# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chuan-Feng Chen' _publ_contact_author_email lipengfei@iccas.ac.cn loop_ _publ_author_name 'Peng-Fei Li' 'Chuan-Feng Chen' data_a _database_code_depnum_ccdc_archive 'CCDC 842676' #TrackingRef 'compound 5a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H75 Cl12 O6' _chemical_formula_weight 1485.74 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.717(3) _cell_length_b 17.240(3) _cell_length_c 18.924(4) _cell_angle_alpha 109.86(3) _cell_angle_beta 100.40(3) _cell_angle_gamma 107.82(3) _cell_volume 3522.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1542 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8586 _exptl_absorpt_correction_T_max 0.8846 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31373 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12871 _reflns_number_gt 10195 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^+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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12871 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2029 _refine_ls_R_factor_gt 0.1819 _refine_ls_wR_factor_ref 0.4428 _refine_ls_wR_factor_gt 0.4300 _refine_ls_goodness_of_fit_ref 2.396 _refine_ls_restrained_S_all 2.396 _refine_ls_shift/su_max 0.398 _refine_ls_shift/su_mean 0.019 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 0.2482(5) -0.2646(4) 0.2209(3) 0.0552(14) Uani 1 1 d . . . O2 O 0.9877(4) -0.2453(3) 0.3146(3) 0.0480(13) Uani 1 1 d . . . O3 O 0.0631(4) -0.6602(3) -0.0654(3) 0.0455(12) Uani 1 1 d . . . O4 O 0.8672(4) -0.5237(3) 0.1855(3) 0.0410(12) Uani 1 1 d . . . H4 H 0.8477 -0.5659 0.1406 0.062 Uiso 1 1 calc R . . O5 O 0.7849(4) -0.6418(3) 0.0243(3) 0.0428(12) Uani 1 1 d . . . O6 O 0.0928(4) -0.5441(3) 0.0884(3) 0.0476(13) Uani 1 1 d . . . H6 H 0.0669 -0.5862 0.0428 0.071 Uiso 1 1 calc R . . C1 C 0.0505(9) -0.6497(7) 0.3760(6) 0.073(3) Uani 1 1 d . . . H1A H 0.0605 -0.6669 0.4203 0.110 Uiso 1 1 calc R . . H1B H -0.0295 -0.6848 0.3398 0.110 Uiso 1 1 calc R . . H1C H 0.0660 -0.5856 0.3962 0.110 Uiso 1 1 calc R . . C2 C 0.6536(10) -0.7541(5) 0.3734(5) 0.069(3) Uani 1 1 d . . . H2A H 0.5867 -0.7722 0.3275 0.103 Uiso 1 1 calc R . . H2B H 0.6260 -0.7697 0.4138 0.103 Uiso 1 1 calc R . . H2C H 0.7035 -0.7854 0.3567 0.103 Uiso 1 1 calc R . . C3 C 0.7064(7) -0.0607(6) 0.6103(5) 0.054(2) Uani 1 1 d . . . H3A H 0.7329 -0.0027 0.6524 0.065 Uiso 1 1 calc R . . C4 C 0.6683(7) -0.1365(6) 0.6251(5) 0.055(2) Uani 1 1 d . . . H4A H 0.6688 -0.1298 0.6771 0.066 Uiso 1 1 calc R . . C5 C 0.2793(8) -0.1849(6) 0.2075(6) 0.061(2) Uani 1 1 d . . . H5A H 0.2095 -0.1840 0.1764 0.092 Uiso 1 1 calc R . . H5B H 0.3358 -0.1842 0.1784 0.092 Uiso 1 1 calc R . . H5C H 0.3140 -0.1319 0.2585 0.092 Uiso 1 1 calc R . . C6 C 0.1136(7) -0.7680(6) 0.3022(5) 0.058(2) Uani 1 1 d . . . H6A H 0.1247 -0.7839 0.3472 0.086 Uiso 1 1 calc R . . H6B H 0.1691 -0.7790 0.2743 0.086 Uiso 1 1 calc R . . H6C H 0.0340 -0.8048 0.2658 0.086 Uiso 1 1 calc R . . C7 C 0.2589(7) -0.6147(6) 0.3889(5) 0.067(3) Uani 1 1 d . . . H7A H 0.2681 -0.6327 0.4327 0.101 Uiso 1 1 calc R . . H7B H 0.2753 -0.5503 0.4100 0.101 Uiso 1 1 calc R . . H7C H 0.3133 -0.6267 0.3604 0.101 Uiso 1 1 calc R . . C8 C 0.6415(8) -0.6070(6) 0.4375(6) 0.063(3) Uani 1 1 d . . . H8A H 0.5734 -0.6244 0.3927 0.094 Uiso 1 1 calc R . . H8B H 0.6842 -0.5416 0.4615 0.094 Uiso 1 1 calc R . . H8C H 0.6159 -0.6259 0.4770 0.094 Uiso 1 1 calc R . . C9 C 0.1671(6) -0.4189(5) 0.2438(5) 0.059(2) Uani 1 1 d . . . H9A H 0.1079 -0.3969 0.2366 0.071 Uiso 1 1 calc R . . C10 C 0.8287(9) -0.6232(7) 0.4821(6) 0.073(3) Uani 1 1 d . . . H10A H 0.8828 -0.6504 0.4659 0.110 Uiso 1 1 calc R . . H10B H 0.8005 -0.6430 0.5205 0.110 Uiso 1 1 calc R . . H10C H 0.8691 -0.5576 0.5065 0.110 Uiso 1 1 calc R . . C11 C 1.0313(7) -0.1642(6) 0.3046(6) 0.061(2) Uani 1 1 d . . . H11A H 1.1034 -0.1586 0.2913 0.092 Uiso 1 1 calc R . . H11B H 1.0471 -0.1127 0.3540 0.092 Uiso 1 1 calc R . . H11C H 0.9733 -0.1658 0.2618 0.092 Uiso 1 1 calc R . . C12 C 0.1342(6) -0.6681(6) 0.3323(5) 0.049(2) Uani 1 1 d . . . C13 C 0.0803(7) -0.6189(6) -0.1191(5) 0.052(2) Uani 1 1 d . . . H13A H 0.0310 -0.5850 -0.1194 0.078 Uiso 1 1 calc R . . H13B H 0.0595 -0.6655 -0.1726 0.078 Uiso 1 1 calc R . . H13C H 0.1623 -0.5780 -0.1020 0.078 Uiso 1 1 calc R . . C14 C 0.8054(7) -0.6004(5) -0.0268(5) 0.0484(19) Uani 1 1 d . . . H14A H 0.8890 -0.5647 -0.0114 0.073 Uiso 1 1 calc R . . H14B H 0.7630 -0.5611 -0.0235 0.073 Uiso 1 1 calc R . . H14C H 0.7785 -0.6465 -0.0813 0.073 Uiso 1 1 calc R . . C15 C 0.6299(7) -0.2215(6) 0.5651(5) 0.0474(19) Uani 1 1 d . . . H15A H 0.6042 -0.2733 0.5752 0.057 Uiso 1 1 calc R . . C16 C 0.2469(7) -1.0291(5) -0.1315(5) 0.0473(19) Uani 1 1 d . . . H16A H 0.2366 -1.0546 -0.0946 0.057 Uiso 1 1 calc R . . C17 C 0.7063(6) -0.0683(5) 0.5350(5) 0.0473(19) Uani 1 1 d . . . H17A H 0.7326 -0.0163 0.5252 0.057 Uiso 1 1 calc R . . C18 C 0.7228(7) -0.6532(5) 0.4075(4) 0.0449(18) Uani 1 1 d . . . C19 C 0.2207(7) -1.0845(5) -0.2122(5) 0.050(2) Uani 1 1 d . . . H19A H 0.1890 -1.1480 -0.2307 0.060 Uiso 1 1 calc R . . C20 C 0.1441(6) -0.5499(5) 0.2801(5) 0.0431(17) Uani 1 1 d . . . H20A H 0.1672 -0.5088 0.3340 0.052 Uiso 1 1 calc R . . C21 C 0.3324(7) -0.2793(5) 0.2633(4) 0.048(2) Uani 1 1 d . . . C22 C 0.1188(6) -0.6402(5) 0.2631(4) 0.0413(17) Uani 1 1 d . . . C23 C 0.2820(6) -0.9536(5) -0.2406(5) 0.0459(18) Uani 1 1 d . . . H23A H 0.2923 -0.9288 -0.2779 0.055 Uiso 1 1 calc R . . C24 C 0.5291(6) -0.2345(4) 0.3428(4) 0.0391(17) Uani 1 1 d . . . C25 C 0.2411(7) -1.0467(5) -0.2641(5) 0.053(2) Uani 1 1 d . . . H25A H 0.2270 -1.0848 -0.3177 0.063 Uiso 1 1 calc R . . C26 C 0.6674(6) -0.1528(4) 0.4746(5) 0.0404(17) Uani 1 1 d . . . C27 C 0.8248(6) -0.2100(4) 0.3422(4) 0.0397(17) Uani 1 1 d . . . H27A H 0.8491 -0.1586 0.3313 0.048 Uiso 1 1 calc R . . C28 C 0.0676(5) -0.6707(5) 0.1237(4) 0.0384(16) Uani 1 1 d . . . C29 C 0.1261(6) -0.7115(5) -0.0574(4) 0.0431(17) Uani 1 1 d . . . C30 C 0.9240(6) -0.3982(4) 0.3397(5) 0.0406(17) Uani 1 1 d . . . H30A H 0.9645 -0.3910 0.3009 0.049 Uiso 1 1 calc R . . H30B H 0.9846 -0.3735 0.3916 0.049 Uiso 1 1 calc R . . C31 C 0.1075(6) -0.7482(5) -0.0028(5) 0.0396(16) Uani 1 1 d . . . C32 C 0.8863(6) -0.2646(4) 0.3340(4) 0.0385(16) Uani 1 1 d . . . C33 C 0.2947(6) -0.3574(5) 0.2753(4) 0.0430(18) Uani 1 1 d . . . C34 C 0.0198(6) -0.7379(5) 0.0397(4) 0.0375(16) Uani 1 1 d . . . H34A H -0.0356 -0.7214 0.0101 0.045 Uiso 1 1 calc R . . H34B H -0.0251 -0.7971 0.0378 0.045 Uiso 1 1 calc R . . C35 C 0.7269(6) -0.2311(4) 0.3667(4) 0.0402(17) Uani 1 1 d . . . C36 C 0.8248(6) -0.5313(4) 0.3684(5) 0.0401(17) Uani 1 1 d . . . H36A H 0.8455 -0.4904 0.4221 0.048 Uiso 1 1 calc R . . C37 C 0.7609(6) -0.7179(5) 0.1325(4) 0.0405(17) Uani 1 1 d . . . H37A H 0.7514 -0.7763 0.1343 0.049 Uiso 1 1 calc R . . H37B H 0.8324 -0.6968 0.1185 0.049 Uiso 1 1 calc R . . C38 C 0.4504(7) -0.2178(5) 0.2955(4) 0.0425(17) Uani 1 1 d . . . H38A H 0.4749 -0.1662 0.2849 0.051 Uiso 1 1 calc R . . C39 C 0.6296(6) -0.2297(5) 0.4876(5) 0.0405(17) Uani 1 1 d . . . C40 C 0.7634(6) -0.6205(5) 0.3469(4) 0.0349(15) Uani 1 1 d . . . C41 C 0.1376(6) -0.5175(5) 0.2243(5) 0.0434(18) Uani 1 1 d . . . C42 C 0.5897(6) -0.3158(5) 0.4142(5) 0.0444(19) Uani 1 1 d . . . H42A H 0.5631 -0.3707 0.4245 0.053 Uiso 1 1 calc R . . C43 C 0.5433(6) -0.7867(4) 0.0580(4) 0.0368(16) Uani 1 1 d . . . H43A H 0.5314 -0.8120 0.0948 0.044 Uiso 1 1 calc R . . C44 C 0.2496(6) -0.8109(4) -0.0292(4) 0.0351(15) Uani 1 1 d . . . C45 C 0.6563(6) -0.1736(5) 0.3876(5) 0.0430(18) Uani 1 1 d . . . H45A H 0.6827 -0.1185 0.3776 0.052 Uiso 1 1 calc R . . C46 C 0.6902(6) -0.3077(4) 0.3818(4) 0.0346(15) Uani 1 1 d . . . C47 C 0.2879(6) -0.9370(5) -0.1070(4) 0.0405(17) Uani 1 1 d . . . C48 C 0.7416(6) -0.6801(4) 0.2694(4) 0.0373(16) Uani 1 1 d . . . H48A H 0.7016 -0.7427 0.2539 0.045 Uiso 1 1 calc R . . C49 C 0.1710(6) -0.7984(4) 0.0105(4) 0.0374(16) Uani 1 1 d . . . H49A H 0.1597 -0.8240 0.0472 0.045 Uiso 1 1 calc R . . C50 C 0.3544(6) -0.7969(4) -0.1230(4) 0.0363(15) Uani 1 1 d . . . H50A H 0.3666 -0.7705 -0.1619 0.044 Uiso 1 1 calc R . . C51 C 0.1003(6) -0.5786(5) 0.1445(5) 0.0404(17) Uani 1 1 d . . . C52 C 0.4483(6) -0.8046(5) -0.0031(4) 0.0375(16) Uani 1 1 d . . . C53 C 0.8513(6) -0.3415(4) 0.3470(4) 0.0362(15) Uani 1 1 d . . . C54 C 0.0795(6) -0.6980(5) 0.1854(4) 0.0401(17) Uani 1 1 d . . . H54A H 0.0592 -0.7601 0.1721 0.048 Uiso 1 1 calc R . . C55 C 0.3073(6) -0.8978(5) -0.1600(4) 0.0385(16) Uani 1 1 d . . . C56 C 0.8585(6) -0.4976(5) 0.3149(4) 0.0364(16) Uani 1 1 d . . . C57 C 0.2674(6) -0.7739(5) -0.0830(4) 0.0356(15) Uani 1 1 d . . . C58 C 0.3220(6) -0.8642(4) -0.0221(4) 0.0377(16) Uani 1 1 d . . . H58A H 0.3097 -0.8902 0.0171 0.045 Uiso 1 1 calc R . . C59 C 0.4935(6) -0.3113(4) 0.3567(4) 0.0360(16) Uani 1 1 d . . . C60 C 0.7765(6) -0.6511(4) 0.2139(4) 0.0328(15) Uani 1 1 d . . . C61 C 0.7513(6) -0.3628(4) 0.3713(4) 0.0354(15) Uani 1 1 d . . . H61A H 0.7258 -0.4154 0.3804 0.043 Uiso 1 1 calc R . . C62 C 0.6555(6) -0.7326(4) 0.0668(4) 0.0330(15) Uani 1 1 d . . . C63 C 0.8328(6) -0.5581(5) 0.2371(4) 0.0363(16) Uani 1 1 d . . . C64 C 0.4658(6) -0.7671(4) -0.0571(4) 0.0354(16) Uani 1 1 d . . . C65 C 0.3768(6) -0.3737(4) 0.3207(5) 0.0410(17) Uani 1 1 d . . . H65A H 0.3539 -0.4278 0.3276 0.049 Uiso 1 1 calc R . . C66 C 0.6718(6) -0.6949(4) 0.0121(4) 0.0356(16) Uani 1 1 d . . . C67 C 0.2060(6) -0.7224(4) -0.0984(4) 0.0364(16) Uani 1 1 d . . . H67A H 0.2182 -0.6965 -0.1348 0.044 Uiso 1 1 calc R . . C68 C 0.5775(6) -0.7122(5) -0.0498(4) 0.0378(16) Uani 1 1 d . . . H68A H 0.5889 -0.6869 -0.0867 0.045 Uiso 1 1 calc R . . C69 C 0.4287(11) -0.0247(9) 0.0833(12) 0.260(16) Uani 1 1 d . . . H69A H 0.4522 0.0240 0.0656 0.312 Uiso 1 1 calc R . . H69B H 0.4713 -0.0638 0.0680 0.312 Uiso 1 1 calc R . . C70 C 0.5980(9) 0.1254(6) 0.5112(7) 0.075(3) Uani 1 1 d . . . H70A H 0.5657 0.1682 0.5028 0.090 Uiso 1 1 calc R . . H70B H 0.5546 0.0969 0.5404 0.090 Uiso 1 1 calc R . . C71 C 0.420(2) 0.3427(8) 0.1925(10) 0.211(12) Uani 1 1 d . . . H71A H 0.4754 0.3419 0.1622 0.253 Uiso 1 1 calc R . . H71B H 0.3490 0.3408 0.1585 0.253 Uiso 1 1 calc R . . C72 C -0.0197(11) -0.9907(7) -0.1836(12) 0.168(9) Uani 1 1 d . . . H72A H 0.0569 -0.9429 -0.1714 0.202 Uiso 1 1 calc R . . H72B H -0.0397 -1.0403 -0.2361 0.202 Uiso 1 1 calc R . . C73 C 0.5256(12) -0.4500(9) 0.1357(10) 0.130(5) Uani 1 1 d . . . H73A H 0.5453 -0.4059 0.1127 0.156 Uiso 1 1 calc R . . H73B H 0.5345 -0.4161 0.1919 0.156 Uiso 1 1 calc R . . C74 C 1.0117(11) 0.0690(19) 0.3918(19) 0.37(2) Uani 1 1 d . . . H74A H 0.9690 0.0353 0.3343 0.440 Uiso 1 1 d R . . H74B H 1.0973 0.0928 0.4032 0.440 Uiso 1 1 d R . . Cl1 Cl 0.2911(6) -0.0803(5) 0.0509(3) 0.198(3) Uani 1 1 d . . . Cl2 Cl 0.4521(3) 0.0268(3) 0.2079(2) 0.1416(17) Uani 1 1 d . . . Cl3 Cl 0.7455(3) 0.18397(18) 0.56799(18) 0.0849(8) Uani 1 1 d . . . Cl4 Cl 0.5787(2) 0.04214(17) 0.41868(15) 0.0719(7) Uani 1 1 d . . . Cl5 Cl 0.4755(5) 0.4370(2) 0.2674(2) 0.1448(18) Uani 1 1 d . . . Cl6 Cl 0.3797(2) 0.24267(16) 0.20484(16) 0.0743(7) Uani 1 1 d . . . Cl7 Cl -0.1229(5) -0.9516(4) -0.1776(3) 0.173(2) Uani 1 1 d . . . Cl8 Cl -0.0253(4) -1.0353(3) -0.0960(3) 0.1391(16) Uani 1 1 d . . . Cl9 Cl 0.3837(3) -0.5197(4) 0.0886(4) 0.236(4) Uani 1 1 d . . . Cl10 Cl 0.6213(4) -0.4949(4) 0.1334(4) 0.172(2) Uani 1 1 d . . . Cl11 Cl 0.9696(11) 0.0317(6) 0.4511(6) 0.318(5) Uani 1 1 d . . . Cl12 Cl 0.9434(7) 0.1764(8) 0.4698(5) 0.325(6) 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 0.058(3) 0.065(4) 0.048(3) 0.022(3) 0.007(3) 0.038(3) O2 0.043(3) 0.041(3) 0.053(3) 0.018(3) 0.022(3) 0.007(2) O3 0.050(3) 0.050(3) 0.044(3) 0.021(3) 0.013(3) 0.028(3) O4 0.041(3) 0.039(3) 0.040(3) 0.018(2) 0.012(2) 0.011(2) O5 0.038(3) 0.048(3) 0.039(3) 0.017(2) 0.013(2) 0.014(2) O6 0.049(3) 0.046(3) 0.048(3) 0.018(3) 0.011(3) 0.024(3) C1 0.081(7) 0.092(7) 0.053(6) 0.031(6) 0.031(5) 0.036(6) C2 0.115(8) 0.044(5) 0.050(6) 0.025(4) 0.035(6) 0.024(5) C3 0.057(5) 0.048(5) 0.052(5) 0.019(4) 0.012(4) 0.019(4) C4 0.053(5) 0.070(6) 0.048(5) 0.028(5) 0.020(4) 0.028(4) C5 0.077(6) 0.060(5) 0.059(6) 0.028(5) 0.015(5) 0.043(5) C6 0.043(5) 0.070(6) 0.055(5) 0.026(5) 0.010(4) 0.020(4) C7 0.052(5) 0.068(6) 0.057(6) 0.016(5) -0.015(4) 0.023(5) C8 0.066(6) 0.065(5) 0.084(7) 0.040(5) 0.051(6) 0.036(5) C9 0.029(4) 0.040(4) 0.078(6) -0.001(4) -0.001(4) 0.017(3) C10 0.083(7) 0.087(7) 0.052(6) 0.040(5) 0.003(5) 0.034(6) C11 0.049(5) 0.062(5) 0.064(6) 0.029(5) 0.027(5) 0.003(4) C12 0.037(4) 0.073(6) 0.035(4) 0.018(4) 0.005(3) 0.027(4) C13 0.063(5) 0.062(5) 0.041(5) 0.024(4) 0.013(4) 0.037(4) C14 0.054(5) 0.057(5) 0.039(5) 0.029(4) 0.015(4) 0.018(4) C15 0.043(4) 0.068(5) 0.053(5) 0.040(4) 0.018(4) 0.031(4) C16 0.044(4) 0.040(4) 0.046(5) 0.011(4) 0.005(4) 0.015(3) C17 0.039(4) 0.040(4) 0.054(5) 0.019(4) 0.007(4) 0.010(3) C18 0.063(5) 0.050(4) 0.036(4) 0.024(4) 0.024(4) 0.030(4) C19 0.047(5) 0.032(4) 0.054(5) 0.008(4) 0.000(4) 0.015(3) C20 0.032(4) 0.051(4) 0.038(4) 0.010(4) 0.005(3) 0.019(3) C21 0.067(5) 0.058(5) 0.028(4) 0.013(4) 0.013(4) 0.047(4) C22 0.022(3) 0.050(4) 0.042(5) 0.010(4) 0.008(3) 0.013(3) C23 0.042(4) 0.047(4) 0.039(4) 0.011(4) 0.005(4) 0.019(4) C24 0.043(4) 0.032(4) 0.044(4) 0.015(3) 0.017(4) 0.016(3) C25 0.054(5) 0.045(4) 0.037(5) -0.004(4) 0.002(4) 0.023(4) C26 0.035(4) 0.032(4) 0.053(5) 0.024(4) 0.007(3) 0.009(3) C27 0.050(4) 0.032(4) 0.039(4) 0.023(3) 0.017(4) 0.008(3) C28 0.022(3) 0.042(4) 0.046(5) 0.013(3) 0.009(3) 0.013(3) C29 0.037(4) 0.045(4) 0.040(4) 0.010(3) 0.002(3) 0.020(3) C30 0.035(4) 0.034(4) 0.039(4) 0.006(3) 0.012(3) 0.007(3) C31 0.030(4) 0.043(4) 0.045(4) 0.019(3) 0.011(3) 0.015(3) C32 0.035(4) 0.034(4) 0.039(4) 0.012(3) 0.007(3) 0.010(3) C33 0.036(4) 0.041(4) 0.037(4) -0.003(3) 0.008(3) 0.019(3) C34 0.032(4) 0.039(4) 0.037(4) 0.014(3) 0.007(3) 0.013(3) C35 0.038(4) 0.026(3) 0.042(4) 0.010(3) 0.003(3) 0.004(3) C36 0.035(4) 0.029(3) 0.045(5) 0.006(3) 0.013(3) 0.009(3) C37 0.046(4) 0.039(4) 0.045(5) 0.019(3) 0.018(4) 0.025(3) C38 0.048(4) 0.037(4) 0.045(5) 0.014(3) 0.011(4) 0.026(3) C39 0.038(4) 0.044(4) 0.047(5) 0.023(4) 0.012(4) 0.021(3) C40 0.030(3) 0.044(4) 0.038(4) 0.019(3) 0.011(3) 0.021(3) C41 0.022(3) 0.047(4) 0.049(5) 0.011(4) 0.001(3) 0.016(3) C42 0.030(4) 0.033(4) 0.081(6) 0.035(4) 0.017(4) 0.014(3) C43 0.043(4) 0.041(4) 0.032(4) 0.018(3) 0.015(3) 0.020(3) C44 0.038(4) 0.030(3) 0.036(4) 0.014(3) 0.010(3) 0.015(3) C45 0.041(4) 0.044(4) 0.054(5) 0.029(4) 0.021(4) 0.018(3) C46 0.029(3) 0.027(3) 0.035(4) 0.009(3) 0.005(3) 0.003(3) C47 0.050(4) 0.036(4) 0.041(4) 0.017(3) 0.018(4) 0.021(3) C48 0.039(4) 0.032(3) 0.047(5) 0.017(3) 0.014(3) 0.020(3) C49 0.031(4) 0.029(3) 0.044(4) 0.014(3) 0.008(3) 0.005(3) C50 0.045(4) 0.038(4) 0.028(4) 0.015(3) 0.012(3) 0.017(3) C51 0.031(4) 0.054(4) 0.043(5) 0.021(4) 0.018(3) 0.021(3) C52 0.032(4) 0.039(4) 0.043(4) 0.015(3) 0.011(3) 0.018(3) C53 0.026(3) 0.032(3) 0.036(4) 0.009(3) 0.001(3) 0.004(3) C54 0.028(4) 0.040(4) 0.046(5) 0.012(4) 0.015(3) 0.012(3) C55 0.035(4) 0.041(4) 0.039(4) 0.014(3) 0.010(3) 0.019(3) C56 0.030(4) 0.038(4) 0.038(4) 0.016(3) 0.007(3) 0.013(3) C57 0.027(3) 0.041(4) 0.039(4) 0.017(3) 0.009(3) 0.015(3) C58 0.042(4) 0.033(4) 0.047(4) 0.024(3) 0.014(4) 0.017(3) C59 0.030(4) 0.039(4) 0.039(4) 0.016(3) 0.008(3) 0.015(3) C60 0.032(3) 0.036(4) 0.034(4) 0.013(3) 0.005(3) 0.021(3) C61 0.040(4) 0.026(3) 0.034(4) 0.012(3) 0.008(3) 0.008(3) C62 0.035(4) 0.039(4) 0.027(4) 0.013(3) 0.009(3) 0.018(3) C63 0.032(4) 0.040(4) 0.043(4) 0.023(3) 0.011(3) 0.016(3) C64 0.036(4) 0.035(4) 0.041(4) 0.018(3) 0.014(3) 0.019(3) C65 0.032(4) 0.028(3) 0.063(5) 0.018(3) 0.010(4) 0.014(3) C66 0.031(4) 0.034(3) 0.039(4) 0.010(3) 0.016(3) 0.013(3) C67 0.039(4) 0.036(4) 0.041(4) 0.021(3) 0.014(3) 0.019(3) C68 0.035(4) 0.049(4) 0.031(4) 0.021(3) 0.010(3) 0.013(3) C69 0.062(7) 0.114(10) 0.35(3) -0.170(14) 0.055(12) 0.013(7) C70 0.072(7) 0.053(5) 0.100(9) 0.029(6) 0.041(6) 0.021(5) C71 0.44(4) 0.057(8) 0.136(14) 0.056(9) 0.13(2) 0.069(15) C72 0.070(8) 0.033(5) 0.29(2) -0.015(9) -0.003(11) 0.013(5) C73 0.113(11) 0.099(10) 0.154(15) 0.055(10) -0.004(10) 0.036(9) C74 0.046(7) 0.60(5) 0.77(6) 0.67(5) 0.121(18) 0.117(15) Cl1 0.227(7) 0.239(6) 0.130(4) 0.054(4) 0.038(4) 0.130(6) Cl2 0.108(3) 0.124(3) 0.117(3) -0.020(2) -0.006(2) 0.053(2) Cl3 0.0870(19) 0.0723(16) 0.080(2) 0.0224(15) 0.0166(16) 0.0276(15) Cl4 0.0845(17) 0.0683(15) 0.0656(16) 0.0289(13) 0.0207(14) 0.0349(13) Cl5 0.228(5) 0.0664(19) 0.090(3) 0.0174(19) 0.043(3) 0.016(3) Cl6 0.0880(18) 0.0642(15) 0.0755(18) 0.0324(13) 0.0318(15) 0.0298(13) Cl7 0.157(4) 0.200(5) 0.158(5) 0.070(4) 0.016(4) 0.092(4) Cl8 0.165(4) 0.108(3) 0.155(4) 0.073(3) 0.061(3) 0.041(3) Cl9 0.068(2) 0.287(7) 0.376(9) 0.282(7) -0.031(3) -0.004(3) Cl10 0.153(4) 0.249(5) 0.297(7) 0.215(5) 0.159(5) 0.153(4) Cl11 0.404(14) 0.253(9) 0.255(10) 0.076(8) 0.048(10) 0.145(10) Cl12 0.220(8) 0.441(14) 0.171(6) -0.025(7) -0.029(6) 0.176(9) _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 C21 1.361(9) . ? O1 C5 1.431(9) . ? O2 C32 1.378(8) . ? O2 C11 1.429(9) . ? O3 C29 1.388(8) . ? O3 C13 1.438(9) . ? O4 C63 1.374(8) . ? O4 H4 0.8400 . ? O5 C66 1.376(8) . ? O5 C14 1.400(8) . ? O6 C51 1.385(9) . ? O6 H6 0.8400 . ? C1 C12 1.504(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C18 1.520(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C17 1.385(11) . ? C3 C4 1.391(11) . ? C3 H3A 0.9500 . ? C4 C15 1.381(11) . ? C4 H4A 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C12 1.538(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.528(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C18 1.560(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C33 1.510(10) . ? C9 C41 1.515(10) . ? C9 H9A 0.9500 . ? C10 C18 1.570(12) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C22 1.540(11) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C39 1.422(10) . ? C15 H15A 0.9500 . ? C16 C47 1.384(10) . ? C16 C19 1.410(11) . ? C16 H16A 0.9500 . ? C17 C26 1.376(10) . ? C17 H17A 0.9500 . ? C18 C40 1.542(9) . ? C19 C25 1.371(11) . ? C19 H19A 0.9500 . ? C20 C41 1.355(10) . ? C20 C22 1.395(10) . ? C20 H20A 0.9500 . ? C21 C33 1.394(11) . ? C21 C38 1.416(11) . ? C22 C54 1.357(10) . ? C23 C25 1.401(11) . ? C23 C55 1.411(10) . ? C23 H23A 0.9500 . ? C24 C38 1.384(10) . ? C24 C59 1.393(9) . ? C24 C45 1.516(10) . ? C25 H25A 0.9500 . ? C26 C39 1.388(9) . ? C26 C45 1.531(11) . ? C27 C32 1.385(9) . ? C27 C35 1.394(9) . ? C27 H27A 0.9500 . ? C28 C51 1.400(10) . ? C28 C54 1.400(10) . ? C28 C34 1.487(10) . ? C29 C31 1.401(10) . ? C29 C67 1.406(9) . ? C30 C56 1.513(9) . ? C30 C53 1.528(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C49 1.402(9) . ? C31 C34 1.507(9) . ? C32 C53 1.385(9) . ? C33 C65 1.389(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C46 1.403(9) . ? C35 C45 1.535(9) . ? C36 C40 1.365(9) . ? C36 C56 1.397(10) . ? C36 H36A 0.9500 . ? C37 C60 1.510(9) . ? C37 C62 1.543(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9500 . ? C39 C42 1.508(10) . ? C40 C48 1.392(10) . ? C41 C51 1.403(10) . ? C42 C46 1.504(9) . ? C42 C59 1.524(10) . ? C42 H42A 1.0000 . ? C43 C62 1.390(9) . ? C43 C52 1.384(10) . ? C43 H43A 0.9500 . ? C44 C49 1.380(9) . ? C44 C57 1.390(9) . ? C44 C58 1.507(8) . ? C45 H45A 1.0000 . ? C46 C61 1.388(9) . ? C47 C55 1.404(10) . ? C47 C58 1.546(10) . ? C48 C60 1.394(9) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 C55 1.503(9) . ? C50 C64 1.519(10) . ? C50 C57 1.525(9) . ? C50 H50A 1.0000 . ? C52 C64 1.399(9) . ? C52 C58 1.515(9) . ? C53 C61 1.415(9) . ? C54 H54A 0.9500 . ? C56 C63 1.390(10) . ? C57 C67 1.413(9) . ? C58 H58A 1.0000 . ? C59 C65 1.408(10) . ? C60 C63 1.408(9) . ? C61 H61A 0.9500 . ? C62 C66 1.409(9) . ? C64 C68 1.396(9) . ? C65 H65A 0.9500 . ? C66 C68 1.392(10) . ? C67 H67A 0.9500 . ? C68 H68A 0.9500 . ? C69 Cl1 1.595(13) . ? C69 Cl2 2.14(2) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 Cl3 1.752(11) . ? C70 Cl4 1.763(10) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 Cl5 1.588(15) . ? C71 Cl6 1.751(12) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 Cl7 1.653(12) . ? C72 Cl8 2.05(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 Cl10 1.629(14) . ? C73 Cl9 1.691(15) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 Cl11 1.567(19) . ? C74 H74A 0.9900 . ? C74 H74B 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 C21 O1 C5 119.3(7) . . ? C32 O2 C11 117.8(6) . . ? C29 O3 C13 117.6(6) . . ? C63 O4 H4 109.5 . . ? C66 O5 C14 118.0(6) . . ? C51 O6 H6 109.5 . . ? C12 C1 H1A 109.5 . . ? C12 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C12 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C18 C2 H2A 109.5 . . ? C18 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C18 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C17 C3 C4 121.0(8) . . ? C17 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C15 C4 C3 120.7(8) . . ? C15 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? O1 C5 H5A 109.5 . . ? O1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 C6 H6A 109.5 . . ? C12 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C12 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 H7A 109.5 . . ? C12 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C12 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C18 C8 H8A 109.5 . . ? C18 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C18 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C33 C9 C41 117.1(6) . . ? C33 C9 H9A 121.5 . . ? C41 C9 H9A 121.5 . . ? C18 C10 H10A 109.5 . . ? C18 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C18 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 C7 109.6(7) . . ? C1 C12 C6 110.2(7) . . ? C7 C12 C6 106.9(7) . . ? C1 C12 C22 109.2(6) . . ? C7 C12 C22 109.9(7) . . ? C6 C12 C22 111.0(7) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.4 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 C39 118.5(7) . . ? C4 C15 H15A 120.7 . . ? C39 C15 H15A 120.7 . . ? C47 C16 C19 118.7(8) . . ? C47 C16 H16A 120.6 . . ? C19 C16 H16A 120.7 . . ? C26 C17 C3 118.7(7) . . ? C26 C17 H17A 120.6 . . ? C3 C17 H17A 120.6 . . ? C2 C18 C40 113.7(6) . . ? C2 C18 C8 107.2(7) . . ? C40 C18 C8 108.1(6) . . ? C2 C18 C10 109.9(7) . . ? C40 C18 C10 111.0(7) . . ? C8 C18 C10 106.7(7) . . ? C25 C19 C16 120.0(7) . . ? C25 C19 H19A 120.0 . . ? C16 C19 H19A 120.0 . . ? C41 C20 C22 123.9(7) . . ? C41 C20 H20A 118.1 . . ? C22 C20 H20A 118.1 . . ? O1 C21 C33 115.8(7) . . ? O1 C21 C38 122.1(7) . . ? C33 C21 C38 122.1(7) . . ? C54 C22 C20 116.5(7) . . ? C54 C22 C12 124.6(7) . . ? C20 C22 C12 118.9(7) . . ? C25 C23 C55 118.1(7) . . ? C25 C23 H23A 120.9 . . ? C55 C23 H23A 120.9 . . ? C38 C24 C59 120.7(7) . . ? C38 C24 C45 126.4(6) . . ? C59 C24 C45 112.8(6) . . ? C19 C25 C23 122.1(7) . . ? C19 C25 H25A 118.9 . . ? C23 C25 H25A 118.9 . . ? C17 C26 C39 121.7(7) . . ? C17 C26 C45 125.6(6) . . ? C39 C26 C45 112.7(6) . . ? C32 C27 C35 119.3(6) . . ? C32 C27 H27A 120.3 . . ? C35 C27 H27A 120.3 . . ? C51 C28 C54 117.5(7) . . ? C51 C28 C34 121.9(7) . . ? C54 C28 C34 120.6(6) . . ? O3 C29 C31 114.9(6) . . ? O3 C29 C67 122.4(7) . . ? C31 C29 C67 122.6(6) . . ? C56 C30 C53 116.4(6) . . ? C56 C30 H30A 108.2 . . ? C53 C30 H30A 108.2 . . ? C56 C30 H30B 108.2 . . ? C53 C30 H30B 108.2 . . ? H30A C30 H30B 107.4 . . ? C29 C31 C49 118.3(6) . . ? C29 C31 C34 122.4(6) . . ? C49 C31 C34 119.3(6) . . ? O2 C32 C27 122.7(6) . . ? O2 C32 C53 115.4(6) . . ? C27 C32 C53 121.9(6) . . ? C65 C33 C21 117.9(7) . . ? C65 C33 C9 121.3(7) . . ? C21 C33 C9 120.6(7) . . ? C28 C34 C31 116.2(6) . . ? C28 C34 H34A 108.2 . . ? C31 C34 H34A 108.2 . . ? C28 C34 H34B 108.2 . . ? C31 C34 H34B 108.2 . . ? H34A C34 H34B 107.4 . . ? C27 C35 C46 120.3(6) . . ? C27 C35 C45 126.6(6) . . ? C46 C35 C45 112.9(6) . . ? C40 C36 C56 122.9(7) . . ? C40 C36 H36A 118.5 . . ? C56 C36 H36A 118.5 . . ? C60 C37 C62 114.0(5) . . ? C60 C37 H37A 108.7 . . ? C62 C37 H37A 108.7 . . ? C60 C37 H37B 108.7 . . ? C62 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C24 C38 C21 118.4(7) . . ? C24 C38 H38A 120.8 . . ? C21 C38 H38A 120.8 . . ? C26 C39 C15 119.3(7) . . ? C26 C39 C42 113.9(7) . . ? C15 C39 C42 126.8(7) . . ? C36 C40 C48 117.7(6) . . ? C36 C40 C18 120.6(6) . . ? C48 C40 C18 121.7(6) . . ? C20 C41 C51 118.1(7) . . ? C20 C41 C9 123.2(7) . . ? C51 C41 C9 118.7(7) . . ? C39 C42 C46 105.9(5) . . ? C39 C42 C59 104.0(5) . . ? C46 C42 C59 107.2(6) . . ? C39 C42 H42A 113.0 . . ? C46 C42 H42A 113.0 . . ? C59 C42 H42A 113.0 . . ? C62 C43 C52 121.5(6) . . ? C62 C43 H43A 119.2 . . ? C52 C43 H43A 119.2 . . ? C49 C44 C57 120.6(6) . . ? C49 C44 C58 126.5(6) . . ? C57 C44 C58 112.9(6) . . ? C24 C45 C35 107.0(6) . . ? C24 C45 C26 104.6(5) . . ? C35 C45 C26 104.6(6) . . ? C24 C45 H45A 113.3 . . ? C35 C45 H45A 113.3 . . ? C26 C45 H45A 113.3 . . ? C61 C46 C35 119.5(6) . . ? C61 C46 C42 127.2(6) . . ? C35 C46 C42 113.1(6) . . ? C16 C47 C55 121.6(7) . . ? C16 C47 C58 127.4(7) . . ? C55 C47 C58 110.9(6) . . ? C60 C48 C40 122.2(6) . . ? C60 C48 H48A 118.9 . . ? C40 C48 H48A 118.9 . . ? C44 C49 C31 120.5(7) . . ? C44 C49 H49A 119.7 . . ? C31 C49 H49A 119.8 . . ? C55 C50 C64 105.1(5) . . ? C55 C50 C57 105.0(5) . . ? C64 C50 C57 106.6(5) . . ? C55 C50 H50A 113.1 . . ? C64 C50 H50A 113.1 . . ? C57 C50 H50A 113.1 . . ? O6 C51 C28 122.4(7) . . ? O6 C51 C41 117.0(7) . . ? C28 C51 C41 120.5(7) . . ? C43 C52 C64 119.2(6) . . ? C43 C52 C58 127.8(7) . . ? C64 C52 C58 112.9(6) . . ? C32 C53 C61 118.4(6) . . ? C32 C53 C30 120.0(6) . . ? C61 C53 C30 121.5(6) . . ? C22 C54 C28 123.4(7) . . ? C22 C54 H54A 118.3 . . ? C28 C54 H54A 118.3 . . ? C47 C55 C23 119.4(7) . . ? C47 C55 C50 114.5(6) . . ? C23 C55 C50 126.2(7) . . ? C63 C56 C36 118.4(6) . . ? C63 C56 C30 119.7(6) . . ? C36 C56 C30 121.9(6) . . ? C44 C57 C67 121.1(6) . . ? C44 C57 C50 113.4(6) . . ? C67 C57 C50 125.5(6) . . ? C44 C58 C52 108.2(5) . . ? C44 C58 C47 105.0(6) . . ? C52 C58 C47 104.9(5) . . ? C44 C58 H58A 112.7 . . ? C52 C58 H58A 112.7 . . ? C47 C58 H58A 112.7 . . ? C24 C59 C65 119.7(6) . . ? C24 C59 C42 113.5(6) . . ? C65 C59 C42 126.8(6) . . ? C48 C60 C63 118.2(6) . . ? C48 C60 C37 120.8(6) . . ? C63 C60 C37 120.9(6) . . ? C46 C61 C53 120.6(6) . . ? C46 C61 H61A 119.7 . . ? C53 C61 H61A 119.7 . . ? C43 C62 C66 118.6(6) . . ? C43 C62 C37 120.6(6) . . ? C66 C62 C37 120.7(6) . . ? O4 C63 C56 117.6(6) . . ? O4 C63 C60 122.0(6) . . ? C56 C63 C60 120.4(6) . . ? C68 C64 C52 120.7(7) . . ? C68 C64 C50 126.3(6) . . ? C52 C64 C50 112.9(6) . . ? C33 C65 C59 121.1(6) . . ? C33 C65 H65A 119.5 . . ? C59 C65 H65A 119.5 . . ? O5 C66 C68 123.6(6) . . ? O5 C66 C62 115.7(6) . . ? C68 C66 C62 120.7(6) . . ? C29 C67 C57 116.8(6) . . ? C29 C67 H67A 121.6 . . ? C57 C67 H67A 121.6 . . ? C64 C68 C66 119.2(6) . . ? C64 C68 H68A 120.4 . . ? C66 C68 H68A 120.4 . . ? Cl1 C69 Cl2 98.8(9) . . ? Cl1 C69 H69A 112.0 . . ? Cl2 C69 H69A 112.0 . . ? Cl1 C69 H69B 112.0 . . ? Cl2 C69 H69B 112.0 . . ? H69A C69 H69B 109.7 . . ? Cl3 C70 Cl4 111.4(5) . . ? Cl3 C70 H70A 109.4 . . ? Cl4 C70 H70A 109.4 . . ? Cl3 C70 H70B 109.4 . . ? Cl4 C70 H70B 109.4 . . ? H70A C70 H70B 108.0 . . ? Cl5 C71 Cl6 120.3(10) . . ? Cl5 C71 H71A 107.3 . . ? Cl6 C71 H71A 107.3 . . ? Cl5 C71 H71B 107.2 . . ? Cl6 C71 H71B 107.2 . . ? H71A C71 H71B 106.9 . . ? Cl7 C72 Cl8 98.3(9) . . ? Cl7 C72 H72A 112.1 . . ? Cl8 C72 H72A 112.1 . . ? Cl7 C72 H72B 112.1 . . ? Cl8 C72 H72B 112.1 . . ? H72A C72 H72B 109.7 . . ? Cl10 C73 Cl9 117.7(9) . . ? Cl10 C73 H73A 107.9 . . ? Cl9 C73 H73A 107.9 . . ? Cl10 C73 H73B 107.9 . . ? Cl9 C73 H73B 107.9 . . ? H73A C73 H73B 107.2 . . ? Cl11 C74 H74A 119.7 . . ? Cl11 C74 H74B 114.1 . . ? H74A C74 H74B 112.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 C3 C4 C15 0.3(12) . . . . ? C3 C4 C15 C39 -0.3(11) . . . . ? C4 C3 C17 C26 0.2(12) . . . . ? C47 C16 C19 C25 3.0(11) . . . . ? C5 O1 C21 C33 178.6(6) . . . . ? C5 O1 C21 C38 0.7(10) . . . . ? C41 C20 C22 C54 -3.7(10) . . . . ? C41 C20 C22 C12 177.6(6) . . . . ? C1 C12 C22 C54 -114.8(8) . . . . ? C7 C12 C22 C54 125.0(8) . . . . ? C6 C12 C22 C54 6.9(9) . . . . ? C1 C12 C22 C20 63.8(9) . . . . ? C7 C12 C22 C20 -56.4(8) . . . . ? C6 C12 C22 C20 -174.5(6) . . . . ? C16 C19 C25 C23 -3.4(12) . . . . ? C55 C23 C25 C19 2.7(11) . . . . ? C3 C17 C26 C39 -0.6(11) . . . . ? C3 C17 C26 C45 177.1(7) . . . . ? C13 O3 C29 C31 178.6(7) . . . . ? C13 O3 C29 C67 1.2(10) . . . . ? O3 C29 C31 C49 -177.9(6) . . . . ? C67 C29 C31 C49 -0.5(11) . . . . ? O3 C29 C31 C34 3.9(10) . . . . ? C67 C29 C31 C34 -178.6(7) . . . . ? C11 O2 C32 C27 1.5(11) . . . . ? C11 O2 C32 C53 -176.8(7) . . . . ? C35 C27 C32 O2 -176.1(7) . . . . ? C35 C27 C32 C53 2.1(11) . . . . ? O1 C21 C33 C65 -177.7(6) . . . . ? C38 C21 C33 C65 0.3(10) . . . . ? O1 C21 C33 C9 -1.3(10) . . . . ? C38 C21 C33 C9 176.6(7) . . . . ? C41 C9 C33 C65 -31.4(11) . . . . ? C41 C9 C33 C21 152.3(7) . . . . ? C51 C28 C34 C31 80.0(8) . . . . ? C54 C28 C34 C31 -101.1(7) . . . . ? C29 C31 C34 C28 -103.3(8) . . . . ? C49 C31 C34 C28 78.6(8) . . . . ? C32 C27 C35 C46 -0.9(11) . . . . ? C32 C27 C35 C45 172.9(7) . . . . ? C59 C24 C38 C21 1.6(10) . . . . ? C45 C24 C38 C21 -174.9(6) . . . . ? O1 C21 C38 C24 175.3(6) . . . . ? C33 C21 C38 C24 -2.6(10) . . . . ? C17 C26 C39 C15 0.6(10) . . . . ? C45 C26 C39 C15 -177.4(6) . . . . ? C17 C26 C39 C42 179.7(6) . . . . ? C45 C26 C39 C42 1.7(8) . . . . ? C4 C15 C39 C26 -0.1(10) . . . . ? C4 C15 C39 C42 -179.1(6) . . . . ? C56 C36 C40 C48 4.8(10) . . . . ? C56 C36 C40 C18 -176.7(6) . . . . ? C2 C18 C40 C36 178.9(7) . . . . ? C8 C18 C40 C36 60.0(9) . . . . ? C10 C18 C40 C36 -56.6(9) . . . . ? C2 C18 C40 C48 -2.7(10) . . . . ? C8 C18 C40 C48 -121.5(7) . . . . ? C10 C18 C40 C48 121.9(7) . . . . ? C22 C20 C41 C51 1.8(10) . . . . ? C22 C20 C41 C9 -179.1(6) . . . . ? C33 C9 C41 C20 77.0(10) . . . . ? C33 C9 C41 C51 -103.8(8) . . . . ? C26 C39 C42 C46 55.4(7) . . . . ? C15 C39 C42 C46 -125.5(7) . . . . ? C26 C39 C42 C59 -57.4(7) . . . . ? C15 C39 C42 C59 121.6(7) . . . . ? C38 C24 C45 C35 -129.3(7) . . . . ? C59 C24 C45 C35 54.0(8) . . . . ? C38 C24 C45 C26 120.2(7) . . . . ? C59 C24 C45 C26 -56.6(7) . . . . ? C27 C35 C45 C24 130.8(8) . . . . ? C46 C35 C45 C24 -55.1(8) . . . . ? C27 C35 C45 C26 -118.6(8) . . . . ? C46 C35 C45 C26 55.5(8) . . . . ? C17 C26 C45 C24 -122.3(7) . . . . ? C39 C26 C45 C24 55.6(7) . . . . ? C17 C26 C45 C35 125.4(7) . . . . ? C39 C26 C45 C35 -56.7(7) . . . . ? C27 C35 C46 C61 -0.7(11) . . . . ? C45 C35 C46 C61 -175.3(6) . . . . ? C27 C35 C46 C42 175.1(7) . . . . ? C45 C35 C46 C42 0.5(9) . . . . ? C39 C42 C46 C61 119.1(7) . . . . ? C59 C42 C46 C61 -130.3(7) . . . . ? C39 C42 C46 C35 -56.3(8) . . . . ? C59 C42 C46 C35 54.2(8) . . . . ? C19 C16 C47 C55 -2.0(11) . . . . ? C19 C16 C47 C58 -179.9(7) . . . . ? C36 C40 C48 C60 -2.4(10) . . . . ? C18 C40 C48 C60 179.1(6) . . . . ? C57 C44 C49 C31 0.1(10) . . . . ? C58 C44 C49 C31 -178.8(7) . . . . ? C29 C31 C49 C44 0.0(10) . . . . ? C34 C31 C49 C44 178.3(6) . . . . ? C54 C28 C51 O6 179.6(6) . . . . ? C34 C28 C51 O6 -1.4(9) . . . . ? C54 C28 C51 C41 -3.4(9) . . . . ? C34 C28 C51 C41 175.6(6) . . . . ? C20 C41 C51 O6 179.1(6) . . . . ? C9 C41 C51 O6 -0.1(9) . . . . ? C20 C41 C51 C28 1.9(10) . . . . ? C9 C41 C51 C28 -177.3(6) . . . . ? C62 C43 C52 C64 -0.2(10) . . . . ? C62 C43 C52 C58 177.9(6) . . . . ? O2 C32 C53 C61 176.7(6) . . . . ? C27 C32 C53 C61 -1.6(11) . . . . ? O2 C32 C53 C30 0.1(10) . . . . ? C27 C32 C53 C30 -178.1(7) . . . . ? C56 C30 C53 C32 -150.9(7) . . . . ? C56 C30 C53 C61 32.6(10) . . . . ? C20 C22 C54 C28 2.1(9) . . . . ? C12 C22 C54 C28 -179.3(6) . . . . ? C51 C28 C54 C22 1.3(9) . . . . ? C34 C28 C54 C22 -177.7(6) . . . . ? C16 C47 C55 C23 1.5(10) . . . . ? C58 C47 C55 C23 179.7(6) . . . . ? C16 C47 C55 C50 -178.7(7) . . . . ? C58 C47 C55 C50 -0.5(8) . . . . ? C25 C23 C55 C47 -1.7(10) . . . . ? C25 C23 C55 C50 178.5(7) . . . . ? C64 C50 C55 C47 56.8(7) . . . . ? C57 C50 C55 C47 -55.5(7) . . . . ? C64 C50 C55 C23 -123.4(7) . . . . ? C57 C50 C55 C23 124.3(7) . . . . ? C40 C36 C56 C63 -3.0(10) . . . . ? C40 C36 C56 C30 178.5(6) . . . . ? C53 C30 C56 C63 102.2(8) . . . . ? C53 C30 C56 C36 -79.3(9) . . . . ? C49 C44 C57 C67 0.2(11) . . . . ? C58 C44 C57 C67 179.2(6) . . . . ? C49 C44 C57 C50 -178.2(6) . . . . ? C58 C44 C57 C50 0.8(8) . . . . ? C55 C50 C57 C44 55.8(8) . . . . ? C64 C50 C57 C44 -55.3(7) . . . . ? C55 C50 C57 C67 -122.5(7) . . . . ? C64 C50 C57 C67 126.3(7) . . . . ? C49 C44 C58 C52 -126.9(7) . . . . ? C57 C44 C58 C52 54.1(8) . . . . ? C49 C44 C58 C47 121.4(7) . . . . ? C57 C44 C58 C47 -57.5(7) . . . . ? C43 C52 C58 C44 128.0(7) . . . . ? C64 C52 C58 C44 -53.8(7) . . . . ? C43 C52 C58 C47 -120.3(7) . . . . ? C64 C52 C58 C47 57.9(7) . . . . ? C16 C47 C58 C44 -124.6(8) . . . . ? C55 C47 C58 C44 57.4(7) . . . . ? C16 C47 C58 C52 121.5(8) . . . . ? C55 C47 C58 C52 -56.6(7) . . . . ? C38 C24 C59 C65 1.6(10) . . . . ? C45 C24 C59 C65 178.6(6) . . . . ? C38 C24 C59 C42 -176.3(6) . . . . ? C45 C24 C59 C42 0.6(8) . . . . ? C39 C42 C59 C24 56.3(7) . . . . ? C46 C42 C59 C24 -55.6(8) . . . . ? C39 C42 C59 C65 -121.5(7) . . . . ? C46 C42 C59 C65 126.7(7) . . . . ? C40 C48 C60 C63 -1.8(10) . . . . ? C40 C48 C60 C37 174.6(6) . . . . ? C62 C37 C60 C48 101.7(7) . . . . ? C62 C37 C60 C63 -82.0(8) . . . . ? C35 C46 C61 C53 1.2(10) . . . . ? C42 C46 C61 C53 -173.9(7) . . . . ? C32 C53 C61 C46 -0.1(10) . . . . ? C30 C53 C61 C46 176.4(6) . . . . ? C52 C43 C62 C66 0.4(10) . . . . ? C52 C43 C62 C37 -176.5(6) . . . . ? C60 C37 C62 C43 -78.2(8) . . . . ? C60 C37 C62 C66 104.9(7) . . . . ? C36 C56 C63 O4 -179.6(6) . . . . ? C30 C56 C63 O4 -1.1(9) . . . . ? C36 C56 C63 C60 -1.4(10) . . . . ? C30 C56 C63 C60 177.2(6) . . . . ? C48 C60 C63 O4 -178.2(6) . . . . ? C37 C60 C63 O4 5.4(9) . . . . ? C48 C60 C63 C56 3.7(9) . . . . ? C37 C60 C63 C56 -172.7(6) . . . . ? C43 C52 C64 C68 0.1(10) . . . . ? C58 C52 C64 C68 -178.3(6) . . . . ? C43 C52 C64 C50 176.9(6) . . . . ? C58 C52 C64 C50 -1.5(8) . . . . ? C55 C50 C64 C68 120.9(7) . . . . ? C57 C50 C64 C68 -128.0(7) . . . . ? C55 C50 C64 C52 -55.7(7) . . . . ? C57 C50 C64 C52 55.3(7) . . . . ? C21 C33 C65 C59 3.0(10) . . . . ? C9 C33 C65 C59 -173.3(6) . . . . ? C24 C59 C65 C33 -4.0(10) . . . . ? C42 C59 C65 C33 173.6(7) . . . . ? C14 O5 C66 C68 2.3(9) . . . . ? C14 O5 C66 C62 -178.0(6) . . . . ? C43 C62 C66 O5 179.8(5) . . . . ? C37 C62 C66 O5 -3.3(8) . . . . ? C43 C62 C66 C68 -0.5(9) . . . . ? C37 C62 C66 C68 176.4(6) . . . . ? O3 C29 C67 C57 177.9(6) . . . . ? C31 C29 C67 C57 0.7(11) . . . . ? C44 C57 C67 C29 -0.5(10) . . . . ? C50 C57 C67 C29 177.7(7) . . . . ? C52 C64 C68 C66 -0.1(10) . . . . ? C50 C64 C68 C66 -176.5(6) . . . . ? O5 C66 C68 C64 -180.0(6) . . . . ? C62 C66 C68 C64 0.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.089 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.150 data_a _database_code_depnum_ccdc_archive 'CCDC 842677' #TrackingRef '- 5a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H75 Cl12 O6' _chemical_formula_weight 1485.74 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.717(3) _cell_length_b 17.240(3) _cell_length_c 18.924(4) _cell_angle_alpha 109.86(3) _cell_angle_beta 100.40(3) _cell_angle_gamma 107.82(3) _cell_volume 3522.6(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1542 _exptl_absorpt_coefficient_mu 0.524 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8586 _exptl_absorpt_correction_T_max 0.8846 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31373 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12871 _reflns_number_gt 10195 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^+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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12871 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2029 _refine_ls_R_factor_gt 0.1819 _refine_ls_wR_factor_ref 0.4428 _refine_ls_wR_factor_gt 0.4300 _refine_ls_goodness_of_fit_ref 2.396 _refine_ls_restrained_S_all 2.396 _refine_ls_shift/su_max 0.398 _refine_ls_shift/su_mean 0.019 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 0.2482(5) -0.2646(4) 0.2209(3) 0.0552(14) Uani 1 1 d . . . O2 O 0.9877(4) -0.2453(3) 0.3146(3) 0.0480(13) Uani 1 1 d . . . O3 O 0.0631(4) -0.6602(3) -0.0654(3) 0.0455(12) Uani 1 1 d . . . O4 O 0.8672(4) -0.5237(3) 0.1855(3) 0.0410(12) Uani 1 1 d . . . H4 H 0.8477 -0.5659 0.1406 0.062 Uiso 1 1 calc R . . O5 O 0.7849(4) -0.6418(3) 0.0243(3) 0.0428(12) Uani 1 1 d . . . O6 O 0.0928(4) -0.5441(3) 0.0884(3) 0.0476(13) Uani 1 1 d . . . H6 H 0.0669 -0.5862 0.0428 0.071 Uiso 1 1 calc R . . C1 C 0.0505(9) -0.6497(7) 0.3760(6) 0.073(3) Uani 1 1 d . . . H1A H 0.0605 -0.6669 0.4203 0.110 Uiso 1 1 calc R . . H1B H -0.0295 -0.6848 0.3398 0.110 Uiso 1 1 calc R . . H1C H 0.0660 -0.5856 0.3962 0.110 Uiso 1 1 calc R . . C2 C 0.6536(10) -0.7541(5) 0.3734(5) 0.069(3) Uani 1 1 d . . . H2A H 0.5867 -0.7722 0.3275 0.103 Uiso 1 1 calc R . . H2B H 0.6260 -0.7697 0.4138 0.103 Uiso 1 1 calc R . . H2C H 0.7035 -0.7854 0.3567 0.103 Uiso 1 1 calc R . . C3 C 0.7064(7) -0.0607(6) 0.6103(5) 0.054(2) Uani 1 1 d . . . H3A H 0.7329 -0.0027 0.6524 0.065 Uiso 1 1 calc R . . C4 C 0.6683(7) -0.1365(6) 0.6251(5) 0.055(2) Uani 1 1 d . . . H4A H 0.6688 -0.1298 0.6771 0.066 Uiso 1 1 calc R . . C5 C 0.2793(8) -0.1849(6) 0.2075(6) 0.061(2) Uani 1 1 d . . . H5A H 0.2095 -0.1840 0.1764 0.092 Uiso 1 1 calc R . . H5B H 0.3358 -0.1842 0.1784 0.092 Uiso 1 1 calc R . . H5C H 0.3140 -0.1319 0.2585 0.092 Uiso 1 1 calc R . . C6 C 0.1136(7) -0.7680(6) 0.3022(5) 0.058(2) Uani 1 1 d . . . H6A H 0.1247 -0.7839 0.3472 0.086 Uiso 1 1 calc R . . H6B H 0.1691 -0.7790 0.2743 0.086 Uiso 1 1 calc R . . H6C H 0.0340 -0.8048 0.2658 0.086 Uiso 1 1 calc R . . C7 C 0.2589(7) -0.6147(6) 0.3889(5) 0.067(3) Uani 1 1 d . . . H7A H 0.2681 -0.6327 0.4327 0.101 Uiso 1 1 calc R . . H7B H 0.2753 -0.5503 0.4100 0.101 Uiso 1 1 calc R . . H7C H 0.3133 -0.6267 0.3604 0.101 Uiso 1 1 calc R . . C8 C 0.6415(8) -0.6070(6) 0.4375(6) 0.063(3) Uani 1 1 d . . . H8A H 0.5734 -0.6244 0.3927 0.094 Uiso 1 1 calc R . . H8B H 0.6842 -0.5416 0.4615 0.094 Uiso 1 1 calc R . . H8C H 0.6159 -0.6259 0.4770 0.094 Uiso 1 1 calc R . . C9 C 0.1671(6) -0.4189(5) 0.2438(5) 0.059(2) Uani 1 1 d . . . H9A H 0.1079 -0.3969 0.2366 0.071 Uiso 1 1 calc R . . C10 C 0.8287(9) -0.6232(7) 0.4821(6) 0.073(3) Uani 1 1 d . . . H10A H 0.8828 -0.6504 0.4659 0.110 Uiso 1 1 calc R . . H10B H 0.8005 -0.6430 0.5205 0.110 Uiso 1 1 calc R . . H10C H 0.8691 -0.5576 0.5065 0.110 Uiso 1 1 calc R . . C11 C 1.0313(7) -0.1642(6) 0.3046(6) 0.061(2) Uani 1 1 d . . . H11A H 1.1034 -0.1586 0.2913 0.092 Uiso 1 1 calc R . . H11B H 1.0471 -0.1127 0.3540 0.092 Uiso 1 1 calc R . . H11C H 0.9733 -0.1658 0.2618 0.092 Uiso 1 1 calc R . . C12 C 0.1342(6) -0.6681(6) 0.3323(5) 0.049(2) Uani 1 1 d . . . C13 C 0.0803(7) -0.6189(6) -0.1191(5) 0.052(2) Uani 1 1 d . . . H13A H 0.0310 -0.5850 -0.1194 0.078 Uiso 1 1 calc R . . H13B H 0.0595 -0.6655 -0.1726 0.078 Uiso 1 1 calc R . . H13C H 0.1623 -0.5780 -0.1020 0.078 Uiso 1 1 calc R . . C14 C 0.8054(7) -0.6004(5) -0.0268(5) 0.0484(19) Uani 1 1 d . . . H14A H 0.8890 -0.5647 -0.0114 0.073 Uiso 1 1 calc R . . H14B H 0.7630 -0.5611 -0.0235 0.073 Uiso 1 1 calc R . . H14C H 0.7785 -0.6465 -0.0813 0.073 Uiso 1 1 calc R . . C15 C 0.6299(7) -0.2215(6) 0.5651(5) 0.0474(19) Uani 1 1 d . . . H15A H 0.6042 -0.2733 0.5752 0.057 Uiso 1 1 calc R . . C16 C 0.2469(7) -1.0291(5) -0.1315(5) 0.0473(19) Uani 1 1 d . . . H16A H 0.2366 -1.0546 -0.0946 0.057 Uiso 1 1 calc R . . C17 C 0.7063(6) -0.0683(5) 0.5350(5) 0.0473(19) Uani 1 1 d . . . H17A H 0.7326 -0.0163 0.5252 0.057 Uiso 1 1 calc R . . C18 C 0.7228(7) -0.6532(5) 0.4075(4) 0.0449(18) Uani 1 1 d . . . C19 C 0.2207(7) -1.0845(5) -0.2122(5) 0.050(2) Uani 1 1 d . . . H19A H 0.1890 -1.1480 -0.2307 0.060 Uiso 1 1 calc R . . C20 C 0.1441(6) -0.5499(5) 0.2801(5) 0.0431(17) Uani 1 1 d . . . H20A H 0.1672 -0.5088 0.3340 0.052 Uiso 1 1 calc R . . C21 C 0.3324(7) -0.2793(5) 0.2633(4) 0.048(2) Uani 1 1 d . . . C22 C 0.1188(6) -0.6402(5) 0.2631(4) 0.0413(17) Uani 1 1 d . . . C23 C 0.2820(6) -0.9536(5) -0.2406(5) 0.0459(18) Uani 1 1 d . . . H23A H 0.2923 -0.9288 -0.2779 0.055 Uiso 1 1 calc R . . C24 C 0.5291(6) -0.2345(4) 0.3428(4) 0.0391(17) Uani 1 1 d . . . C25 C 0.2411(7) -1.0467(5) -0.2641(5) 0.053(2) Uani 1 1 d . . . H25A H 0.2270 -1.0848 -0.3177 0.063 Uiso 1 1 calc R . . C26 C 0.6674(6) -0.1528(4) 0.4746(5) 0.0404(17) Uani 1 1 d . . . C27 C 0.8248(6) -0.2100(4) 0.3422(4) 0.0397(17) Uani 1 1 d . . . H27A H 0.8491 -0.1586 0.3313 0.048 Uiso 1 1 calc R . . C28 C 0.0676(5) -0.6707(5) 0.1237(4) 0.0384(16) Uani 1 1 d . . . C29 C 0.1261(6) -0.7115(5) -0.0574(4) 0.0431(17) Uani 1 1 d . . . C30 C 0.9240(6) -0.3982(4) 0.3397(5) 0.0406(17) Uani 1 1 d . . . H30A H 0.9645 -0.3910 0.3009 0.049 Uiso 1 1 calc R . . H30B H 0.9846 -0.3735 0.3916 0.049 Uiso 1 1 calc R . . C31 C 0.1075(6) -0.7482(5) -0.0028(5) 0.0396(16) Uani 1 1 d . . . C32 C 0.8863(6) -0.2646(4) 0.3340(4) 0.0385(16) Uani 1 1 d . . . C33 C 0.2947(6) -0.3574(5) 0.2753(4) 0.0430(18) Uani 1 1 d . . . C34 C 0.0198(6) -0.7379(5) 0.0397(4) 0.0375(16) Uani 1 1 d . . . H34A H -0.0356 -0.7214 0.0101 0.045 Uiso 1 1 calc R . . H34B H -0.0251 -0.7971 0.0378 0.045 Uiso 1 1 calc R . . C35 C 0.7269(6) -0.2311(4) 0.3667(4) 0.0402(17) Uani 1 1 d . . . C36 C 0.8248(6) -0.5313(4) 0.3684(5) 0.0401(17) Uani 1 1 d . . . H36A H 0.8455 -0.4904 0.4221 0.048 Uiso 1 1 calc R . . C37 C 0.7609(6) -0.7179(5) 0.1325(4) 0.0405(17) Uani 1 1 d . . . H37A H 0.7514 -0.7763 0.1343 0.049 Uiso 1 1 calc R . . H37B H 0.8324 -0.6968 0.1185 0.049 Uiso 1 1 calc R . . C38 C 0.4504(7) -0.2178(5) 0.2955(4) 0.0425(17) Uani 1 1 d . . . H38A H 0.4749 -0.1662 0.2849 0.051 Uiso 1 1 calc R . . C39 C 0.6296(6) -0.2297(5) 0.4876(5) 0.0405(17) Uani 1 1 d . . . C40 C 0.7634(6) -0.6205(5) 0.3469(4) 0.0349(15) Uani 1 1 d . . . C41 C 0.1376(6) -0.5175(5) 0.2243(5) 0.0434(18) Uani 1 1 d . . . C42 C 0.5897(6) -0.3158(5) 0.4142(5) 0.0444(19) Uani 1 1 d . . . H42A H 0.5631 -0.3707 0.4245 0.053 Uiso 1 1 calc R . . C43 C 0.5433(6) -0.7867(4) 0.0580(4) 0.0368(16) Uani 1 1 d . . . H43A H 0.5314 -0.8120 0.0948 0.044 Uiso 1 1 calc R . . C44 C 0.2496(6) -0.8109(4) -0.0292(4) 0.0351(15) Uani 1 1 d . . . C45 C 0.6563(6) -0.1736(5) 0.3876(5) 0.0430(18) Uani 1 1 d . . . H45A H 0.6827 -0.1185 0.3776 0.052 Uiso 1 1 calc R . . C46 C 0.6902(6) -0.3077(4) 0.3818(4) 0.0346(15) Uani 1 1 d . . . C47 C 0.2879(6) -0.9370(5) -0.1070(4) 0.0405(17) Uani 1 1 d . . . C48 C 0.7416(6) -0.6801(4) 0.2694(4) 0.0373(16) Uani 1 1 d . . . H48A H 0.7016 -0.7427 0.2539 0.045 Uiso 1 1 calc R . . C49 C 0.1710(6) -0.7984(4) 0.0105(4) 0.0374(16) Uani 1 1 d . . . H49A H 0.1597 -0.8240 0.0472 0.045 Uiso 1 1 calc R . . C50 C 0.3544(6) -0.7969(4) -0.1230(4) 0.0363(15) Uani 1 1 d . . . H50A H 0.3666 -0.7705 -0.1619 0.044 Uiso 1 1 calc R . . C51 C 0.1003(6) -0.5786(5) 0.1445(5) 0.0404(17) Uani 1 1 d . . . C52 C 0.4483(6) -0.8046(5) -0.0031(4) 0.0375(16) Uani 1 1 d . . . C53 C 0.8513(6) -0.3415(4) 0.3470(4) 0.0362(15) Uani 1 1 d . . . C54 C 0.0795(6) -0.6980(5) 0.1854(4) 0.0401(17) Uani 1 1 d . . . H54A H 0.0592 -0.7601 0.1721 0.048 Uiso 1 1 calc R . . C55 C 0.3073(6) -0.8978(5) -0.1600(4) 0.0385(16) Uani 1 1 d . . . C56 C 0.8585(6) -0.4976(5) 0.3149(4) 0.0364(16) Uani 1 1 d . . . C57 C 0.2674(6) -0.7739(5) -0.0830(4) 0.0356(15) Uani 1 1 d . . . C58 C 0.3220(6) -0.8642(4) -0.0221(4) 0.0377(16) Uani 1 1 d . . . H58A H 0.3097 -0.8902 0.0171 0.045 Uiso 1 1 calc R . . C59 C 0.4935(6) -0.3113(4) 0.3567(4) 0.0360(16) Uani 1 1 d . . . C60 C 0.7765(6) -0.6511(4) 0.2139(4) 0.0328(15) Uani 1 1 d . . . C61 C 0.7513(6) -0.3628(4) 0.3713(4) 0.0354(15) Uani 1 1 d . . . H61A H 0.7258 -0.4154 0.3804 0.043 Uiso 1 1 calc R . . C62 C 0.6555(6) -0.7326(4) 0.0668(4) 0.0330(15) Uani 1 1 d . . . C63 C 0.8328(6) -0.5581(5) 0.2371(4) 0.0363(16) Uani 1 1 d . . . C64 C 0.4658(6) -0.7671(4) -0.0571(4) 0.0354(16) Uani 1 1 d . . . C65 C 0.3768(6) -0.3737(4) 0.3207(5) 0.0410(17) Uani 1 1 d . . . H65A H 0.3539 -0.4278 0.3276 0.049 Uiso 1 1 calc R . . C66 C 0.6718(6) -0.6949(4) 0.0121(4) 0.0356(16) Uani 1 1 d . . . C67 C 0.2060(6) -0.7224(4) -0.0984(4) 0.0364(16) Uani 1 1 d . . . H67A H 0.2182 -0.6965 -0.1348 0.044 Uiso 1 1 calc R . . C68 C 0.5775(6) -0.7122(5) -0.0498(4) 0.0378(16) Uani 1 1 d . . . H68A H 0.5889 -0.6869 -0.0867 0.045 Uiso 1 1 calc R . . C69 C 0.4287(11) -0.0247(9) 0.0833(12) 0.260(16) Uani 1 1 d . . . H69A H 0.4522 0.0240 0.0656 0.312 Uiso 1 1 calc R . . H69B H 0.4713 -0.0638 0.0680 0.312 Uiso 1 1 calc R . . C70 C 0.5980(9) 0.1254(6) 0.5112(7) 0.075(3) Uani 1 1 d . . . H70A H 0.5657 0.1682 0.5028 0.090 Uiso 1 1 calc R . . H70B H 0.5546 0.0969 0.5404 0.090 Uiso 1 1 calc R . . C71 C 0.420(2) 0.3427(8) 0.1925(10) 0.211(12) Uani 1 1 d . . . H71A H 0.4754 0.3419 0.1622 0.253 Uiso 1 1 calc R . . H71B H 0.3490 0.3408 0.1585 0.253 Uiso 1 1 calc R . . C72 C -0.0197(11) -0.9907(7) -0.1836(12) 0.168(9) Uani 1 1 d . . . H72A H 0.0569 -0.9429 -0.1714 0.202 Uiso 1 1 calc R . . H72B H -0.0397 -1.0403 -0.2361 0.202 Uiso 1 1 calc R . . C73 C 0.5256(12) -0.4500(9) 0.1357(10) 0.130(5) Uani 1 1 d . . . H73A H 0.5453 -0.4059 0.1127 0.156 Uiso 1 1 calc R . . H73B H 0.5345 -0.4161 0.1919 0.156 Uiso 1 1 calc R . . C74 C 1.0117(11) 0.0690(19) 0.3918(19) 0.37(2) Uani 1 1 d . . . H74A H 0.9690 0.0353 0.3343 0.440 Uiso 1 1 d R . . H74B H 1.0973 0.0928 0.4032 0.440 Uiso 1 1 d R . . Cl1 Cl 0.2911(6) -0.0803(5) 0.0509(3) 0.198(3) Uani 1 1 d . . . Cl2 Cl 0.4521(3) 0.0268(3) 0.2079(2) 0.1416(17) Uani 1 1 d . . . Cl3 Cl 0.7455(3) 0.18397(18) 0.56799(18) 0.0849(8) Uani 1 1 d . . . Cl4 Cl 0.5787(2) 0.04214(17) 0.41868(15) 0.0719(7) Uani 1 1 d . . . Cl5 Cl 0.4755(5) 0.4370(2) 0.2674(2) 0.1448(18) Uani 1 1 d . . . Cl6 Cl 0.3797(2) 0.24267(16) 0.20484(16) 0.0743(7) Uani 1 1 d . . . Cl7 Cl -0.1229(5) -0.9516(4) -0.1776(3) 0.173(2) Uani 1 1 d . . . Cl8 Cl -0.0253(4) -1.0353(3) -0.0960(3) 0.1391(16) Uani 1 1 d . . . Cl9 Cl 0.3837(3) -0.5197(4) 0.0886(4) 0.236(4) Uani 1 1 d . . . Cl10 Cl 0.6213(4) -0.4949(4) 0.1334(4) 0.172(2) Uani 1 1 d . . . Cl11 Cl 0.9696(11) 0.0317(6) 0.4511(6) 0.318(5) Uani 1 1 d . . . Cl12 Cl 0.9434(7) 0.1764(8) 0.4698(5) 0.325(6) 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 0.058(3) 0.065(4) 0.048(3) 0.022(3) 0.007(3) 0.038(3) O2 0.043(3) 0.041(3) 0.053(3) 0.018(3) 0.022(3) 0.007(2) O3 0.050(3) 0.050(3) 0.044(3) 0.021(3) 0.013(3) 0.028(3) O4 0.041(3) 0.039(3) 0.040(3) 0.018(2) 0.012(2) 0.011(2) O5 0.038(3) 0.048(3) 0.039(3) 0.017(2) 0.013(2) 0.014(2) O6 0.049(3) 0.046(3) 0.048(3) 0.018(3) 0.011(3) 0.024(3) C1 0.081(7) 0.092(7) 0.053(6) 0.031(6) 0.031(5) 0.036(6) C2 0.115(8) 0.044(5) 0.050(6) 0.025(4) 0.035(6) 0.024(5) C3 0.057(5) 0.048(5) 0.052(5) 0.019(4) 0.012(4) 0.019(4) C4 0.053(5) 0.070(6) 0.048(5) 0.028(5) 0.020(4) 0.028(4) C5 0.077(6) 0.060(5) 0.059(6) 0.028(5) 0.015(5) 0.043(5) C6 0.043(5) 0.070(6) 0.055(5) 0.026(5) 0.010(4) 0.020(4) C7 0.052(5) 0.068(6) 0.057(6) 0.016(5) -0.015(4) 0.023(5) C8 0.066(6) 0.065(5) 0.084(7) 0.040(5) 0.051(6) 0.036(5) C9 0.029(4) 0.040(4) 0.078(6) -0.001(4) -0.001(4) 0.017(3) C10 0.083(7) 0.087(7) 0.052(6) 0.040(5) 0.003(5) 0.034(6) C11 0.049(5) 0.062(5) 0.064(6) 0.029(5) 0.027(5) 0.003(4) C12 0.037(4) 0.073(6) 0.035(4) 0.018(4) 0.005(3) 0.027(4) C13 0.063(5) 0.062(5) 0.041(5) 0.024(4) 0.013(4) 0.037(4) C14 0.054(5) 0.057(5) 0.039(5) 0.029(4) 0.015(4) 0.018(4) C15 0.043(4) 0.068(5) 0.053(5) 0.040(4) 0.018(4) 0.031(4) C16 0.044(4) 0.040(4) 0.046(5) 0.011(4) 0.005(4) 0.015(3) C17 0.039(4) 0.040(4) 0.054(5) 0.019(4) 0.007(4) 0.010(3) C18 0.063(5) 0.050(4) 0.036(4) 0.024(4) 0.024(4) 0.030(4) C19 0.047(5) 0.032(4) 0.054(5) 0.008(4) 0.000(4) 0.015(3) C20 0.032(4) 0.051(4) 0.038(4) 0.010(4) 0.005(3) 0.019(3) C21 0.067(5) 0.058(5) 0.028(4) 0.013(4) 0.013(4) 0.047(4) C22 0.022(3) 0.050(4) 0.042(5) 0.010(4) 0.008(3) 0.013(3) C23 0.042(4) 0.047(4) 0.039(4) 0.011(4) 0.005(4) 0.019(4) C24 0.043(4) 0.032(4) 0.044(4) 0.015(3) 0.017(4) 0.016(3) C25 0.054(5) 0.045(4) 0.037(5) -0.004(4) 0.002(4) 0.023(4) C26 0.035(4) 0.032(4) 0.053(5) 0.024(4) 0.007(3) 0.009(3) C27 0.050(4) 0.032(4) 0.039(4) 0.023(3) 0.017(4) 0.008(3) C28 0.022(3) 0.042(4) 0.046(5) 0.013(3) 0.009(3) 0.013(3) C29 0.037(4) 0.045(4) 0.040(4) 0.010(3) 0.002(3) 0.020(3) C30 0.035(4) 0.034(4) 0.039(4) 0.006(3) 0.012(3) 0.007(3) C31 0.030(4) 0.043(4) 0.045(4) 0.019(3) 0.011(3) 0.015(3) C32 0.035(4) 0.034(4) 0.039(4) 0.012(3) 0.007(3) 0.010(3) C33 0.036(4) 0.041(4) 0.037(4) -0.003(3) 0.008(3) 0.019(3) C34 0.032(4) 0.039(4) 0.037(4) 0.014(3) 0.007(3) 0.013(3) C35 0.038(4) 0.026(3) 0.042(4) 0.010(3) 0.003(3) 0.004(3) C36 0.035(4) 0.029(3) 0.045(5) 0.006(3) 0.013(3) 0.009(3) C37 0.046(4) 0.039(4) 0.045(5) 0.019(3) 0.018(4) 0.025(3) C38 0.048(4) 0.037(4) 0.045(5) 0.014(3) 0.011(4) 0.026(3) C39 0.038(4) 0.044(4) 0.047(5) 0.023(4) 0.012(4) 0.021(3) C40 0.030(3) 0.044(4) 0.038(4) 0.019(3) 0.011(3) 0.021(3) C41 0.022(3) 0.047(4) 0.049(5) 0.011(4) 0.001(3) 0.016(3) C42 0.030(4) 0.033(4) 0.081(6) 0.035(4) 0.017(4) 0.014(3) C43 0.043(4) 0.041(4) 0.032(4) 0.018(3) 0.015(3) 0.020(3) C44 0.038(4) 0.030(3) 0.036(4) 0.014(3) 0.010(3) 0.015(3) C45 0.041(4) 0.044(4) 0.054(5) 0.029(4) 0.021(4) 0.018(3) C46 0.029(3) 0.027(3) 0.035(4) 0.009(3) 0.005(3) 0.003(3) C47 0.050(4) 0.036(4) 0.041(4) 0.017(3) 0.018(4) 0.021(3) C48 0.039(4) 0.032(3) 0.047(5) 0.017(3) 0.014(3) 0.020(3) C49 0.031(4) 0.029(3) 0.044(4) 0.014(3) 0.008(3) 0.005(3) C50 0.045(4) 0.038(4) 0.028(4) 0.015(3) 0.012(3) 0.017(3) C51 0.031(4) 0.054(4) 0.043(5) 0.021(4) 0.018(3) 0.021(3) C52 0.032(4) 0.039(4) 0.043(4) 0.015(3) 0.011(3) 0.018(3) C53 0.026(3) 0.032(3) 0.036(4) 0.009(3) 0.001(3) 0.004(3) C54 0.028(4) 0.040(4) 0.046(5) 0.012(4) 0.015(3) 0.012(3) C55 0.035(4) 0.041(4) 0.039(4) 0.014(3) 0.010(3) 0.019(3) C56 0.030(4) 0.038(4) 0.038(4) 0.016(3) 0.007(3) 0.013(3) C57 0.027(3) 0.041(4) 0.039(4) 0.017(3) 0.009(3) 0.015(3) C58 0.042(4) 0.033(4) 0.047(4) 0.024(3) 0.014(4) 0.017(3) C59 0.030(4) 0.039(4) 0.039(4) 0.016(3) 0.008(3) 0.015(3) C60 0.032(3) 0.036(4) 0.034(4) 0.013(3) 0.005(3) 0.021(3) C61 0.040(4) 0.026(3) 0.034(4) 0.012(3) 0.008(3) 0.008(3) C62 0.035(4) 0.039(4) 0.027(4) 0.013(3) 0.009(3) 0.018(3) C63 0.032(4) 0.040(4) 0.043(4) 0.023(3) 0.011(3) 0.016(3) C64 0.036(4) 0.035(4) 0.041(4) 0.018(3) 0.014(3) 0.019(3) C65 0.032(4) 0.028(3) 0.063(5) 0.018(3) 0.010(4) 0.014(3) C66 0.031(4) 0.034(3) 0.039(4) 0.010(3) 0.016(3) 0.013(3) C67 0.039(4) 0.036(4) 0.041(4) 0.021(3) 0.014(3) 0.019(3) C68 0.035(4) 0.049(4) 0.031(4) 0.021(3) 0.010(3) 0.013(3) C69 0.062(7) 0.114(10) 0.35(3) -0.170(14) 0.055(12) 0.013(7) C70 0.072(7) 0.053(5) 0.100(9) 0.029(6) 0.041(6) 0.021(5) C71 0.44(4) 0.057(8) 0.136(14) 0.056(9) 0.13(2) 0.069(15) C72 0.070(8) 0.033(5) 0.29(2) -0.015(9) -0.003(11) 0.013(5) C73 0.113(11) 0.099(10) 0.154(15) 0.055(10) -0.004(10) 0.036(9) C74 0.046(7) 0.60(5) 0.77(6) 0.67(5) 0.121(18) 0.117(15) Cl1 0.227(7) 0.239(6) 0.130(4) 0.054(4) 0.038(4) 0.130(6) Cl2 0.108(3) 0.124(3) 0.117(3) -0.020(2) -0.006(2) 0.053(2) Cl3 0.0870(19) 0.0723(16) 0.080(2) 0.0224(15) 0.0166(16) 0.0276(15) Cl4 0.0845(17) 0.0683(15) 0.0656(16) 0.0289(13) 0.0207(14) 0.0349(13) Cl5 0.228(5) 0.0664(19) 0.090(3) 0.0174(19) 0.043(3) 0.016(3) Cl6 0.0880(18) 0.0642(15) 0.0755(18) 0.0324(13) 0.0318(15) 0.0298(13) Cl7 0.157(4) 0.200(5) 0.158(5) 0.070(4) 0.016(4) 0.092(4) Cl8 0.165(4) 0.108(3) 0.155(4) 0.073(3) 0.061(3) 0.041(3) Cl9 0.068(2) 0.287(7) 0.376(9) 0.282(7) -0.031(3) -0.004(3) Cl10 0.153(4) 0.249(5) 0.297(7) 0.215(5) 0.159(5) 0.153(4) Cl11 0.404(14) 0.253(9) 0.255(10) 0.076(8) 0.048(10) 0.145(10) Cl12 0.220(8) 0.441(14) 0.171(6) -0.025(7) -0.029(6) 0.176(9) _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 C21 1.361(9) . ? O1 C5 1.431(9) . ? O2 C32 1.378(8) . ? O2 C11 1.429(9) . ? O3 C29 1.388(8) . ? O3 C13 1.438(9) . ? O4 C63 1.374(8) . ? O4 H4 0.8400 . ? O5 C66 1.376(8) . ? O5 C14 1.400(8) . ? O6 C51 1.385(9) . ? O6 H6 0.8400 . ? C1 C12 1.504(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C18 1.520(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C17 1.385(11) . ? C3 C4 1.391(11) . ? C3 H3A 0.9500 . ? C4 C15 1.381(11) . ? C4 H4A 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C12 1.538(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.528(11) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C18 1.560(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C33 1.510(10) . ? C9 C41 1.515(10) . ? C9 H9A 0.9500 . ? C10 C18 1.570(12) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C22 1.540(11) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C39 1.422(10) . ? C15 H15A 0.9500 . ? C16 C47 1.384(10) . ? C16 C19 1.410(11) . ? C16 H16A 0.9500 . ? C17 C26 1.376(10) . ? C17 H17A 0.9500 . ? C18 C40 1.542(9) . ? C19 C25 1.371(11) . ? C19 H19A 0.9500 . ? C20 C41 1.355(10) . ? C20 C22 1.395(10) . ? C20 H20A 0.9500 . ? C21 C33 1.394(11) . ? C21 C38 1.416(11) . ? C22 C54 1.357(10) . ? C23 C25 1.401(11) . ? C23 C55 1.411(10) . ? C23 H23A 0.9500 . ? C24 C38 1.384(10) . ? C24 C59 1.393(9) . ? C24 C45 1.516(10) . ? C25 H25A 0.9500 . ? C26 C39 1.388(9) . ? C26 C45 1.531(11) . ? C27 C32 1.385(9) . ? C27 C35 1.394(9) . ? C27 H27A 0.9500 . ? C28 C51 1.400(10) . ? C28 C54 1.400(10) . ? C28 C34 1.487(10) . ? C29 C31 1.401(10) . ? C29 C67 1.406(9) . ? C30 C56 1.513(9) . ? C30 C53 1.528(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C49 1.402(9) . ? C31 C34 1.507(9) . ? C32 C53 1.385(9) . ? C33 C65 1.389(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C46 1.403(9) . ? C35 C45 1.535(9) . ? C36 C40 1.365(9) . ? C36 C56 1.397(10) . ? C36 H36A 0.9500 . ? C37 C60 1.510(9) . ? C37 C62 1.543(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9500 . ? C39 C42 1.508(10) . ? C40 C48 1.392(10) . ? C41 C51 1.403(10) . ? C42 C46 1.504(9) . ? C42 C59 1.524(10) . ? C42 H42A 1.0000 . ? C43 C62 1.390(9) . ? C43 C52 1.384(10) . ? C43 H43A 0.9500 . ? C44 C49 1.380(9) . ? C44 C57 1.390(9) . ? C44 C58 1.507(8) . ? C45 H45A 1.0000 . ? C46 C61 1.388(9) . ? C47 C55 1.404(10) . ? C47 C58 1.546(10) . ? C48 C60 1.394(9) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 C55 1.503(9) . ? C50 C64 1.519(10) . ? C50 C57 1.525(9) . ? C50 H50A 1.0000 . ? C52 C64 1.399(9) . ? C52 C58 1.515(9) . ? C53 C61 1.415(9) . ? C54 H54A 0.9500 . ? C56 C63 1.390(10) . ? C57 C67 1.413(9) . ? C58 H58A 1.0000 . ? C59 C65 1.408(10) . ? C60 C63 1.408(9) . ? C61 H61A 0.9500 . ? C62 C66 1.409(9) . ? C64 C68 1.396(9) . ? C65 H65A 0.9500 . ? C66 C68 1.392(10) . ? C67 H67A 0.9500 . ? C68 H68A 0.9500 . ? C69 Cl1 1.595(13) . ? C69 Cl2 2.14(2) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 Cl3 1.752(11) . ? C70 Cl4 1.763(10) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 Cl5 1.588(15) . ? C71 Cl6 1.751(12) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 Cl7 1.653(12) . ? C72 Cl8 2.05(2) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 Cl10 1.629(14) . ? C73 Cl9 1.691(15) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 Cl11 1.567(19) . ? C74 H74A 0.9900 . ? C74 H74B 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 C21 O1 C5 119.3(7) . . ? C32 O2 C11 117.8(6) . . ? C29 O3 C13 117.6(6) . . ? C63 O4 H4 109.5 . . ? C66 O5 C14 118.0(6) . . ? C51 O6 H6 109.5 . . ? C12 C1 H1A 109.5 . . ? C12 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C12 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C18 C2 H2A 109.5 . . ? C18 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C18 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C17 C3 C4 121.0(8) . . ? C17 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C15 C4 C3 120.7(8) . . ? C15 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? O1 C5 H5A 109.5 . . ? O1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C12 C6 H6A 109.5 . . ? C12 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C12 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 H7A 109.5 . . ? C12 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C12 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C18 C8 H8A 109.5 . . ? C18 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C18 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C33 C9 C41 117.1(6) . . ? C33 C9 H9A 121.5 . . ? C41 C9 H9A 121.5 . . ? C18 C10 H10A 109.5 . . ? C18 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C18 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 C7 109.6(7) . . ? C1 C12 C6 110.2(7) . . ? C7 C12 C6 106.9(7) . . ? C1 C12 C22 109.2(6) . . ? C7 C12 C22 109.9(7) . . ? C6 C12 C22 111.0(7) . . ? O3 C13 H13A 109.5 . . ? O3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.4 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 C39 118.5(7) . . ? C4 C15 H15A 120.7 . . ? C39 C15 H15A 120.7 . . ? C47 C16 C19 118.7(8) . . ? C47 C16 H16A 120.6 . . ? C19 C16 H16A 120.7 . . ? C26 C17 C3 118.7(7) . . ? C26 C17 H17A 120.6 . . ? C3 C17 H17A 120.6 . . ? C2 C18 C40 113.7(6) . . ? C2 C18 C8 107.2(7) . . ? C40 C18 C8 108.1(6) . . ? C2 C18 C10 109.9(7) . . ? C40 C18 C10 111.0(7) . . ? C8 C18 C10 106.7(7) . . ? C25 C19 C16 120.0(7) . . ? C25 C19 H19A 120.0 . . ? C16 C19 H19A 120.0 . . ? C41 C20 C22 123.9(7) . . ? C41 C20 H20A 118.1 . . ? C22 C20 H20A 118.1 . . ? O1 C21 C33 115.8(7) . . ? O1 C21 C38 122.1(7) . . ? C33 C21 C38 122.1(7) . . ? C54 C22 C20 116.5(7) . . ? C54 C22 C12 124.6(7) . . ? C20 C22 C12 118.9(7) . . ? C25 C23 C55 118.1(7) . . ? C25 C23 H23A 120.9 . . ? C55 C23 H23A 120.9 . . ? C38 C24 C59 120.7(7) . . ? C38 C24 C45 126.4(6) . . ? C59 C24 C45 112.8(6) . . ? C19 C25 C23 122.1(7) . . ? C19 C25 H25A 118.9 . . ? C23 C25 H25A 118.9 . . ? C17 C26 C39 121.7(7) . . ? C17 C26 C45 125.6(6) . . ? C39 C26 C45 112.7(6) . . ? C32 C27 C35 119.3(6) . . ? C32 C27 H27A 120.3 . . ? C35 C27 H27A 120.3 . . ? C51 C28 C54 117.5(7) . . ? C51 C28 C34 121.9(7) . . ? C54 C28 C34 120.6(6) . . ? O3 C29 C31 114.9(6) . . ? O3 C29 C67 122.4(7) . . ? C31 C29 C67 122.6(6) . . ? C56 C30 C53 116.4(6) . . ? C56 C30 H30A 108.2 . . ? C53 C30 H30A 108.2 . . ? C56 C30 H30B 108.2 . . ? C53 C30 H30B 108.2 . . ? H30A C30 H30B 107.4 . . ? C29 C31 C49 118.3(6) . . ? C29 C31 C34 122.4(6) . . ? C49 C31 C34 119.3(6) . . ? O2 C32 C27 122.7(6) . . ? O2 C32 C53 115.4(6) . . ? C27 C32 C53 121.9(6) . . ? C65 C33 C21 117.9(7) . . ? C65 C33 C9 121.3(7) . . ? C21 C33 C9 120.6(7) . . ? C28 C34 C31 116.2(6) . . ? C28 C34 H34A 108.2 . . ? C31 C34 H34A 108.2 . . ? C28 C34 H34B 108.2 . . ? C31 C34 H34B 108.2 . . ? H34A C34 H34B 107.4 . . ? C27 C35 C46 120.3(6) . . ? C27 C35 C45 126.6(6) . . ? C46 C35 C45 112.9(6) . . ? C40 C36 C56 122.9(7) . . ? C40 C36 H36A 118.5 . . ? C56 C36 H36A 118.5 . . ? C60 C37 C62 114.0(5) . . ? C60 C37 H37A 108.7 . . ? C62 C37 H37A 108.7 . . ? C60 C37 H37B 108.7 . . ? C62 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C24 C38 C21 118.4(7) . . ? C24 C38 H38A 120.8 . . ? C21 C38 H38A 120.8 . . ? C26 C39 C15 119.3(7) . . ? C26 C39 C42 113.9(7) . . ? C15 C39 C42 126.8(7) . . ? C36 C40 C48 117.7(6) . . ? C36 C40 C18 120.6(6) . . ? C48 C40 C18 121.7(6) . . ? C20 C41 C51 118.1(7) . . ? C20 C41 C9 123.2(7) . . ? C51 C41 C9 118.7(7) . . ? C39 C42 C46 105.9(5) . . ? C39 C42 C59 104.0(5) . . ? C46 C42 C59 107.2(6) . . ? C39 C42 H42A 113.0 . . ? C46 C42 H42A 113.0 . . ? C59 C42 H42A 113.0 . . ? C62 C43 C52 121.5(6) . . ? C62 C43 H43A 119.2 . . ? C52 C43 H43A 119.2 . . ? C49 C44 C57 120.6(6) . . ? C49 C44 C58 126.5(6) . . ? C57 C44 C58 112.9(6) . . ? C24 C45 C35 107.0(6) . . ? C24 C45 C26 104.6(5) . . ? C35 C45 C26 104.6(6) . . ? C24 C45 H45A 113.3 . . ? C35 C45 H45A 113.3 . . ? C26 C45 H45A 113.3 . . ? C61 C46 C35 119.5(6) . . ? C61 C46 C42 127.2(6) . . ? C35 C46 C42 113.1(6) . . ? C16 C47 C55 121.6(7) . . ? C16 C47 C58 127.4(7) . . ? C55 C47 C58 110.9(6) . . ? C60 C48 C40 122.2(6) . . ? C60 C48 H48A 118.9 . . ? C40 C48 H48A 118.9 . . ? C44 C49 C31 120.5(7) . . ? C44 C49 H49A 119.7 . . ? C31 C49 H49A 119.8 . . ? C55 C50 C64 105.1(5) . . ? C55 C50 C57 105.0(5) . . ? C64 C50 C57 106.6(5) . . ? C55 C50 H50A 113.1 . . ? C64 C50 H50A 113.1 . . ? C57 C50 H50A 113.1 . . ? O6 C51 C28 122.4(7) . . ? O6 C51 C41 117.0(7) . . ? C28 C51 C41 120.5(7) . . ? C43 C52 C64 119.2(6) . . ? C43 C52 C58 127.8(7) . . ? C64 C52 C58 112.9(6) . . ? C32 C53 C61 118.4(6) . . ? C32 C53 C30 120.0(6) . . ? C61 C53 C30 121.5(6) . . ? C22 C54 C28 123.4(7) . . ? C22 C54 H54A 118.3 . . ? C28 C54 H54A 118.3 . . ? C47 C55 C23 119.4(7) . . ? C47 C55 C50 114.5(6) . . ? C23 C55 C50 126.2(7) . . ? C63 C56 C36 118.4(6) . . ? C63 C56 C30 119.7(6) . . ? C36 C56 C30 121.9(6) . . ? C44 C57 C67 121.1(6) . . ? C44 C57 C50 113.4(6) . . ? C67 C57 C50 125.5(6) . . ? C44 C58 C52 108.2(5) . . ? C44 C58 C47 105.0(6) . . ? C52 C58 C47 104.9(5) . . ? C44 C58 H58A 112.7 . . ? C52 C58 H58A 112.7 . . ? C47 C58 H58A 112.7 . . ? C24 C59 C65 119.7(6) . . ? C24 C59 C42 113.5(6) . . ? C65 C59 C42 126.8(6) . . ? C48 C60 C63 118.2(6) . . ? C48 C60 C37 120.8(6) . . ? C63 C60 C37 120.9(6) . . ? C46 C61 C53 120.6(6) . . ? C46 C61 H61A 119.7 . . ? C53 C61 H61A 119.7 . . ? C43 C62 C66 118.6(6) . . ? C43 C62 C37 120.6(6) . . ? C66 C62 C37 120.7(6) . . ? O4 C63 C56 117.6(6) . . ? O4 C63 C60 122.0(6) . . ? C56 C63 C60 120.4(6) . . ? C68 C64 C52 120.7(7) . . ? C68 C64 C50 126.3(6) . . ? C52 C64 C50 112.9(6) . . ? C33 C65 C59 121.1(6) . . ? C33 C65 H65A 119.5 . . ? C59 C65 H65A 119.5 . . ? O5 C66 C68 123.6(6) . . ? O5 C66 C62 115.7(6) . . ? C68 C66 C62 120.7(6) . . ? C29 C67 C57 116.8(6) . . ? C29 C67 H67A 121.6 . . ? C57 C67 H67A 121.6 . . ? C64 C68 C66 119.2(6) . . ? C64 C68 H68A 120.4 . . ? C66 C68 H68A 120.4 . . ? Cl1 C69 Cl2 98.8(9) . . ? Cl1 C69 H69A 112.0 . . ? Cl2 C69 H69A 112.0 . . ? Cl1 C69 H69B 112.0 . . ? Cl2 C69 H69B 112.0 . . ? H69A C69 H69B 109.7 . . ? Cl3 C70 Cl4 111.4(5) . . ? Cl3 C70 H70A 109.4 . . ? Cl4 C70 H70A 109.4 . . ? Cl3 C70 H70B 109.4 . . ? Cl4 C70 H70B 109.4 . . ? H70A C70 H70B 108.0 . . ? Cl5 C71 Cl6 120.3(10) . . ? Cl5 C71 H71A 107.3 . . ? Cl6 C71 H71A 107.3 . . ? Cl5 C71 H71B 107.2 . . ? Cl6 C71 H71B 107.2 . . ? H71A C71 H71B 106.9 . . ? Cl7 C72 Cl8 98.3(9) . . ? Cl7 C72 H72A 112.1 . . ? Cl8 C72 H72A 112.1 . . ? Cl7 C72 H72B 112.1 . . ? Cl8 C72 H72B 112.1 . . ? H72A C72 H72B 109.7 . . ? Cl10 C73 Cl9 117.7(9) . . ? Cl10 C73 H73A 107.9 . . ? Cl9 C73 H73A 107.9 . . ? Cl10 C73 H73B 107.9 . . ? Cl9 C73 H73B 107.9 . . ? H73A C73 H73B 107.2 . . ? Cl11 C74 H74A 119.7 . . ? Cl11 C74 H74B 114.1 . . ? H74A C74 H74B 112.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 C3 C4 C15 0.3(12) . . . . ? C3 C4 C15 C39 -0.3(11) . . . . ? C4 C3 C17 C26 0.2(12) . . . . ? C47 C16 C19 C25 3.0(11) . . . . ? C5 O1 C21 C33 178.6(6) . . . . ? C5 O1 C21 C38 0.7(10) . . . . ? C41 C20 C22 C54 -3.7(10) . . . . ? C41 C20 C22 C12 177.6(6) . . . . ? C1 C12 C22 C54 -114.8(8) . . . . ? C7 C12 C22 C54 125.0(8) . . . . ? C6 C12 C22 C54 6.9(9) . . . . ? C1 C12 C22 C20 63.8(9) . . . . ? C7 C12 C22 C20 -56.4(8) . . . . ? C6 C12 C22 C20 -174.5(6) . . . . ? C16 C19 C25 C23 -3.4(12) . . . . ? C55 C23 C25 C19 2.7(11) . . . . ? C3 C17 C26 C39 -0.6(11) . . . . ? C3 C17 C26 C45 177.1(7) . . . . ? C13 O3 C29 C31 178.6(7) . . . . ? C13 O3 C29 C67 1.2(10) . . . . ? O3 C29 C31 C49 -177.9(6) . . . . ? C67 C29 C31 C49 -0.5(11) . . . . ? O3 C29 C31 C34 3.9(10) . . . . ? C67 C29 C31 C34 -178.6(7) . . . . ? C11 O2 C32 C27 1.5(11) . . . . ? C11 O2 C32 C53 -176.8(7) . . . . ? C35 C27 C32 O2 -176.1(7) . . . . ? C35 C27 C32 C53 2.1(11) . . . . ? O1 C21 C33 C65 -177.7(6) . . . . ? C38 C21 C33 C65 0.3(10) . . . . ? O1 C21 C33 C9 -1.3(10) . . . . ? C38 C21 C33 C9 176.6(7) . . . . ? C41 C9 C33 C65 -31.4(11) . . . . ? C41 C9 C33 C21 152.3(7) . . . . ? C51 C28 C34 C31 80.0(8) . . . . ? C54 C28 C34 C31 -101.1(7) . . . . ? C29 C31 C34 C28 -103.3(8) . . . . ? C49 C31 C34 C28 78.6(8) . . . . ? C32 C27 C35 C46 -0.9(11) . . . . ? C32 C27 C35 C45 172.9(7) . . . . ? C59 C24 C38 C21 1.6(10) . . . . ? C45 C24 C38 C21 -174.9(6) . . . . ? O1 C21 C38 C24 175.3(6) . . . . ? C33 C21 C38 C24 -2.6(10) . . . . ? C17 C26 C39 C15 0.6(10) . . . . ? C45 C26 C39 C15 -177.4(6) . . . . ? C17 C26 C39 C42 179.7(6) . . . . ? C45 C26 C39 C42 1.7(8) . . . . ? C4 C15 C39 C26 -0.1(10) . . . . ? C4 C15 C39 C42 -179.1(6) . . . . ? C56 C36 C40 C48 4.8(10) . . . . ? C56 C36 C40 C18 -176.7(6) . . . . ? C2 C18 C40 C36 178.9(7) . . . . ? C8 C18 C40 C36 60.0(9) . . . . ? C10 C18 C40 C36 -56.6(9) . . . . ? C2 C18 C40 C48 -2.7(10) . . . . ? C8 C18 C40 C48 -121.5(7) . . . . ? C10 C18 C40 C48 121.9(7) . . . . ? C22 C20 C41 C51 1.8(10) . . . . ? C22 C20 C41 C9 -179.1(6) . . . . ? C33 C9 C41 C20 77.0(10) . . . . ? C33 C9 C41 C51 -103.8(8) . . . . ? C26 C39 C42 C46 55.4(7) . . . . ? C15 C39 C42 C46 -125.5(7) . . . . ? C26 C39 C42 C59 -57.4(7) . . . . ? C15 C39 C42 C59 121.6(7) . . . . ? C38 C24 C45 C35 -129.3(7) . . . . ? C59 C24 C45 C35 54.0(8) . . . . ? C38 C24 C45 C26 120.2(7) . . . . ? C59 C24 C45 C26 -56.6(7) . . . . ? C27 C35 C45 C24 130.8(8) . . . . ? C46 C35 C45 C24 -55.1(8) . . . . ? C27 C35 C45 C26 -118.6(8) . . . . ? C46 C35 C45 C26 55.5(8) . . . . ? C17 C26 C45 C24 -122.3(7) . . . . ? C39 C26 C45 C24 55.6(7) . . . . ? C17 C26 C45 C35 125.4(7) . . . . ? C39 C26 C45 C35 -56.7(7) . . . . ? C27 C35 C46 C61 -0.7(11) . . . . ? C45 C35 C46 C61 -175.3(6) . . . . ? C27 C35 C46 C42 175.1(7) . . . . ? C45 C35 C46 C42 0.5(9) . . . . ? C39 C42 C46 C61 119.1(7) . . . . ? C59 C42 C46 C61 -130.3(7) . . . . ? C39 C42 C46 C35 -56.3(8) . . . . ? C59 C42 C46 C35 54.2(8) . . . . ? C19 C16 C47 C55 -2.0(11) . . . . ? C19 C16 C47 C58 -179.9(7) . . . . ? C36 C40 C48 C60 -2.4(10) . . . . ? C18 C40 C48 C60 179.1(6) . . . . ? C57 C44 C49 C31 0.1(10) . . . . ? C58 C44 C49 C31 -178.8(7) . . . . ? C29 C31 C49 C44 0.0(10) . . . . ? C34 C31 C49 C44 178.3(6) . . . . ? C54 C28 C51 O6 179.6(6) . . . . ? C34 C28 C51 O6 -1.4(9) . . . . ? C54 C28 C51 C41 -3.4(9) . . . . ? C34 C28 C51 C41 175.6(6) . . . . ? C20 C41 C51 O6 179.1(6) . . . . ? C9 C41 C51 O6 -0.1(9) . . . . ? C20 C41 C51 C28 1.9(10) . . . . ? C9 C41 C51 C28 -177.3(6) . . . . ? C62 C43 C52 C64 -0.2(10) . . . . ? C62 C43 C52 C58 177.9(6) . . . . ? O2 C32 C53 C61 176.7(6) . . . . ? C27 C32 C53 C61 -1.6(11) . . . . ? O2 C32 C53 C30 0.1(10) . . . . ? C27 C32 C53 C30 -178.1(7) . . . . ? C56 C30 C53 C32 -150.9(7) . . . . ? C56 C30 C53 C61 32.6(10) . . . . ? C20 C22 C54 C28 2.1(9) . . . . ? C12 C22 C54 C28 -179.3(6) . . . . ? C51 C28 C54 C22 1.3(9) . . . . ? C34 C28 C54 C22 -177.7(6) . . . . ? C16 C47 C55 C23 1.5(10) . . . . ? C58 C47 C55 C23 179.7(6) . . . . ? C16 C47 C55 C50 -178.7(7) . . . . ? C58 C47 C55 C50 -0.5(8) . . . . ? C25 C23 C55 C47 -1.7(10) . . . . ? C25 C23 C55 C50 178.5(7) . . . . ? C64 C50 C55 C47 56.8(7) . . . . ? C57 C50 C55 C47 -55.5(7) . . . . ? C64 C50 C55 C23 -123.4(7) . . . . ? C57 C50 C55 C23 124.3(7) . . . . ? C40 C36 C56 C63 -3.0(10) . . . . ? C40 C36 C56 C30 178.5(6) . . . . ? C53 C30 C56 C63 102.2(8) . . . . ? C53 C30 C56 C36 -79.3(9) . . . . ? C49 C44 C57 C67 0.2(11) . . . . ? C58 C44 C57 C67 179.2(6) . . . . ? C49 C44 C57 C50 -178.2(6) . . . . ? C58 C44 C57 C50 0.8(8) . . . . ? C55 C50 C57 C44 55.8(8) . . . . ? C64 C50 C57 C44 -55.3(7) . . . . ? C55 C50 C57 C67 -122.5(7) . . . . ? C64 C50 C57 C67 126.3(7) . . . . ? C49 C44 C58 C52 -126.9(7) . . . . ? C57 C44 C58 C52 54.1(8) . . . . ? C49 C44 C58 C47 121.4(7) . . . . ? C57 C44 C58 C47 -57.5(7) . . . . ? C43 C52 C58 C44 128.0(7) . . . . ? C64 C52 C58 C44 -53.8(7) . . . . ? C43 C52 C58 C47 -120.3(7) . . . . ? C64 C52 C58 C47 57.9(7) . . . . ? C16 C47 C58 C44 -124.6(8) . . . . ? C55 C47 C58 C44 57.4(7) . . . . ? C16 C47 C58 C52 121.5(8) . . . . ? C55 C47 C58 C52 -56.6(7) . . . . ? C38 C24 C59 C65 1.6(10) . . . . ? C45 C24 C59 C65 178.6(6) . . . . ? C38 C24 C59 C42 -176.3(6) . . . . ? C45 C24 C59 C42 0.6(8) . . . . ? C39 C42 C59 C24 56.3(7) . . . . ? C46 C42 C59 C24 -55.6(8) . . . . ? C39 C42 C59 C65 -121.5(7) . . . . ? C46 C42 C59 C65 126.7(7) . . . . ? C40 C48 C60 C63 -1.8(10) . . . . ? C40 C48 C60 C37 174.6(6) . . . . ? C62 C37 C60 C48 101.7(7) . . . . ? C62 C37 C60 C63 -82.0(8) . . . . ? C35 C46 C61 C53 1.2(10) . . . . ? C42 C46 C61 C53 -173.9(7) . . . . ? C32 C53 C61 C46 -0.1(10) . . . . ? C30 C53 C61 C46 176.4(6) . . . . ? C52 C43 C62 C66 0.4(10) . . . . ? C52 C43 C62 C37 -176.5(6) . . . . ? C60 C37 C62 C43 -78.2(8) . . . . ? C60 C37 C62 C66 104.9(7) . . . . ? C36 C56 C63 O4 -179.6(6) . . . . ? C30 C56 C63 O4 -1.1(9) . . . . ? C36 C56 C63 C60 -1.4(10) . . . . ? C30 C56 C63 C60 177.2(6) . . . . ? C48 C60 C63 O4 -178.2(6) . . . . ? C37 C60 C63 O4 5.4(9) . . . . ? C48 C60 C63 C56 3.7(9) . . . . ? C37 C60 C63 C56 -172.7(6) . . . . ? C43 C52 C64 C68 0.1(10) . . . . ? C58 C52 C64 C68 -178.3(6) . . . . ? C43 C52 C64 C50 176.9(6) . . . . ? C58 C52 C64 C50 -1.5(8) . . . . ? C55 C50 C64 C68 120.9(7) . . . . ? C57 C50 C64 C68 -128.0(7) . . . . ? C55 C50 C64 C52 -55.7(7) . . . . ? C57 C50 C64 C52 55.3(7) . . . . ? C21 C33 C65 C59 3.0(10) . . . . ? C9 C33 C65 C59 -173.3(6) . . . . ? C24 C59 C65 C33 -4.0(10) . . . . ? C42 C59 C65 C33 173.6(7) . . . . ? C14 O5 C66 C68 2.3(9) . . . . ? C14 O5 C66 C62 -178.0(6) . . . . ? C43 C62 C66 O5 179.8(5) . . . . ? C37 C62 C66 O5 -3.3(8) . . . . ? C43 C62 C66 C68 -0.5(9) . . . . ? C37 C62 C66 C68 176.4(6) . . . . ? O3 C29 C67 C57 177.9(6) . . . . ? C31 C29 C67 C57 0.7(11) . . . . ? C44 C57 C67 C29 -0.5(10) . . . . ? C50 C57 C67 C29 177.7(7) . . . . ? C52 C64 C68 C66 -0.1(10) . . . . ? C50 C64 C68 C66 -176.5(6) . . . . ? O5 C66 C68 C64 -180.0(6) . . . . ? C62 C66 C68 C64 0.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.089 _refine_diff_density_min -1.223 _refine_diff_density_rms 0.150 # Attachment '- 6a.cif' data_mx995 _database_code_depnum_ccdc_archive 'CCDC 842678' #TrackingRef '- 6a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H56 O6, 3(C3 H6 O)' _chemical_formula_sum 'C73 H74 O9' _chemical_formula_weight 1095.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.531(3) _cell_length_b 38.597(8) _cell_length_c 14.299(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.405(2) _cell_angle_gamma 90.00 _cell_volume 6858(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14793 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 25.34 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9763 _exptl_absorpt_correction_T_max 0.9857 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007-HF CCD(Saturn 724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41470 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.34 _reflns_number_total 12518 _reflns_number_gt 9948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.1312P)^2^+14.9063P] 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 12518 _refine_ls_number_parameters 767 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.1167 _refine_ls_wR_factor_ref 0.3140 _refine_ls_wR_factor_gt 0.3025 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.001 _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 0.7885(3) 0.05964(8) 1.1501(2) 0.0549(9) Uani 1 1 d . . . H1A H 0.7591 0.0592 1.0939 0.082 Uiso 1 1 calc R . . O2 O 0.6956(2) 0.06189(8) 0.9657(2) 0.0444(7) Uani 1 1 d . . . H2A H 0.7209 0.0448 0.9396 0.053 Uiso 1 1 d R . . O3 O 0.7801(3) 0.00444(8) 0.8763(3) 0.0554(9) Uani 1 1 d . . . H3A H 0.8036 -0.0144 0.8999 0.066 Uiso 1 1 d R . . O4 O 1.4367(3) 0.08830(9) 0.9198(3) 0.0598(9) Uani 1 1 d . . . H4A H 1.4500 0.0728 0.9608 0.072 Uiso 1 1 d R . . O5 O 1.4330(2) 0.15455(8) 0.9934(2) 0.0496(8) Uani 1 1 d . . . H5A H 1.4351 0.1343 0.9724 0.060 Uiso 1 1 d R . . O6 O 1.4389(3) 0.14740(10) 1.1844(3) 0.0600(10) Uani 1 1 d . . . H6A H 1.4481 0.1484 1.1273 0.090 Uiso 1 1 calc R . . O7 O 0.1420(5) 0.05726(12) 1.0473(4) 0.0982(17) Uani 1 1 d . . . O8 O 0.6690(4) 0.10064(18) 0.5230(4) 0.1125(19) Uani 1 1 d . . . O9 O 0.4824(7) 0.0354(2) 0.0556(8) 0.173(4) Uani 1 1 d . . . C1 C 0.9905(4) 0.20986(13) 1.4054(3) 0.0492(11) Uani 1 1 d . . . H1B H 0.9592 0.2306 1.3789 0.059 Uiso 1 1 calc R . . C2 C 1.0047(4) 0.20461(15) 1.5029(4) 0.0596(13) Uani 1 1 d . . . H2B H 0.9825 0.2222 1.5428 0.072 Uiso 1 1 calc R . . C3 C 1.0502(5) 0.17446(14) 1.5431(3) 0.0578(13) Uani 1 1 d . . . H3B H 1.0596 0.1715 1.6096 0.069 Uiso 1 1 calc R . . C4 C 1.0821(4) 0.14832(13) 1.4840(3) 0.0475(11) Uani 1 1 d . . . H4B H 1.1135 0.1275 1.5103 0.057 Uiso 1 1 calc R . . C5 C 1.0677(3) 0.15306(11) 1.3883(3) 0.0392(9) Uani 1 1 d . . . C6 C 1.0232(3) 0.18400(11) 1.3483(3) 0.0390(9) Uani 1 1 d . . . C7 C 0.7934(3) 0.12188(11) 1.1305(3) 0.0364(9) Uani 1 1 d . . . C8 C 0.9469(3) 0.15277(10) 1.2087(3) 0.0356(9) Uani 1 1 d . . . C10 C 0.9903(3) 0.12184(10) 1.2489(3) 0.0332(9) Uani 1 1 d . . . C11 C 0.9374(4) 0.09098(11) 1.2272(3) 0.0395(10) Uani 1 1 d . . . H11A H 0.9673 0.0697 1.2519 0.047 Uiso 1 1 calc R . . C12 C 0.8393(4) 0.09136(11) 1.1684(3) 0.0402(10) Uani 1 1 d . . . C13 C 0.8502(3) 0.15266(11) 1.1519(3) 0.0369(9) Uani 1 1 d . . . H13A H 0.8210 0.1739 1.1266 0.044 Uiso 1 1 calc R . . C14 C 0.6834(3) 0.12291(11) 1.0723(3) 0.0402(10) Uani 1 1 d . . . H14A H 0.6450 0.1439 1.0896 0.048 Uiso 1 1 calc R . . H14B H 0.6416 0.1025 1.0885 0.048 Uiso 1 1 calc R . . C15 C 0.6869(3) 0.12312(11) 0.9661(3) 0.0377(9) Uani 1 1 d . . . C16 C 0.6864(3) 0.15430(11) 0.9173(3) 0.0404(10) Uani 1 1 d . . . H16A H 0.6849 0.1753 0.9520 0.048 Uiso 1 1 calc R . . C17 C 0.6881(3) 0.15635(11) 0.8213(3) 0.0414(10) Uani 1 1 d . A . C18 C 0.6885(3) 0.12503(11) 0.7722(3) 0.0402(10) Uani 1 1 d . . . H18A H 0.6876 0.1255 0.7057 0.048 Uiso 1 1 calc R . . C19 C 0.6899(3) 0.09337(11) 0.8173(3) 0.0391(9) Uani 1 1 d . . . C20 C 0.6927(3) 0.09261(10) 0.9151(3) 0.0383(9) Uani 1 1 d . . . C21 C 0.6939(4) 0.05983(12) 0.7611(3) 0.0472(11) Uani 1 1 d . . . H21A H 0.6613 0.0639 0.6952 0.057 Uiso 1 1 calc R . . H21B H 0.6508 0.0419 0.7885 0.057 Uiso 1 1 calc R . . C22 C 0.8093(3) 0.04669(11) 0.7615(3) 0.0385(9) Uani 1 1 d . . . C23 C 0.8769(4) 0.06355(10) 0.7077(3) 0.0382(9) Uani 1 1 d . . . H23A H 0.8504 0.0824 0.6688 0.046 Uiso 1 1 calc R . . C24 C 0.9833(3) 0.05327(10) 0.7097(3) 0.0357(9) Uani 1 1 d . . . C25 C 1.0220(3) 0.02509(10) 0.7665(3) 0.0353(9) Uani 1 1 d . . . C26 C 0.9550(4) 0.00815(10) 0.8207(3) 0.0393(10) Uani 1 1 d . . . H26A H 0.9806 -0.0110 0.8590 0.047 Uiso 1 1 calc R . . C27 C 0.8493(4) 0.01948(10) 0.8183(3) 0.0414(10) Uani 1 1 d . . . C28 C 1.0664(4) 0.06851(10) 0.6527(3) 0.0378(9) Uani 1 1 d . . . H28A H 1.0386 0.0886 0.6124 0.045 Uiso 1 1 calc R . . C29 C 1.1652(4) 0.07757(11) 0.7245(3) 0.0381(9) Uani 1 1 d . . . C30 C 1.2018(3) 0.04956(10) 0.7807(3) 0.0357(9) Uani 1 1 d . . . C31 C 1.1385(4) 0.01656(10) 0.7584(3) 0.0378(9) Uani 1 1 d . . . H31A H 1.1664 -0.0034 0.7989 0.045 Uiso 1 1 calc R . . C32 C 1.1439(3) 0.01047(11) 0.6545(3) 0.0388(9) Uani 1 1 d . . . C33 C 1.1825(4) -0.01880(11) 0.6130(3) 0.0461(11) Uani 1 1 d . . . H33A H 1.2082 -0.0379 0.6512 0.055 Uiso 1 1 calc R . . C34 C 1.1837(4) -0.02022(13) 0.5169(4) 0.0548(13) Uani 1 1 d . . . H34A H 1.2117 -0.0401 0.4893 0.066 Uiso 1 1 calc R . . C35 C 1.1442(4) 0.00733(13) 0.4602(3) 0.0521(12) Uani 1 1 d . . . H35A H 1.1446 0.0063 0.3939 0.063 Uiso 1 1 calc R . . C36 C 1.1038(4) 0.03670(12) 0.5014(3) 0.0469(11) Uani 1 1 d . . . H36A H 1.0762 0.0556 0.4630 0.056 Uiso 1 1 calc R . . C37 C 1.1041(4) 0.03808(11) 0.5962(3) 0.0389(9) Uani 1 1 d . . . C38 C 1.2910(3) 0.05330(11) 0.8472(3) 0.0405(10) Uani 1 1 d . . . H38A H 1.3142 0.0346 0.8881 0.049 Uiso 1 1 calc R . . C39 C 1.3473(4) 0.08465(12) 0.8543(3) 0.0433(10) Uani 1 1 d . . . C40 C 1.3168(4) 0.11207(12) 0.7939(3) 0.0430(10) Uani 1 1 d . . . C41 C 1.2229(4) 0.10819(11) 0.7298(3) 0.0383(9) Uani 1 1 d . . . H41A H 1.1987 0.1269 0.6894 0.046 Uiso 1 1 calc R . . C42 C 1.3841(4) 0.14489(12) 0.7926(3) 0.0516(12) Uani 1 1 d . . . H42A H 1.4586 0.1397 0.8210 0.062 Uiso 1 1 calc R . . H42B H 1.3866 0.1518 0.7263 0.062 Uiso 1 1 calc R . . C43 C 1.3426(4) 0.17525(12) 0.8449(3) 0.0460(11) Uani 1 1 d . . . C44 C 1.2798(4) 0.20059(12) 0.7960(4) 0.0555(13) Uani 1 1 d . . . H44A H 1.2622 0.1983 0.7297 0.067 Uiso 1 1 calc R . . C45 C 1.2414(4) 0.22915(12) 0.8400(4) 0.0540(13) Uani 1 1 d . . . C46 C 1.2679(4) 0.23148(11) 0.9393(4) 0.0459(11) Uani 1 1 d . . . H46A H 1.2409 0.2504 0.9717 0.055 Uiso 1 1 calc R . . C47 C 1.3316(3) 0.20709(10) 0.9903(3) 0.0352(9) Uani 1 1 d . . . C48 C 1.3676(3) 0.17875(11) 0.9418(3) 0.0384(9) Uani 1 1 d . . . C49 C 1.3598(3) 0.21080(11) 1.0961(3) 0.0403(10) Uani 1 1 d . . . H49A H 1.4370 0.2052 1.1131 0.048 Uiso 1 1 calc R . . H49B H 1.3495 0.2353 1.1135 0.048 Uiso 1 1 calc R . . C50 C 1.2946(3) 0.18813(11) 1.1529(3) 0.0359(9) Uani 1 1 d . . . C51 C 1.1897(4) 0.19732(10) 1.1657(3) 0.0389(9) Uani 1 1 d . . . H51A H 1.1600 0.2181 1.1375 0.047 Uiso 1 1 calc R . . C52 C 1.1284(3) 0.17752(10) 1.2174(3) 0.0360(9) Uani 1 1 d . . . C53 C 1.0159(3) 0.18450(10) 1.2418(3) 0.0368(9) Uani 1 1 d . . . H53A H 0.9849 0.2066 1.2138 0.044 Uiso 1 1 calc R . . C54 C 1.0945(3) 0.12704(11) 1.3145(3) 0.0367(9) Uani 1 1 d . . . H54A H 1.1250 0.1049 1.3429 0.044 Uiso 1 1 calc R . . C55 C 1.1722(3) 0.14610(10) 1.2577(3) 0.0351(9) Uani 1 1 d . . . C56 C 1.2746(3) 0.13634(11) 1.2463(3) 0.0407(10) Uani 1 1 d . . . H56A H 1.3040 0.1155 1.2738 0.049 Uiso 1 1 calc R . . C57 C 1.3357(3) 0.15734(11) 1.1939(3) 0.0386(9) Uani 1 1 d . . . C58 C 0.6919(4) 0.19116(12) 0.7706(3) 0.0503(11) Uani 1 1 d D . . C59 C 0.8014(7) 0.2057(3) 0.7945(8) 0.080(3) Uani 0.654(12) 1 d PDU A 1 H59A H 0.8191 0.2070 0.8632 0.119 Uiso 0.654(12) 1 calc PR A 1 H59B H 0.8041 0.2290 0.7675 0.119 Uiso 0.654(12) 1 calc PR A 1 H59C H 0.8536 0.1907 0.7686 0.119 Uiso 0.654(12) 1 calc PR A 1 C60 C 0.6542(14) 0.1883(3) 0.6673(7) 0.104(4) Uani 0.654(12) 1 d PDU A 1 H60A H 0.5813 0.1786 0.6579 0.155 Uiso 0.654(12) 1 calc PR A 1 H60B H 0.7028 0.1730 0.6379 0.155 Uiso 0.654(12) 1 calc PR A 1 H60C H 0.6536 0.2113 0.6383 0.155 Uiso 0.654(12) 1 calc PR A 1 C61 C 0.6092(8) 0.2157(2) 0.8044(8) 0.068(3) Uani 0.654(12) 1 d PDU A 1 H61A H 0.5368 0.2061 0.7880 0.102 Uiso 0.654(12) 1 calc PR A 1 H61B H 0.6134 0.2383 0.7738 0.102 Uiso 0.654(12) 1 calc PR A 1 H61C H 0.6242 0.2185 0.8729 0.102 Uiso 0.654(12) 1 calc PR A 1 C59' C 0.750(2) 0.1900(5) 0.6815(13) 0.086(6) Uani 0.346(12) 1 d PDU A 2 H59D H 0.8250 0.1834 0.6992 0.130 Uiso 0.346(12) 1 calc PR A 2 H59E H 0.7461 0.2129 0.6517 0.130 Uiso 0.346(12) 1 calc PR A 2 H59F H 0.7142 0.1729 0.6371 0.130 Uiso 0.346(12) 1 calc PR A 2 C60' C 0.5817(13) 0.2048(6) 0.734(2) 0.091(6) Uani 0.346(12) 1 d PDU A 2 H60D H 0.5888 0.2271 0.7024 0.137 Uiso 0.346(12) 1 calc PR A 2 H60E H 0.5398 0.2080 0.7866 0.137 Uiso 0.346(12) 1 calc PR A 2 H60F H 0.5448 0.1883 0.6888 0.137 Uiso 0.346(12) 1 calc PR A 2 C61' C 0.735(3) 0.2215(5) 0.8321(17) 0.113(8) Uani 0.346(12) 1 d PDU A 2 H61D H 0.8055 0.2155 0.8660 0.170 Uiso 0.346(12) 1 calc PR A 2 H61E H 0.6849 0.2267 0.8776 0.170 Uiso 0.346(12) 1 calc PR A 2 H61F H 0.7419 0.2419 0.7924 0.170 Uiso 0.346(12) 1 calc PR A 2 C62 C 1.1671(5) 0.25609(16) 0.7859(5) 0.081(2) Uani 1 1 d . . . C63 C 1.1906(6) 0.2585(2) 0.6808(6) 0.112(3) Uani 1 1 d . . . H63A H 1.1429 0.2758 0.6471 0.168 Uiso 1 1 calc R . . H63B H 1.1778 0.2359 0.6503 0.168 Uiso 1 1 calc R . . H63C H 1.2657 0.2653 0.6794 0.168 Uiso 1 1 calc R . . C64 C 1.1853(8) 0.29179(18) 0.8271(8) 0.133(4) Uani 1 1 d . . . H64A H 1.1701 0.2917 0.8926 0.200 Uiso 1 1 calc R . . H64B H 1.1372 0.3083 0.7903 0.200 Uiso 1 1 calc R . . H64C H 1.2602 0.2987 0.8251 0.200 Uiso 1 1 calc R . . C65 C 1.0518(5) 0.2435(2) 0.7859(6) 0.102(3) Uani 1 1 d . . . H65A H 1.0354 0.2420 0.8510 0.154 Uiso 1 1 calc R . . H65B H 1.0437 0.2206 0.7563 0.154 Uiso 1 1 calc R . . H65C H 1.0022 0.2598 0.7505 0.154 Uiso 1 1 calc R . . C66 C 0.6308(8) 0.1063(3) 0.3583(7) 0.152(5) Uani 1 1 d . . . H66A H 0.5589 0.0981 0.3673 0.229 Uiso 1 1 calc R . . H66B H 0.6655 0.0893 0.3213 0.229 Uiso 1 1 calc R . . H66C H 0.6248 0.1285 0.3246 0.229 Uiso 1 1 calc R . . C67 C 0.6978(5) 0.11111(18) 0.4535(5) 0.0747(17) Uani 1 1 d . . . C68 C 0.8054(7) 0.1226(2) 0.4464(6) 0.100(2) Uani 1 1 d . . . H68A H 0.8448 0.1253 0.5098 0.150 Uiso 1 1 calc R . . H68B H 0.8030 0.1448 0.4133 0.150 Uiso 1 1 calc R . . H68C H 0.8419 0.1054 0.4113 0.150 Uiso 1 1 calc R . . C69 C -0.0187(5) 0.0836(2) 0.9721(5) 0.083(2) Uani 1 1 d . . . H69A H -0.0513 0.0610 0.9825 0.124 Uiso 1 1 calc R . . H69B H -0.0272 0.0886 0.9044 0.124 Uiso 1 1 calc R . . H69C H -0.0544 0.1016 1.0050 0.124 Uiso 1 1 calc R . . C70 C 0.0995(4) 0.08261(13) 1.0098(3) 0.0490(11) Uani 1 1 d . . . C71 C 0.1593(5) 0.11564(16) 0.9994(5) 0.0724(16) Uani 1 1 d . . . H71A H 0.2348 0.1127 1.0260 0.109 Uiso 1 1 calc R . . H71B H 0.1272 0.1343 1.0331 0.109 Uiso 1 1 calc R . . H71C H 0.1552 0.1216 0.9325 0.109 Uiso 1 1 calc R . . C72 C 0.4520(12) 0.0708(4) 0.1939(10) 0.178(5) Uani 1 1 d U . . H72A H 0.4614 0.0675 0.2624 0.268 Uiso 1 1 calc R . . H72B H 0.3776 0.0778 0.1726 0.268 Uiso 1 1 calc R . . H72C H 0.5012 0.0889 0.1776 0.268 Uiso 1 1 calc R . . C73 C 0.4750(8) 0.0391(3) 0.1488(15) 0.190(9) Uani 1 1 d . . . C74 C 0.5318(8) 0.0145(3) 0.2198(11) 0.187(7) Uani 1 1 d . . . H74A H 0.5269 0.0230 0.2836 0.280 Uiso 1 1 calc R . . H74B H 0.6076 0.0127 0.2102 0.280 Uiso 1 1 calc R . . H74C H 0.4980 -0.0084 0.2119 0.280 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 0.074(2) 0.0326(16) 0.054(2) 0.0083(14) -0.0089(17) -0.0080(15) O2 0.0460(17) 0.0347(15) 0.0522(18) 0.0040(13) 0.0054(14) -0.0010(13) O3 0.052(2) 0.0393(17) 0.078(2) 0.0097(16) 0.0190(17) -0.0012(14) O4 0.0458(19) 0.059(2) 0.071(2) 0.0105(18) -0.0066(17) -0.0031(16) O5 0.0353(16) 0.0467(18) 0.066(2) 0.0049(15) 0.0045(15) 0.0046(13) O6 0.0415(18) 0.073(2) 0.067(2) 0.0247(19) 0.0096(16) 0.0169(16) O7 0.131(4) 0.077(3) 0.094(3) 0.030(3) 0.045(3) 0.043(3) O8 0.098(4) 0.173(6) 0.072(3) 0.022(4) 0.030(3) 0.026(4) O9 0.128(6) 0.100(5) 0.279(12) 0.041(7) -0.018(7) -0.028(4) C1 0.056(3) 0.050(3) 0.041(2) -0.010(2) 0.004(2) 0.008(2) C2 0.061(3) 0.066(3) 0.053(3) -0.016(3) 0.012(2) 0.011(3) C3 0.074(4) 0.067(3) 0.032(2) -0.007(2) 0.004(2) 0.012(3) C4 0.057(3) 0.052(3) 0.032(2) 0.0008(19) 0.003(2) 0.010(2) C5 0.041(2) 0.045(2) 0.032(2) -0.0043(18) 0.0056(17) 0.0015(18) C6 0.041(2) 0.042(2) 0.035(2) -0.0034(18) 0.0072(17) 0.0053(18) C7 0.037(2) 0.038(2) 0.035(2) 0.0028(17) 0.0099(17) 0.0061(17) C8 0.040(2) 0.032(2) 0.035(2) -0.0013(16) 0.0084(17) 0.0054(17) C10 0.037(2) 0.035(2) 0.0290(19) 0.0049(16) 0.0092(16) 0.0071(16) C11 0.050(3) 0.032(2) 0.038(2) 0.0017(17) 0.0096(19) 0.0072(18) C12 0.052(3) 0.036(2) 0.032(2) 0.0043(17) 0.0067(18) -0.0061(19) C13 0.038(2) 0.035(2) 0.039(2) 0.0035(17) 0.0112(18) 0.0099(17) C14 0.043(2) 0.035(2) 0.044(2) 0.0021(18) 0.0115(19) 0.0017(18) C15 0.032(2) 0.037(2) 0.044(2) 0.0021(18) 0.0031(17) -0.0005(17) C16 0.036(2) 0.039(2) 0.045(2) 0.0012(18) -0.0023(18) 0.0026(17) C17 0.039(2) 0.040(2) 0.044(2) 0.0039(19) -0.0002(18) 0.0025(18) C18 0.038(2) 0.046(2) 0.037(2) 0.0014(18) 0.0037(17) 0.0018(18) C19 0.032(2) 0.042(2) 0.042(2) -0.0008(18) -0.0016(17) -0.0024(17) C20 0.028(2) 0.031(2) 0.055(3) 0.0052(18) 0.0006(18) -0.0008(16) C21 0.040(2) 0.049(3) 0.050(3) -0.011(2) -0.004(2) -0.003(2) C22 0.046(2) 0.033(2) 0.036(2) -0.0060(17) 0.0013(18) 0.0002(18) C23 0.053(3) 0.031(2) 0.029(2) -0.0065(16) -0.0005(18) 0.0012(18) C24 0.046(2) 0.031(2) 0.030(2) -0.0055(16) 0.0059(17) -0.0034(17) C25 0.048(2) 0.0275(19) 0.030(2) -0.0038(16) 0.0042(17) -0.0025(17) C26 0.052(3) 0.027(2) 0.039(2) -0.0007(17) 0.0059(19) -0.0041(18) C27 0.050(3) 0.029(2) 0.047(2) -0.0065(18) 0.014(2) -0.0047(18) C28 0.050(2) 0.031(2) 0.031(2) 0.0031(16) 0.0006(18) -0.0006(18) C29 0.048(2) 0.037(2) 0.029(2) 0.0001(17) 0.0062(18) -0.0009(18) C30 0.042(2) 0.033(2) 0.034(2) -0.0042(16) 0.0126(17) -0.0016(17) C31 0.052(3) 0.030(2) 0.033(2) 0.0041(16) 0.0097(18) 0.0008(18) C32 0.037(2) 0.035(2) 0.046(2) -0.0042(18) 0.0101(18) -0.0048(17) C33 0.056(3) 0.035(2) 0.048(3) -0.0076(19) 0.013(2) -0.001(2) C34 0.071(3) 0.045(3) 0.051(3) -0.025(2) 0.014(2) -0.005(2) C35 0.068(3) 0.052(3) 0.038(2) -0.012(2) 0.016(2) -0.011(2) C36 0.058(3) 0.043(2) 0.039(2) -0.0118(19) 0.006(2) -0.007(2) C37 0.048(2) 0.036(2) 0.034(2) -0.0021(17) 0.0086(18) -0.0062(18) C38 0.042(2) 0.044(2) 0.038(2) 0.0000(18) 0.0137(18) 0.0016(19) C39 0.037(2) 0.045(2) 0.047(3) -0.006(2) 0.0065(19) -0.0036(19) C40 0.052(3) 0.045(2) 0.035(2) -0.0056(19) 0.0152(19) -0.012(2) C41 0.055(3) 0.033(2) 0.027(2) -0.0012(16) 0.0088(18) -0.0032(18) C42 0.067(3) 0.050(3) 0.040(2) -0.003(2) 0.015(2) -0.024(2) C43 0.046(3) 0.042(2) 0.048(3) 0.008(2) 0.003(2) -0.018(2) C44 0.069(3) 0.042(3) 0.049(3) 0.008(2) -0.016(2) -0.025(2) C45 0.051(3) 0.041(3) 0.061(3) 0.017(2) -0.025(2) -0.018(2) C46 0.040(2) 0.034(2) 0.061(3) 0.008(2) -0.003(2) -0.0031(18) C47 0.030(2) 0.036(2) 0.038(2) 0.0073(17) -0.0002(16) -0.0107(16) C48 0.029(2) 0.038(2) 0.049(2) 0.0099(19) 0.0060(18) -0.0080(17) C49 0.036(2) 0.040(2) 0.043(2) -0.0037(18) -0.0005(18) -0.0063(18) C50 0.040(2) 0.038(2) 0.029(2) -0.0050(16) -0.0016(16) -0.0041(17) C51 0.048(2) 0.030(2) 0.038(2) -0.0014(17) 0.0034(18) 0.0033(18) C52 0.044(2) 0.031(2) 0.033(2) 0.0004(16) 0.0017(17) 0.0044(17) C53 0.046(2) 0.029(2) 0.036(2) 0.0012(16) 0.0087(18) 0.0071(17) C54 0.043(2) 0.036(2) 0.032(2) 0.0083(17) 0.0057(17) 0.0093(17) C55 0.043(2) 0.034(2) 0.029(2) -0.0015(16) 0.0069(17) 0.0044(17) C56 0.042(2) 0.044(2) 0.036(2) 0.0113(18) 0.0040(18) 0.0101(19) C57 0.036(2) 0.048(2) 0.031(2) 0.0031(18) 0.0022(17) 0.0002(18) C58 0.059(3) 0.044(3) 0.048(3) 0.006(2) 0.006(2) -0.001(2) C59 0.057(5) 0.076(6) 0.104(7) 0.041(5) 0.008(5) -0.021(4) C60 0.150(9) 0.076(6) 0.079(6) 0.020(5) -0.004(6) 0.004(6) C61 0.073(5) 0.046(4) 0.089(6) 0.026(4) 0.030(5) 0.011(4) C59' 0.113(11) 0.070(9) 0.079(9) 0.022(7) 0.024(8) -0.009(8) C60' 0.087(9) 0.078(9) 0.105(10) 0.030(8) -0.002(8) -0.004(7) C61' 0.126(12) 0.099(11) 0.112(11) 0.006(8) 0.005(9) -0.015(9) C62 0.067(4) 0.060(3) 0.101(5) 0.026(3) -0.042(3) -0.017(3) C63 0.099(5) 0.123(6) 0.107(6) 0.077(5) -0.018(4) -0.028(5) C64 0.132(7) 0.060(4) 0.184(10) 0.035(5) -0.071(7) 0.020(4) C65 0.060(4) 0.112(6) 0.125(6) 0.077(5) -0.024(4) -0.013(4) C66 0.099(7) 0.222(12) 0.129(8) 0.089(8) -0.011(6) -0.001(7) C67 0.065(4) 0.084(4) 0.074(4) 0.031(3) 0.002(3) 0.007(3) C68 0.099(6) 0.098(6) 0.106(6) 0.012(5) 0.022(5) 0.003(4) C69 0.061(4) 0.123(6) 0.065(4) -0.032(4) 0.014(3) -0.016(4) C70 0.056(3) 0.053(3) 0.040(2) -0.002(2) 0.015(2) 0.001(2) C71 0.076(4) 0.068(4) 0.073(4) -0.003(3) 0.013(3) -0.017(3) C72 0.192(6) 0.170(6) 0.184(6) 0.020(5) 0.067(5) 0.031(5) C73 0.080(6) 0.138(9) 0.38(2) 0.169(13) 0.124(10) 0.057(6) C74 0.111(7) 0.108(7) 0.343(19) 0.125(10) 0.037(9) 0.047(6) _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 C12 1.389(5) . ? O1 H1A 0.8400 . ? O2 C20 1.387(5) . ? O2 H2A 0.8399 . ? O3 C27 1.400(5) . ? O3 H3A 0.8397 . ? O4 C39 1.372(5) . ? O4 H4A 0.8399 . ? O5 C48 1.390(5) . ? O5 H5A 0.8399 . ? O6 C57 1.373(5) . ? O6 H6A 0.8400 . ? O7 C70 1.206(6) . ? O8 C67 1.172(8) . ? O9 C73 1.356(19) . ? C1 C6 1.384(6) . ? C1 C2 1.398(7) . ? C1 H1B 0.9500 . ? C2 C3 1.388(8) . ? C2 H2B 0.9500 . ? C3 C4 1.407(7) . ? C3 H3B 0.9500 . ? C4 C5 1.370(6) . ? C4 H4B 0.9500 . ? C5 C6 1.408(6) . ? C5 C54 1.524(6) . ? C6 C53 1.514(6) . ? C7 C12 1.390(6) . ? C7 C13 1.398(6) . ? C7 C14 1.517(6) . ? C8 C13 1.369(6) . ? C8 C10 1.404(5) . ? C8 C53 1.538(6) . ? C10 C11 1.379(6) . ? C10 C54 1.520(6) . ? C11 C12 1.397(6) . ? C11 H11A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.525(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.391(6) . ? C15 C20 1.392(6) . ? C16 C17 1.378(6) . ? C16 H16A 0.9500 . ? C17 C18 1.398(6) . ? C17 C58 1.530(6) . ? C18 C19 1.381(6) . ? C18 H18A 0.9500 . ? C19 C20 1.395(6) . ? C19 C21 1.528(6) . ? C21 C22 1.532(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.379(6) . ? C22 C27 1.382(6) . ? C23 C24 1.388(6) . ? C23 H23A 0.9500 . ? C24 C25 1.406(6) . ? C24 C28 1.520(6) . ? C25 C26 1.379(6) . ? C25 C31 1.515(6) . ? C26 C27 1.391(6) . ? C26 H26A 0.9500 . ? C28 C37 1.535(6) . ? C28 C29 1.543(6) . ? C28 H28A 1.0000 . ? C29 C41 1.383(6) . ? C29 C30 1.389(6) . ? C30 C38 1.379(6) . ? C30 C31 1.513(6) . ? C31 C32 1.514(6) . ? C31 H31A 1.0000 . ? C32 C33 1.391(6) . ? C32 C37 1.404(6) . ? C33 C34 1.377(7) . ? C33 H33A 0.9500 . ? C34 C35 1.389(7) . ? C34 H34A 0.9500 . ? C35 C36 1.402(7) . ? C35 H35A 0.9500 . ? C36 C37 1.356(6) . ? C36 H36A 0.9500 . ? C38 C39 1.398(6) . ? C38 H38A 0.9500 . ? C39 C40 1.388(7) . ? C40 C41 1.404(6) . ? C40 C42 1.523(6) . ? C41 H41A 0.9500 . ? C42 C43 1.516(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.387(7) . ? C43 C48 1.388(6) . ? C44 C45 1.385(8) . ? C44 H44A 0.9500 . ? C45 C46 1.418(7) . ? C45 C62 1.536(7) . ? C46 C47 1.380(6) . ? C46 H46A 0.9500 . ? C47 C48 1.401(6) . ? C47 C49 1.515(6) . ? C49 C50 1.505(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C57 1.394(6) . ? C50 C51 1.396(6) . ? C51 C52 1.366(6) . ? C51 H51A 0.9500 . ? C52 C55 1.422(5) . ? C52 C53 1.519(6) . ? C53 H53A 1.0000 . ? C54 C55 1.534(6) . ? C54 H54A 1.0000 . ? C55 C56 1.368(6) . ? C56 C57 1.397(6) . ? C56 H56A 0.9500 . ? C58 C59 1.481(9) . ? C58 C60 1.496(10) . ? C58 C60' 1.509(13) . ? C58 C61' 1.521(14) . ? C58 C61 1.529(8) . ? C58 C59' 1.544(13) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C59' H59D 0.9800 . ? C59' H59E 0.9800 . ? C59' H59F 0.9800 . ? C60' H60D 0.9800 . ? C60' H60E 0.9800 . ? C60' H60F 0.9800 . ? C61' H61D 0.9800 . ? C61' H61E 0.9800 . ? C61' H61F 0.9800 . ? C62 C64 1.504(10) . ? C62 C65 1.525(9) . ? C62 C63 1.572(11) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.516(12) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C68 1.435(10) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.510(8) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C71 1.496(7) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.429(19) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.503(15) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? 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 C12 O1 H1A 109.5 . . ? C20 O2 H2A 115.1 . . ? C27 O3 H3A 112.7 . . ? C39 O4 H4A 118.3 . . ? C48 O5 H5A 118.6 . . ? C57 O6 H6A 109.5 . . ? C6 C1 C2 118.3(5) . . ? C6 C1 H1B 120.8 . . ? C2 C1 H1B 120.8 . . ? C3 C2 C1 121.8(5) . . ? C3 C2 H2B 119.1 . . ? C1 C2 H2B 119.1 . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3B 120.5 . . ? C4 C3 H3B 120.5 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4B 120.2 . . ? C3 C4 H4B 120.2 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 C54 126.2(4) . . ? C6 C5 C54 112.9(3) . . ? C1 C6 C5 120.3(4) . . ? C1 C6 C53 126.8(4) . . ? C5 C6 C53 112.9(3) . . ? C12 C7 C13 117.5(4) . . ? C12 C7 C14 122.5(4) . . ? C13 C7 C14 119.9(4) . . ? C13 C8 C10 120.5(4) . . ? C13 C8 C53 127.2(4) . . ? C10 C8 C53 112.2(4) . . ? C11 C10 C8 119.5(4) . . ? C11 C10 C54 127.1(4) . . ? C8 C10 C54 113.4(4) . . ? C10 C11 C12 119.1(4) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? O1 C12 C7 121.1(4) . . ? O1 C12 C11 116.8(4) . . ? C7 C12 C11 122.1(4) . . ? C8 C13 C7 121.3(4) . . ? C8 C13 H13A 119.4 . . ? C7 C13 H13A 119.4 . . ? C7 C14 C15 114.0(3) . . ? C7 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? C7 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.6 . . ? C16 C15 C20 117.8(4) . . ? C16 C15 C14 120.3(4) . . ? C20 C15 C14 121.8(4) . . ? C17 C16 C15 123.3(4) . . ? C17 C16 H16A 118.3 . . ? C15 C16 H16A 118.3 . . ? C16 C17 C18 116.9(4) . . ? C16 C17 C58 121.9(4) . . ? C18 C17 C58 121.3(4) . . ? C19 C18 C17 122.1(4) . . ? C19 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? C18 C19 C20 118.9(4) . . ? C18 C19 C21 120.3(4) . . ? C20 C19 C21 120.8(4) . . ? O2 C20 C15 116.7(4) . . ? O2 C20 C19 122.5(4) . . ? C15 C20 C19 120.8(4) . . ? C19 C21 C22 111.9(3) . . ? C19 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C19 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C27 119.0(4) . . ? C23 C22 C21 119.3(4) . . ? C27 C22 C21 121.7(4) . . ? C22 C23 C24 120.8(4) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C23 C24 C25 119.4(4) . . ? C23 C24 C28 126.9(4) . . ? C25 C24 C28 113.6(4) . . ? C26 C25 C24 120.2(4) . . ? C26 C25 C31 127.1(4) . . ? C24 C25 C31 112.8(4) . . ? C25 C26 C27 119.0(4) . . ? C25 C26 H26A 120.5 . . ? C27 C26 H26A 120.5 . . ? C22 C27 C26 121.7(4) . . ? C22 C27 O3 117.2(4) . . ? C26 C27 O3 121.0(4) . . ? C24 C28 C37 105.4(3) . . ? C24 C28 C29 106.1(3) . . ? C37 C28 C29 104.4(3) . . ? C24 C28 H28A 113.4 . . ? C37 C28 H28A 113.4 . . ? C29 C28 H28A 113.4 . . ? C41 C29 C30 120.1(4) . . ? C41 C29 C28 126.9(4) . . ? C30 C29 C28 112.7(4) . . ? C38 C30 C29 119.7(4) . . ? C38 C30 C31 126.2(4) . . ? C29 C30 C31 114.1(4) . . ? C30 C31 C32 104.4(3) . . ? C30 C31 C25 106.6(3) . . ? C32 C31 C25 105.9(3) . . ? C30 C31 H31A 113.1 . . ? C32 C31 H31A 113.1 . . ? C25 C31 H31A 113.1 . . ? C33 C32 C37 118.7(4) . . ? C33 C32 C31 127.3(4) . . ? C37 C32 C31 114.0(4) . . ? C34 C33 C32 120.4(5) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 C36 119.6(4) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? C37 C36 C35 119.8(5) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C36 C37 C32 121.2(4) . . ? C36 C37 C28 126.5(4) . . ? C32 C37 C28 112.2(4) . . ? C30 C38 C39 119.8(4) . . ? C30 C38 H38A 120.1 . . ? C39 C38 H38A 120.1 . . ? O4 C39 C40 118.8(4) . . ? O4 C39 C38 119.9(4) . . ? C40 C39 C38 121.3(4) . . ? C39 C40 C41 117.7(4) . . ? C39 C40 C42 122.3(4) . . ? C41 C40 C42 120.0(4) . . ? C29 C41 C40 121.1(4) . . ? C29 C41 H41A 119.5 . . ? C40 C41 H41A 119.5 . . ? C43 C42 C40 114.3(4) . . ? C43 C42 H42A 108.7 . . ? C40 C42 H42A 108.7 . . ? C43 C42 H42B 108.7 . . ? C40 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C44 C43 C48 118.3(5) . . ? C44 C43 C42 120.4(4) . . ? C48 C43 C42 121.3(4) . . ? C45 C44 C43 122.7(5) . . ? C45 C44 H44A 118.6 . . ? C43 C44 H44A 118.6 . . ? C44 C45 C46 117.1(4) . . ? C44 C45 C62 122.2(5) . . ? C46 C45 C62 120.6(5) . . ? C47 C46 C45 122.0(5) . . ? C47 C46 H46A 119.0 . . ? C45 C46 H46A 119.0 . . ? C46 C47 C48 118.2(4) . . ? C46 C47 C49 120.5(4) . . ? C48 C47 C49 121.3(4) . . ? C43 C48 O5 120.4(4) . . ? C43 C48 C47 121.7(4) . . ? O5 C48 C47 117.9(4) . . ? C50 C49 C47 114.2(3) . . ? C50 C49 H49A 108.7 . . ? C47 C49 H49A 108.7 . . ? C50 C49 H49B 108.7 . . ? C47 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? C57 C50 C51 117.7(4) . . ? C57 C50 C49 121.7(4) . . ? C51 C50 C49 120.6(4) . . ? C52 C51 C50 122.2(4) . . ? C52 C51 H51A 118.9 . . ? C50 C51 H51A 118.9 . . ? C51 C52 C55 118.8(4) . . ? C51 C52 C53 128.9(4) . . ? C55 C52 C53 112.3(4) . . ? C6 C53 C52 106.9(3) . . ? C6 C53 C8 105.0(3) . . ? C52 C53 C8 106.8(3) . . ? C6 C53 H53A 112.5 . . ? C52 C53 H53A 112.5 . . ? C8 C53 H53A 112.5 . . ? C10 C54 C5 105.4(3) . . ? C10 C54 C55 106.8(3) . . ? C5 C54 C55 105.2(3) . . ? C10 C54 H54A 112.9 . . ? C5 C54 H54A 112.9 . . ? C55 C54 H54A 112.9 . . ? C56 C55 C52 120.4(4) . . ? C56 C55 C54 126.9(4) . . ? C52 C55 C54 112.7(4) . . ? C55 C56 C57 119.4(4) . . ? C55 C56 H56A 120.3 . . ? C57 C56 H56A 120.3 . . ? O6 C57 C50 119.9(4) . . ? O6 C57 C56 118.6(4) . . ? C50 C57 C56 121.5(4) . . ? C59 C58 C60 115.0(8) . . ? C59 C58 C60' 136.7(10) . . ? C60 C58 C60' 61.5(12) . . ? C59 C58 C61' 47.7(12) . . ? C60 C58 C61' 132.2(12) . . ? C60' C58 C61' 99.9(15) . . ? C59 C58 C61 109.8(7) . . ? C60 C58 C61 102.5(8) . . ? C60' C58 C61 42.7(11) . . ? C61' C58 C61 62.8(13) . . ? C59 C58 C17 107.9(5) . . ? C60 C58 C17 112.2(6) . . ? C60' C58 C17 112.9(9) . . ? C61' C58 C17 115.6(11) . . ? C61 C58 C17 109.3(5) . . ? C59 C58 C59' 71.5(11) . . ? C60 C58 C59' 46.0(9) . . ? C60' C58 C59' 103.2(14) . . ? C61' C58 C59' 109.3(15) . . ? C61 C58 C59' 133.4(9) . . ? C17 C58 C59' 114.3(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 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C58 C61 H61A 109.5 . . ? C58 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C58 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C58 C59' H59D 109.5 . . ? C58 C59' H59E 109.5 . . ? H59D C59' H59E 109.5 . . ? C58 C59' H59F 109.5 . . ? H59D C59' H59F 109.5 . . ? H59E C59' H59F 109.5 . . ? C58 C60' H60D 109.5 . . ? C58 C60' H60E 109.5 . . ? H60D C60' H60E 109.5 . . ? C58 C60' H60F 109.5 . . ? H60D C60' H60F 109.5 . . ? H60E C60' H60F 109.5 . . ? C58 C61' H61D 109.5 . . ? C58 C61' H61E 109.5 . . ? H61D C61' H61E 109.5 . . ? C58 C61' H61F 109.5 . . ? H61D C61' H61F 109.5 . . ? H61E C61' H61F 109.5 . . ? C64 C62 C65 112.8(8) . . ? C64 C62 C45 111.9(5) . . ? C65 C62 C45 107.3(5) . . ? C64 C62 C63 106.4(7) . . ? C65 C62 C63 108.2(6) . . ? C45 C62 C63 110.2(6) . . ? 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 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 H66A 109.5 . . ? C67 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C67 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O8 C67 C68 124.1(7) . . ? O8 C67 C66 121.6(7) . . ? C68 C67 C66 113.0(7) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? O7 C70 C71 122.5(6) . . ? O7 C70 C69 122.4(6) . . ? C71 C70 C69 115.2(5) . . ? C70 C71 H71A 109.5 . . ? 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 . . ? C73 C72 H72A 109.5 . . ? C73 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C73 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O9 C73 C72 125.4(10) . . ? O9 C73 C74 120.6(12) . . ? C72 C73 C74 110.0(18) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0(8) . . . . ? C1 C2 C3 C4 -0.5(9) . . . . ? C2 C3 C4 C5 -0.1(8) . . . . ? C3 C4 C5 C6 1.3(7) . . . . ? C3 C4 C5 C54 -178.0(5) . . . . ? C2 C1 C6 C5 1.2(7) . . . . ? C2 C1 C6 C53 -179.6(5) . . . . ? C4 C5 C6 C1 -1.8(7) . . . . ? C54 C5 C6 C1 177.5(4) . . . . ? C4 C5 C6 C53 178.9(4) . . . . ? C54 C5 C6 C53 -1.8(5) . . . . ? C13 C8 C10 C11 3.2(6) . . . . ? C53 C8 C10 C11 179.3(4) . . . . ? C13 C8 C10 C54 -176.5(4) . . . . ? C53 C8 C10 C54 -0.4(5) . . . . ? C8 C10 C11 C12 -2.6(6) . . . . ? C54 C10 C11 C12 177.1(4) . . . . ? C13 C7 C12 O1 -179.6(4) . . . . ? C14 C7 C12 O1 3.7(6) . . . . ? C13 C7 C12 C11 1.1(6) . . . . ? C14 C7 C12 C11 -175.6(4) . . . . ? C10 C11 C12 O1 -178.9(4) . . . . ? C10 C11 C12 C7 0.4(6) . . . . ? C10 C8 C13 C7 -1.7(6) . . . . ? C53 C8 C13 C7 -177.1(4) . . . . ? C12 C7 C13 C8 -0.5(6) . . . . ? C14 C7 C13 C8 176.4(4) . . . . ? C12 C7 C14 C15 -98.3(5) . . . . ? C13 C7 C14 C15 85.1(5) . . . . ? C7 C14 C15 C16 -92.7(5) . . . . ? C7 C14 C15 C20 86.0(5) . . . . ? C20 C15 C16 C17 2.0(6) . . . . ? C14 C15 C16 C17 -179.2(4) . . . . ? C15 C16 C17 C18 1.1(6) . . . . ? C15 C16 C17 C58 -177.6(4) . . . . ? C16 C17 C18 C19 -1.7(6) . . . . ? C58 C17 C18 C19 177.0(4) . . . . ? C17 C18 C19 C20 -0.9(6) . . . . ? C17 C18 C19 C21 -178.1(4) . . . . ? C16 C15 C20 O2 178.5(4) . . . . ? C14 C15 C20 O2 -0.3(6) . . . . ? C16 C15 C20 C19 -4.7(6) . . . . ? C14 C15 C20 C19 176.5(4) . . . . ? C18 C19 C20 O2 -179.2(4) . . . . ? C21 C19 C20 O2 -2.1(6) . . . . ? C18 C19 C20 C15 4.2(6) . . . . ? C21 C19 C20 C15 -178.7(4) . . . . ? C18 C19 C21 C22 94.5(5) . . . . ? C20 C19 C21 C22 -82.6(5) . . . . ? C19 C21 C22 C23 -73.9(5) . . . . ? C19 C21 C22 C27 102.7(5) . . . . ? C27 C22 C23 C24 0.5(6) . . . . ? C21 C22 C23 C24 177.2(4) . . . . ? C22 C23 C24 C25 0.7(6) . . . . ? C22 C23 C24 C28 178.2(4) . . . . ? C23 C24 C25 C26 -0.8(6) . . . . ? C28 C24 C25 C26 -178.6(4) . . . . ? C23 C24 C25 C31 178.3(3) . . . . ? C28 C24 C25 C31 0.5(5) . . . . ? C24 C25 C26 C27 -0.2(6) . . . . ? C31 C25 C26 C27 -179.2(4) . . . . ? C23 C22 C27 C26 -1.7(6) . . . . ? C21 C22 C27 C26 -178.2(4) . . . . ? C23 C22 C27 O3 176.1(4) . . . . ? C21 C22 C27 O3 -0.5(6) . . . . ? C25 C26 C27 C22 1.5(6) . . . . ? C25 C26 C27 O3 -176.2(4) . . . . ? C23 C24 C28 C37 -122.1(4) . . . . ? C25 C24 C28 C37 55.5(4) . . . . ? C23 C24 C28 C29 127.6(4) . . . . ? C25 C24 C28 C29 -54.8(4) . . . . ? C24 C28 C29 C41 -133.0(4) . . . . ? C37 C28 C29 C41 116.0(5) . . . . ? C24 C28 C29 C30 54.0(4) . . . . ? C37 C28 C29 C30 -57.0(4) . . . . ? C41 C29 C30 C38 5.3(6) . . . . ? C28 C29 C30 C38 178.7(4) . . . . ? C41 C29 C30 C31 -172.6(4) . . . . ? C28 C29 C30 C31 0.9(5) . . . . ? C38 C30 C31 C32 -121.7(4) . . . . ? C29 C30 C31 C32 55.9(5) . . . . ? C38 C30 C31 C25 126.4(4) . . . . ? C29 C30 C31 C25 -55.9(4) . . . . ? C26 C25 C31 C30 -126.0(4) . . . . ? C24 C25 C31 C30 54.9(4) . . . . ? C26 C25 C31 C32 123.2(4) . . . . ? C24 C25 C31 C32 -55.9(4) . . . . ? C30 C31 C32 C33 123.1(5) . . . . ? C25 C31 C32 C33 -124.6(5) . . . . ? C30 C31 C32 C37 -57.2(5) . . . . ? C25 C31 C32 C37 55.1(4) . . . . ? C37 C32 C33 C34 1.4(7) . . . . ? C31 C32 C33 C34 -178.9(4) . . . . ? C32 C33 C34 C35 -1.4(7) . . . . ? C33 C34 C35 C36 0.4(8) . . . . ? C34 C35 C36 C37 0.4(7) . . . . ? C35 C36 C37 C32 -0.4(7) . . . . ? C35 C36 C37 C28 178.0(4) . . . . ? C33 C32 C37 C36 -0.5(6) . . . . ? C31 C32 C37 C36 179.8(4) . . . . ? C33 C32 C37 C28 -179.1(4) . . . . ? C31 C32 C37 C28 1.2(5) . . . . ? C24 C28 C37 C36 125.4(5) . . . . ? C29 C28 C37 C36 -123.1(5) . . . . ? C24 C28 C37 C32 -56.2(4) . . . . ? C29 C28 C37 C32 55.4(4) . . . . ? C29 C30 C38 C39 -3.3(6) . . . . ? C31 C30 C38 C39 174.2(4) . . . . ? C30 C38 C39 O4 -179.3(4) . . . . ? C30 C38 C39 C40 -1.6(7) . . . . ? O4 C39 C40 C41 -177.8(4) . . . . ? C38 C39 C40 C41 4.5(6) . . . . ? O4 C39 C40 C42 4.9(7) . . . . ? C38 C39 C40 C42 -172.8(4) . . . . ? C30 C29 C41 C40 -2.3(6) . . . . ? C28 C29 C41 C40 -174.8(4) . . . . ? C39 C40 C41 C29 -2.5(6) . . . . ? C42 C40 C41 C29 174.8(4) . . . . ? C39 C40 C42 C43 -101.0(5) . . . . ? C41 C40 C42 C43 81.8(5) . . . . ? C40 C42 C43 C44 -97.7(5) . . . . ? C40 C42 C43 C48 83.3(6) . . . . ? C48 C43 C44 C45 0.2(7) . . . . ? C42 C43 C44 C45 -178.8(4) . . . . ? C43 C44 C45 C46 -0.9(7) . . . . ? C43 C44 C45 C62 -176.8(5) . . . . ? C44 C45 C46 C47 1.9(7) . . . . ? C62 C45 C46 C47 177.9(4) . . . . ? C45 C46 C47 C48 -2.1(6) . . . . ? C45 C46 C47 C49 178.9(4) . . . . ? C44 C43 C48 O5 -178.1(4) . . . . ? C42 C43 C48 O5 0.9(6) . . . . ? C44 C43 C48 C47 -0.4(6) . . . . ? C42 C43 C48 C47 178.6(4) . . . . ? C46 C47 C48 C43 1.3(6) . . . . ? C49 C47 C48 C43 -179.6(4) . . . . ? C46 C47 C48 O5 179.1(4) . . . . ? C49 C47 C48 O5 -1.9(5) . . . . ? C46 C47 C49 C50 101.5(5) . . . . ? C48 C47 C49 C50 -77.6(5) . . . . ? C47 C49 C50 C57 101.1(5) . . . . ? C47 C49 C50 C51 -78.5(5) . . . . ? C57 C50 C51 C52 0.9(6) . . . . ? C49 C50 C51 C52 -179.5(4) . . . . ? C50 C51 C52 C55 -1.4(6) . . . . ? C50 C51 C52 C53 176.9(4) . . . . ? C1 C6 C53 C52 125.4(5) . . . . ? C5 C6 C53 C52 -55.4(5) . . . . ? C1 C6 C53 C8 -121.4(5) . . . . ? C5 C6 C53 C8 57.8(4) . . . . ? C51 C52 C53 C6 -122.7(5) . . . . ? C55 C52 C53 C6 55.7(4) . . . . ? C51 C52 C53 C8 125.3(4) . . . . ? C55 C52 C53 C8 -56.3(4) . . . . ? C13 C8 C53 C6 119.1(4) . . . . ? C10 C8 C53 C6 -56.7(4) . . . . ? C13 C8 C53 C52 -127.6(4) . . . . ? C10 C8 C53 C52 56.6(4) . . . . ? C11 C10 C54 C5 -123.3(4) . . . . ? C8 C10 C54 C5 56.4(4) . . . . ? C11 C10 C54 C55 125.1(4) . . . . ? C8 C10 C54 C55 -55.2(4) . . . . ? C4 C5 C54 C10 124.0(5) . . . . ? C6 C5 C54 C10 -55.3(5) . . . . ? C4 C5 C54 C55 -123.3(5) . . . . ? C6 C5 C54 C55 57.4(4) . . . . ? C51 C52 C55 C56 1.3(6) . . . . ? C53 C52 C55 C56 -177.3(4) . . . . ? C51 C52 C55 C54 179.2(4) . . . . ? C53 C52 C55 C54 0.6(5) . . . . ? C10 C54 C55 C56 -127.1(4) . . . . ? C5 C54 C55 C56 121.2(4) . . . . ? C10 C54 C55 C52 55.1(4) . . . . ? C5 C54 C55 C52 -56.6(4) . . . . ? C52 C55 C56 C57 -0.7(6) . . . . ? C54 C55 C56 C57 -178.3(4) . . . . ? C51 C50 C57 O6 -179.1(4) . . . . ? C49 C50 C57 O6 1.3(6) . . . . ? C51 C50 C57 C56 -0.2(6) . . . . ? C49 C50 C57 C56 -179.8(4) . . . . ? C55 C56 C57 O6 179.0(4) . . . . ? C55 C56 C57 C50 0.1(6) . . . . ? C16 C17 C58 C59 72.9(8) . . . . ? C18 C17 C58 C59 -105.8(7) . . . . ? C16 C17 C58 C60 -159.5(8) . . . . ? C18 C17 C58 C60 21.9(9) . . . . ? C16 C17 C58 C60' -92.2(14) . . . . ? C18 C17 C58 C60' 89.1(14) . . . . ? C16 C17 C58 C61' 21.9(15) . . . . ? C18 C17 C58 C61' -156.7(15) . . . . ? C16 C17 C58 C61 -46.5(7) . . . . ? C18 C17 C58 C61 134.9(6) . . . . ? C16 C17 C58 C59' 150.2(12) . . . . ? C18 C17 C58 C59' -28.4(12) . . . . ? C44 C45 C62 C64 -147.8(7) . . . . ? C46 C45 C62 C64 36.4(9) . . . . ? C44 C45 C62 C65 88.0(8) . . . . ? C46 C45 C62 C65 -87.8(7) . . . . ? C44 C45 C62 C63 -29.6(7) . . . . ? C46 C45 C62 C63 154.6(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O2 0.84 1.90 2.743(5) 175.4 . O2 H2A O3 0.84 1.99 2.832(5) 179.4 . O3 H3A O7 0.84 1.91 2.746(5) 179.5 3_657 O4 H4A O9 0.84 1.99 2.826(10) 178.8 1_656 O5 H5A O4 0.84 1.93 2.768(5) 177.8 . O6 H6A O5 0.84 1.91 2.736(5) 165.8 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.375 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.074 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 1.000 681 142 ' ' 2 0.500 0.000 0.500 681 142 ' '