ? C23 C24 1.399(8) . ? C24 C25 1.397(8) . ? C24 H24 0.9500 . ? C25 C26 1.376(8) . ? C25 C28 1.516(8) . ? C26 C27 1.409(8) . ? C27 H27 0.9500 . ? C28 C29 1.530(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.373(7) . ? C29 C30 1.403(8) . ? C30 C31 1.391(7) . ? C31 C32 1.394(7) . ? C31 H31 0.9500 . ? C32 C33 1.384(7) . ? C32 C35 1.518(7) . ? C33 C34 1.387(7) . ? C34 H34 0.9500 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.494(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.496(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.503(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.480(10) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.481(11) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.460(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.511(17) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.504(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.507(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.507(8) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.505(8) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.510(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.494(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.512(11) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.503(7) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.497(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.518(8) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.498(9) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.526(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.514(11) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.484(12) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.516(8) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.483(8) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.526(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.502(9) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.513(9) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.514(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.510(12) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.504(8) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.524(9) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.520(9) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.520(10) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.513(11) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.527(13) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.541(16) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C77 1.505(10) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.462(13) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C79 1.476(15) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C80 1.561(15) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 C81 1.434(17) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 C82 1.530(16) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.255(13) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C85 1.512(8) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C86 1.501(9) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 C87 1.540(11) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.499(12) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 C89 1.578(17) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.486(19) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 C91 1.44(2) . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 C93 1.497(8) . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.508(9) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 C95 1.519(9) . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.533(10) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 C97 1.508(12) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.90(2) . ? C97 H97A 0.9900 . ? C97 H97B 0.9900 . ? C98 C99 1.366(17) . ? C98 H98A 0.9900 . ? C98 H98B 0.9900 . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 C101 1.486(9) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.558(12) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 C103 1.339(13) . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? C103 C104 1.540(12) . ? C103 H10G 0.9900 . ? C103 H10H 0.9900 . ? C104 C105 1.479(16) . ? C104 H10I 0.9900 . ? C104 H10J 0.9900 . ? C105 C106 1.545(14) . ? C105 H10K 0.9900 . ? C105 H10L 0.9900 . ? C106 C107 1.288(17) . ? C106 H10Q 0.9900 . ? C106 H10R 0.9900 . ? C108 C109 1.492(8) . ? C108 H10M 0.9900 . ? C108 H10N 0.9900 . ? C109 C110 1.509(9) . ? C109 H10O 0.9900 . ? C109 H10P 0.9900 . ? C110 C111 1.516(8) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.514(10) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 C113 1.512(10) . ? C112 H11E 0.9900 . ? C112 H11F 0.9900 . ? C113 C114 1.539(13) . ? C113 H11G 0.9900 . ? C113 H11H 0.9900 . ? C114 C115 1.505(14) . ? C114 H11I 0.9900 . ? C114 H11J 0.9900 . ? C115 H11K 0.9800 . ? C115 H11L 0.9800 . ? C115 H11M 0.9800 . ? C117 C116 1.399(12) . ? C117 C118 1.482(12) . ? C117 H11N 0.9900 . ? C117 H11O 0.9900 . ? C118 C119 1.308(13) . ? C118 H11P 0.9900 . ? C118 H11Q 0.9900 . ? Cl1 C116 1.718(10) . ? Cl2 C119 1.877(12) . ? C107 H10S 0.9800 . ? C107 H10T 0.9800 . ? C107 H10U 0.9800 . ? C116 H11R 0.9900 . ? C116 H11S 0.9900 . ? C119 H11T 0.9900 . ? C119 H11U 0.9900 . ? 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 C1 O1 C36 118.0(4) . . ? C4 O2 C44 116.9(4) . . ? C12 O3 C52 118.2(4) . . ? C9 O4 C60 119.1(4) . . ? C19 O5 C68 116.5(4) . . ? C16 O6 C76 119.5(5) . . ? C26 O7 C84 118.7(4) . . ? C23 O8 C92 118.0(4) . . ? C33 O9 C100 117.2(4) . . ? C30 O10 C108 118.2(4) . . ? O1 C1 C6 124.7(5) . . ? O1 C1 C2 116.0(5) . . ? C6 C1 C2 119.3(5) . . ? C3 C2 C1 118.8(5) . . ? C3 C2 C7 120.3(5) . . ? C1 C2 C7 120.8(5) . . ? C4 C3 C2 121.7(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.1 . . ? O2 C4 C3 124.2(5) . . ? O2 C4 C5 115.9(5) . . ? C3 C4 C5 119.9(5) . . ? C6 C5 C4 118.0(5) . . ? C6 C5 C35 122.1(5) . . ? C4 C5 C35 119.9(5) . . ? C1 C6 C5 122.1(5) . . ? C1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C2 C7 C8 112.0(4) . . ? C2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C13 C8 C9 117.9(5) . . ? C13 C8 C7 120.5(5) . . ? C9 C8 C7 121.5(5) . . ? C10 C9 O4 124.9(5) . . ? C10 C9 C8 120.0(5) . . ? O4 C9 C8 115.1(5) . . ? C11 C10 C9 121.7(5) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 118.7(5) . . ? C10 C11 C14 120.6(5) . . ? C12 C11 C14 120.6(5) . . ? O3 C12 C13 124.7(5) . . ? O3 C12 C11 116.0(5) . . ? C13 C12 C11 119.3(5) . . ? C12 C13 C8 122.5(5) . . ? C12 C13 H13 118.8 . . ? C8 C13 H13 118.8 . . ? C15 C14 C11 109.1(4) . . ? C15 C14 H14A 109.9 . . ? C11 C14 H14A 109.9 . . ? C15 C14 H14B 109.9 . . ? C11 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C20 C15 C16 117.9(5) . . ? C20 C15 C14 121.4(5) . . ? C16 C15 C14 120.4(5) . . ? O6 C16 C17 122.9(5) . . ? O6 C16 C15 116.3(5) . . ? C17 C16 C15 120.7(5) . . ? C16 C17 C18 120.9(5) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 118.2(5) . . ? C17 C18 C21 121.2(5) . . ? C19 C18 C21 120.7(5) . . ? C20 C19 O5 123.0(5) . . ? C20 C19 C18 120.2(5) . . ? O5 C19 C18 116.8(5) . . ? C19 C20 C15 122.0(5) . . ? C19 C20 H20 119.0 . . ? C15 C20 H20 119.0 . . ? C22 C21 C18 114.8(4) . . ? C22 C21 H21A 108.6 . . ? C18 C21 H21A 108.6 . . ? C22 C21 H21B 108.6 . . ? C18 C21 H21B 108.6 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C27 116.8(5) . . ? C23 C22 C21 122.8(5) . . ? C27 C22 C21 120.4(5) . . ? C22 C23 C24 122.2(5) . . ? C22 C23 O8 115.2(5) . . ? C24 C23 O8 122.6(5) . . ? C25 C24 C23 120.5(5) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 118.1(5) . . ? C26 C25 C28 121.9(5) . . ? C24 C25 C28 120.0(5) . . ? C25 C26 O7 116.2(5) . . ? C25 C26 C27 121.4(5) . . ? O7 C26 C27 122.5(5) . . ? C22 C27 C26 121.0(5) . . ? C22 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C25 C28 C29 108.6(4) . . ? C25 C28 H28A 110.0 . . ? C29 C28 H28A 110.0 . . ? C25 C28 H28B 110.0 . . ? C29 C28 H28B 110.0 . . ? H28A C28 H28B 108.3 . . ? C34 C29 C30 119.6(5) . . ? C34 C29 C28 120.4(5) . . ? C30 C29 C28 119.7(5) . . ? O10 C30 C31 124.1(5) . . ? O10 C30 C29 116.7(5) . . ? C31 C30 C29 119.2(5) . . ? C30 C31 C32 121.2(5) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C33 C32 C31 118.5(5) . . ? C33 C32 C35 120.9(5) . . ? C31 C32 C35 120.5(5) . . ? C32 C33 C34 120.8(5) . . ? C32 C33 O9 116.5(4) . . ? C34 C33 O9 122.6(5) . . ? C29 C34 C33 120.7(5) . . ? C29 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C32 C35 C5 112.5(4) . . ? C32 C35 H35A 109.1 . . ? C5 C35 H35A 109.1 . . ? C32 C35 H35B 109.1 . . ? C5 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? O1 C36 C37 108.6(5) . . ? O1 C36 H36A 110.0 . . ? C37 C36 H36A 110.0 . . ? O1 C36 H36B 110.0 . . ? C37 C36 H36B 110.0 . . ? H36A C36 H36B 108.3 . . ? C36 C37 C38 113.4(5) . . ? C36 C37 H37A 108.9 . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37B 108.9 . . ? C38 C37 H37B 108.9 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 115.4(6) . . ? C37 C38 H38A 108.4 . . ? C39 C38 H38A 108.4 . . ? C37 C38 H38B 108.4 . . ? C39 C38 H38B 108.4 . . ? H38A C38 H38B 107.5 . . ? C40 C39 C38 117.3(7) . . ? C40 C39 H39A 108.0 . . ? C38 C39 H39A 108.0 . . ? C40 C39 H39B 108.0 . . ? C38 C39 H39B 108.0 . . ? H39A C39 H39B 107.2 . . ? C41 C40 C39 117.2(8) . . ? C41 C40 H40A 108.0 . . ? C39 C40 H40A 108.0 . . ? C41 C40 H40B 108.0 . . ? C39 C40 H40B 108.0 . . ? H40A C40 H40B 107.2 . . ? C42 C41 C40 117.7(9) . . ? C42 C41 H41A 107.9 . . ? C40 C41 H41A 107.9 . . ? C42 C41 H41B 107.9 . . ? C40 C41 H41B 107.9 . . ? H41A C41 H41B 107.2 . . ? C41 C42 C43 114.2(12) . . ? C41 C42 H42A 108.7 . . ? C43 C42 H42A 108.7 . . ? C41 C42 H42B 108.7 . . ? C43 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O2 C44 C45 109.0(4) . . ? O2 C44 H44A 109.9 . . ? C45 C44 H44A 109.9 . . ? O2 C44 H44B 109.9 . . ? C45 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? C44 C45 C46 113.4(5) . . ? C44 C45 H45A 108.9 . . ? C46 C45 H45A 108.9 . . ? C44 C45 H45B 108.9 . . ? C46 C45 H45B 108.9 . . ? H45A C45 H45B 107.7 . . ? C45 C46 C47 113.4(5) . . ? C45 C46 H46A 108.9 . . ? C47 C46 H46A 108.9 . . ? C45 C46 H46B 108.9 . . ? C47 C46 H46B 108.9 . . ? H46A C46 H46B 107.7 . . ? C48 C47 C46 117.1(5) . . ? C48 C47 H47A 108.0 . . ? C46 C47 H47A 108.0 . . ? C48 C47 H47B 108.0 . . ? C46 C47 H47B 108.0 . . ? H47A C47 H47B 107.3 . . ? C47 C48 C49 115.5(6) . . ? C47 C48 H48A 108.4 . . ? C49 C48 H48A 108.4 . . ? C47 C48 H48B 108.4 . . ? C49 C48 H48B 108.4 . . ? H48A C48 H48B 107.5 . . ? C50 C49 C48 116.3(6) . . ? C50 C49 H49A 108.2 . . ? C48 C49 H49A 108.2 . . ? C50 C49 H49B 108.2 . . ? C48 C49 H49B 108.2 . . ? H49A C49 H49B 107.4 . . ? C49 C50 C51 114.9(7) . . ? C49 C50 H50A 108.5 . . ? C51 C50 H50A 108.6 . . ? C49 C50 H50B 108.5 . . ? C51 C50 H50B 108.5 . . ? H50A C50 H50B 107.5 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O3 C52 C53 108.8(5) . . ? O3 C52 H52A 109.9 . . ? C53 C52 H52A 109.9 . . ? O3 C52 H52B 109.9 . . ? C53 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? C54 C53 C52 112.8(5) . . ? C54 C53 H53A 109.0 . . ? C52 C53 H53A 109.0 . . ? C54 C53 H53B 109.0 . . ? C52 C53 H53B 109.0 . . ? H53A C53 H53B 107.8 . . ? C53 C54 C55 114.2(5) . . ? C53 C54 H54A 108.7 . . ? C55 C54 H54A 108.7 . . ? C53 C54 H54B 108.7 . . ? C55 C54 H54B 108.7 . . ? H54A C54 H54B 107.6 . . ? C56 C55 C54 114.3(6) . . ? C56 C55 H55A 108.7 . . ? C54 C55 H55A 108.7 . . ? C56 C55 H55B 108.7 . . ? C54 C55 H55B 108.7 . . ? H55A C55 H55B 107.6 . . ? C55 C56 C57 114.9(6) . . ? C55 C56 H56A 108.5 . . ? C57 C56 H56A 108.5 . . ? C55 C56 H56B 108.5 . . ? C57 C56 H56B 108.5 . . ? H56A C56 H56B 107.5 . . ? C58 C57 C56 113.9(7) . . ? C58 C57 H57A 108.8 . . ? C56 C57 H57A 108.8 . . ? C58 C57 H57B 108.8 . . ? C56 C57 H57B 108.8 . . ? H57A C57 H57B 107.7 . . ? C59 C58 C57 112.9(9) . . ? C59 C58 H58A 109.0 . . ? C57 C58 H58A 109.0 . . ? C59 C58 H58B 109.0 . . ? C57 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O4 C60 C61 108.0(5) . . ? O4 C60 H60A 110.1 . . ? C61 C60 H60A 110.1 . . ? O4 C60 H60B 110.1 . . ? C61 C60 H60B 110.1 . . ? H60A C60 H60B 108.4 . . ? C62 C61 C60 113.2(5) . . ? C62 C61 H61A 108.9 . . ? C60 C61 H61A 108.9 . . ? C62 C61 H61B 108.9 . . ? C60 C61 H61B 108.9 . . ? H61A C61 H61B 107.7 . . ? C61 C62 C63 113.4(6) . . ? C61 C62 H62A 108.9 . . ? C63 C62 H62A 108.9 . . ? C61 C62 H62B 108.9 . . ? C63 C62 H62B 108.9 . . ? H62A C62 H62B 107.7 . . ? C64 C63 C62 114.1(6) . . ? C64 C63 H63A 108.7 . . ? C62 C63 H63A 108.7 . . ? C64 C63 H63B 108.7 . . ? C62 C63 H63B 108.7 . . ? H63A C63 H63B 107.6 . . ? C63 C64 C65 115.4(6) . . ? C63 C64 H64A 108.4 . . ? C65 C64 H64A 108.4 . . ? C63 C64 H64B 108.4 . . ? C65 C64 H64B 108.4 . . ? H64A C64 H64B 107.5 . . ? C64 C65 C66 114.2(6) . . ? C64 C65 H65A 108.7 . . ? C66 C65 H65A 108.7 . . ? C64 C65 H65B 108.7 . . ? C66 C65 H65B 108.7 . . ? H65A C65 H65B 107.6 . . ? C67 C66 C65 113.8(8) . . ? C67 C66 H66A 108.8 . . ? C65 C66 H66A 108.8 . . ? C67 C66 H66B 108.8 . . ? C65 C66 H66B 108.8 . . ? H66A C66 H66B 107.7 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O5 C68 C69 109.9(5) . . ? O5 C68 H68A 109.7 . . ? C69 C68 H68A 109.7 . . ? O5 C68 H68B 109.7 . . ? C69 C68 H68B 109.7 . . ? H68A C68 H68B 108.2 . . ? C68 C69 C70 109.7(5) . . ? C68 C69 H69A 109.7 . . ? C70 C69 H69A 109.7 . . ? C68 C69 H69B 109.7 . . ? C70 C69 H69B 109.7 . . ? H69A C69 H69B 108.2 . . ? C71 C70 C69 114.2(6) . . ? C71 C70 H70A 108.7 . . ? C69 C70 H70A 108.7 . . ? C71 C70 H70B 108.7 . . ? C69 C70 H70B 108.7 . . ? H70A C70 H70B 107.6 . . ? C72 C71 C70 113.2(6) . . ? C72 C71 H71A 108.9 . . ? C70 C71 H71A 108.9 . . ? C72 C71 H71B 108.9 . . ? C70 C71 H71B 108.9 . . ? H71A C71 H71B 107.8 . . ? C73 C72 C71 113.3(7) . . ? C73 C72 H72A 108.9 . . ? C71 C72 H72A 108.9 . . ? C73 C72 H72B 108.9 . . ? C71 C72 H72B 108.9 . . ? H72A C72 H72B 107.7 . . ? C72 C73 C74 114.0(9) . . ? C72 C73 H73A 108.7 . . ? C74 C73 H73A 108.7 . . ? C72 C73 H73B 108.7 . . ? C74 C73 H73B 108.7 . . ? H73A C73 H73B 107.6 . . ? C73 C74 C75 113.2(12) . . ? C73 C74 H74A 108.9 . . ? C75 C74 H74A 108.9 . . ? C73 C74 H74B 108.9 . . ? C75 C74 H74B 108.9 . . ? H74A C74 H74B 107.7 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O6 C76 C77 106.3(6) . . ? O6 C76 H76A 110.5 . . ? C77 C76 H76A 110.5 . . ? O6 C76 H76B 110.5 . . ? C77 C76 H76B 110.5 . . ? H76A C76 H76B 108.7 . . ? C78 C77 C76 116.2(9) . . ? C78 C77 H77A 108.2 . . ? C76 C77 H77A 108.2 . . ? C78 C77 H77B 108.2 . . ? C76 C77 H77B 108.2 . . ? H77A C77 H77B 107.4 . . ? C77 C78 C79 113.1(10) . . ? C77 C78 H78A 109.0 . . ? C79 C78 H78A 109.0 . . ? C77 C78 H78B 109.0 . . ? C79 C78 H78B 109.0 . . ? H78A C78 H78B 107.8 . . ? C78 C79 C80 112.2(10) . . ? C78 C79 H79A 109.2 . . ? C80 C79 H79A 109.2 . . ? C78 C79 H79B 109.2 . . ? C80 C79 H79B 109.2 . . ? H79A C79 H79B 107.9 . . ? C81 C80 C79 117.8(11) . . ? C81 C80 H80A 107.9 . . ? C79 C80 H80A 107.9 . . ? C81 C80 H80B 107.9 . . ? C79 C80 H80B 107.9 . . ? H80A C80 H80B 107.2 . . ? C80 C81 C82 119.7(14) . . ? C80 C81 H81A 107.4 . . ? C82 C81 H81A 107.4 . . ? C80 C81 H81B 107.4 . . ? C82 C81 H81B 107.4 . . ? H81A C81 H81B 106.9 . . ? C83 C82 C81 119.3(15) . . ? C83 C82 H82A 107.5 . . ? C81 C82 H82A 107.5 . . ? C83 C82 H82B 107.5 . . ? C81 C82 H82B 107.5 . . ? H82A C82 H82B 107.0 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? O7 C84 C85 108.8(5) . . ? O7 C84 H84A 109.9 . . ? C85 C84 H84A 109.9 . . ? O7 C84 H84B 109.9 . . ? C85 C84 H84B 109.9 . . ? H84A C84 H84B 108.3 . . ? C86 C85 C84 111.8(6) . . ? C86 C85 H85A 109.3 . . ? C84 C85 H85A 109.3 . . ? C86 C85 H85B 109.3 . . ? C84 C85 H85B 109.3 . . ? H85A C85 H85B 107.9 . . ? C85 C86 C87 112.4(7) . . ? C85 C86 H86A 109.1 . . ? C87 C86 H86A 109.1 . . ? C85 C86 H86B 109.1 . . ? C87 C86 H86B 109.1 . . ? H86A C86 H86B 107.9 . . ? C88 C87 C86 113.9(9) . . ? C88 C87 H87A 108.8 . . ? C86 C87 H87A 108.8 . . ? C88 C87 H87B 108.8 . . ? C86 C87 H87B 108.8 . . ? H87A C87 H87B 107.7 . . ? C87 C88 C89 113.0(12) . . ? C87 C88 H88A 109.0 . . ? C89 C88 H88A 109.0 . . ? C87 C88 H88B 109.0 . . ? C89 C88 H88B 109.0 . . ? H88A C88 H88B 107.8 . . ? C90 C89 C88 112.7(16) . . ? C90 C89 H89A 109.1 . . ? C88 C89 H89A 109.1 . . ? C90 C89 H89B 109.1 . . ? C88 C89 H89B 109.1 . . ? H89A C89 H89B 107.8 . . ? C91 C90 C89 108.6(18) . . ? C91 C90 H90A 110.0 . . ? C89 C90 H90A 110.0 . . ? C91 C90 H90B 110.0 . . ? C89 C90 H90B 110.0 . . ? H90A C90 H90B 108.3 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? O8 C92 C93 109.6(5) . . ? O8 C92 H92A 109.8 . . ? C93 C92 H92A 109.8 . . ? O8 C92 H92B 109.8 . . ? C93 C92 H92B 109.8 . . ? H92A C92 H92B 108.2 . . ? C92 C93 C94 111.7(6) . . ? C92 C93 H93A 109.3 . . ? C94 C93 H93A 109.3 . . ? C92 C93 H93B 109.3 . . ? C94 C93 H93B 109.3 . . ? H93A C93 H93B 107.9 . . ? C93 C94 C95 113.7(6) . . ? C93 C94 H94A 108.8 . . ? C95 C94 H94A 108.8 . . ? C93 C94 H94B 108.8 . . ? C95 C94 H94B 108.8 . . ? H94A C94 H94B 107.7 . . ? C94 C95 C96 112.4(7) . . ? C94 C95 H95A 109.1 . . ? C96 C95 H95A 109.1 . . ? C94 C95 H95B 109.1 . . ? C96 C95 H95B 109.1 . . ? H95A C95 H95B 107.9 . . ? C97 C96 C95 112.1(8) . . ? C97 C96 H96A 109.2 . . ? C95 C96 H96A 109.2 . . ? C97 C96 H96B 109.2 . . ? C95 C96 H96B 109.2 . . ? H96A C96 H96B 107.9 . . ? C96 C97 C98 104.2(8) . . ? C96 C97 H97A 110.9 . . ? C98 C97 H97A 111.0 . . ? C96 C97 H97B 110.9 . . ? C98 C97 H97B 110.8 . . ? H97A C97 H97B 108.9 . . ? C99 C98 C97 85.2(15) . . ? C99 C98 H98A 114.3 . . ? C97 C98 H98A 114.4 . . ? C99 C98 H98B 114.6 . . ? C97 C98 H98B 114.5 . . ? H98A C98 H98B 111.6 . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.6 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.3 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? O9 C100 C101 110.4(5) . . ? O9 C100 H10A 109.6 . . ? C101 C100 H10A 109.6 . . ? O9 C100 H10B 109.6 . . ? C101 C100 H10B 109.6 . . ? H10A C100 H10B 108.1 . . ? C100 C101 C102 109.6(7) . . ? C100 C101 H10C 109.8 . . ? C102 C101 H10C 109.7 . . ? C100 C101 H10D 109.8 . . ? C102 C101 H10D 109.8 . . ? H10C C101 H10D 108.2 . . ? C103 C102 C101 118.9(10) . . ? C103 C102 H10E 107.6 . . ? C101 C102 H10E 107.6 . . ? C103 C102 H10F 107.6 . . ? C101 C102 H10F 107.6 . . ? H10E C102 H10F 107.0 . . ? C102 C103 C104 118.9(11) . . ? C102 C103 H10G 107.6 . . ? C104 C103 H10G 107.6 . . ? C102 C103 H10H 107.6 . . ? C104 C103 H10H 107.6 . . ? H10G C103 H10H 107.0 . . ? C105 C104 C103 118.6(11) . . ? C105 C104 H10I 107.7 . . ? C103 C104 H10I 107.7 . . ? C105 C104 H10J 107.6 . . ? C103 C104 H10J 107.7 . . ? H10I C104 H10J 107.1 . . ? C104 C105 C106 119.7(14) . . ? C104 C105 H10K 107.4 . . ? C106 C105 H10K 107.4 . . ? C104 C105 H10L 107.4 . . ? C106 C105 H10L 107.5 . . ? H10K C105 H10L 106.9 . . ? C107 C106 C105 109.2(16) . . ? C107 C106 H10Q 109.4 . . ? C105 C106 H10Q 109.7 . . ? C107 C106 H10R 110.3 . . ? C105 C106 H10R 109.9 . . ? H10Q C106 H10R 108.3 . . ? O10 C108 C109 109.1(5) . . ? O10 C108 H10M 109.9 . . ? C109 C108 H10M 109.9 . . ? O10 C108 H10N 109.9 . . ? C109 C108 H10N 109.9 . . ? H10M C108 H10N 108.3 . . ? C108 C109 C110 111.6(5) . . ? C108 C109 H10O 109.3 . . ? C110 C109 H10O 109.3 . . ? C108 C109 H10P 109.3 . . ? C110 C109 H10P 109.3 . . ? H10O C109 H10P 108.0 . . ? C109 C110 C111 114.1(6) . . ? C109 C110 H11A 108.7 . . ? C111 C110 H11A 108.7 . . ? C109 C110 H11B 108.7 . . ? C111 C110 H11B 108.7 . . ? H11A C110 H11B 107.6 . . ? C112 C111 C110 113.5(6) . . ? C112 C111 H11C 108.9 . . ? C110 C111 H11C 108.9 . . ? C112 C111 H11D 108.9 . . ? C110 C111 H11D 108.9 . . ? H11C C111 H11D 107.7 . . ? C113 C112 C111 113.4(7) . . ? C113 C112 H11E 108.9 . . ? C111 C112 H11E 108.9 . . ? C113 C112 H11F 108.9 . . ? C111 C112 H11F 108.9 . . ? H11E C112 H11F 107.7 . . ? C112 C113 C114 113.1(9) . . ? C112 C113 H11G 109.0 . . ? C114 C113 H11G 108.9 . . ? C112 C113 H11H 108.9 . . ? C114 C113 H11H 109.0 . . ? H11G C113 H11H 107.8 . . ? C115 C114 C113 113.1(12) . . ? C115 C114 H11I 109.0 . . ? C113 C114 H11I 109.0 . . ? C115 C114 H11J 109.0 . . ? C113 C114 H11J 109.0 . . ? H11I C114 H11J 107.8 . . ? C114 C115 H11K 109.5 . . ? C114 C115 H11L 109.5 . . ? H11K C115 H11L 109.5 . . ? C114 C115 H11M 109.5 . . ? H11K C115 H11M 109.5 . . ? H11L C115 H11M 109.5 . . ? C116 C117 C118 120.3(12) . . ? C116 C117 H11N 107.2 . . ? C118 C117 H11N 107.2 . . ? C116 C117 H11O 107.2 . . ? C118 C117 H11O 107.2 . . ? H11N C117 H11O 106.9 . . ? C119 C118 C117 123.8(12) . . ? C119 C118 H11P 106.4 . . ? C117 C118 H11P 106.4 . . ? C119 C118 H11Q 106.4 . . ? C117 C118 H11Q 106.4 . . ? H11P C118 H11Q 106.5 . . ? C106 C107 H10S 109.4 . . ? C106 C107 H10T 109.9 . . ? H10S C107 H10T 109.5 . . ? C106 C107 H10U 109.1 . . ? H10S C107 H10U 109.5 . . ? H10T C107 H10U 109.5 . . ? C117 C116 Cl1 114.3(10) . . ? C117 C116 H11R 108.7 . . ? Cl1 C116 H11R 108.7 . . ? C117 C116 H11S 108.7 . . ? Cl1 C116 H11S 108.7 . . ? H11R C116 H11S 107.6 . . ? C118 C119 Cl2 122.1(12) . . ? C118 C119 H11T 106.8 . . ? Cl2 C119 H11T 106.8 . . ? C118 C119 H11U 106.8 . . ? Cl2 C119 H11U 106.8 . . ? H11T C119 H11U 106.7 . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.130 _refine_diff_density_min -0.723 _refine_diff_density_rms 0.086 # Attachment 'DFBu-BuP5A.cif' data_mo_11019a_0m _database_code_depnum_ccdc_archive 'CCDC 863690' #TrackingRef 'DFBu-BuP5A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19.75 H29.50 F O2.50' _chemical_formula_weight 325.93 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2219(11) _cell_length_b 14.4860(13) _cell_length_c 21.9366(19) _cell_angle_alpha 89.672(2) _cell_angle_beta 89.514(2) _cell_angle_gamma 76.1320(10) _cell_volume 3770.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4267 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9802 _exptl_absorpt_correction_T_max 0.9841 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24029 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 25.50 _reflns_number_total 13910 _reflns_number_gt 7999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^2^+10.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13910 _refine_ls_number_parameters 820 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1521 _refine_ls_R_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.2913 _refine_ls_wR_factor_gt 0.2284 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.379 _refine_ls_shift/su_mean 0.023 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 -0.0093(3) 0.7711(2) 0.31658(13) 0.0409(7) Uani 1 1 d . . . O2 O 0.0225(3) 0.3991(2) 0.38721(14) 0.0424(8) Uani 1 1 d . . . O3 O 0.3035(2) 0.6098(2) 0.46109(13) 0.0367(7) Uani 1 1 d . . . O4 O 0.4417(2) 0.2422(2) 0.37268(14) 0.0405(7) Uani 1 1 d . . . O5 O 0.6631(3) 0.5168(2) 0.34633(12) 0.0377(7) Uani 1 1 d . . . O6 O 0.5878(3) 0.2926(2) 0.15515(13) 0.0390(7) Uani 1 1 d . . . O7 O 0.5605(2) 0.6580(2) 0.13429(14) 0.0375(7) Uani 1 1 d . . . O8 O 0.2821(2) 0.4667(2) 0.01674(13) 0.0357(7) Uani 1 1 d . . . O9 O 0.1419(3) 0.8157(2) 0.11268(15) 0.0484(8) Uani 1 1 d . . . O10 O -0.0461(3) 0.5107(2) 0.15929(15) 0.0447(8) Uani 1 1 d . . . C1 C 0.0057(3) 0.6781(3) 0.33424(18) 0.0306(9) Uani 1 1 d . . . C2 C -0.0442(3) 0.6216(3) 0.29684(17) 0.0287(9) Uani 1 1 d . . . C3 C -0.0382(3) 0.5285(3) 0.31414(19) 0.0332(9) Uani 1 1 d . . . H3A H -0.0709 0.4905 0.2897 0.040 Uiso 1 1 calc R . . C4 C 0.0162(3) 0.4907(3) 0.36766(18) 0.0306(9) Uani 1 1 d . . . C5 C 0.0699(3) 0.5455(3) 0.40354(17) 0.0301(9) Uani 1 1 d . . . C6 C 0.0626(3) 0.6389(3) 0.38662(18) 0.0313(9) Uani 1 1 d . . . H6A H 0.0965 0.6765 0.4108 0.038 Uiso 1 1 calc R . . C7 C 0.1389(3) 0.5030(3) 0.45832(18) 0.0318(9) Uani 1 1 d . . . H7A H 0.1083 0.4527 0.4758 0.038 Uiso 1 1 calc R . . H7B H 0.1349 0.5515 0.4891 0.038 Uiso 1 1 calc R . . C8 C 0.2621(3) 0.4626(3) 0.43944(17) 0.0285(9) Uani 1 1 d . . . C9 C 0.2956(3) 0.3701(3) 0.41697(17) 0.0313(9) Uani 1 1 d . . . H9A H 0.2434 0.3328 0.4156 0.038 Uiso 1 1 calc R . . C10 C 0.4047(3) 0.3327(3) 0.39675(17) 0.0302(9) Uani 1 1 d . . . C11 C 0.4843(3) 0.3864(3) 0.39990(17) 0.0288(9) Uani 1 1 d . . . C12 C 0.4511(3) 0.4794(3) 0.42216(17) 0.0286(8) Uani 1 1 d . . . H12A H 0.5036 0.5163 0.4244 0.034 Uiso 1 1 calc R . . C13 C 0.3407(3) 0.5171(3) 0.44096(17) 0.0296(9) Uani 1 1 d . . . C14 C 0.6052(3) 0.3487(3) 0.37709(17) 0.0302(9) Uani 1 1 d . . . H14A H 0.6561 0.3735 0.4025 0.036 Uiso 1 1 calc R . . H14B H 0.6256 0.2800 0.3805 0.036 Uiso 1 1 calc R . . C15 C 0.6184(3) 0.3771(3) 0.31172(17) 0.0285(9) Uani 1 1 d . . . C16 C 0.6006(3) 0.3188(3) 0.26435(18) 0.0314(9) Uani 1 1 d . . . H16A H 0.5846 0.2605 0.2733 0.038 Uiso 1 1 calc R . . C17 C 0.6064(3) 0.3467(3) 0.20373(17) 0.0292(9) Uani 1 1 d . . . C18 C 0.6327(3) 0.4323(3) 0.18946(17) 0.0255(8) Uani 1 1 d . . . C19 C 0.6501(3) 0.4903(3) 0.23661(17) 0.0287(9) Uani 1 1 d . . . H19A H 0.6664 0.5484 0.2275 0.034 Uiso 1 1 calc R . . C20 C 0.6437(3) 0.4634(3) 0.29701(18) 0.0285(8) Uani 1 1 d . . . C21 C 0.6404(3) 0.4630(3) 0.12288(17) 0.0300(9) Uani 1 1 d . . . H21A H 0.6923 0.5041 0.1199 0.036 Uiso 1 1 calc R . . H21B H 0.6704 0.4072 0.0982 0.036 Uiso 1 1 calc R . . C22 C 0.5270(3) 0.5150(3) 0.09779(17) 0.0284(9) Uani 1 1 d . . . C23 C 0.4580(3) 0.4661(3) 0.06862(17) 0.0299(9) Uani 1 1 d . . . H23A H 0.4824 0.4006 0.0641 0.036 Uiso 1 1 calc R . . C24 C 0.3533(3) 0.5127(3) 0.04589(17) 0.0296(9) Uani 1 1 d . . . C25 C 0.3158(3) 0.6107(3) 0.05152(17) 0.0296(9) Uani 1 1 d . . . C26 C 0.3856(3) 0.6606(3) 0.08051(17) 0.0299(9) Uani 1 1 d . . . H26A H 0.3622 0.7263 0.0842 0.036 Uiso 1 1 calc R . . C27 C 0.4896(3) 0.6130(3) 0.10398(18) 0.0304(9) Uani 1 1 d . . . C28 C 0.1987(3) 0.6624(3) 0.03140(18) 0.0325(9) Uani 1 1 d . . . H28A H 0.1989 0.7266 0.0186 0.039 Uiso 1 1 calc R . . H28B H 0.1759 0.6297 -0.0030 0.039 Uiso 1 1 calc R . . C29 C 0.1164(3) 0.6656(3) 0.08384(17) 0.0284(9) Uani 1 1 d . . . C30 C 0.0686(3) 0.5891(3) 0.09456(18) 0.0320(9) Uani 1 1 d . . . H30A H 0.0830 0.5386 0.0674 0.038 Uiso 1 1 calc R . . C31 C 0.0000(3) 0.5864(3) 0.14483(18) 0.0316(9) Uani 1 1 d . . . C32 C -0.0263(3) 0.6637(3) 0.18459(18) 0.0299(9) Uani 1 1 d . . . C33 C 0.0203(3) 0.7397(3) 0.17333(18) 0.0326(9) Uani 1 1 d . . . H33A H 0.0030 0.7918 0.1993 0.039 Uiso 1 1 calc R . . C34 C 0.0921(3) 0.7410(3) 0.12432(18) 0.0326(9) Uani 1 1 d . . . C35 C -0.1039(3) 0.6629(3) 0.23854(18) 0.0322(9) Uani 1 1 d . . . H35A H -0.1579 0.6263 0.2279 0.039 Uiso 1 1 calc R . . H35B H -0.1458 0.7276 0.2465 0.039 Uiso 1 1 calc R . . C36 C 0.0420(4) 0.8323(3) 0.3515(2) 0.0443(11) Uani 1 1 d . . . H36A H 0.1234 0.8133 0.3471 0.053 Uiso 1 1 calc R . . H36B H 0.0229 0.8288 0.3944 0.053 Uiso 1 1 calc R . . C37 C -0.0019(5) 0.9320(3) 0.3279(2) 0.0526(13) Uani 1 1 d . . . H37A H 0.0097 0.9325 0.2841 0.063 Uiso 1 1 calc R . . H37B H 0.0409 0.9732 0.3459 0.063 Uiso 1 1 calc R . . C38 C -0.1264(5) 0.9714(3) 0.3419(2) 0.0551(13) Uani 1 1 d . . . H38A H -0.1364 0.9763 0.3858 0.066 Uiso 1 1 calc R . . H38B H -0.1679 0.9266 0.3275 0.066 Uiso 1 1 calc R . . C39 C -0.1769(7) 1.0684(4) 0.3136(3) 0.087(2) Uani 1 1 d . . . H39A H -0.2553 1.0882 0.3244 0.130 Uiso 1 1 calc R . . H39B H -0.1692 1.0642 0.2701 0.130 Uiso 1 1 calc R . . H39C H -0.1380 1.1139 0.3285 0.130 Uiso 1 1 calc R . . C40 C -0.0623(5) 0.3543(4) 0.3653(3) 0.0580(14) Uani 1 1 d . . . H40A H -0.0434 0.3301 0.3244 0.070 Uiso 1 1 calc R . . H40B H -0.1349 0.3996 0.3642 0.070 Uiso 1 1 calc R . . C41 C -0.0664(5) 0.2719(4) 0.4094(3) 0.0676(17) Uani 1 1 d . . . H41A H -0.0823 0.2973 0.4502 0.081 Uiso 1 1 calc R . . H41B H -0.1278 0.2441 0.3978 0.081 Uiso 1 1 calc R . . C42 C 0.0366(5) 0.1986(4) 0.4104(3) 0.0745(18) Uani 1 1 d . . . H42A H 0.0985 0.2256 0.4222 0.089 Uiso 1 1 calc R . . H42B H 0.0526 0.1719 0.3699 0.089 Uiso 1 1 calc R . . C43 C 0.0259(6) 0.1183(4) 0.4565(3) 0.0710(17) Uani 1 1 d . . . H43A H 0.0943 0.0691 0.4560 0.106 Uiso 1 1 calc R . . H43B H -0.0360 0.0921 0.4449 0.106 Uiso 1 1 calc R . . H43C H 0.0127 0.1444 0.4967 0.106 Uiso 1 1 calc R . . C44 C 0.3787(3) 0.6702(3) 0.45595(18) 0.0323(9) Uani 1 1 d . . . H44A H 0.4029 0.6728 0.4139 0.039 Uiso 1 1 calc R . . H44B H 0.4448 0.6456 0.4807 0.039 Uiso 1 1 calc R . . C45 C 0.3191(4) 0.7687(3) 0.47736(19) 0.0361(10) Uani 1 1 d . . . H45A H 0.2609 0.7968 0.4484 0.043 Uiso 1 1 calc R . . H45B H 0.2830 0.7638 0.5164 0.043 Uiso 1 1 calc R . . C46 C 0.3998(4) 0.8326(3) 0.4838(2) 0.0494(12) Uani 1 1 d . . . H46A H 0.4295 0.8429 0.4439 0.059 Uiso 1 1 calc R . . H46B H 0.4626 0.8008 0.5090 0.059 Uiso 1 1 calc R . . C47 C 0.3448(5) 0.9286(4) 0.5120(3) 0.0726(18) Uani 1 1 d . . . H47A H 0.3997 0.9658 0.5155 0.109 Uiso 1 1 calc R . . H47B H 0.3157 0.9190 0.5517 0.109 Uiso 1 1 calc R . . H47C H 0.2843 0.9616 0.4865 0.109 Uiso 1 1 calc R . . C48 C 0.3624(4) 0.1851(3) 0.3687(2) 0.0456(11) Uani 1 1 d . . . H48A H 0.2994 0.2167 0.3436 0.055 Uiso 1 1 calc R . . H48B H 0.3339 0.1753 0.4090 0.055 Uiso 1 1 calc R . . C49 C 0.4204(5) 0.0906(4) 0.3408(3) 0.0558(13) Uani 1 1 d . . . H49A H 0.4437 0.1008 0.2995 0.067 Uiso 1 1 calc R . . H49B H 0.4874 0.0624 0.3640 0.067 Uiso 1 1 calc R . . C50 C 0.3440(6) 0.0231(4) 0.3401(3) 0.082(2) Uani 1 1 d . . . H50A H 0.3197 0.0148 0.3815 0.099 Uiso 1 1 calc R . . H50B H 0.2775 0.0518 0.3167 0.099 Uiso 1 1 calc R . . C51 C 0.3965(8) -0.0732(5) 0.3138(4) 0.108(3) Uani 1 1 d . . . H51A H 0.3424 -0.1116 0.3146 0.162 Uiso 1 1 calc R . . H51B H 0.4609 -0.1034 0.3375 0.162 Uiso 1 1 calc R . . H51C H 0.4196 -0.0660 0.2724 0.162 Uiso 1 1 calc R . . C52 C 0.6635(3) 0.6141(3) 0.33679(19) 0.0331(9) Uani 1 1 d . . . H52A H 0.5891 0.6501 0.3251 0.040 Uiso 1 1 calc R . . H52B H 0.7162 0.6196 0.3044 0.040 Uiso 1 1 calc R . . C53 C 0.6981(4) 0.6521(3) 0.39541(19) 0.0366(10) Uani 1 1 d . . . H53A H 0.7714 0.6139 0.4073 0.044 Uiso 1 1 calc R . . H53B H 0.6445 0.6464 0.4272 0.044 Uiso 1 1 calc R . . C54 C 0.7038(4) 0.7551(3) 0.3898(2) 0.0422(11) Uani 1 1 d . . . H54A H 0.6291 0.7937 0.3810 0.051 Uiso 1 1 calc R . . H54B H 0.7527 0.7614 0.3558 0.051 Uiso 1 1 calc R . . C55 C 0.7470(5) 0.7923(4) 0.4469(2) 0.0608(15) Uani 1 1 d . . . H55A H 0.7490 0.8576 0.4408 0.091 Uiso 1 1 calc R . . H55B H 0.8216 0.7552 0.4555 0.091 Uiso 1 1 calc R . . H55C H 0.6979 0.7878 0.4805 0.091 Uiso 1 1 calc R . . C56 C 0.5595(4) 0.2042(3) 0.1684(2) 0.0441(11) Uani 1 1 d . . . H56A H 0.4920 0.2150 0.1936 0.053 Uiso 1 1 calc R . . H56B H 0.6205 0.1623 0.1903 0.053 Uiso 1 1 calc R . . C57 C 0.5400(5) 0.1601(3) 0.1089(2) 0.0503(12) Uani 1 1 d . . . H57A H 0.4785 0.2031 0.0880 0.060 Uiso 1 1 calc R . . H57B H 0.5168 0.1018 0.1173 0.060 Uiso 1 1 calc R . . C58 C 0.6412(6) 0.1378(5) 0.0669(3) 0.081(2) Uani 1 1 d . . . H58A H 0.7057 0.1008 0.0888 0.098 Uiso 1 1 calc R . . H58B H 0.6590 0.1966 0.0537 0.098 Uiso 1 1 calc R . . C59 C 0.6193(8) 0.0821(6) 0.0110(3) 0.109(3) Uani 1 1 d . . . H59A H 0.6847 0.0693 -0.0151 0.164 Uiso 1 1 calc R . . H59B H 0.5560 0.1190 -0.0110 0.164 Uiso 1 1 calc R . . H59C H 0.6036 0.0232 0.0239 0.164 Uiso 1 1 calc R . . C60 C 0.5290(4) 0.7584(3) 0.1388(2) 0.0420(11) Uani 1 1 d . . . H60A H 0.4580 0.7783 0.1606 0.050 Uiso 1 1 calc R . . H60B H 0.5202 0.7868 0.0984 0.050 Uiso 1 1 calc R . . C61 C 0.6211(4) 0.7894(3) 0.1726(2) 0.0471(12) Uani 1 1 d . . . H61A H 0.6204 0.7694 0.2149 0.057 Uiso 1 1 calc R . . H61B H 0.6935 0.7582 0.1551 0.057 Uiso 1 1 calc R . . C62 C 0.6072(5) 0.8958(3) 0.1700(3) 0.0611(15) Uani 1 1 d . . . H62A H 0.5321 0.9272 0.1840 0.073 Uiso 1 1 calc R . . H62B H 0.6151 0.9151 0.1281 0.073 Uiso 1 1 calc R . . C63 C 0.6935(7) 0.9273(4) 0.2090(4) 0.102(3) Uani 1 1 d . . . H63A H 0.6813 0.9952 0.2069 0.153 Uiso 1 1 calc R . . H63B H 0.7680 0.8983 0.1943 0.153 Uiso 1 1 calc R . . H63C H 0.6860 0.9084 0.2506 0.153 Uiso 1 1 calc R . . C64 C 0.3111(4) 0.3655(3) 0.0189(2) 0.0364(10) Uani 1 1 d . . . H64A H 0.3188 0.3440 0.0609 0.044 Uiso 1 1 calc R . . H64B H 0.3826 0.3413 -0.0018 0.044 Uiso 1 1 calc R . . C65 C 0.2195(4) 0.3287(3) -0.0118(2) 0.0472(12) Uani 1 1 d . . . H65A H 0.1475 0.3570 0.0072 0.057 Uiso 1 1 calc R . . H65B H 0.2153 0.3475 -0.0544 0.057 Uiso 1 1 calc R . . C66 C 0.2422(5) 0.2210(4) -0.0073(3) 0.0601(14) Uani 1 1 d . . . H66A H 0.3144 0.1936 -0.0264 0.072 Uiso 1 1 calc R . . H66B H 0.2482 0.2030 0.0355 0.072 Uiso 1 1 calc R . . C67 C 0.1551(6) 0.1788(5) -0.0358(4) 0.090(2) Uani 1 1 d . . . H67A H 0.1767 0.1109 -0.0316 0.135 Uiso 1 1 calc R . . H67B H 0.1488 0.1956 -0.0782 0.135 Uiso 1 1 calc R . . H67C H 0.0839 0.2029 -0.0158 0.135 Uiso 1 1 calc R . . C68 C 0.1273(5) 0.8891(4) 0.1561(3) 0.0689(17) Uani 1 1 d . . . H68A H 0.1484 0.8619 0.1960 0.083 Uiso 1 1 calc R . . H68B H 0.0485 0.9228 0.1578 0.083 Uiso 1 1 calc R . . C69 C 0.1979(7) 0.9576(5) 0.1400(4) 0.101(3) Uani 1 1 d . . . H69A H 0.2753 0.9224 0.1339 0.122 Uiso 1 1 calc R . . H69B H 0.1714 0.9891 0.1019 0.122 Uiso 1 1 calc R . . C70 C 0.1949(7) 1.0314(5) 0.1880(4) 0.099(2) Uani 1 1 d . . . H70A H 0.1183 1.0696 0.1920 0.119 Uiso 1 1 calc R . . H70B H 0.2161 0.9999 0.2267 0.119 Uiso 1 1 calc R . . C71 C 0.2711(7) 1.0955(6) 0.1744(5) 0.136(4) Uani 1 1 d . . . H71A H 0.2639 1.1421 0.2061 0.203 Uiso 1 1 calc R . . H71B H 0.2508 1.1270 0.1361 0.203 Uiso 1 1 calc R . . H71C H 0.3476 1.0588 0.1723 0.203 Uiso 1 1 calc R . . C72 C -0.0162(4) 0.4281(3) 0.1221(3) 0.0507(13) Uani 1 1 d . . . H72A H 0.0649 0.4087 0.1166 0.061 Uiso 1 1 calc R . . H72B H -0.0509 0.4407 0.0823 0.061 Uiso 1 1 calc R . . C73 C -0.0591(5) 0.3506(4) 0.1551(4) 0.076(2) Uani 1 1 d . . . H73A H -0.0244 0.3418 0.1950 0.091 Uiso 1 1 calc R . . H73B H -0.1395 0.3742 0.1616 0.091 Uiso 1 1 calc R . . C74 C -0.0413(8) 0.2604(6) 0.1275(4) 0.114(3) Uani 1 1 d . . . H74A H 0.0382 0.2345 0.1195 0.137 Uiso 1 1 calc R . . H74B H -0.0818 0.2649 0.0894 0.137 Uiso 1 1 calc R . . C75 C -0.0878(9) 0.1951(8) 0.1749(9) 0.299(13) Uani 1 1 d . . . H75A H -0.0795 0.1328 0.1580 0.448 Uiso 1 1 calc R . . H75B H -0.1661 0.2227 0.1832 0.448 Uiso 1 1 calc R . . H75C H -0.0460 0.1905 0.2121 0.448 Uiso 1 1 calc R . . C76 C 0.2620(8) 0.4040(7) 0.2335(5) 0.125(4) Uani 1 1 d . . . H76A H 0.3030 0.3755 0.2693 0.149 Uiso 1 1 calc R . . H76B H 0.1840 0.4248 0.2465 0.149 Uiso 1 1 calc R . . C77 C 0.2947(7) 0.4843(6) 0.2252(5) 0.111(3) Uani 1 1 d . . . H77A H 0.2516 0.5134 0.1902 0.133 Uiso 1 1 calc R . . H77B H 0.3718 0.4632 0.2106 0.133 Uiso 1 1 calc R . . C78 C 0.2972(8) 0.5617(7) 0.2630(5) 0.118(3) Uani 1 1 d . . . H78A H 0.2205 0.5819 0.2783 0.141 Uiso 1 1 calc R . . H78B H 0.3416 0.5326 0.2976 0.141 Uiso 1 1 calc R . . C79 C 0.3281(8) 0.6418(6) 0.2546(5) 0.112(3) Uani 1 1 d . . . H79A H 0.4057 0.6219 0.2407 0.134 Uiso 1 1 calc R . . H79B H 0.2854 0.6704 0.2194 0.134 Uiso 1 1 calc R . . F1 F 0.2631(5) 0.3346(4) 0.1992(3) 0.156(2) Uani 1 1 d . . . F2 F 0.3273(5) 0.7108(4) 0.2891(3) 0.144(2) Uani 1 1 d . . . 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 0.059(2) 0.0295(16) 0.0342(16) -0.0034(13) -0.0086(14) -0.0114(14) O2 0.0444(18) 0.0371(17) 0.0499(19) 0.0084(14) -0.0125(15) -0.0178(14) O3 0.0353(16) 0.0341(16) 0.0410(17) -0.0087(13) 0.0025(13) -0.0087(13) O4 0.0385(17) 0.0331(17) 0.0508(19) -0.0070(14) 0.0048(14) -0.0103(13) O5 0.0512(18) 0.0399(17) 0.0272(15) 0.0011(13) -0.0083(13) -0.0212(14) O6 0.0563(19) 0.0325(16) 0.0290(15) -0.0032(12) -0.0008(14) -0.0124(14) O7 0.0378(16) 0.0283(15) 0.0469(18) 0.0009(13) -0.0129(14) -0.0081(13) O8 0.0344(15) 0.0394(17) 0.0334(16) -0.0047(13) -0.0065(12) -0.0083(13) O9 0.067(2) 0.0404(19) 0.0438(18) -0.0061(15) 0.0178(16) -0.0250(16) O10 0.0441(18) 0.0392(18) 0.055(2) -0.0099(15) 0.0102(15) -0.0179(14) C1 0.030(2) 0.032(2) 0.029(2) -0.0054(17) 0.0056(17) -0.0047(17) C2 0.0231(19) 0.034(2) 0.028(2) -0.0037(17) 0.0041(16) -0.0040(16) C3 0.027(2) 0.036(2) 0.036(2) -0.0066(18) 0.0013(17) -0.0070(17) C4 0.028(2) 0.031(2) 0.034(2) 0.0014(17) 0.0046(17) -0.0092(17) C5 0.0230(19) 0.039(2) 0.026(2) -0.0032(17) 0.0025(16) -0.0041(17) C6 0.033(2) 0.035(2) 0.027(2) -0.0074(17) 0.0024(17) -0.0105(18) C7 0.033(2) 0.037(2) 0.027(2) -0.0012(17) 0.0057(17) -0.0109(18) C8 0.029(2) 0.036(2) 0.0205(19) 0.0005(16) -0.0035(15) -0.0068(17) C9 0.034(2) 0.037(2) 0.025(2) 0.0030(17) -0.0019(17) -0.0122(18) C10 0.037(2) 0.030(2) 0.0229(19) 0.0000(16) -0.0006(17) -0.0066(17) C11 0.030(2) 0.036(2) 0.0198(18) 0.0049(16) -0.0078(16) -0.0068(17) C12 0.031(2) 0.031(2) 0.0247(19) 0.0018(16) -0.0037(16) -0.0107(17) C13 0.033(2) 0.033(2) 0.0224(19) -0.0017(16) -0.0022(16) -0.0066(17) C14 0.029(2) 0.033(2) 0.028(2) 0.0037(17) -0.0043(16) -0.0050(17) C15 0.0233(19) 0.031(2) 0.028(2) 0.0016(16) -0.0017(16) -0.0007(16) C16 0.031(2) 0.028(2) 0.034(2) 0.0024(17) -0.0006(17) -0.0029(17) C17 0.028(2) 0.031(2) 0.027(2) -0.0013(16) 0.0016(16) -0.0039(16) C18 0.0197(18) 0.028(2) 0.028(2) 0.0029(16) -0.0010(15) -0.0035(15) C19 0.0249(19) 0.034(2) 0.029(2) 0.0041(17) 0.0002(16) -0.0101(16) C20 0.0253(19) 0.033(2) 0.028(2) 0.0003(17) -0.0042(16) -0.0083(16) C21 0.027(2) 0.034(2) 0.027(2) -0.0019(17) 0.0015(16) -0.0043(17) C22 0.028(2) 0.034(2) 0.0201(19) 0.0003(16) 0.0006(15) -0.0022(17) C23 0.035(2) 0.030(2) 0.025(2) -0.0012(16) 0.0053(17) -0.0074(17) C24 0.031(2) 0.039(2) 0.0199(19) -0.0027(16) 0.0028(16) -0.0102(18) C25 0.027(2) 0.038(2) 0.0200(19) 0.0021(16) 0.0013(16) -0.0011(17) C26 0.031(2) 0.029(2) 0.028(2) 0.0024(16) 0.0002(17) -0.0047(17) C27 0.030(2) 0.035(2) 0.027(2) 0.0025(17) -0.0018(16) -0.0105(17) C28 0.033(2) 0.039(2) 0.023(2) 0.0023(17) -0.0019(17) -0.0035(18) C29 0.0243(19) 0.034(2) 0.0248(19) 0.0010(16) -0.0049(15) -0.0026(16) C30 0.028(2) 0.037(2) 0.030(2) -0.0053(17) -0.0033(17) -0.0047(17) C31 0.025(2) 0.039(2) 0.031(2) -0.0015(18) -0.0022(17) -0.0092(17) C32 0.0224(19) 0.038(2) 0.029(2) -0.0004(17) -0.0041(16) -0.0053(17) C33 0.033(2) 0.035(2) 0.029(2) -0.0054(17) -0.0002(17) -0.0063(18) C34 0.032(2) 0.035(2) 0.030(2) 0.0009(18) -0.0016(17) -0.0081(18) C35 0.026(2) 0.039(2) 0.031(2) -0.0009(18) -0.0002(17) -0.0061(17) C36 0.052(3) 0.040(3) 0.044(3) -0.008(2) -0.001(2) -0.018(2) C37 0.082(4) 0.039(3) 0.044(3) -0.009(2) 0.002(3) -0.029(3) C38 0.072(4) 0.040(3) 0.054(3) -0.004(2) -0.007(3) -0.015(3) C39 0.125(6) 0.044(3) 0.090(5) -0.001(3) -0.042(4) -0.016(4) C40 0.057(3) 0.049(3) 0.074(4) 0.007(3) -0.027(3) -0.024(3) C41 0.055(3) 0.061(4) 0.093(5) -0.022(3) 0.015(3) -0.026(3) C42 0.056(4) 0.070(4) 0.098(5) -0.015(4) -0.010(3) -0.017(3) C43 0.101(5) 0.056(4) 0.061(4) 0.014(3) -0.024(3) -0.028(3) C44 0.034(2) 0.036(2) 0.027(2) -0.0006(17) -0.0015(17) -0.0081(18) C45 0.040(2) 0.033(2) 0.032(2) -0.0012(18) -0.0011(18) -0.0046(19) C46 0.053(3) 0.038(3) 0.058(3) -0.007(2) 0.003(2) -0.012(2) C47 0.083(4) 0.043(3) 0.092(5) -0.018(3) 0.006(4) -0.016(3) C48 0.052(3) 0.044(3) 0.044(3) -0.012(2) 0.009(2) -0.018(2) C49 0.064(3) 0.043(3) 0.058(3) -0.014(2) -0.001(3) -0.010(2) C50 0.112(6) 0.057(4) 0.086(5) -0.024(3) 0.016(4) -0.036(4) C51 0.153(8) 0.061(5) 0.110(6) -0.009(4) -0.008(6) -0.027(5) C52 0.031(2) 0.036(2) 0.033(2) -0.0005(18) -0.0013(17) -0.0088(18) C53 0.039(2) 0.044(3) 0.030(2) -0.0061(19) -0.0006(18) -0.016(2) C54 0.048(3) 0.041(3) 0.038(2) -0.007(2) 0.006(2) -0.012(2) C55 0.086(4) 0.056(3) 0.051(3) -0.015(3) 0.006(3) -0.037(3) C56 0.063(3) 0.031(2) 0.039(3) -0.0007(19) 0.002(2) -0.011(2) C57 0.070(3) 0.035(3) 0.047(3) -0.004(2) -0.006(2) -0.014(2) C58 0.098(5) 0.083(5) 0.059(4) -0.030(3) 0.010(4) -0.013(4) C59 0.168(8) 0.098(6) 0.046(4) -0.018(4) 0.005(4) 0.001(5) C60 0.047(3) 0.030(2) 0.049(3) 0.004(2) -0.011(2) -0.009(2) C61 0.051(3) 0.035(3) 0.054(3) -0.001(2) -0.022(2) -0.006(2) C62 0.078(4) 0.031(3) 0.074(4) 0.003(2) -0.034(3) -0.011(3) C63 0.127(6) 0.033(3) 0.148(7) -0.002(4) -0.082(6) -0.023(4) C64 0.039(2) 0.039(3) 0.032(2) -0.0048(19) -0.0020(18) -0.0101(19) C65 0.044(3) 0.051(3) 0.046(3) -0.013(2) -0.003(2) -0.009(2) C66 0.060(3) 0.052(3) 0.071(4) -0.006(3) -0.015(3) -0.017(3) C67 0.078(5) 0.070(4) 0.121(6) -0.010(4) -0.038(4) -0.017(4) C68 0.083(4) 0.050(3) 0.079(4) -0.017(3) 0.025(3) -0.029(3) C69 0.113(6) 0.072(5) 0.124(7) -0.021(5) 0.046(5) -0.033(4) C70 0.091(5) 0.083(5) 0.126(7) 0.002(5) -0.019(5) -0.024(4) C71 0.101(6) 0.101(7) 0.219(12) 0.051(7) -0.018(7) -0.054(5) C72 0.047(3) 0.040(3) 0.068(3) -0.013(2) 0.003(2) -0.014(2) C73 0.040(3) 0.043(3) 0.148(6) -0.009(4) 0.028(3) -0.019(2) C74 0.114(7) 0.085(6) 0.146(8) 0.008(5) -0.030(6) -0.032(5) C75 0.097(7) 0.124(9) 0.64(4) 0.197(15) 0.131(13) 0.033(6) C76 0.115(7) 0.097(7) 0.170(10) -0.046(7) -0.015(7) -0.039(6) C77 0.073(5) 0.095(6) 0.160(9) -0.021(6) 0.005(5) -0.011(4) C78 0.108(7) 0.108(7) 0.143(8) -0.043(6) 0.045(6) -0.039(6) C79 0.108(7) 0.095(6) 0.140(8) -0.036(6) 0.016(6) -0.037(5) F1 0.134(5) 0.114(4) 0.222(7) -0.060(4) -0.005(4) -0.030(3) F2 0.151(5) 0.130(4) 0.162(5) -0.062(4) 0.024(4) -0.052(4) _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 1.370(5) . ? O1 C36 1.431(5) . ? O2 C4 1.376(5) . ? O2 C40 1.436(5) . ? O3 C13 1.385(5) . ? O3 C44 1.416(5) . ? O4 C10 1.387(5) . ? O4 C48 1.419(5) . ? O5 C20 1.388(5) . ? O5 C52 1.425(5) . ? O6 C17 1.379(5) . ? O6 C56 1.432(5) . ? O7 C27 1.379(5) . ? O7 C60 1.416(5) . ? O8 C24 1.379(5) . ? O8 C64 1.423(5) . ? O9 C34 1.384(5) . ? O9 C68 1.409(6) . ? O10 C31 1.382(5) . ? O10 C72 1.425(5) . ? C1 C6 1.394(6) . ? C1 C2 1.403(5) . ? C2 C3 1.383(6) . ? C2 C35 1.525(5) . ? C3 C4 1.397(6) . ? C3 H3A 0.9300 . ? C4 C5 1.395(6) . ? C5 C6 1.383(6) . ? C5 C7 1.514(6) . ? C6 H6A 0.9300 . ? C7 C8 1.533(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C13 1.383(6) . ? C8 C9 1.395(6) . ? C9 C10 1.384(6) . ? C9 H9A 0.9300 . ? C10 C11 1.386(6) . ? C11 C12 1.399(5) . ? C11 C14 1.529(5) . ? C12 C13 1.389(5) . ? C12 H12A 0.9300 . ? C14 C15 1.507(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.394(6) . ? C15 C16 1.394(5) . ? C16 C17 1.394(6) . ? C16 H16A 0.9300 . ? C17 C18 1.386(5) . ? C18 C19 1.386(5) . ? C18 C21 1.533(5) . ? C19 C20 1.386(5) . ? C19 H19A 0.9300 . ? C21 C22 1.516(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.389(6) . ? C22 C23 1.387(6) . ? C23 C24 1.391(6) . ? C23 H23A 0.9300 . ? C24 C25 1.389(6) . ? C25 C26 1.401(6) . ? C25 C28 1.516(5) . ? C26 C27 1.394(5) . ? C26 H26A 0.9300 . ? C28 C29 1.515(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.388(6) . ? C29 C34 1.386(5) . ? C30 C31 1.386(6) . ? C30 H30A 0.9300 . ? C31 C32 1.397(6) . ? C32 C33 1.376(6) . ? C32 C35 1.512(5) . ? C33 C34 1.385(6) . ? C33 H33A 0.9300 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.507(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.521(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.524(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.542(8) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.440(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.565(9) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.514(6) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.513(6) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.525(7) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 C49 1.513(6) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.505(8) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.505(9) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.504(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.514(6) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.514(6) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.503(6) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.508(8) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.532(9) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.509(6) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.511(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.518(7) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65 1.515(6) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C66 1.521(7) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.491(7) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 C69 1.502(8) . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.498(10) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.492(10) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 C73 1.525(7) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.411(9) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.592(13) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 F1 1.257(9) . ? C76 C77 1.328(11) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C78 1.406(11) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C79 1.315(11) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C79 F2 1.255(8) . ? C79 H79A 0.9700 . ? C79 H79B 0.9700 . ? 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 C1 O1 C36 118.8(3) . . ? C4 O2 C40 116.8(3) . . ? C13 O3 C44 117.7(3) . . ? C10 O4 C48 117.7(3) . . ? C20 O5 C52 118.8(3) . . ? C17 O6 C56 117.7(3) . . ? C27 O7 C60 118.4(3) . . ? C24 O8 C64 117.0(3) . . ? C34 O9 C68 118.1(4) . . ? C31 O10 C72 117.9(3) . . ? O1 C1 C6 124.5(4) . . ? O1 C1 C2 115.8(4) . . ? C6 C1 C2 119.7(4) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C35 121.1(4) . . ? C1 C2 C35 120.2(4) . . ? C2 C3 C4 121.2(4) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? O2 C4 C3 123.2(4) . . ? O2 C4 C5 116.6(4) . . ? C3 C4 C5 120.2(4) . . ? C6 C5 C4 118.5(4) . . ? C6 C5 C7 120.4(4) . . ? C4 C5 C7 121.0(4) . . ? C5 C6 C1 121.7(4) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? C5 C7 C8 110.2(3) . . ? C5 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? C5 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C13 C8 C9 118.4(4) . . ? C13 C8 C7 121.8(4) . . ? C9 C8 C7 119.7(4) . . ? C10 C9 C8 121.4(4) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C9 C10 O4 123.8(4) . . ? C9 C10 C11 120.1(4) . . ? O4 C10 C11 116.1(3) . . ? C10 C11 C12 118.7(4) . . ? C10 C11 C14 121.9(4) . . ? C12 C11 C14 119.3(4) . . ? C13 C12 C11 120.7(4) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C8 C13 O3 116.9(3) . . ? C8 C13 C12 120.5(4) . . ? O3 C13 C12 122.5(4) . . ? C15 C14 C11 111.4(3) . . ? C15 C14 H14A 109.3 . . ? C11 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C11 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C20 C15 C16 118.4(4) . . ? C20 C15 C14 121.2(4) . . ? C16 C15 C14 120.3(4) . . ? C17 C16 C15 120.8(4) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C18 C17 O6 116.3(3) . . ? C18 C17 C16 120.5(4) . . ? O6 C17 C16 123.2(4) . . ? C17 C18 C19 118.7(4) . . ? C17 C18 C21 120.7(3) . . ? C19 C18 C21 120.6(3) . . ? C20 C19 C18 121.3(4) . . ? C20 C19 H19A 119.4 . . ? C18 C19 H19A 119.4 . . ? C19 C20 C15 120.4(4) . . ? C19 C20 O5 124.2(4) . . ? C15 C20 O5 115.4(3) . . ? C22 C21 C18 112.5(3) . . ? C22 C21 H21A 109.1 . . ? C18 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C18 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C27 C22 C23 118.5(4) . . ? C27 C22 C21 120.5(4) . . ? C23 C22 C21 120.9(4) . . ? C24 C23 C22 121.6(4) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? O8 C24 C23 123.4(4) . . ? O8 C24 C25 116.4(3) . . ? C23 C24 C25 120.1(4) . . ? C24 C25 C26 118.5(4) . . ? C24 C25 C28 121.2(4) . . ? C26 C25 C28 120.1(4) . . ? C27 C26 C25 120.9(4) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? O7 C27 C22 116.3(3) . . ? O7 C27 C26 123.4(4) . . ? C22 C27 C26 120.3(4) . . ? C29 C28 C25 109.5(3) . . ? C29 C28 H28A 109.8 . . ? C25 C28 H28A 109.8 . . ? C29 C28 H28B 109.8 . . ? C25 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C34 118.3(4) . . ? C30 C29 C28 120.0(4) . . ? C34 C29 C28 121.6(4) . . ? C29 C30 C31 121.6(4) . . ? C29 C30 H30A 119.2 . . ? C31 C30 H30A 119.2 . . ? C30 C31 O10 124.2(4) . . ? C30 C31 C32 119.8(4) . . ? O10 C31 C32 115.9(3) . . ? C33 C32 C31 118.3(4) . . ? C33 C32 C35 121.3(4) . . ? C31 C32 C35 120.4(4) . . ? C32 C33 C34 121.9(4) . . ? C32 C33 H33A 119.1 . . ? C34 C33 H33A 119.1 . . ? C33 C34 C29 120.1(4) . . ? C33 C34 O9 123.0(4) . . ? C29 C34 O9 116.9(4) . . ? C32 C35 C2 114.4(3) . . ? C32 C35 H35A 108.7 . . ? C2 C35 H35A 108.7 . . ? C32 C35 H35B 108.7 . . ? C2 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? O1 C36 C37 107.4(4) . . ? O1 C36 H36A 110.2 . . ? C37 C36 H36A 110.2 . . ? O1 C36 H36B 110.2 . . ? C37 C36 H36B 110.2 . . ? H36A C36 H36B 108.5 . . ? C36 C37 C38 112.7(4) . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? C36 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 C39 114.4(5) . . ? C37 C38 H38A 108.7 . . ? C39 C38 H38A 108.7 . . ? C37 C38 H38B 108.7 . . ? C39 C38 H38B 108.7 . . ? H38A C38 H38B 107.6 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O2 C40 C41 107.2(4) . . ? O2 C40 H40A 110.3 . . ? C41 C40 H40A 110.3 . . ? O2 C40 H40B 110.3 . . ? C41 C40 H40B 110.3 . . ? H40A C40 H40B 108.5 . . ? C42 C41 C40 113.4(5) . . ? C42 C41 H41A 108.8 . . ? C40 C41 H41A 108.9 . . ? C42 C41 H41B 108.9 . . ? C40 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C41 C42 C43 110.3(6) . . ? C41 C42 H42A 109.6 . . ? C43 C42 H42A 109.6 . . ? C41 C42 H42B 109.6 . . ? C43 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.4 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O3 C44 C45 108.9(3) . . ? O3 C44 H44A 109.9 . . ? C45 C44 H44A 109.9 . . ? O3 C44 H44B 109.9 . . ? C45 C44 H44B 109.9 . . ? H44A C44 H44B 108.3 . . ? C46 C45 C44 111.8(4) . . ? C46 C45 H45A 109.2 . . ? C44 C45 H45A 109.2 . . ? C46 C45 H45B 109.2 . . ? C44 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C45 C46 C47 113.0(4) . . ? C45 C46 H46A 109.0 . . ? C47 C46 H46A 109.0 . . ? C45 C46 H46B 109.0 . . ? C47 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O4 C48 C49 108.6(4) . . ? O4 C48 H48A 110.0 . . ? C49 C48 H48A 110.0 . . ? O4 C48 H48B 110.0 . . ? C49 C48 H48B 110.0 . . ? H48A C48 H48B 108.3 . . ? C50 C49 C48 111.5(5) . . ? C50 C49 H49A 109.3 . . ? C48 C49 H49A 109.3 . . ? C50 C49 H49B 109.3 . . ? C48 C49 H49B 109.3 . . ? H49A C49 H49B 108.0 . . ? C51 C50 C49 114.6(6) . . ? C51 C50 H50A 108.6 . . ? C49 C50 H50A 108.6 . . ? C51 C50 H50B 108.6 . . ? C49 C50 H50B 108.6 . . ? H50A C50 H50B 107.6 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O5 C52 C53 108.0(3) . . ? O5 C52 H52A 110.1 . . ? C53 C52 H52A 110.1 . . ? O5 C52 H52B 110.1 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C52 C53 C54 112.3(4) . . ? C52 C53 H53A 109.2 . . ? C54 C53 H53A 109.2 . . ? C52 C53 H53B 109.1 . . ? C54 C53 H53B 109.1 . . ? H53A C53 H53B 107.9 . . ? C53 C54 C55 113.0(4) . . ? C53 C54 H54A 109.0 . . ? C55 C54 H54A 109.0 . . ? C53 C54 H54B 109.0 . . ? C55 C54 H54B 109.0 . . ? H54A C54 H54B 107.8 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O6 C56 C57 107.8(4) . . ? O6 C56 H56A 110.1 . . ? C57 C56 H56A 110.1 . . ? O6 C56 H56B 110.2 . . ? C57 C56 H56B 110.1 . . ? H56A C56 H56B 108.5 . . ? C56 C57 C58 114.4(5) . . ? C56 C57 H57A 108.6 . . ? C58 C57 H57A 108.6 . . ? C56 C57 H57B 108.7 . . ? C58 C57 H57B 108.7 . . ? H57A C57 H57B 107.6 . . ? C57 C58 C59 111.2(6) . . ? C57 C58 H58A 109.4 . . ? C59 C58 H58A 109.4 . . ? C57 C58 H58B 109.4 . . ? C59 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O7 C60 C61 107.7(4) . . ? O7 C60 H60A 110.2 . . ? C61 C60 H60A 110.2 . . ? O7 C60 H60B 110.2 . . ? C61 C60 H60B 110.2 . . ? H60A C60 H60B 108.5 . . ? C62 C61 C60 112.2(4) . . ? C62 C61 H61A 109.2 . . ? C60 C61 H61A 109.2 . . ? C62 C61 H61B 109.2 . . ? C60 C61 H61B 109.2 . . ? H61A C61 H61B 107.9 . . ? C61 C62 C63 111.8(4) . . ? C61 C62 H62A 109.3 . . ? C63 C62 H62A 109.2 . . ? C61 C62 H62B 109.2 . . ? C63 C62 H62B 109.3 . . ? H62A C62 H62B 107.9 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O8 C64 C65 109.1(4) . . ? O8 C64 H64A 109.9 . . ? C65 C64 H64A 109.9 . . ? O8 C64 H64B 109.9 . . ? C65 C64 H64B 109.9 . . ? H64A C64 H64B 108.3 . . ? C66 C65 C64 111.4(4) . . ? C66 C65 H65A 109.3 . . ? C64 C65 H65A 109.4 . . ? C66 C65 H65B 109.4 . . ? C64 C65 H65B 109.3 . . ? H65A C65 H65B 108.0 . . ? C67 C66 C65 114.9(5) . . ? C67 C66 H66A 108.5 . . ? C65 C66 H66A 108.5 . . ? C67 C66 H66B 108.5 . . ? C65 C66 H66B 108.6 . . ? H66A C66 H66B 107.5 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O9 C68 C69 110.9(5) . . ? O9 C68 H68A 109.5 . . ? C69 C68 H68A 109.4 . . ? O9 C68 H68B 109.4 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? C70 C69 C68 113.1(6) . . ? C70 C69 H69A 109.0 . . ? C68 C69 H69A 109.0 . . ? C70 C69 H69B 108.9 . . ? C68 C69 H69B 108.9 . . ? H69A C69 H69B 107.8 . . ? C71 C70 C69 113.4(8) . . ? C71 C70 H70A 108.9 . . ? C69 C70 H70A 108.9 . . ? C71 C70 H70B 108.9 . . ? C69 C70 H70B 108.8 . . ? H70A C70 H70B 107.7 . . ? C70 C71 H71A 109.4 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O10 C72 C73 106.5(4) . . ? O10 C72 H72A 110.4 . . ? C73 C72 H72A 110.4 . . ? O10 C72 H72B 110.4 . . ? C73 C72 H72B 110.4 . . ? H72A C72 H72B 108.6 . . ? C74 C73 C72 118.4(6) . . ? C74 C73 H73A 107.7 . . ? C72 C73 H73A 107.7 . . ? C74 C73 H73B 107.7 . . ? C72 C73 H73B 107.7 . . ? H73A C73 H73B 107.1 . . ? C73 C74 C75 105.8(10) . . ? C73 C74 H74A 110.6 . . ? C75 C74 H74A 110.6 . . ? C73 C74 H74B 110.5 . . ? C75 C74 H74B 110.6 . . ? H74A C74 H74B 108.7 . . ? C74 C75 H75A 109.4 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? F1 C76 C77 132.4(11) . . ? F1 C76 H76A 104.1 . . ? C77 C76 H76A 104.2 . . ? F1 C76 H76B 104.1 . . ? C77 C76 H76B 104.1 . . ? H76A C76 H76B 105.5 . . ? C76 C77 C78 133.6(10) . . ? C76 C77 H77A 103.8 . . ? C78 C77 H77A 103.8 . . ? C76 C77 H77B 103.8 . . ? C78 C77 H77B 103.8 . . ? H77A C77 H77B 105.4 . . ? C79 C78 C77 133.7(10) . . ? C79 C78 H78A 103.8 . . ? C77 C78 H78A 103.8 . . ? C79 C78 H78B 103.9 . . ? C77 C78 H78B 103.8 . . ? H78A C78 H78B 105.4 . . ? F2 C79 C78 132.3(10) . . ? F2 C79 H79A 104.1 . . ? C78 C79 H79A 104.1 . . ? F2 C79 H79B 104.2 . . ? C78 C79 H79B 104.2 . . ? H79A C79 H79B 105.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.396 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.103 # Attachment 'DIBu-BuP5A.cif' data_mo_10902a_0m _database_code_depnum_ccdc_archive 'CCDC 863691' #TrackingRef 'DIBu-BuP5A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H118 I2 O10' _chemical_formula_weight 1481.53 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.136(2) _cell_length_b 24.590(4) _cell_length_c 24.775(4) _cell_angle_alpha 61.226(2) _cell_angle_beta 81.302(2) _cell_angle_gamma 74.159(2) _cell_volume 7774(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9626 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.44 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7522 _exptl_absorpt_correction_T_max 0.7818 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42356 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 25.01 _reflns_number_total 26098 _reflns_number_gt 16646 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _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^)+(0.2000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26098 _refine_ls_number_parameters 1639 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.2447 _refine_ls_R_factor_gt 0.1970 _refine_ls_wR_factor_ref 0.5428 _refine_ls_wR_factor_gt 0.4940 _refine_ls_goodness_of_fit_ref 2.082 _refine_ls_restrained_S_all 2.090 _refine_ls_shift/su_max 14.977 _refine_ls_shift/su_mean 0.289 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 I3 I 0.28617(15) 0.30757(9) 0.20723(8) 0.1012(7) Uani 1 1 d D . . O1 O 0.8436(6) 0.1543(4) 0.6314(4) 0.0243(19) Uani 1 1 d . . . O2 O 1.0303(6) 0.3477(4) 0.5197(4) 0.0252(19) Uani 1 1 d . . . O3 O 0.9817(6) 0.0002(4) 0.8507(4) 0.0253(19) Uani 1 1 d . . . O4 O 1.2014(6) 0.1224(4) 0.6512(4) 0.0263(19) Uani 1 1 d . . . O5 O 0.8941(5) 0.1269(4) 0.9628(4) 0.0209(17) Uani 1 1 d . . . O6 O 1.2435(5) 0.0925(4) 0.8713(4) 0.0226(18) Uani 1 1 d . . . O7 O 0.7290(6) 0.3503(4) 0.8202(4) 0.030(2) Uani 1 1 d . . . O8 O 1.0909(6) 0.3025(4) 0.8746(4) 0.035(2) Uani 1 1 d . . . O9 O 0.6900(7) 0.3756(5) 0.6117(4) 0.036(2) Uani 1 1 d . . . O10 O 0.9697(6) 0.4526(4) 0.6548(4) 0.034(2) Uani 1 1 d . . . O11 O -0.2025(7) 0.3767(5) 0.3514(4) 0.038(2) Uani 1 1 d . . . O12 O 0.0213(6) 0.4975(4) 0.1544(4) 0.029(2) Uani 1 1 d . . . O13 O -0.2512(6) 0.4098(5) 0.1302(4) 0.037(2) Uani 1 1 d . . . O14 O 0.1052(6) 0.3771(4) 0.0365(4) 0.0233(18) Uani 1 1 d . . . O15 O -0.0945(6) 0.2031(4) 0.1208(4) 0.036(2) Uani 1 1 d . . . O16 O 0.2696(6) 0.1531(5) 0.1724(4) 0.032(2) Uani 1 1 d . . . O17 O 0.0249(6) 0.0520(4) 0.3362(4) 0.028(2) Uani 1 1 d . . . O18 O 0.3132(6) 0.1184(4) 0.3858(4) 0.029(2) Uani 1 1 d . . . O19 O -0.0314(6) 0.1478(4) 0.4816(4) 0.0258(19) Uani 1 1 d . . . O20 O 0.1580(7) 0.3406(4) 0.3688(4) 0.031(2) Uani 1 1 d . . . C1 C 0.8869(8) 0.2044(5) 0.6022(5) 0.018(2) Uani 1 1 d . . . C2 C 0.9831(8) 0.1870(5) 0.5980(5) 0.016(2) Uani 1 1 d . . . C3 C 1.0305(8) 0.2349(5) 0.5706(5) 0.016(2) Uani 1 1 d . . . H3A H 1.0956 0.2234 0.5675 0.019 Uiso 1 1 calc R . . C4 C 0.9873(8) 0.2985(6) 0.5476(5) 0.019(2) Uani 1 1 d . . . C5 C 0.8886(8) 0.3179(5) 0.5508(5) 0.018(2) Uani 1 1 d . . . C6 C 0.8409(8) 0.2687(5) 0.5783(5) 0.018(2) Uani 1 1 d . . . H6A H 0.7757 0.2794 0.5808 0.022 Uiso 1 1 calc R . . C7 C 0.8414(8) 0.3854(5) 0.5300(5) 0.020(2) Uani 1 1 d . . . H7A H 0.7794 0.3933 0.5155 0.025 Uiso 1 1 calc R . . H7B H 0.8765 0.4129 0.4952 0.025 Uiso 1 1 calc R . . C8 C 0.8331(8) 0.4015(5) 0.5826(5) 0.018(2) Uani 1 1 d . . . C9 C 0.9044(8) 0.4226(5) 0.5918(5) 0.020(2) Uani 1 1 d . . . H9A H 0.9552 0.4290 0.5636 0.023 Uiso 1 1 calc R . . C10 C 0.9013(8) 0.4341(5) 0.6415(5) 0.020(2) Uani 1 1 d . . . C11 C 0.8266(8) 0.4260(6) 0.6836(5) 0.021(3) Uani 1 1 d . . . C12 C 0.7564(8) 0.4080(6) 0.6724(5) 0.022(3) Uani 1 1 d . . . H12A H 0.7038 0.4043 0.6991 0.026 Uiso 1 1 calc R . . C13 C 0.7586(8) 0.3949(5) 0.6241(5) 0.021(3) Uani 1 1 d . . . C14 C 0.8243(9) 0.4387(5) 0.7381(5) 0.022(3) Uani 1 1 d . . . H14A H 0.7597 0.4530 0.7491 0.027 Uiso 1 1 calc R . . H14B H 0.8556 0.4736 0.7261 0.027 Uiso 1 1 calc R . . C15 C 0.8708(8) 0.3799(5) 0.7941(5) 0.016(2) Uani 1 1 d . . . C16 C 0.9585(8) 0.3690(5) 0.8080(5) 0.021(3) Uani 1 1 d . . . H16A H 0.9930 0.3994 0.7813 0.025 Uiso 1 1 calc R . . C17 C 1.0022(8) 0.3149(6) 0.8601(5) 0.021(3) Uani 1 1 d . . . C18 C 0.9504(8) 0.2693(5) 0.9003(5) 0.017(2) Uani 1 1 d . . . C19 C 0.8589(8) 0.2817(5) 0.8872(5) 0.018(2) Uani 1 1 d . . . H19A H 0.8231 0.2521 0.9138 0.021 Uiso 1 1 calc R . . C20 C 0.8180(8) 0.3366(5) 0.8357(5) 0.017(2) Uani 1 1 d . . . C21 C 0.9952(9) 0.2091(5) 0.9544(5) 0.022(3) Uani 1 1 d . . . H21A H 0.9494 0.1963 0.9885 0.027 Uiso 1 1 calc R . . H21B H 1.0453 0.2174 0.9689 0.027 Uiso 1 1 calc R . . C22 C 1.0348(8) 0.1544(5) 0.9375(5) 0.016(2) Uani 1 1 d . . . C23 C 0.9826(8) 0.1165(5) 0.9397(5) 0.016(2) Uani 1 1 d . . . C24 C 1.0212(8) 0.0681(5) 0.9235(5) 0.016(2) Uani 1 1 d . . . H24A H 0.9854 0.0393 0.9293 0.019 Uiso 1 1 calc R . . C25 C 1.1099(8) 0.0600(5) 0.8991(5) 0.016(2) Uani 1 1 d . . . C26 C 1.1563(7) 0.1013(5) 0.8954(5) 0.017(2) Uani 1 1 d . . . C27 C 1.1240(8) 0.1479(6) 0.9130(5) 0.020(3) Uani 1 1 d . . . H27A H 1.1612 0.1752 0.9088 0.024 Uiso 1 1 calc R . . C28 C 1.1459(8) 0.0093(5) 0.8776(5) 0.017(2) Uani 1 1 d . . . H28A H 1.2137 -0.0041 0.8802 0.021 Uiso 1 1 calc R . . H28B H 1.1205 -0.0285 0.9047 0.021 Uiso 1 1 calc R . . C29 C 1.1184(7) 0.0355(5) 0.8121(5) 0.014(2) Uani 1 1 d . . . C30 C 1.1744(8) 0.0650(5) 0.7633(5) 0.019(2) Uani 1 1 d . . . H30A H 1.2321 0.0675 0.7714 0.023 Uiso 1 1 calc R . . C31 C 1.1490(8) 0.0916(5) 0.7018(5) 0.018(2) Uani 1 1 d . . . C32 C 1.0647(7) 0.0889(5) 0.6891(5) 0.013(2) Uani 1 1 d . . . C33 C 1.0070(8) 0.0584(5) 0.7383(5) 0.016(2) Uani 1 1 d . . . H33A H 0.9497 0.0558 0.7297 0.019 Uiso 1 1 calc R . . C34 C 1.0316(7) 0.0317(5) 0.8000(5) 0.013(2) Uani 1 1 d . . . C35 C 1.0340(8) 0.1169(5) 0.6237(5) 0.016(2) Uani 1 1 d . . . H35A H 0.9933 0.0921 0.6227 0.020 Uiso 1 1 calc R . . H35B H 1.0885 0.1130 0.5970 0.020 Uiso 1 1 calc R . . C36 C 0.7457(9) 0.1707(6) 0.6326(6) 0.030(3) Uani 1 1 d . . . H36A H 0.7228 0.1953 0.5901 0.036 Uiso 1 1 calc R . . H36B H 0.7229 0.1974 0.6538 0.036 Uiso 1 1 calc R . . C37 C 0.7110(9) 0.1096(7) 0.6667(6) 0.033(3) Uani 1 1 d . . . H37A H 0.7394 0.0816 0.6474 0.040 Uiso 1 1 calc R . . H37B H 0.7313 0.0870 0.7098 0.040 Uiso 1 1 calc R . . C38 C 0.6106(11) 0.1203(8) 0.6667(8) 0.048(4) Uani 1 1 d . . . H38A H 0.5903 0.1408 0.6237 0.058 Uiso 1 1 calc R . . H38B H 0.5818 0.1499 0.6842 0.058 Uiso 1 1 calc R . . C39 C 0.5783(15) 0.0593(10) 0.7034(10) 0.073(6) Uani 1 1 d . . . H39A H 0.5112 0.0687 0.7019 0.110 Uiso 1 1 calc R . . H39B H 0.5967 0.0395 0.7463 0.110 Uiso 1 1 calc R . . H39C H 0.6060 0.0301 0.6860 0.110 Uiso 1 1 calc R . . C40 C 1.1273(9) 0.3310(6) 0.5196(5) 0.025(3) Uani 1 1 d . . . H40A H 1.1503 0.3059 0.4968 0.030 Uiso 1 1 calc R . . H40B H 1.1485 0.3042 0.5625 0.030 Uiso 1 1 calc R . . C41 C 1.1649(9) 0.3892(6) 0.4901(6) 0.028(3) Uani 1 1 d . . . H41A H 1.1369 0.4161 0.5106 0.034 Uiso 1 1 calc R . . H41B H 1.1474 0.4140 0.4464 0.034 Uiso 1 1 calc R . . C42 C 1.2704(10) 0.3738(7) 0.4937(7) 0.037(3) Uani 1 1 d . . . H42A H 1.2874 0.3492 0.5376 0.044 Uiso 1 1 calc R . . H42B H 1.2980 0.3463 0.4738 0.044 Uiso 1 1 calc R . . C43 C 1.3118(14) 0.4323(9) 0.4634(9) 0.063(5) Uani 1 1 d . . . H43A H 1.3787 0.4185 0.4673 0.094 Uiso 1 1 calc R . . H43B H 1.2868 0.4591 0.4838 0.094 Uiso 1 1 calc R . . H43C H 1.2964 0.4567 0.4197 0.094 Uiso 1 1 calc R . . C44 C 0.8882(8) 0.0024(6) 0.8410(5) 0.021(3) Uani 1 1 d . . . H44A H 0.8878 -0.0119 0.8100 0.025 Uiso 1 1 calc R . . H44B H 0.8502 0.0465 0.8260 0.025 Uiso 1 1 calc R . . C45 C 0.8507(8) -0.0407(6) 0.9012(5) 0.024(3) Uani 1 1 d . . . H45A H 0.8545 -0.0273 0.9324 0.029 Uiso 1 1 calc R . . H45B H 0.8883 -0.0848 0.9151 0.029 Uiso 1 1 calc R . . C46 C 0.7508(9) -0.0395(7) 0.8958(6) 0.032(3) Uani 1 1 d . . . H46A H 0.7469 -0.0504 0.8628 0.038 Uiso 1 1 calc R . . H46B H 0.7131 0.0042 0.8838 0.038 Uiso 1 1 calc R . . C47 C 0.7109(11) -0.0858(8) 0.9555(7) 0.046(4) Uani 1 1 d . . . H47A H 0.6471 -0.0830 0.9494 0.068 Uiso 1 1 calc R . . H47B H 0.7129 -0.0746 0.9883 0.068 Uiso 1 1 calc R . . H47C H 0.7471 -0.1293 0.9673 0.068 Uiso 1 1 calc R . . C48 C 1.2878(10) 0.1266(7) 0.6602(6) 0.037(3) Uani 1 1 d D . . H48A H 1.3283 0.0833 0.6789 0.044 Uiso 1 1 calc R . . H48B H 1.2813 0.1442 0.6895 0.044 Uiso 1 1 calc R . . C49 C 1.3310(13) 0.1667(8) 0.6031(7) 0.057(5) Uani 1 1 d D . . H49A H 1.2963 0.2117 0.5872 0.068 Uiso 1 1 calc R . . H49B H 1.3947 0.1642 0.6108 0.068 Uiso 1 1 calc R . . C50 C 1.332(2) 0.1452(18) 0.5593(11) 0.153(15) Uani 1 1 d D . . H50A H 1.2793 0.1252 0.5678 0.184 Uiso 1 1 calc R . . H50B H 1.3252 0.1819 0.5174 0.184 Uiso 1 1 calc R . . C51 C 1.415(3) 0.100(2) 0.563(2) 0.26(3) Uani 1 1 d D . . H51A H 1.4156 0.0854 0.5324 0.383 Uiso 1 1 calc R . . H51B H 1.4213 0.0642 0.6040 0.383 Uiso 1 1 calc R . . H51C H 1.4669 0.1207 0.5535 0.383 Uiso 1 1 calc R . . C52 C 0.8338(8) 0.0910(6) 0.9611(5) 0.021(3) Uani 1 1 d . . . H52A H 0.8561 0.0450 0.9889 0.026 Uiso 1 1 calc R . . H52B H 0.8325 0.0968 0.9187 0.026 Uiso 1 1 calc R . . C53 C 0.7395(9) 0.1149(6) 0.9812(6) 0.030(3) Uani 1 1 d . . . H53A H 0.7156 0.1596 0.9506 0.036 Uiso 1 1 calc R . . H53B H 0.7434 0.1143 1.0210 0.036 Uiso 1 1 calc R . . C54 C 0.6725(11) 0.0754(8) 0.9886(7) 0.043(4) Uani 1 1 d . . . H54A H 0.6697 0.0746 0.9493 0.052 Uiso 1 1 calc R . . H54B H 0.6944 0.0310 1.0207 0.052 Uiso 1 1 calc R . . C55 C 0.5786(15) 0.1028(12) 1.0063(11) 0.085(7) Uani 1 1 d . . . H55A H 0.5366 0.0767 1.0110 0.127 Uiso 1 1 calc R . . H55B H 0.5565 0.1465 0.9742 0.127 Uiso 1 1 calc R . . H55C H 0.5813 0.1032 1.0454 0.127 Uiso 1 1 calc R . . C56 C 1.3044(10) 0.1382(7) 0.8557(6) 0.034(3) Uani 1 1 d . . . H56A H 1.2708 0.1824 0.8295 0.041 Uiso 1 1 calc R . . H56B H 1.3212 0.1359 0.8940 0.041 Uiso 1 1 calc R . . C57 C 1.3876(11) 0.1213(8) 0.8230(8) 0.047(4) Uani 1 1 d D . . H57A H 1.3681 0.1168 0.7893 0.056 Uiso 1 1 calc R . . H57B H 1.4171 0.1579 0.8036 0.056 Uiso 1 1 calc R . . C58 C 1.4564(19) 0.0655(12) 0.8562(13) 0.133(12) Uani 1 1 d D . . H58A H 1.5071 0.0609 0.8272 0.159 Uiso 1 1 calc R . . H58B H 1.4297 0.0277 0.8731 0.159 Uiso 1 1 calc R . . C59 C 1.493(2) 0.0665(16) 0.9059(14) 0.136(12) Uani 1 1 d D . . H59A H 1.5430 0.0285 0.9249 0.204 Uiso 1 1 calc R . . H59B H 1.4448 0.0669 0.9368 0.204 Uiso 1 1 calc R . . H59C H 1.5175 0.1048 0.8898 0.204 Uiso 1 1 calc R . . C60 C 0.6682(11) 0.3111(8) 0.8651(7) 0.047(4) Uani 1 1 d . . . H60A H 0.6657 0.3131 0.9043 0.057 Uiso 1 1 calc R . . H60B H 0.6916 0.2660 0.8736 0.057 Uiso 1 1 calc R . . C61 C 0.5738(11) 0.3366(8) 0.8383(8) 0.048(4) Uani 1 1 d . . . H61A H 0.5334 0.3078 0.8653 0.057 Uiso 1 1 calc R . . H61B H 0.5779 0.3383 0.7973 0.057 Uiso 1 1 calc R . . C62 C 0.5328(12) 0.4033(9) 0.8322(9) 0.056(5) Uani 1 1 d . . . H62A H 0.5251 0.4013 0.8735 0.068 Uiso 1 1 calc R . . H62B H 0.5750 0.4315 0.8073 0.068 Uiso 1 1 calc R . . C63 C 0.4394(15) 0.4309(12) 0.8012(11) 0.083(7) Uani 1 1 d . . . H63A H 0.4130 0.4732 0.7985 0.124 Uiso 1 1 calc R . . H63B H 0.3979 0.4027 0.8257 0.124 Uiso 1 1 calc R . . H63C H 0.4474 0.4344 0.7598 0.124 Uiso 1 1 calc R . . C64 C 1.1351(13) 0.3563(9) 0.8476(9) 0.057(5) Uani 1 1 d . . . H64A H 1.0911 0.3946 0.8472 0.069 Uiso 1 1 calc R . . H64B H 1.1555 0.3661 0.8047 0.069 Uiso 1 1 calc R . . C65 C 1.2161(16) 0.3383(12) 0.8860(12) 0.085(7) Uani 1 1 d . . . H65A H 1.2472 0.3741 0.8683 0.102 Uiso 1 1 calc R . . H65B H 1.1944 0.3306 0.9283 0.102 Uiso 1 1 calc R . . C66 C 1.276(2) 0.2857(17) 0.8884(19) 0.135(12) Uani 1 1 d . . . H66A H 1.3046 0.2944 0.8471 0.162 Uiso 1 1 calc R . . H66B H 1.2450 0.2506 0.9022 0.162 Uiso 1 1 calc R . . C67 C 1.3569(17) 0.2656(13) 0.9381(11) 0.094(8) Uani 1 1 d . . . H67A H 1.4044 0.2291 0.9387 0.140 Uiso 1 1 calc R . . H67B H 1.3289 0.2541 0.9794 0.140 Uiso 1 1 calc R . . H67C H 1.3846 0.3018 0.9255 0.140 Uiso 1 1 calc R . . C68 C 0.6104(14) 0.3664(10) 0.6530(9) 0.068(5) Uani 1 1 d . . . H68A H 0.5838 0.4039 0.6603 0.081 Uiso 1 1 calc R . . H68B H 0.6261 0.3279 0.6930 0.081 Uiso 1 1 calc R . . C69 C 0.545(3) 0.358(3) 0.618(2) 0.21(2) Uani 1 1 d . . . H69A H 0.5779 0.3344 0.5957 0.251 Uiso 1 1 calc R . . H69B H 0.5079 0.3999 0.5892 0.251 Uiso 1 1 calc R . . C70 C 0.480(3) 0.315(2) 0.6786(19) 0.161(16) Uani 1 1 d . . . H70A H 0.5214 0.2810 0.7118 0.194 Uiso 1 1 calc R . . H70B H 0.4404 0.3437 0.6949 0.194 Uiso 1 1 calc R . . C71 C 0.415(3) 0.283(2) 0.660(2) 0.190(19) Uani 1 1 d . . . H71A H 0.3802 0.2585 0.6972 0.285 Uiso 1 1 calc R . . H71B H 0.4531 0.2545 0.6446 0.285 Uiso 1 1 calc R . . H71C H 0.3713 0.3167 0.6289 0.285 Uiso 1 1 calc R . . C72 C 1.0568(9) 0.4534(6) 0.6196(6) 0.026(3) Uani 1 1 d . . . H72A H 1.0759 0.4156 0.6123 0.032 Uiso 1 1 calc R . . H72B H 1.0501 0.4922 0.5792 0.032 Uiso 1 1 calc R . . C73 C 1.1256(11) 0.4527(8) 0.6562(8) 0.050(4) Uani 1 1 d . . . H73A H 1.1312 0.4137 0.6963 0.060 Uiso 1 1 calc R . . H73B H 1.1043 0.4899 0.6642 0.060 Uiso 1 1 calc R . . C74 C 1.2176(12) 0.4544(9) 0.6246(8) 0.056(5) Uani 1 1 d . . . H74A H 1.2125 0.4929 0.5840 0.067 Uiso 1 1 calc R . . H74B H 1.2405 0.4165 0.6176 0.067 Uiso 1 1 calc R . . C75 C 1.2852(19) 0.4552(17) 0.6643(16) 0.142(12) Uani 1 1 d . . . H75A H 1.3453 0.4570 0.6431 0.212 Uiso 1 1 calc R . . H75B H 1.2914 0.4164 0.7039 0.212 Uiso 1 1 calc R . . H75C H 1.2622 0.4926 0.6713 0.212 Uiso 1 1 calc R . . C76 C -0.1479(9) 0.4080(6) 0.3006(5) 0.025(3) Uani 1 1 d . . . C77 C -0.1739(9) 0.4346(6) 0.2407(6) 0.026(3) Uani 1 1 d . . . H77A H -0.2321 0.4325 0.2327 0.032 Uiso 1 1 calc R . . C78 C -0.1168(8) 0.4650(5) 0.1908(5) 0.021(2) Uani 1 1 d . . . C79 C -0.0297(8) 0.4672(5) 0.2041(5) 0.018(2) Uani 1 1 d . . . C80 C -0.0055(8) 0.4381(5) 0.2657(5) 0.022(3) Uani 1 1 d . . . H80A H 0.0531 0.4383 0.2748 0.026 Uiso 1 1 calc R . . C81 C -0.0638(8) 0.4088(5) 0.3143(5) 0.018(2) Uani 1 1 d . . . C82 C -0.1431(9) 0.4916(6) 0.1246(5) 0.025(3) Uani 1 1 d . . . H82A H -0.2108 0.5057 0.1216 0.031 Uiso 1 1 calc R . . H82B H -0.1169 0.5292 0.0981 0.031 Uiso 1 1 calc R . . C83 C -0.1085(9) 0.4423(6) 0.1018(5) 0.023(3) Uani 1 1 d . . . C84 C -0.1627(7) 0.4043(5) 0.1052(4) 0.012(2) Uani 1 1 d . . . C85 C -0.1261(9) 0.3574(6) 0.0834(5) 0.024(3) Uani 1 1 d . . . H85A H -0.1643 0.3318 0.0848 0.029 Uiso 1 1 calc R . . C86 C -0.0352(8) 0.3487(6) 0.0602(5) 0.020(3) Uani 1 1 d . . . C87 C 0.0171(8) 0.3880(6) 0.0586(5) 0.021(3) Uani 1 1 d . . . C88 C -0.0223(8) 0.4336(6) 0.0783(5) 0.020(3) Uani 1 1 d . . . H88A H 0.0144 0.4610 0.0749 0.025 Uiso 1 1 calc R . . C89 C -0.0008(9) 0.2972(6) 0.0420(5) 0.024(3) Uani 1 1 d . . . H89A H -0.0529 0.2904 0.0281 0.029 Uiso 1 1 calc R . . H89B H 0.0434 0.3106 0.0070 0.029 Uiso 1 1 calc R . . C90 C 0.0450(8) 0.2359(5) 0.0937(5) 0.016(2) Uani 1 1 d . . . C91 C -0.0039(8) 0.1887(5) 0.1354(5) 0.020(2) Uani 1 1 d . . . C92 C 0.0370(9) 0.1351(6) 0.1858(5) 0.024(3) Uani 1 1 d . . . H92A H 0.0017 0.1053 0.2126 0.029 Uiso 1 1 calc R . . C93 C 0.1256(8) 0.1236(5) 0.1983(5) 0.019(2) Uani 1 1 d . . . C94 C 0.1803(8) 0.1674(5) 0.1575(5) 0.019(2) Uani 1 1 d . . . C95 C 0.1404(8) 0.2224(5) 0.1059(5) 0.020(2) Uani 1 1 d . . . H95A H 0.1769 0.2512 0.0785 0.024 Uiso 1 1 calc R . . C96 C 0.1720(9) 0.0635(6) 0.2544(5) 0.024(3) Uani 1 1 d . . . H96A H 0.2367 0.0494 0.2433 0.029 Uiso 1 1 calc R . . H96B H 0.1407 0.0289 0.2654 0.029 Uiso 1 1 calc R . . C97 C 0.1697(8) 0.0745(5) 0.3111(5) 0.019(2) Uani 1 1 d . . . C98 C 0.0952(9) 0.0694(6) 0.3497(5) 0.024(3) Uani 1 1 d . . . C99 C 0.0919(9) 0.0785(6) 0.4022(5) 0.023(3) Uani 1 1 d . . . H99A H 0.0402 0.0734 0.4297 0.028 Uiso 1 1 calc R . . C100 C 0.1677(8) 0.0955(5) 0.4130(5) 0.021(3) Uani 1 1 d . . . C101 C 0.2410(8) 0.1028(6) 0.3714(5) 0.025(3) Uani 1 1 d . . . C102 C 0.2434(9) 0.0909(5) 0.3226(5) 0.023(3) Uani 1 1 d . . . H10A H 0.2962 0.0939 0.2961 0.028 Uiso 1 1 calc R . . C103 C 0.1606(9) 0.1098(5) 0.4670(5) 0.023(3) Uani 1 1 d . . . H10B H 0.1271 0.0811 0.5019 0.027 Uiso 1 1 calc R . . H10C H 0.2229 0.1024 0.4807 0.027 Uiso 1 1 calc R . . C104 C 0.1101(8) 0.1787(6) 0.4475(5) 0.021(2) Uani 1 1 d . . . C105 C 0.0128(8) 0.1978(5) 0.4530(5) 0.020(2) Uani 1 1 d . . . C106 C -0.0290(9) 0.2606(6) 0.4314(5) 0.022(3) Uani 1 1 d . . . H10D H -0.0940 0.2723 0.4354 0.027 Uiso 1 1 calc R . . C107 C 0.0190(9) 0.3080(6) 0.4040(6) 0.027(3) Uani 1 1 d . . . C108 C 0.1135(9) 0.2914(6) 0.3977(5) 0.022(3) Uani 1 1 d . . . C109 C 0.1586(9) 0.2257(6) 0.4202(5) 0.022(3) Uani 1 1 d . . . H10E H 0.2235 0.2141 0.4162 0.027 Uiso 1 1 calc R . . C110 C -0.0310(9) 0.3773(6) 0.3806(5) 0.022(3) Uani 1 1 d . . . H11A H 0.0105 0.4012 0.3826 0.027 Uiso 1 1 calc R . . H11B H -0.0847 0.3803 0.4080 0.027 Uiso 1 1 calc R . . C111 C -0.2882(15) 0.3784(11) 0.3414(10) 0.074(6) Uani 1 1 d . . . H11C H -0.2866 0.3567 0.3163 0.088 Uiso 1 1 calc R . . H11D H -0.3232 0.4231 0.3192 0.088 Uiso 1 1 calc R . . C112 C -0.335(3) 0.3427(18) 0.4074(18) 0.150(15) Uani 1 1 d . . . H11E H -0.3558 0.3096 0.4041 0.181 Uiso 1 1 calc R . . H11T H -0.2820 0.3191 0.4351 0.181 Uiso 1 1 calc R . . C113 C -0.385(6) 0.356(4) 0.434(3) 0.45(8) Uani 1 1 d D . . H11U H -0.4377 0.3836 0.4067 0.544 Uiso 1 1 calc R . . H11V H -0.3619 0.3826 0.4453 0.544 Uiso 1 1 calc R . . C114 C -0.420(4) 0.308(3) 0.490(2) 0.32(4) Uani 1 1 d D . . H11F H -0.4520 0.3280 0.5158 0.484 Uiso 1 1 calc R . . H11G H -0.3686 0.2731 0.5127 0.484 Uiso 1 1 calc R . . H11H H -0.4626 0.2914 0.4793 0.484 Uiso 1 1 calc R . . C115 C 0.1143(8) 0.4938(6) 0.1649(5) 0.020(2) Uani 1 1 d . . . H11I H 0.1514 0.4496 0.1789 0.025 Uiso 1 1 calc R . . H11J H 0.1152 0.5066 0.1970 0.025 Uiso 1 1 calc R . . C116 C 0.1535(9) 0.5387(6) 0.1042(6) 0.028(3) Uani 1 1 d . . . H11K H 0.1494 0.5269 0.0719 0.034 Uiso 1 1 calc R . . H11L H 0.1172 0.5830 0.0913 0.034 Uiso 1 1 calc R . . C117 C 0.2533(9) 0.5347(7) 0.1119(6) 0.032(3) Uani 1 1 d . . . H11M H 0.2895 0.4906 0.1235 0.039 Uiso 1 1 calc R . . H11N H 0.2572 0.5444 0.1458 0.039 Uiso 1 1 calc R . . C118 C 0.2951(12) 0.5815(9) 0.0523(8) 0.054(4) Uani 1 1 d . . . H11O H 0.3595 0.5771 0.0589 0.081 Uiso 1 1 calc R . . H11P H 0.2607 0.6253 0.0415 0.081 Uiso 1 1 calc R . . H11Q H 0.2917 0.5719 0.0188 0.081 Uiso 1 1 calc R . . C119 C -0.3177(17) 0.3768(11) 0.1341(9) 0.075(6) Uani 1 1 d . . . H11R H -0.3315 0.3868 0.0921 0.090 Uiso 1 1 calc R . . H11S H -0.2921 0.3303 0.1571 0.090 Uiso 1 1 calc R . . C120 C -0.3973(11) 0.3933(9) 0.1630(8) 0.051(4) Uani 1 1 d D . . H12B H -0.4062 0.4382 0.1543 0.062 Uiso 1 1 calc R . . H12S H -0.3910 0.3663 0.2081 0.062 Uiso 1 1 calc R . . C121 C -0.477(2) 0.3865(17) 0.144(2) 0.203(19) Uani 1 1 d D . . H12C H -0.4730 0.3975 0.1001 0.243 Uiso 1 1 calc R . . H12D H -0.5339 0.4141 0.1518 0.243 Uiso 1 1 calc R . . C122 C -0.478(3) 0.3197(19) 0.183(2) 0.28(3) Uani 1 1 d D . . H12E H -0.5307 0.3106 0.1728 0.415 Uiso 1 1 calc R . . H12F H -0.4817 0.3098 0.2261 0.415 Uiso 1 1 calc R . . H12G H -0.4210 0.2933 0.1748 0.415 Uiso 1 1 calc R . . C123 C 0.1656(9) 0.4125(6) 0.0407(6) 0.026(3) Uani 1 1 d . . . H12H H 0.1682 0.4039 0.0839 0.032 Uiso 1 1 calc R . . H12I H 0.1424 0.4589 0.0150 0.032 Uiso 1 1 calc R . . C124 C 0.2595(10) 0.3901(7) 0.0178(6) 0.033(3) Uani 1 1 d . . . H12J H 0.2846 0.3447 0.0463 0.040 Uiso 1 1 calc R . . H12K H 0.2546 0.3938 -0.0233 0.040 Uiso 1 1 calc R . . C125 C 0.3227(12) 0.4289(9) 0.0136(8) 0.051(4) Uani 1 1 d . . . H12L H 0.3266 0.4252 0.0548 0.062 Uiso 1 1 calc R . . H12M H 0.2967 0.4742 -0.0146 0.062 Uiso 1 1 calc R . . C126 C 0.4224(18) 0.4083(14) -0.0101(13) 0.107(9) Uani 1 1 d . . . H12N H 0.4606 0.4355 -0.0118 0.160 Uiso 1 1 calc R . . H12O H 0.4193 0.4129 -0.0513 0.160 Uiso 1 1 calc R . . H12P H 0.4493 0.3638 0.0181 0.160 Uiso 1 1 calc R . . C127 C -0.1329(12) 0.1506(8) 0.1400(8) 0.051(4) Uani 1 1 d . . . H12Q H -0.1440 0.1312 0.1852 0.061 Uiso 1 1 calc R . . H12R H -0.0896 0.1181 0.1302 0.061 Uiso 1 1 calc R . . C128 C -0.2207(17) 0.1715(11) 0.1084(11) 0.088(7) Uani 1 1 d . . . H12V H -0.2043 0.1677 0.0699 0.106 Uiso 1 1 calc R . . H12W H -0.2558 0.1386 0.1346 0.106 Uiso 1 1 calc R . . C129 C -0.280(3) 0.226(2) 0.093(3) 0.22(3) Uani 1 1 d . . . H12T H -0.2451 0.2602 0.0694 0.264 Uiso 1 1 calc R . . H12U H -0.3030 0.2290 0.1312 0.264 Uiso 1 1 calc R . . C130 C -0.3626(15) 0.2440(11) 0.0552(11) 0.076(6) Uani 1 1 d . . . H13A H -0.4050 0.2824 0.0546 0.114 Uiso 1 1 calc R . . H13B H -0.3938 0.2088 0.0737 0.114 Uiso 1 1 calc R . . H13C H -0.3426 0.2523 0.0130 0.114 Uiso 1 1 calc R . . C131 C 0.3297(11) 0.1887(8) 0.1291(8) 0.049(4) Uani 1 1 d . . . H13D H 0.3070 0.2342 0.1189 0.058 Uiso 1 1 calc R . . H13E H 0.3322 0.1851 0.0908 0.058 Uiso 1 1 calc R . . C132 C 0.4259(13) 0.1637(9) 0.1557(8) 0.057(5) Uani 1 1 d . . . H13F H 0.4668 0.1911 0.1267 0.069 Uiso 1 1 calc R . . H13G H 0.4228 0.1656 0.1950 0.069 Uiso 1 1 calc R . . C133 C 0.4642(12) 0.0973(9) 0.1665(8) 0.052(4) Uani 1 1 d . . . H13H H 0.4701 0.0960 0.1267 0.063 Uiso 1 1 calc R . . H13I H 0.4214 0.0705 0.1936 0.063 Uiso 1 1 calc R . . C134 C 0.5589(16) 0.0699(12) 0.1964(11) 0.082(7) Uani 1 1 d . . . H13J H 0.5823 0.0260 0.2029 0.124 Uiso 1 1 calc R . . H13K H 0.5529 0.0704 0.2362 0.124 Uiso 1 1 calc R . . H13L H 0.6016 0.0959 0.1693 0.124 Uiso 1 1 calc R . . C135 C -0.0580(9) 0.0515(6) 0.3715(6) 0.026(3) Uani 1 1 d . . . H13M H -0.0753 0.0887 0.3798 0.031 Uiso 1 1 calc R . . H13N H -0.0517 0.0120 0.4113 0.031 Uiso 1 1 calc R . . C136 C -0.1297(10) 0.0549(7) 0.3316(7) 0.035(3) Uani 1 1 d . . . H13O H -0.1380 0.0965 0.2940 0.042 Uiso 1 1 calc R . . H13P H -0.1055 0.0212 0.3187 0.042 Uiso 1 1 calc R . . C137 C -0.2218(13) 0.0472(9) 0.3627(8) 0.057(5) Uani 1 1 d . . . H13Q H -0.2448 0.0791 0.3782 0.069 Uiso 1 1 calc R . . H13R H -0.2150 0.0043 0.3986 0.069 Uiso 1 1 calc R . . C138 C -0.2916(14) 0.0558(11) 0.3192(10) 0.074(6) Uani 1 1 d . . . H13S H -0.3505 0.0500 0.3412 0.111 Uiso 1 1 calc R . . H13T H -0.2692 0.0241 0.3040 0.111 Uiso 1 1 calc R . . H13U H -0.2999 0.0987 0.2843 0.111 Uiso 1 1 calc R . . C139 C 0.3972(13) 0.1129(11) 0.3502(9) 0.069(6) Uani 1 1 d . . . H13V H 0.3891 0.1453 0.3065 0.082 Uiso 1 1 calc R . . H13W H 0.4173 0.0700 0.3526 0.082 Uiso 1 1 calc R . . C140 C 0.4677(17) 0.1246(14) 0.3811(12) 0.088(7) Uani 1 1 d . . . H14C H 0.4528 0.1093 0.4256 0.106 Uiso 1 1 calc R . . H14D H 0.5305 0.1013 0.3763 0.106 Uiso 1 1 calc R . . C141 C 0.463(4) 0.189(3) 0.353(3) 0.32(5) Uani 1 1 d . . . H14E H 0.3996 0.2131 0.3556 0.384 Uiso 1 1 calc R . . H14F H 0.4817 0.2045 0.3086 0.384 Uiso 1 1 calc R . . C142 C 0.538(3) 0.197(2) 0.393(2) 0.21(2) Uani 1 1 d . . . H14G H 0.5529 0.2385 0.3690 0.312 Uiso 1 1 calc R . . H14H H 0.5948 0.1631 0.3997 0.312 Uiso 1 1 calc R . . H14I H 0.5101 0.1923 0.4325 0.312 Uiso 1 1 calc R . . C143 C -0.1267(9) 0.1658(6) 0.4796(6) 0.027(3) Uani 1 1 d . . . H14J H -0.1463 0.1931 0.4364 0.032 Uiso 1 1 calc R . . H14K H -0.1509 0.1905 0.5027 0.032 Uiso 1 1 calc R . . C144 C -0.1638(8) 0.1064(6) 0.5080(6) 0.025(3) Uani 1 1 d . . . H14L H -0.1490 0.0819 0.5522 0.030 Uiso 1 1 calc R . . H14M H -0.1323 0.0794 0.4881 0.030 Uiso 1 1 calc R . . C145 C -0.2682(11) 0.1199(7) 0.5017(7) 0.042(4) Uani 1 1 d . . . H14N H -0.2993 0.1466 0.5219 0.050 Uiso 1 1 calc R . . H14X H -0.2827 0.1452 0.4574 0.050 Uiso 1 1 calc R . . C146 C -0.3068(13) 0.0643(9) 0.5274(9) 0.060(5) Uani 1 1 d . . . H14O H -0.3731 0.0779 0.5210 0.090 Uiso 1 1 calc R . . H14P H -0.2951 0.0395 0.5716 0.090 Uiso 1 1 calc R . . H14Q H -0.2781 0.0379 0.5070 0.090 Uiso 1 1 calc R . . C147 C 0.2537(10) 0.3257(7) 0.3642(7) 0.036(3) Uani 1 1 d . . . H14R H 0.2742 0.2987 0.3432 0.043 Uiso 1 1 calc R . . H14S H 0.2799 0.3017 0.4059 0.043 Uiso 1 1 calc R . . C148 C 0.2865(10) 0.3872(7) 0.3277(6) 0.036(3) Uani 1 1 d . . . H14T H 0.2636 0.4093 0.2853 0.044 Uiso 1 1 calc R . . H14U H 0.2606 0.4156 0.3469 0.044 Uiso 1 1 calc R . . C149 C 0.3866(12) 0.3754(9) 0.3255(9) 0.057(5) Uani 1 1 d . . . H14V H 0.4124 0.3451 0.3084 0.068 Uiso 1 1 calc R . . H14W H 0.4090 0.3553 0.3679 0.068 Uiso 1 1 calc R . . C150 C 0.4224(14) 0.4383(10) 0.2850(10) 0.070(6) Uani 1 1 d . . . H15Q H 0.4897 0.4278 0.2847 0.105 Uiso 1 1 calc R . . H15R H 0.3985 0.4680 0.3024 0.105 Uiso 1 1 calc R . . H15S H 0.4012 0.4582 0.2428 0.105 Uiso 1 1 calc R . . I1 I 0.68974(9) 0.18047(7) 0.79636(6) 0.0619(5) Uani 1 1 d D . . I2 I 1.14587(9) 0.26606(6) 0.70955(6) 0.0594(5) Uani 1 1 d D . . C151 C 0.790(2) 0.222(3) 0.754(2) 0.36(6) Uani 1 1 d D . . H15A H 0.7976 0.2204 0.7145 0.437 Uiso 1 1 calc R . . H15B H 0.7642 0.2671 0.7439 0.437 Uiso 1 1 calc R . . C152 C 0.8843(10) 0.2095(8) 0.7719(7) 0.046(4) Uani 1 1 d D . . H15C H 0.8819 0.2123 0.8107 0.055 Uiso 1 1 calc R . . H15D H 0.9158 0.1653 0.7806 0.055 Uiso 1 1 calc R . . C153 C 0.9369(18) 0.2502(15) 0.7287(12) 0.128(12) Uani 1 1 d D . . H15E H 0.9067 0.2944 0.7210 0.153 Uiso 1 1 calc R . . H15F H 0.9380 0.2485 0.6895 0.153 Uiso 1 1 calc R . . C154 C 1.032(2) 0.236(3) 0.746(2) 0.26(3) Uani 1 1 d D . . H15G H 1.0526 0.1895 0.7603 0.307 Uiso 1 1 calc R . . H15H H 1.0238 0.2402 0.7848 0.307 Uiso 1 1 calc R . . I4 I -0.18221(18) 0.23704(9) 0.29104(9) 0.1135(8) Uani 1 1 d D . . C155 C 0.1761(18) 0.276(2) 0.240(2) 0.29(4) Uani 1 1 d D . . H15I H 0.1970 0.2325 0.2444 0.346 Uiso 1 1 calc R . . H15J H 0.1742 0.2706 0.2823 0.346 Uiso 1 1 calc R . . C156 C 0.0781(19) 0.2899(17) 0.2291(19) 0.23(3) Uani 1 1 d D . . H15K H 0.0470 0.3309 0.2292 0.274 Uiso 1 1 calc R . . H15L H 0.0707 0.2947 0.1879 0.274 Uiso 1 1 calc R . . C157 C 0.0358(17) 0.2429(16) 0.2728(14) 0.152(13) Uani 1 1 d D . . H15M H 0.0433 0.2383 0.3139 0.183 Uiso 1 1 calc R . . H15N H 0.0675 0.2019 0.2729 0.183 Uiso 1 1 calc R . . C158 C -0.0615(15) 0.255(2) 0.263(2) 0.23(3) Uani 1 1 d D . . H15O H -0.0566 0.2514 0.2246 0.273 Uiso 1 1 calc R . . H15P H -0.0784 0.3011 0.2496 0.273 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 I3 0.1246(15) 0.0903(13) 0.0729(11) -0.0409(10) -0.0300(10) 0.0200(10) O1 0.023(5) 0.020(5) 0.025(4) -0.007(4) -0.004(4) -0.003(4) O2 0.032(5) 0.020(5) 0.019(4) -0.005(3) 0.004(4) -0.010(4) O3 0.025(5) 0.028(5) 0.021(4) -0.007(4) -0.006(3) -0.010(4) O4 0.027(5) 0.030(5) 0.014(4) -0.004(3) 0.003(3) -0.008(4) O5 0.016(4) 0.023(4) 0.025(4) -0.011(3) 0.000(3) -0.005(3) O6 0.011(4) 0.027(5) 0.036(5) -0.012(4) -0.003(3) -0.017(3) O7 0.026(5) 0.034(5) 0.024(5) -0.009(4) 0.001(4) -0.009(4) O8 0.032(5) 0.025(5) 0.041(5) -0.007(4) -0.007(4) -0.009(4) O9 0.039(6) 0.044(6) 0.039(5) -0.025(5) 0.000(4) -0.020(5) O10 0.035(6) 0.036(5) 0.035(5) -0.021(4) 0.005(4) -0.010(4) O11 0.035(6) 0.038(6) 0.030(5) -0.009(4) 0.012(4) -0.015(4) O12 0.028(5) 0.035(5) 0.023(5) -0.010(4) -0.003(4) -0.009(4) O13 0.015(5) 0.050(6) 0.043(5) -0.025(5) 0.004(4) 0.002(4) O14 0.017(4) 0.024(5) 0.031(4) -0.014(4) 0.001(3) -0.007(3) O15 0.031(5) 0.031(5) 0.041(5) -0.013(4) -0.005(4) -0.007(4) O16 0.022(5) 0.038(6) 0.031(5) -0.011(4) 0.002(4) -0.008(4) O17 0.030(5) 0.034(5) 0.029(5) -0.020(4) 0.001(4) -0.011(4) O18 0.026(5) 0.035(5) 0.033(5) -0.021(4) -0.002(4) -0.006(4) O19 0.034(5) 0.020(5) 0.021(4) -0.008(4) 0.004(4) -0.008(4) O20 0.040(6) 0.019(5) 0.031(5) -0.009(4) 0.000(4) -0.006(4) C1 0.025(6) 0.016(6) 0.010(5) -0.004(4) -0.001(4) -0.004(5) C2 0.022(6) 0.014(6) 0.011(5) -0.005(4) -0.003(4) -0.002(5) C3 0.016(6) 0.019(6) 0.010(5) -0.006(4) 0.003(4) -0.004(4) C4 0.021(6) 0.021(6) 0.015(6) -0.008(5) -0.001(5) -0.004(5) C5 0.021(6) 0.017(6) 0.014(5) -0.006(4) 0.001(5) -0.005(5) C6 0.023(6) 0.017(6) 0.012(5) -0.005(4) -0.003(5) -0.003(5) C7 0.022(6) 0.021(6) 0.013(5) -0.005(5) -0.002(5) -0.001(5) C8 0.024(6) 0.013(6) 0.012(5) -0.001(4) -0.002(4) -0.003(5) C9 0.020(6) 0.016(6) 0.018(6) -0.003(5) 0.003(5) -0.009(5) C10 0.020(6) 0.019(6) 0.021(6) -0.008(5) 0.002(5) -0.008(5) C11 0.027(7) 0.018(6) 0.020(6) -0.009(5) -0.003(5) -0.007(5) C12 0.017(6) 0.020(6) 0.022(6) -0.007(5) -0.002(5) 0.000(5) C13 0.019(6) 0.020(6) 0.021(6) -0.008(5) -0.002(5) -0.004(5) C14 0.030(7) 0.013(6) 0.019(6) -0.006(5) -0.001(5) -0.001(5) C15 0.012(6) 0.016(6) 0.021(6) -0.007(5) 0.003(4) -0.007(4) C16 0.026(7) 0.017(6) 0.019(6) -0.008(5) 0.003(5) -0.006(5) C17 0.017(6) 0.019(6) 0.026(6) -0.009(5) -0.006(5) -0.001(5) C18 0.016(6) 0.019(6) 0.018(6) -0.008(5) -0.002(4) -0.006(5) C19 0.019(6) 0.014(6) 0.019(6) -0.006(4) -0.003(5) -0.003(4) C20 0.014(6) 0.021(6) 0.015(5) -0.007(5) 0.002(4) -0.005(5) C21 0.027(7) 0.018(6) 0.020(6) -0.008(5) -0.001(5) -0.003(5) C22 0.018(6) 0.019(6) 0.010(5) -0.006(4) -0.006(4) 0.001(5) C23 0.015(6) 0.017(6) 0.010(5) -0.003(4) 0.001(4) -0.003(4) C24 0.021(6) 0.011(5) 0.011(5) -0.001(4) -0.004(4) -0.003(4) C25 0.020(6) 0.013(6) 0.009(5) 0.000(4) -0.003(4) -0.001(4) C26 0.000(5) 0.027(6) 0.021(6) -0.010(5) 0.003(4) -0.006(4) C27 0.023(7) 0.019(6) 0.016(6) -0.004(5) -0.003(5) -0.006(5) C28 0.019(6) 0.018(6) 0.013(5) -0.004(4) -0.002(4) -0.004(5) C29 0.016(6) 0.012(5) 0.012(5) -0.004(4) -0.006(4) 0.000(4) C30 0.018(6) 0.022(6) 0.017(6) -0.008(5) -0.004(5) -0.002(5) C31 0.023(6) 0.015(6) 0.012(5) -0.006(4) 0.002(4) -0.003(5) C32 0.013(6) 0.014(5) 0.011(5) -0.005(4) 0.003(4) -0.003(4) C33 0.018(6) 0.015(6) 0.013(5) -0.005(4) -0.005(4) -0.003(4) C34 0.017(6) 0.010(5) 0.010(5) -0.003(4) 0.001(4) -0.005(4) C35 0.022(6) 0.016(6) 0.010(5) -0.006(4) -0.002(4) -0.002(5) C36 0.024(7) 0.027(7) 0.034(7) -0.010(6) -0.005(6) -0.005(6) C37 0.029(8) 0.032(8) 0.030(7) -0.009(6) 0.001(6) -0.006(6) C38 0.040(9) 0.033(9) 0.059(10) -0.012(7) 0.001(8) -0.008(7) C39 0.059(13) 0.066(14) 0.078(14) -0.024(11) 0.005(11) -0.013(11) C40 0.030(7) 0.024(7) 0.017(6) -0.007(5) 0.001(5) -0.006(5) C41 0.032(7) 0.021(7) 0.028(7) -0.009(5) -0.005(5) -0.001(5) C42 0.038(9) 0.029(8) 0.036(8) -0.008(6) -0.004(6) -0.008(6) C43 0.059(12) 0.046(11) 0.080(13) -0.026(10) -0.006(10) -0.011(9) C44 0.021(6) 0.022(6) 0.021(6) -0.010(5) 0.003(5) -0.008(5) C45 0.027(7) 0.024(6) 0.021(6) -0.008(5) 0.001(5) -0.009(5) C46 0.027(7) 0.036(8) 0.031(7) -0.016(6) 0.005(6) -0.009(6) C47 0.042(9) 0.047(10) 0.045(9) -0.016(7) 0.002(7) -0.020(7) C48 0.029(8) 0.042(9) 0.038(8) -0.019(7) 0.003(6) -0.009(7) C49 0.053(11) 0.054(11) 0.049(10) -0.012(8) 0.005(8) -0.018(9) C50 0.15(4) 0.20(4) 0.10(3) -0.06(3) -0.01(3) -0.05(3) C51 0.28(7) 0.31(7) 0.18(5) -0.17(5) 0.07(5) -0.03(6) C52 0.025(7) 0.020(6) 0.014(6) -0.003(5) -0.003(5) -0.005(5) C53 0.029(8) 0.031(7) 0.024(7) -0.008(5) -0.001(5) -0.006(6) C54 0.039(9) 0.044(9) 0.047(9) -0.017(7) -0.003(7) -0.016(7) C55 0.058(15) 0.108(19) 0.092(16) -0.052(14) 0.008(12) -0.020(13) C56 0.028(8) 0.036(8) 0.033(7) -0.015(6) 0.009(6) -0.009(6) C57 0.030(9) 0.065(11) 0.058(10) -0.034(8) 0.007(7) -0.021(8) C58 0.16(3) 0.13(3) 0.11(2) -0.06(2) 0.04(2) -0.04(2) C59 0.10(3) 0.17(3) 0.15(3) -0.09(3) 0.00(2) -0.02(2) C60 0.044(10) 0.033(9) 0.043(9) 0.000(7) -0.001(7) -0.010(7) C61 0.035(9) 0.052(10) 0.050(9) -0.016(8) 0.004(7) -0.018(7) C62 0.042(11) 0.059(11) 0.067(11) -0.028(9) 0.002(9) -0.013(9) C63 0.061(14) 0.070(16) 0.091(16) -0.016(13) -0.011(12) -0.011(12) C64 0.043(11) 0.047(11) 0.071(12) -0.014(9) -0.010(9) -0.015(9) C65 0.069(15) 0.085(18) 0.101(17) -0.037(14) -0.012(13) -0.023(13) C66 0.07(2) 0.13(3) 0.24(4) -0.11(3) 0.02(2) -0.028(19) C67 0.068(17) 0.099(19) 0.086(17) -0.016(14) -0.003(13) -0.029(14) C68 0.063(14) 0.075(14) 0.063(12) -0.031(10) -0.006(10) -0.010(10) C69 0.18(4) 0.40(7) 0.19(4) -0.22(5) 0.07(3) -0.16(5) C70 0.13(3) 0.15(4) 0.22(4) -0.10(3) -0.11(3) 0.02(3) C71 0.16(4) 0.16(4) 0.25(5) -0.09(4) -0.06(4) -0.04(3) C72 0.022(7) 0.030(7) 0.027(6) -0.012(5) 0.006(5) -0.013(5) C73 0.036(9) 0.044(10) 0.077(11) -0.037(9) -0.005(8) -0.004(7) C74 0.041(10) 0.048(11) 0.067(11) -0.015(9) -0.001(8) -0.014(8) C75 0.07(2) 0.19(3) 0.25(4) -0.16(3) 0.01(2) -0.03(2) C76 0.027(7) 0.020(6) 0.023(6) -0.008(5) 0.005(5) -0.003(5) C77 0.024(7) 0.026(7) 0.030(7) -0.015(6) 0.001(5) -0.005(5) C78 0.023(6) 0.016(6) 0.019(6) -0.007(5) -0.005(5) 0.002(5) C79 0.024(6) 0.011(6) 0.014(6) -0.003(4) 0.003(5) -0.004(5) C80 0.023(6) 0.022(6) 0.021(6) -0.011(5) -0.003(5) -0.003(5) C81 0.022(6) 0.015(6) 0.013(6) -0.005(5) 0.003(5) -0.002(5) C82 0.028(7) 0.018(6) 0.025(6) -0.005(5) -0.005(5) -0.003(5) C83 0.028(7) 0.018(6) 0.014(6) -0.002(5) -0.007(5) -0.002(5) C84 0.007(5) 0.013(5) 0.012(5) -0.002(4) 0.001(4) -0.005(4) C85 0.026(7) 0.026(7) 0.020(6) -0.009(5) -0.007(5) -0.006(5) C86 0.021(6) 0.023(6) 0.016(6) -0.006(5) -0.005(5) -0.006(5) C87 0.024(7) 0.020(6) 0.015(6) -0.005(5) -0.004(5) -0.003(5) C88 0.021(7) 0.023(6) 0.017(6) -0.007(5) -0.005(5) -0.004(5) C89 0.033(7) 0.020(6) 0.016(6) -0.006(5) -0.001(5) -0.005(5) C90 0.016(6) 0.016(6) 0.016(5) -0.006(4) -0.001(4) -0.005(4) C91 0.021(6) 0.015(6) 0.022(6) -0.005(5) 0.000(5) -0.006(5) C92 0.026(7) 0.024(7) 0.023(6) -0.011(5) 0.005(5) -0.007(5) C93 0.020(6) 0.016(6) 0.018(6) -0.007(5) 0.003(5) -0.004(5) C94 0.017(6) 0.021(6) 0.018(6) -0.008(5) 0.000(5) -0.006(5) C95 0.022(6) 0.022(6) 0.018(6) -0.009(5) 0.001(5) -0.010(5) C96 0.031(7) 0.016(6) 0.021(6) -0.008(5) -0.004(5) 0.003(5) C97 0.024(6) 0.016(6) 0.014(6) -0.004(5) -0.003(5) -0.003(5) C98 0.032(7) 0.024(7) 0.017(6) -0.010(5) 0.002(5) -0.007(5) C99 0.031(7) 0.022(6) 0.019(6) -0.012(5) -0.005(5) -0.004(5) C100 0.025(7) 0.015(6) 0.020(6) -0.006(5) -0.004(5) -0.002(5) C101 0.022(7) 0.026(7) 0.024(6) -0.013(5) 0.000(5) -0.001(5) C102 0.029(7) 0.016(6) 0.021(6) -0.008(5) -0.004(5) 0.000(5) C103 0.030(7) 0.020(6) 0.013(6) -0.006(5) -0.005(5) -0.001(5) C104 0.021(6) 0.021(6) 0.019(6) -0.010(5) -0.003(5) -0.002(5) C105 0.027(7) 0.018(6) 0.012(5) -0.005(4) -0.002(5) -0.003(5) C106 0.025(7) 0.024(7) 0.017(6) -0.009(5) -0.002(5) -0.003(5) C107 0.035(8) 0.027(7) 0.019(6) -0.013(5) 0.001(5) -0.002(6) C108 0.030(7) 0.018(6) 0.017(6) -0.006(5) -0.005(5) -0.003(5) C109 0.029(7) 0.020(6) 0.015(6) -0.006(5) -0.004(5) -0.003(5) C110 0.027(7) 0.024(6) 0.014(6) -0.007(5) 0.003(5) -0.007(5) C111 0.066(15) 0.076(15) 0.075(14) -0.036(12) 0.018(11) -0.019(11) C112 0.12(3) 0.11(3) 0.18(4) -0.03(3) 0.04(3) -0.05(2) C113 0.39(13) 0.57(16) 0.16(6) -0.05(8) 0.19(7) -0.10(11) C114 0.22(6) 0.42(10) 0.20(6) -0.10(6) 0.07(5) 0.01(7) C115 0.018(6) 0.023(6) 0.020(6) -0.008(5) 0.002(5) -0.010(5) C116 0.029(7) 0.029(7) 0.025(7) -0.011(5) 0.002(5) -0.008(6) C117 0.029(8) 0.037(8) 0.034(7) -0.019(6) 0.004(6) -0.011(6) C118 0.047(10) 0.062(11) 0.055(10) -0.022(8) 0.008(8) -0.032(9) C119 0.115(19) 0.069(14) 0.050(12) -0.023(10) 0.003(12) -0.047(13) C120 0.033(10) 0.069(12) 0.066(11) -0.041(9) 0.012(8) -0.019(8) C121 0.11(3) 0.29(6) 0.28(5) -0.19(5) 0.02(3) -0.06(4) C122 0.20(6) 0.46(9) 0.32(7) -0.28(7) 0.11(5) -0.16(7) C123 0.028(7) 0.022(7) 0.025(6) -0.006(5) -0.010(5) -0.003(5) C124 0.036(8) 0.033(8) 0.027(7) -0.012(6) 0.000(6) -0.005(6) C125 0.042(10) 0.056(11) 0.054(10) -0.023(8) 0.003(8) -0.015(8) C126 0.085(19) 0.13(2) 0.12(2) -0.078(19) 0.028(16) -0.037(17) C127 0.045(10) 0.046(10) 0.057(10) -0.014(8) -0.010(8) -0.015(8) C128 0.075(16) 0.070(16) 0.090(16) 0.000(12) -0.029(13) -0.029(13) C129 0.12(4) 0.10(3) 0.38(7) -0.07(4) -0.04(4) 0.04(3) C130 0.054(14) 0.080(16) 0.080(15) -0.023(12) -0.004(11) -0.022(11) C131 0.041(10) 0.040(9) 0.048(10) -0.006(7) -0.005(8) -0.010(7) C132 0.054(11) 0.051(11) 0.059(11) -0.014(9) -0.007(9) -0.020(9) C133 0.041(10) 0.053(11) 0.058(11) -0.023(9) -0.004(8) -0.007(8) C134 0.065(15) 0.084(17) 0.081(16) -0.024(13) -0.014(12) -0.013(12) C135 0.024(7) 0.028(7) 0.026(6) -0.012(5) 0.002(5) -0.008(5) C136 0.032(8) 0.033(8) 0.044(8) -0.022(6) -0.001(6) -0.004(6) C137 0.055(12) 0.054(12) 0.060(11) -0.021(9) -0.003(9) -0.019(9) C138 0.053(13) 0.084(15) 0.106(15) -0.056(12) 0.003(11) -0.027(11) C139 0.049(12) 0.101(16) 0.067(13) -0.049(12) 0.001(10) -0.014(11) C140 0.063(16) 0.13(2) 0.099(18) -0.077(17) 0.003(13) -0.018(14) C141 0.28(9) 0.20(7) 0.51(13) -0.10(8) -0.21(8) -0.11(7) C142 0.16(4) 0.13(4) 0.33(6) -0.10(4) -0.07(4) -0.02(3) C143 0.028(7) 0.026(7) 0.023(6) -0.010(5) 0.001(5) -0.005(5) C144 0.022(7) 0.025(7) 0.025(6) -0.008(5) -0.002(5) -0.006(5) C145 0.042(9) 0.039(9) 0.036(8) -0.010(7) -0.008(7) -0.006(7) C146 0.049(12) 0.057(12) 0.065(12) -0.022(10) -0.009(9) -0.006(9) C147 0.037(8) 0.030(8) 0.038(8) -0.014(6) -0.007(6) -0.004(6) C148 0.037(8) 0.037(8) 0.028(7) -0.013(6) 0.005(6) -0.006(6) C149 0.047(11) 0.050(11) 0.063(11) -0.021(9) -0.005(8) -0.004(8) C150 0.048(12) 0.061(13) 0.077(13) -0.016(10) 0.010(10) -0.015(10) I1 0.0613(9) 0.0642(9) 0.0532(8) -0.0236(6) -0.0070(6) -0.0078(6) I2 0.0674(9) 0.0521(8) 0.0529(8) -0.0196(6) -0.0037(6) -0.0128(6) C151 0.50(16) 0.20(7) 0.31(10) 0.00(6) -0.27(11) -0.06(8) C152 0.048(10) 0.045(9) 0.039(9) -0.016(7) 0.002(7) -0.009(8) C153 0.18(4) 0.14(3) 0.10(2) -0.07(2) 0.01(2) -0.06(3) C154 0.19(7) 0.34(9) 0.29(8) -0.17(7) 0.04(6) -0.11(7) I4 0.188(2) 0.0684(12) 0.0781(12) -0.0277(10) -0.0288(12) -0.0192(12) C155 0.56(13) 0.12(4) 0.15(5) -0.05(4) -0.17(7) 0.03(6) C156 0.29(7) 0.21(6) 0.15(5) -0.11(4) -0.08(4) 0.09(5) C157 0.20(4) 0.18(3) 0.09(2) -0.05(2) 0.01(2) -0.08(3) C158 0.09(3) 0.31(6) 0.23(5) -0.10(5) 0.00(3) 0.00(4) _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 I3 C155 1.926(17) . ? O1 C1 1.382(14) . ? O1 C36 1.426(15) . ? O2 C4 1.361(14) . ? O2 C40 1.411(15) . ? O3 C34 1.357(13) . ? O3 C44 1.454(14) . ? O4 C31 1.374(14) . ? O4 C48 1.399(17) . ? O5 C23 1.382(14) . ? O5 C52 1.449(14) . ? O6 C26 1.369(14) . ? O6 C56 1.517(16) . ? O7 C20 1.363(14) . ? O7 C60 1.470(17) . ? O8 C17 1.357(15) . ? O8 C64 1.46(2) . ? O9 C13 1.379(15) . ? O9 C68 1.45(2) . ? O10 C10 1.376(15) . ? O10 C72 1.467(15) . ? O11 C111 1.34(2) . ? O11 C76 1.400(15) . ? O12 C79 1.346(14) . ? O12 C115 1.440(14) . ? O13 C84 1.387(14) . ? O13 C119 1.42(2) . ? O14 C87 1.370(15) . ? O14 C123 1.468(15) . ? O15 C127 1.401(19) . ? O15 C91 1.378(15) . ? O16 C94 1.361(15) . ? O16 C131 1.407(18) . ? O17 C98 1.386(15) . ? O17 C135 1.415(15) . ? O18 C101 1.394(15) . ? O18 C139 1.45(2) . ? O19 C105 1.389(14) . ? O19 C143 1.390(16) . ? O20 C108 1.378(15) . ? O20 C147 1.394(17) . ? C1 C6 1.398(16) . ? C1 C2 1.405(16) . ? C2 C3 1.380(16) . ? C2 C35 1.528(15) . ? C3 C4 1.378(16) . ? C3 H3A 0.9500 . ? C4 C5 1.441(16) . ? C5 C6 1.409(16) . ? C5 C7 1.474(16) . ? C6 H6A 0.9500 . ? C7 C8 1.514(15) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.393(16) . ? C8 C9 1.407(17) . ? C9 C10 1.382(16) . ? C9 H9A 0.9500 . ? C10 C11 1.402(17) . ? C11 C12 1.367(17) . ? C11 C14 1.520(16) . ? C12 C13 1.376(17) . ? C12 H12A 0.9500 . ? C14 C15 1.523(15) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.344(16) . ? C15 C20 1.412(16) . ? C16 C17 1.413(16) . ? C16 H16A 0.9500 . ? C17 C18 1.426(16) . ? C18 C19 1.388(16) . ? C18 C21 1.506(15) . ? C19 C20 1.399(15) . ? C19 H19A 0.9500 . ? C21 C22 1.540(15) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.354(16) . ? C22 C27 1.394(17) . ? C23 C24 1.388(15) . ? C24 C25 1.390(16) . ? C24 H24A 0.9500 . ? C25 C26 1.346(16) . ? C25 C28 1.522(15) . ? C26 C27 1.362(16) . ? C27 H27A 0.9500 . ? C28 C29 1.509(14) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.373(16) . ? C29 C34 1.427(15) . ? C30 C31 1.407(15) . ? C30 H30A 0.9500 . ? C31 C32 1.386(16) . ? C32 C33 1.402(15) . ? C32 C35 1.512(14) . ? C33 C34 1.408(14) . ? C33 H33A 0.9500 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.522(18) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.47(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.51(3) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.489(17) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.543(19) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.53(2) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.489(16) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.529(18) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.526(19) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.460(15) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.414(18) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.416(19) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.497(17) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.52(2) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.50(3) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.46(2) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.426(18) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.441(18) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.51(2) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.53(2) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.53(3) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.50(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.34(4) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.67(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C69 1.51(4) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.71(6) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 C71 1.65(5) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.47(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.49(2) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.53(3) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C77 1.374(17) . ? C76 C81 1.374(17) . ? C77 C78 1.405(17) . ? C77 H77A 0.9500 . ? C78 C79 1.427(17) . ? C78 C82 1.517(16) . ? C79 C80 1.396(15) . ? C80 C81 1.393(16) . ? C80 H80A 0.9500 . ? C81 C110 1.534(15) . ? C82 C83 1.512(17) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C88 1.351(18) . ? C83 C84 1.369(16) . ? C84 C85 1.445(16) . ? C85 C86 1.410(18) . ? C85 H85A 0.9500 . ? C86 C87 1.390(17) . ? C86 C89 1.482(17) . ? C87 C88 1.387(17) . ? C88 H88A 0.9500 . ? C89 C90 1.495(15) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 C91 1.429(16) . ? C90 C95 1.436(16) . ? C91 C92 1.372(16) . ? C92 C93 1.345(17) . ? C92 H92A 0.9500 . ? C93 C94 1.433(16) . ? C93 C96 1.536(15) . ? C94 C95 1.397(16) . ? C95 H95A 0.9500 . ? C96 C97 1.548(16) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C98 1.355(17) . ? C97 C102 1.393(17) . ? C98 C99 1.416(16) . ? C99 C100 1.423(17) . ? C99 H99A 0.9500 . ? C100 C101 1.383(17) . ? C100 C103 1.520(16) . ? C101 C102 1.367(17) . ? C102 H10A 0.9500 . ? C103 C104 1.518(16) . ? C103 H10B 0.9900 . ? C103 H10C 0.9900 . ? C104 C109 1.374(17) . ? C104 C105 1.425(17) . ? C105 C106 1.360(17) . ? C106 C107 1.378(18) . ? C106 H10D 0.9500 . ? C107 C108 1.383(18) . ? C107 C110 1.512(17) . ? C108 C109 1.426(16) . ? C109 H10E 0.9500 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.60(4) . ? C111 H11C 0.9900 . ? C111 H11D 0.9900 . ? C112 C113 1.00(7) . ? C112 H11E 0.9900 . ? C112 H11T 0.9900 . ? C113 C114 1.47(2) . ? C113 H11U 0.9900 . ? C113 H11V 0.9900 . ? C114 H11F 0.9800 . ? C114 H11G 0.9800 . ? C114 H11H 0.9800 . ? C115 C116 1.523(16) . ? C115 H11I 0.9900 . ? C115 H11J 0.9900 . ? C116 C117 1.522(19) . ? C116 H11K 0.9900 . ? C116 H11L 0.9900 . ? C117 C118 1.54(2) . ? C117 H11M 0.9900 . ? C117 H11N 0.9900 . ? C118 H11O 0.9800 . ? C118 H11P 0.9800 . ? C118 H11Q 0.9800 . ? C119 C120 1.37(3) . ? C119 H11R 0.9900 . ? C119 H11S 0.9900 . ? C120 C121 1.438(19) . ? C120 H12B 0.9900 . ? C120 H12S 0.9900 . ? C121 C122 1.450(19) . ? C121 H12C 0.9900 . ? C121 H12D 0.9900 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? C122 H12G 0.9800 . ? C123 C124 1.509(19) . ? C123 H12H 0.9900 . ? C123 H12I 0.9900 . ? C124 C125 1.49(2) . ? C124 H12J 0.9900 . ? C124 H12K 0.9900 . ? C125 C126 1.57(3) . ? C125 H12L 0.9900 . ? C125 H12M 0.9900 . ? C126 H12N 0.9800 . ? C126 H12O 0.9800 . ? C126 H12P 0.9800 . ? C127 C128 1.48(3) . ? C127 H12Q 0.9900 . ? C127 H12R 0.9900 . ? C128 C129 1.31(4) . ? C128 H12V 0.9900 . ? C128 H12W 0.9900 . ? C129 C130 1.51(5) . ? C129 H12T 0.9900 . ? C129 H12U 0.9900 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? C131 C132 1.53(2) . ? C131 H13D 0.9900 . ? C131 H13E 0.9900 . ? C132 C133 1.48(2) . ? C132 H13F 0.9900 . ? C132 H13G 0.9900 . ? C133 C134 1.54(3) . ? C133 H13H 0.9900 . ? C133 H13I 0.9900 . ? C134 H13J 0.9800 . ? C134 H13K 0.9800 . ? C134 H13L 0.9800 . ? C135 C136 1.535(18) . ? C135 H13M 0.9900 . ? C135 H13N 0.9900 . ? C136 C137 1.50(2) . ? C136 H13O 0.9900 . ? C136 H13P 0.9900 . ? C137 C138 1.53(3) . ? C137 H13Q 0.9900 . ? C137 H13R 0.9900 . ? C138 H13S 0.9800 . ? C138 H13T 0.9800 . ? C138 H13U 0.9800 . ? C139 C140 1.56(3) . ? C139 H13V 0.9900 . ? C139 H13W 0.9900 . ? C140 C141 1.37(6) . ? C140 H14C 0.9900 . ? C140 H14D 0.9900 . ? C141 C142 1.72(6) . ? C141 H14E 0.9900 . ? C141 H14F 0.9900 . ? C142 H14G 0.9800 . ? C142 H14H 0.9800 . ? C142 H14I 0.9800 . ? C143 C144 1.513(17) . ? C143 H14J 0.9900 . ? C143 H14K 0.9900 . ? C144 C145 1.539(19) . ? C144 H14L 0.9900 . ? C144 H14M 0.9900 . ? C145 C146 1.45(2) . ? C145 H14N 0.9900 . ? C145 H14X 0.9900 . ? C146 H14O 0.9800 . ? C146 H14P 0.9800 . ? C146 H14Q 0.9800 . ? C147 C148 1.520(19) . ? C147 H14R 0.9900 . ? C147 H14S 0.9900 . ? C148 C149 1.46(2) . ? C148 H14T 0.9900 . ? C148 H14U 0.9900 . ? C149 C150 1.58(3) . ? C149 H14V 0.9900 . ? C149 H14W 0.9900 . ? C150 H15Q 0.9800 . ? C150 H15R 0.9800 . ? C150 H15S 0.9800 . ? I1 C151 1.944(18) . ? I2 C154 1.980(17) . ? C151 C152 1.461(18) . ? C151 H15A 0.9900 . ? C151 H15B 0.9900 . ? C152 C153 1.388(17) . ? C152 H15C 0.9900 . ? C152 H15D 0.9900 . ? C153 C154 1.469(19) . ? C153 H15E 0.9900 . ? C153 H15F 0.9900 . ? C154 H15G 0.9900 . ? C154 H15H 0.9900 . ? I4 C158 1.939(17) . ? C155 C156 1.465(19) . ? C155 H15I 0.9900 . ? C155 H15J 0.9900 . ? C156 C157 1.381(19) . ? C156 H15K 0.9900 . ? C156 H15L 0.9900 . ? C157 C158 1.454(18) . ? C157 H15M 0.9900 . ? C157 H15N 0.9900 . ? C158 H15O 0.9900 . ? C158 H15P 0.9900 . ? 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 C1 O1 C36 116.5(9) . . ? C4 O2 C40 116.4(9) . . ? C34 O3 C44 116.9(8) . . ? C31 O4 C48 118.9(9) . . ? C23 O5 C52 117.2(9) . . ? C26 O6 C56 122.4(9) . . ? C20 O7 C60 118.0(10) . . ? C17 O8 C64 117.3(11) . . ? C13 O9 C68 118.7(11) . . ? C10 O10 C72 119.6(9) . . ? C111 O11 C76 118.3(12) . . ? C79 O12 C115 117.1(9) . . ? C84 O13 C119 127.7(13) . . ? C87 O14 C123 115.9(9) . . ? C127 O15 C91 115.6(11) . . ? C94 O16 C131 119.1(10) . . ? C98 O17 C135 118.7(9) . . ? C101 O18 C139 115.0(11) . . ? C105 O19 C143 115.1(9) . . ? C108 O20 C147 118.5(10) . . ? C6 C1 O1 124.1(10) . . ? C6 C1 C2 120.5(10) . . ? O1 C1 C2 115.4(10) . . ? C3 C2 C1 118.2(10) . . ? C3 C2 C35 120.9(10) . . ? C1 C2 C35 120.9(10) . . ? C4 C3 C2 122.7(11) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.5 . . ? O2 C4 C3 125.2(11) . . ? O2 C4 C5 114.4(10) . . ? C3 C4 C5 120.4(10) . . ? C6 C5 C4 116.4(10) . . ? C6 C5 C7 122.2(11) . . ? C4 C5 C7 121.2(10) . . ? C1 C6 C5 121.8(11) . . ? C1 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C5 C7 C8 109.8(9) . . ? C5 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? C5 C7 H7B 109.7 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? C13 C8 C9 117.6(10) . . ? C13 C8 C7 123.0(11) . . ? C9 C8 C7 119.4(10) . . ? C10 C9 C8 120.7(11) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.7 . . ? C9 C10 O10 124.0(10) . . ? C9 C10 C11 121.1(11) . . ? O10 C10 C11 114.9(10) . . ? C12 C11 C10 117.3(11) . . ? C12 C11 C14 122.2(11) . . ? C10 C11 C14 120.4(11) . . ? C11 C12 C13 122.8(11) . . ? C11 C12 H12A 118.5 . . ? C13 C12 H12A 118.7 . . ? O9 C13 C12 124.7(11) . . ? O9 C13 C8 114.8(10) . . ? C12 C13 C8 120.5(11) . . ? C11 C14 C15 112.2(10) . . ? C11 C14 H14A 109.3 . . ? C15 C14 H14A 109.0 . . ? C11 C14 H14B 109.0 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C20 118.0(10) . . ? C16 C15 C14 123.2(10) . . ? C20 C15 C14 118.7(10) . . ? C15 C16 C17 123.8(11) . . ? C15 C16 H16A 118.1 . . ? C17 C16 H16A 118.1 . . ? O8 C17 C16 124.8(11) . . ? O8 C17 C18 117.0(10) . . ? C16 C17 C18 118.2(11) . . ? C19 C18 C17 118.1(10) . . ? C19 C18 C21 121.6(10) . . ? C17 C18 C21 120.3(10) . . ? C18 C19 C20 121.7(10) . . ? C18 C19 H19A 119.3 . . ? C20 C19 H19A 119.0 . . ? O7 C20 C19 123.9(10) . . ? O7 C20 C15 115.9(10) . . ? C19 C20 C15 120.1(11) . . ? C18 C21 C22 111.6(9) . . ? C18 C21 H21A 109.5 . . ? C22 C21 H21A 109.8 . . ? C18 C21 H21B 109.0 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C27 118.7(10) . . ? C23 C22 C21 122.0(10) . . ? C27 C22 C21 119.0(10) . . ? C22 C23 C24 119.9(10) . . ? C22 C23 O5 115.6(10) . . ? C24 C23 O5 124.4(10) . . ? C23 C24 C25 122.8(10) . . ? C23 C24 H24A 118.5 . . ? C25 C24 H24A 118.7 . . ? C26 C25 C24 114.0(10) . . ? C26 C25 C28 125.5(10) . . ? C24 C25 C28 120.4(10) . . ? C27 C26 C25 126.0(11) . . ? C27 C26 O6 120.8(10) . . ? C25 C26 O6 113.1(10) . . ? C26 C27 C22 118.3(11) . . ? C26 C27 H27A 121.1 . . ? C22 C27 H27A 120.7 . . ? C29 C28 C25 109.9(9) . . ? C29 C28 H28A 109.7 . . ? C25 C28 H28A 109.8 . . ? C29 C28 H28B 109.6 . . ? C25 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C34 119.1(9) . . ? C30 C29 C28 121.0(10) . . ? C34 C29 C28 119.9(10) . . ? C29 C30 C31 122.1(11) . . ? C29 C30 H30A 118.9 . . ? C31 C30 H30A 119.0 . . ? O4 C31 C30 124.8(10) . . ? O4 C31 C32 115.4(9) . . ? C30 C31 C32 119.9(10) . . ? C33 C32 C31 118.8(9) . . ? C33 C32 C35 119.3(10) . . ? C31 C32 C35 121.9(10) . . ? C32 C33 C34 122.0(10) . . ? C32 C33 H33A 119.0 . . ? C34 C33 H33A 119.1 . . ? O3 C34 C33 126.5(10) . . ? O3 C34 C29 115.2(9) . . ? C33 C34 C29 118.3(10) . . ? C32 C35 C2 112.8(9) . . ? C32 C35 H35A 109.1 . . ? C2 C35 H35A 109.1 . . ? C32 C35 H35B 108.9 . . ? C2 C35 H35B 108.9 . . ? H35A C35 H35B 107.8 . . ? O1 C36 C37 108.8(10) . . ? O1 C36 H36A 109.8 . . ? C37 C36 H36A 109.9 . . ? O1 C36 H36B 109.9 . . ? C37 C36 H36B 110.0 . . ? H36A C36 H36B 108.3 . . ? C38 C37 C36 113.7(12) . . ? C38 C37 H37A 108.9 . . ? C36 C37 H37A 109.0 . . ? C38 C37 H37B 108.6 . . ? C36 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C37 C38 C39 112.3(14) . . ? C37 C38 H38A 108.9 . . ? C39 C38 H38A 108.9 . . ? C37 C38 H38B 109.3 . . ? C39 C38 H38B 109.4 . . ? H38A C38 H38B 107.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.2 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.7 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O2 C40 C41 110.6(10) . . ? O2 C40 H40A 109.5 . . ? C41 C40 H40A 109.5 . . ? O2 C40 H40B 109.5 . . ? C41 C40 H40B 109.6 . . ? H40A C40 H40B 108.0 . . ? C40 C41 C42 112.9(11) . . ? C40 C41 H41A 109.0 . . ? C42 C41 H41A 109.0 . . ? C40 C41 H41B 109.1 . . ? C42 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C43 C42 C41 114.5(13) . . ? C43 C42 H42A 108.5 . . ? C41 C42 H42A 108.6 . . ? C43 C42 H42B 108.8 . . ? C41 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 H43A 109.4 . . ? C42 C43 H43B 109.6 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.4 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O3 C44 C45 107.5(9) . . ? O3 C44 H44A 110.2 . . ? C45 C44 H44A 110.4 . . ? O3 C44 H44B 110.1 . . ? C45 C44 H44B 110.1 . . ? H44A C44 H44B 108.5 . . ? C44 C45 C46 111.1(10) . . ? C44 C45 H45A 109.6 . . ? C46 C45 H45A 109.4 . . ? C44 C45 H45B 109.3 . . ? C46 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? C45 C46 C47 113.1(11) . . ? C45 C46 H46A 109.0 . . ? C47 C46 H46A 108.9 . . ? C45 C46 H46B 108.9 . . ? C47 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? C46 C47 H47A 109.7 . . ? C46 C47 H47B 109.3 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.4 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O4 C48 C49 112.8(12) . . ? O4 C48 H48A 109.1 . . ? C49 C48 H48A 109.3 . . ? O4 C48 H48B 109.1 . . ? C49 C48 H48B 108.7 . . ? H48A C48 H48B 107.8 . . ? C50 C49 C48 108.8(16) . . ? C50 C49 H49A 109.7 . . ? C48 C49 H49A 110.3 . . ? C50 C49 H49B 109.8 . . ? C48 C49 H49B 109.9 . . ? H49A C49 H49B 108.4 . . ? C51 C50 C49 109.5(19) . . ? C51 C50 H50A 108.3 . . ? C49 C50 H50A 109.4 . . ? C51 C50 H50B 111.1 . . ? C49 C50 H50B 110.2 . . ? H50A C50 H50B 108.2 . . ? C50 C51 H51A 109.6 . . ? C50 C51 H51B 110.8 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 108.0 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O5 C52 C53 108.2(10) . . ? O5 C52 H52A 110.2 . . ? C53 C52 H52A 110.1 . . ? O5 C52 H52B 109.9 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? C52 C53 C54 112.9(12) . . ? C52 C53 H53A 109.0 . . ? C54 C53 H53A 108.8 . . ? C52 C53 H53B 109.1 . . ? C54 C53 H53B 109.1 . . ? H53A C53 H53B 107.7 . . ? C55 C54 C53 110.7(15) . . ? C55 C54 H54A 109.6 . . ? C53 C54 H54A 109.6 . . ? C55 C54 H54B 109.7 . . ? C53 C54 H54B 109.3 . . ? H54A C54 H54B 108.0 . . ? C54 C55 H55A 108.9 . . ? C54 C55 H55B 109.8 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.7 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 O6 109.4(12) . . ? C57 C56 H56A 109.3 . . ? O6 C56 H56A 110.0 . . ? C57 C56 H56B 110.1 . . ? O6 C56 H56B 109.7 . . ? H56A C56 H56B 108.3 . . ? C58 C57 C56 119.5(18) . . ? C58 C57 H57A 107.1 . . ? C56 C57 H57A 107.2 . . ? C58 C57 H57B 108.0 . . ? C56 C57 H57B 107.7 . . ? H57A C57 H57B 106.8 . . ? C57 C58 C59 113(2) . . ? C57 C58 H58A 108.3 . . ? C59 C58 H58A 108.4 . . ? C57 C58 H58B 109.8 . . ? C59 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? C58 C59 H59A 110.1 . . ? C58 C59 H59B 108.9 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.4 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O7 C60 C61 108.0(12) . . ? O7 C60 H60A 109.8 . . ? C61 C60 H60A 109.8 . . ? O7 C60 H60B 110.4 . . ? C61 C60 H60B 110.4 . . ? H60A C60 H60B 108.4 . . ? C60 C61 C62 110.3(14) . . ? C60 C61 H61A 109.4 . . ? C62 C61 H61A 110.1 . . ? C60 C61 H61B 109.5 . . ? C62 C61 H61B 109.3 . . ? H61A C61 H61B 108.2 . . ? C63 C62 C61 110.2(16) . . ? C63 C62 H62A 109.5 . . ? C61 C62 H62A 109.3 . . ? C63 C62 H62B 109.6 . . ? C61 C62 H62B 110.0 . . ? H62A C62 H62B 108.1 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.4 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O8 C64 C65 108.0(15) . . ? O8 C64 H64A 110.1 . . ? C65 C64 H64A 110.4 . . ? O8 C64 H64B 110.0 . . ? C65 C64 H64B 109.9 . . ? H64A C64 H64B 108.4 . . ? C66 C65 C64 112(2) . . ? C66 C65 H65A 109.5 . . ? C64 C65 H65A 109.7 . . ? C66 C65 H65B 108.3 . . ? C64 C65 H65B 109.4 . . ? H65A C65 H65B 108.2 . . ? C65 C66 C67 107(3) . . ? C65 C66 H66A 109.4 . . ? C67 C66 H66A 110.1 . . ? C65 C66 H66B 110.3 . . ? C67 C66 H66B 110.8 . . ? H66A C66 H66B 108.7 . . ? C66 C67 H67A 109.7 . . ? C66 C67 H67B 109.0 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.7 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O9 C68 C69 103(2) . . ? O9 C68 H68A 111.6 . . ? C69 C68 H68A 113.8 . . ? O9 C68 H68B 110.8 . . ? C69 C68 H68B 108.8 . . ? H68A C68 H68B 109.1 . . ? C68 C69 C70 100(3) . . ? C68 C69 H69A 114.0 . . ? C70 C69 H69A 113.6 . . ? C68 C69 H69B 109.4 . . ? C70 C69 H69B 110.0 . . ? H69A C69 H69B 109.8 . . ? C71 C70 C69 114(3) . . ? C71 C70 H70A 109.0 . . ? C69 C70 H70A 107.1 . . ? C71 C70 H70B 107.9 . . ? C69 C70 H70B 110.8 . . ? H70A C70 H70B 107.9 . . ? C70 C71 H71A 110.8 . . ? C70 C71 H71B 108.3 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.4 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 O10 107.2(11) . . ? C73 C72 H72A 110.3 . . ? O10 C72 H72A 110.1 . . ? C73 C72 H72B 110.3 . . ? O10 C72 H72B 110.5 . . ? H72A C72 H72B 108.5 . . ? C72 C73 C74 112.4(14) . . ? C72 C73 H73A 109.1 . . ? C74 C73 H73A 108.9 . . ? C72 C73 H73B 109.1 . . ? C74 C73 H73B 109.4 . . ? H73A C73 H73B 107.8 . . ? C73 C74 C75 109.8(18) . . ? C73 C74 H74A 109.5 . . ? C75 C74 H74A 110.0 . . ? C73 C74 H74B 109.9 . . ? C75 C74 H74B 109.5 . . ? H74A C74 H74B 108.1 . . ? C74 C75 H75A 109.1 . . ? C74 C75 H75B 109.9 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.4 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 C76 C81 121.3(11) . . ? C77 C76 O11 123.3(12) . . ? C81 C76 O11 115.4(10) . . ? C76 C77 C78 121.7(12) . . ? C76 C77 H77A 119.1 . . ? C78 C77 H77A 119.3 . . ? C77 C78 C79 117.9(10) . . ? C77 C78 C82 121.9(11) . . ? C79 C78 C82 120.1(10) . . ? O12 C79 C80 126.7(11) . . ? O12 C79 C78 115.0(10) . . ? C80 C79 C78 118.3(10) . . ? C81 C80 C79 122.7(11) . . ? C81 C80 H80A 118.6 . . ? C79 C80 H80A 118.7 . . ? C76 C81 C80 118.1(10) . . ? C76 C81 C110 122.8(10) . . ? C80 C81 C110 119.1(11) . . ? C83 C82 C78 111.4(10) . . ? C83 C82 H82A 109.3 . . ? C78 C82 H82A 109.5 . . ? C83 C82 H82B 109.4 . . ? C78 C82 H82B 109.2 . . ? H82A C82 H82B 108.0 . . ? C88 C83 C84 117.9(11) . . ? C88 C83 C82 120.9(11) . . ? C84 C83 C82 121.2(11) . . ? C83 C84 O13 120.7(10) . . ? C83 C84 C85 119.1(10) . . ? O13 C84 C85 120.2(10) . . ? C86 C85 C84 121.6(11) . . ? C86 C85 H85A 119.1 . . ? C84 C85 H85A 119.4 . . ? C87 C86 C85 116.8(11) . . ? C87 C86 C89 124.7(11) . . ? C85 C86 C89 118.5(11) . . ? C86 C87 O14 114.5(10) . . ? C86 C87 C88 119.3(11) . . ? O14 C87 C88 126.2(11) . . ? C83 C88 C87 125.3(12) . . ? C83 C88 H88A 117.4 . . ? C87 C88 H88A 117.4 . . ? C90 C89 C86 112.3(10) . . ? C90 C89 H89A 109.0 . . ? C86 C89 H89A 108.7 . . ? C90 C89 H89B 109.3 . . ? C86 C89 H89B 109.6 . . ? H89A C89 H89B 107.8 . . ? C91 C90 C95 116.2(10) . . ? C91 C90 C89 122.3(10) . . ? C95 C90 C89 121.4(10) . . ? C92 C91 O15 124.3(11) . . ? C92 C91 C90 121.8(11) . . ? O15 C91 C90 113.9(10) . . ? C93 C92 C91 122.0(11) . . ? C93 C92 H92A 119.1 . . ? C91 C92 H92A 119.0 . . ? C92 C93 C94 119.7(11) . . ? C92 C93 C96 122.3(11) . . ? C94 C93 C96 118.1(10) . . ? O16 C94 C95 123.3(10) . . ? O16 C94 C93 117.0(10) . . ? C95 C94 C93 119.6(11) . . ? C94 C95 C90 120.7(10) . . ? C94 C95 H95A 119.7 . . ? C90 C95 H95A 119.6 . . ? C93 C96 C97 112.7(9) . . ? C93 C96 H96A 108.9 . . ? C97 C96 H96A 109.2 . . ? C93 C96 H96B 109.1 . . ? C97 C96 H96B 109.0 . . ? H96A C96 H96B 107.8 . . ? C98 C97 C102 119.1(11) . . ? C98 C97 C96 120.4(11) . . ? C102 C97 C96 120.5(11) . . ? C97 C98 O17 116.3(10) . . ? C97 C98 C99 121.4(12) . . ? O17 C98 C99 122.3(11) . . ? C98 C99 C100 118.6(11) . . ? C98 C99 H99A 120.6 . . ? C100 C99 H99A 120.8 . . ? C101 C100 C99 118.4(11) . . ? C101 C100 C103 123.2(11) . . ? C99 C100 C103 118.2(11) . . ? C102 C101 O18 123.7(11) . . ? C102 C101 C100 121.2(12) . . ? O18 C101 C100 114.9(10) . . ? C101 C102 C97 121.1(12) . . ? C101 C102 H10A 119.4 . . ? C97 C102 H10A 119.5 . . ? C104 C103 C100 109.6(9) . . ? C104 C103 H10B 110.0 . . ? C100 C103 H10B 109.8 . . ? C104 C103 H10C 109.6 . . ? C100 C103 H10C 109.6 . . ? H10B C103 H10C 108.2 . . ? C109 C104 C105 117.8(11) . . ? C109 C104 C103 119.5(11) . . ? C105 C104 C103 122.6(11) . . ? C106 C105 O19 125.4(11) . . ? C106 C105 C104 120.0(11) . . ? O19 C105 C104 114.6(10) . . ? C105 C106 C107 122.6(12) . . ? C105 C106 H10D 118.8 . . ? C107 C106 H10D 118.6 . . ? C108 C107 C106 119.0(12) . . ? C108 C107 C110 120.4(12) . . ? C106 C107 C110 120.6(12) . . ? O20 C108 C107 116.7(11) . . ? O20 C108 C109 124.1(11) . . ? C107 C108 C109 119.1(11) . . ? C104 C109 C108 121.5(12) . . ? C104 C109 H10E 119.2 . . ? C108 C109 H10E 119.4 . . ? C107 C110 C81 113.5(10) . . ? C107 C110 H11A 108.9 . . ? C81 C110 H11A 108.8 . . ? C107 C110 H11B 108.8 . . ? C81 C110 H11B 108.9 . . ? H11A C110 H11B 107.7 . . ? O11 C111 C112 107(2) . . ? O11 C111 H11C 110.3 . . ? C112 C111 H11C 110.7 . . ? O11 C111 H11D 109.8 . . ? C112 C111 H11D 110.6 . . ? H11C C111 H11D 108.5 . . ? C113 C112 C111 136(6) . . ? C113 C112 H11E 101.8 . . ? C111 C112 H11E 102.4 . . ? C113 C112 H11T 105.1 . . ? C111 C112 H11T 103.6 . . ? H11E C112 H11T 105.1 . . ? C112 C113 C114 121(8) . . ? C112 C113 H11U 109.2 . . ? C114 C113 H11U 107.1 . . ? C112 C113 H11V 105.6 . . ? C114 C113 H11V 106.1 . . ? H11U C113 H11V 106.7 . . ? C113 C114 H11F 110.3 . . ? C113 C114 H11G 109.4 . . ? H11F C114 H11G 109.5 . . ? C113 C114 H11H 108.7 . . ? H11F C114 H11H 109.5 . . ? H11G C114 H11H 109.5 . . ? O12 C115 C116 107.5(9) . . ? O12 C115 H11I 110.2 . . ? C116 C115 H11I 110.1 . . ? O12 C115 H11J 110.1 . . ? C116 C115 H11J 110.4 . . ? H11I C115 H11J 108.5 . . ? C117 C116 C115 109.8(10) . . ? C117 C116 H11K 109.7 . . ? C115 C116 H11K 110.0 . . ? C117 C116 H11L 109.5 . . ? C115 C116 H11L 109.6 . . ? H11K C116 H11L 108.2 . . ? C116 C117 C118 111.8(12) . . ? C116 C117 H11M 109.0 . . ? C118 C117 H11M 109.4 . . ? C116 C117 H11N 109.3 . . ? C118 C117 H11N 109.3 . . ? H11M C117 H11N 107.9 . . ? C117 C118 H11O 109.4 . . ? C117 C118 H11P 109.5 . . ? H11O C118 H11P 109.5 . . ? C117 C118 H11Q 109.5 . . ? H11O C118 H11Q 109.5 . . ? H11P C118 H11Q 109.5 . . ? C120 C119 O13 111.8(17) . . ? C120 C119 H11R 108.0 . . ? O13 C119 H11R 108.6 . . ? C120 C119 H11S 109.8 . . ? O13 C119 H11S 110.7 . . ? H11R C119 H11S 107.8 . . ? C119 C120 C121 114(3) . . ? C119 C120 H12B 109.4 . . ? C121 C120 H12B 108.5 . . ? C119 C120 H12S 107.9 . . ? C121 C120 H12S 109.4 . . ? H12B C120 H12S 107.8 . . ? C120 C121 C122 103.9(18) . . ? C120 C121 H12C 111.3 . . ? C122 C121 H12C 110.3 . . ? C120 C121 H12D 111.2 . . ? C122 C121 H12D 111.0 . . ? H12C C121 H12D 109.0 . . ? C121 C122 H12E 110.1 . . ? C121 C122 H12F 108.8 . . ? H12E C122 H12F 109.5 . . ? C121 C122 H12G 109.5 . . ? H12E C122 H12G 109.5 . . ? H12F C122 H12G 109.5 . . ? O14 C123 C124 106.8(10) . . ? O14 C123 H12H 110.1 . . ? C124 C123 H12H 110.3 . . ? O14 C123 H12I 110.5 . . ? C124 C123 H12I 110.5 . . ? H12H C123 H12I 108.6 . . ? C125 C124 C123 110.4(12) . . ? C125 C124 H12J 109.8 . . ? C123 C124 H12J 109.6 . . ? C125 C124 H12K 109.5 . . ? C123 C124 H12K 109.5 . . ? H12J C124 H12K 108.1 . . ? C124 C125 C126 113.4(16) . . ? C124 C125 H12L 108.8 . . ? C126 C125 H12L 108.7 . . ? C124 C125 H12M 109.1 . . ? C126 C125 H12M 109.1 . . ? H12L C125 H12M 107.7 . . ? C125 C126 H12N 109.4 . . ? C125 C126 H12O 109.3 . . ? H12N C126 H12O 109.5 . . ? C125 C126 H12P 109.7 . . ? H12N C126 H12P 109.5 . . ? H12O C126 H12P 109.5 . . ? O15 C127 C128 109.7(15) . . ? O15 C127 H12Q 109.6 . . ? C128 C127 H12Q 109.3 . . ? O15 C127 H12R 109.6 . . ? C128 C127 H12R 110.3 . . ? H12Q C127 H12R 108.2 . . ? C129 C128 C127 126(3) . . ? C129 C128 H12V 103.1 . . ? C127 C128 H12V 105.6 . . ? C129 C128 H12W 107.8 . . ? C127 C128 H12W 106.3 . . ? H12V C128 H12W 106.4 . . ? C128 C129 C130 121(4) . . ? C128 C129 H12T 109.1 . . ? C130 C129 H12T 109.0 . . ? C128 C129 H12U 104.6 . . ? C130 C129 H12U 105.5 . . ? H12T C129 H12U 107.1 . . ? C129 C130 H13A 110.6 . . ? C129 C130 H13B 110.6 . . ? H13A C130 H13B 109.5 . . ? C129 C130 H13C 107.2 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? O16 C131 C132 109.7(13) . . ? O16 C131 H13D 109.9 . . ? C132 C131 H13D 109.6 . . ? O16 C131 H13E 109.8 . . ? C132 C131 H13E 109.6 . . ? H13D C131 H13E 108.2 . . ? C133 C132 C131 110.5(15) . . ? C133 C132 H13F 109.7 . . ? C131 C132 H13F 109.6 . . ? C133 C132 H13G 109.4 . . ? C131 C132 H13G 109.5 . . ? H13F C132 H13G 108.1 . . ? C132 C133 C134 111.5(17) . . ? C132 C133 H13H 109.2 . . ? C134 C133 H13H 109.7 . . ? C132 C133 H13I 109.4 . . ? C134 C133 H13I 109.0 . . ? H13H C133 H13I 108.0 . . ? C133 C134 H13J 109.5 . . ? C133 C134 H13K 109.9 . . ? H13J C134 H13K 109.5 . . ? C133 C134 H13L 109.1 . . ? H13J C134 H13L 109.5 . . ? H13K C134 H13L 109.5 . . ? O17 C135 C136 104.8(10) . . ? O17 C135 H13M 110.6 . . ? C136 C135 H13M 110.9 . . ? O17 C135 H13N 110.8 . . ? C136 C135 H13N 110.9 . . ? H13M C135 H13N 108.8 . . ? C137 C136 C135 114.7(12) . . ? C137 C136 H13O 108.7 . . ? C135 C136 H13O 108.6 . . ? C137 C136 H13P 108.4 . . ? C135 C136 H13P 108.7 . . ? H13O C136 H13P 107.5 . . ? C136 C137 C138 112.0(15) . . ? C136 C137 H13Q 109.0 . . ? C138 C137 H13Q 108.8 . . ? C136 C137 H13R 109.3 . . ? C138 C137 H13R 109.8 . . ? H13Q C137 H13R 107.8 . . ? C137 C138 H13S 109.1 . . ? C137 C138 H13T 109.1 . . ? H13S C138 H13T 109.5 . . ? C137 C138 H13U 110.2 . . ? H13S C138 H13U 109.5 . . ? H13T C138 H13U 109.5 . . ? O18 C139 C140 103.8(15) . . ? O18 C139 H13V 111.0 . . ? C140 C139 H13V 110.9 . . ? O18 C139 H13W 110.8 . . ? C140 C139 H13W 111.3 . . ? H13V C139 H13W 109.0 . . ? C141 C140 C139 108(3) . . ? C141 C140 H14C 108.1 . . ? C139 C140 H14C 110.5 . . ? C141 C140 H14D 112.0 . . ? C139 C140 H14D 109.9 . . ? H14C C140 H14D 108.5 . . ? C140 C141 C142 104(4) . . ? C140 C141 H14E 113.0 . . ? C142 C141 H14E 112.7 . . ? C140 C141 H14F 109.2 . . ? C142 C141 H14F 108.9 . . ? H14E C141 H14F 109.3 . . ? C141 C142 H14G 111.2 . . ? C141 C142 H14H 110.2 . . ? H14G C142 H14H 109.5 . . ? C141 C142 H14I 107.0 . . ? H14G C142 H14I 109.5 . . ? H14H C142 H14I 109.5 . . ? O19 C143 C144 108.6(10) . . ? O19 C143 H14J 110.0 . . ? C144 C143 H14J 110.2 . . ? O19 C143 H14K 109.8 . . ? C144 C143 H14K 109.9 . . ? H14J C143 H14K 108.3 . . ? C143 C144 C145 113.8(11) . . ? C143 C144 H14L 108.9 . . ? C145 C144 H14L 108.8 . . ? C143 C144 H14M 108.7 . . ? C145 C144 H14M 108.9 . . ? H14L C144 H14M 107.6 . . ? C146 C145 C144 115.8(13) . . ? C146 C145 H14N 108.3 . . ? C144 C145 H14N 108.4 . . ? C146 C145 H14X 108.3 . . ? C144 C145 H14X 108.4 . . ? H14N C145 H14X 107.4 . . ? C145 C146 H14O 109.3 . . ? C145 C146 H14P 109.5 . . ? H14O C146 H14P 109.5 . . ? C145 C146 H14Q 109.6 . . ? H14O C146 H14Q 109.5 . . ? H14P C146 H14Q 109.5 . . ? O20 C147 C148 108.9(11) . . ? O20 C147 H14R 110.1 . . ? C148 C147 H14R 110.0 . . ? O20 C147 H14S 109.8 . . ? C148 C147 H14S 109.8 . . ? H14R C147 H14S 108.3 . . ? C149 C148 C147 111.8(13) . . ? C149 C148 H14T 109.1 . . ? C147 C148 H14T 109.2 . . ? C149 C148 H14U 109.3 . . ? C147 C148 H14U 109.4 . . ? H14T C148 H14U 108.0 . . ? C148 C149 C150 112.7(15) . . ? C148 C149 H14V 109.1 . . ? C150 C149 H14V 109.5 . . ? C148 C149 H14W 108.8 . . ? C150 C149 H14W 108.9 . . ? H14V C149 H14W 107.8 . . ? C149 C150 H15Q 109.3 . . ? C149 C150 H15R 109.9 . . ? H15Q C150 H15R 109.5 . . ? C149 C150 H15S 109.3 . . ? H15Q C150 H15S 109.5 . . ? H15R C150 H15S 109.5 . . ? C152 C151 I1 132(2) . . ? C152 C151 H15A 105.8 . . ? I1 C151 H15A 105.4 . . ? C152 C151 H15B 102.2 . . ? I1 C151 H15B 102.8 . . ? H15A C151 H15B 105.7 . . ? C153 C152 C151 115.6(16) . . ? C153 C152 H15C 108.9 . . ? C151 C152 H15C 110.2 . . ? C153 C152 H15D 107.8 . . ? C151 C152 H15D 106.4 . . ? H15C C152 H15D 107.7 . . ? C152 C153 C154 114.8(18) . . ? C152 C153 H15E 107.9 . . ? C154 C153 H15E 107.5 . . ? C152 C153 H15F 109.0 . . ? C154 C153 H15F 109.7 . . ? H15E C153 H15F 107.7 . . ? C153 C154 I2 138(3) . . ? C153 C154 H15G 101.3 . . ? I2 C154 H15G 102.2 . . ? C153 C154 H15H 103.4 . . ? I2 C154 H15H 103.1 . . ? H15G C154 H15H 105.0 . . ? C156 C155 I3 144(3) . . ? C156 C155 H15I 98.8 . . ? I3 C155 H15I 99.9 . . ? C156 C155 H15J 102.9 . . ? I3 C155 H15J 102.2 . . ? H15I C155 H15J 104.4 . . ? C157 C156 C155 113(2) . . ? C157 C156 H15K 107.4 . . ? C155 C156 H15K 106.9 . . ? C157 C156 H15L 110.2 . . ? C155 C156 H15L 111.2 . . ? H15K C156 H15L 107.9 . . ? C156 C157 C158 115(2) . . ? C156 C157 H15M 109.8 . . ? C158 C157 H15M 110.3 . . ? C156 C157 H15N 107.0 . . ? C158 C157 H15N 107.3 . . ? H15M C157 H15N 107.6 . . ? C157 C158 I4 152(3) . . ? C157 C158 H15O 99.9 . . ? I4 C158 H15O 98.9 . . ? C157 C158 H15P 97.3 . . ? I4 C158 H15P 98.1 . . ? H15O C158 H15P 103.8 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 10.302 _refine_diff_density_min -2.728 _refine_diff_density_rms 0.282