data_katya3lm _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H93 N3 O18' _chemical_formula_weight 1432.61 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' 'N' 'N' 0.0061 0.0033 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.231(3) _cell_length_b 14.444(4) _cell_length_c 23.916(6) _cell_angle_alpha 82.718(6) _cell_angle_beta 87.233(6) _cell_angle_gamma 69.734(5) _cell_volume 3931.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9849 _exptl_absorpt_correction_T_max 0.9941 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45239 _diffrn_reflns_av_R_equivalents 0.1016 _diffrn_reflns_av_sigmaI/netI 0.2508 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.00 _reflns_number_total 17039 _reflns_number_gt 5724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^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 17039 _refine_ls_number_parameters 970 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1817 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 0.730 _refine_ls_restrained_S_all 0.730 _refine_ls_shift/su_max 0.371 _refine_ls_shift/su_mean 0.010 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 C1 C 0.1660(3) 0.4709(2) 0.33000(14) 0.0222(8) Uani 1 1 d . . . C2 C 0.1321(3) 0.5189(2) 0.37781(13) 0.0210(8) Uani 1 1 d . . . C3 C 0.0253(3) 0.5954(2) 0.37764(14) 0.0259(9) Uani 1 1 d . . . H3 H 0.0026 0.6297 0.4100 0.031 Uiso 1 1 calc R . . C4 C -0.0498(3) 0.6236(2) 0.33148(14) 0.0245(9) Uani 1 1 d . . . C5 C -0.0108(3) 0.5752(2) 0.28353(14) 0.0267(9) Uani 1 1 d . . . H5 H -0.0586 0.5949 0.2509 0.032 Uiso 1 1 calc R . . C6 C 0.0961(3) 0.4988(2) 0.28236(14) 0.0233(9) Uani 1 1 d . . . C7 C 0.1372(3) 0.4489(3) 0.22995(14) 0.0277(9) Uani 1 1 d . . . C8 C 0.0626(3) 0.4125(2) 0.14054(14) 0.0235(9) Uani 1 1 d . . . C9 C 0.0502(3) 0.4245(2) 0.19798(14) 0.0235(9) Uani 1 1 d . . . C10 C -0.0474(3) 0.4110(2) 0.22536(14) 0.0306(9) Uani 1 1 d . . . H10 H -0.0558 0.4165 0.2646 0.037 Uiso 1 1 calc R . . C11 C -0.1335(3) 0.3900(2) 0.19858(14) 0.0252(9) Uani 1 1 d . . . C12 C -0.1149(3) 0.3764(2) 0.14172(14) 0.0273(9) Uani 1 1 d . . . H12 H -0.1706 0.3606 0.1221 0.033 Uiso 1 1 calc R . . C13 C -0.0163(3) 0.3856(2) 0.11308(14) 0.0231(9) Uani 1 1 d . . . C14 C -0.0010(3) 0.3710(3) 0.05171(14) 0.0248(9) Uani 1 1 d . . . C15 C 0.1524(3) 0.1962(3) 0.06165(13) 0.0225(8) Uani 1 1 d . . . C16 C 0.1060(3) 0.2914(2) 0.03313(13) 0.0225(8) Uani 1 1 d . . . C17 C 0.1607(3) 0.3155(3) -0.01621(14) 0.0266(9) Uani 1 1 d . . . H17 H 0.1288 0.3801 -0.0362 0.032 Uiso 1 1 calc R . . C18 C 0.2609(3) 0.2477(3) -0.03710(14) 0.0287(9) Uani 1 1 d . . . C19 C 0.3041(3) 0.1539(3) -0.00692(14) 0.0295(9) Uani 1 1 d . . . H19 H 0.3722 0.1066 -0.0205 0.035 Uiso 1 1 calc R . . C20 C 0.2520(3) 0.1259(2) 0.04260(13) 0.0224(8) Uani 1 1 d . . . C21 C 0.3061(3) 0.0208(3) 0.06955(14) 0.0270(9) Uani 1 1 d . . . C22 C 0.3164(3) 0.0512(2) 0.17169(14) 0.0212(8) Uani 1 1 d . . . C23 C 0.3038(3) -0.0072(2) 0.13218(13) 0.0210(8) Uani 1 1 d . . . C24 C 0.3014(3) -0.1026(2) 0.15139(14) 0.0239(9) Uani 1 1 d . . . H24 H 0.2956 -0.1437 0.1245 0.029 Uiso 1 1 calc R . . C25 C 0.3069(3) -0.1390(2) 0.20802(14) 0.0211(8) Uani 1 1 d . . . C26 C 0.3153(3) -0.0754(2) 0.24539(14) 0.0228(8) Uani 1 1 d . . . H26 H 0.3180 -0.0979 0.2845 0.027 Uiso 1 1 calc R . . C27 C 0.3199(3) 0.0186(2) 0.22919(14) 0.0197(8) Uani 1 1 d . . . C28 C 0.3344(3) 0.0813(3) 0.27139(14) 0.0240(9) Uani 1 1 d . . . C29 C 0.3088(3) 0.0992(2) 0.37524(14) 0.0195(8) Uani 1 1 d . . . C30 C 0.2688(3) 0.0804(2) 0.32578(13) 0.0191(8) Uani 1 1 d . . . C31 C 0.1622(3) 0.0632(2) 0.32876(13) 0.0205(8) Uani 1 1 d . . . H31 H 0.1316 0.0537 0.2950 0.025 Uiso 1 1 calc R . . C32 C 0.0993(3) 0.0595(2) 0.37843(14) 0.0210(8) Uani 1 1 d . . . C33 C 0.1431(3) 0.0806(2) 0.42623(14) 0.0214(8) Uani 1 1 d . . . H33 H 0.1014 0.0801 0.4608 0.026 Uiso 1 1 calc R . . C34 C 0.2448(3) 0.1022(2) 0.42523(13) 0.0196(8) Uani 1 1 d . . . C35 C 0.2895(3) 0.1238(3) 0.47755(14) 0.0220(8) Uani 1 1 d . . . C36 C 0.2489(3) 0.3083(3) 0.45125(13) 0.0189(8) Uani 1 1 d . . . C37 C 0.3187(3) 0.2162(2) 0.47614(13) 0.0195(8) Uani 1 1 d . . . C38 C 0.4224(3) 0.2087(2) 0.50177(13) 0.0225(8) Uani 1 1 d . . . H38 H 0.4700 0.1460 0.5196 0.027 Uiso 1 1 calc R . . C39 C 0.4578(3) 0.2900(3) 0.50200(13) 0.0212(8) Uani 1 1 d . . . C40 C 0.3846(3) 0.3811(2) 0.47678(13) 0.0228(8) Uani 1 1 d . . . H40 H 0.4070 0.4379 0.4766 0.027 Uiso 1 1 calc R . . C41 C 0.2801(3) 0.3922(2) 0.45184(13) 0.0198(8) Uani 1 1 d . . . C42 C 0.2060(3) 0.4959(3) 0.42966(14) 0.0242(9) Uani 1 1 d . . . C43 C -0.1692(3) 0.7042(3) 0.33463(15) 0.0319(10) Uani 1 1 d . . . C44 C -0.2379(3) 0.6697(3) 0.38375(18) 0.0779(16) Uani 1 1 d . . . H44A H -0.3137 0.7217 0.3876 0.117 Uiso 1 1 calc R . . H44B H -0.1939 0.6565 0.4188 0.117 Uiso 1 1 calc R . . H44C H -0.2498 0.6088 0.3760 0.117 Uiso 1 1 calc R . . C45 C -0.1551(4) 0.7981(3) 0.3466(2) 0.100(2) Uani 1 1 d . . . H45A H -0.1118 0.8211 0.3157 0.150 Uiso 1 1 calc R . . H45B H -0.1122 0.7861 0.3819 0.150 Uiso 1 1 calc R . . H45C H -0.2320 0.8488 0.3501 0.150 Uiso 1 1 calc R . . C46 C -0.2408(3) 0.7197(3) 0.28265(18) 0.0696(15) Uani 1 1 d . . . H46A H -0.2052 0.7485 0.2507 0.104 Uiso 1 1 calc R . . H46B H -0.3200 0.7649 0.2888 0.104 Uiso 1 1 calc R . . H46C H -0.2436 0.6557 0.2746 0.104 Uiso 1 1 calc R . . C47 C -0.2414(3) 0.3819(3) 0.23074(15) 0.0326(10) Uani 1 1 d . . . C48 C -0.2901(4) 0.4646(3) 0.26920(18) 0.0690(15) Uani 1 1 d . . . H48A H -0.3117 0.5295 0.2463 0.104 Uiso 1 1 calc R . . H48B H -0.2305 0.4596 0.2965 0.104 Uiso 1 1 calc R . . H48C H -0.3590 0.4575 0.2893 0.104 Uiso 1 1 calc R . . C49 C -0.2029(4) 0.2845(3) 0.26979(18) 0.0700(15) Uani 1 1 d . . . H49A H -0.2647 0.2841 0.2974 0.105 Uiso 1 1 calc R . . H49B H -0.1317 0.2779 0.2895 0.105 Uiso 1 1 calc R . . H49C H -0.1876 0.2287 0.2476 0.105 Uiso 1 1 calc R . . C50 C -0.3370(3) 0.3893(4) 0.19209(17) 0.0774(17) Uani 1 1 d . . . H50A H -0.3561 0.4516 0.1668 0.116 Uiso 1 1 calc R . . H50B H -0.4061 0.3882 0.2143 0.116 Uiso 1 1 calc R . . H50C H -0.3116 0.3330 0.1698 0.116 Uiso 1 1 calc R . . C51 C 0.3227(3) 0.2754(3) -0.09059(15) 0.0411(11) Uani 1 1 d . . . C52 C 0.4414(7) 0.2863(6) -0.0700(3) 0.040(2) Uiso 0.50 1 d P . . H52A H 0.4874 0.2245 -0.0476 0.060 Uiso 0.50 1 calc PR . . H52B H 0.4217 0.3414 -0.0469 0.060 Uiso 0.50 1 calc PR . . H52C H 0.4868 0.2995 -0.1029 0.060 Uiso 0.50 1 calc PR . . C53 C 0.2575(7) 0.3703(6) -0.1227(4) 0.050(3) Uiso 0.50 1 d P . . H53A H 0.3008 0.3805 -0.1571 0.075 Uiso 0.50 1 calc PR . . H53B H 0.2469 0.4243 -0.0997 0.075 Uiso 0.50 1 calc PR . . H53C H 0.1812 0.3695 -0.1327 0.075 Uiso 0.50 1 calc PR . . C54 C 0.3619(7) 0.1828(6) -0.1272(3) 0.026(2) Uiso 0.50 1 d P . . H54A H 0.4002 0.1996 -0.1620 0.039 Uiso 0.50 1 calc PR . . H54B H 0.2931 0.1679 -0.1366 0.039 Uiso 0.50 1 calc PR . . H54C H 0.4163 0.1245 -0.1053 0.039 Uiso 0.50 1 calc PR . . C55 C 0.3087(3) -0.2437(2) 0.23000(14) 0.0239(9) Uani 1 1 d . . . C56 C 0.2901(3) -0.3003(3) 0.18321(14) 0.0382(10) Uani 1 1 d . . . H56A H 0.2144 -0.2639 0.1654 0.057 Uiso 1 1 calc R . . H56B H 0.2920 -0.3666 0.1995 0.057 Uiso 1 1 calc R . . H56C H 0.3522 -0.3066 0.1549 0.057 Uiso 1 1 calc R . . C57 C 0.4273(3) -0.3022(3) 0.25686(15) 0.0415(11) Uani 1 1 d . . . H57A H 0.4887 -0.3071 0.2283 0.062 Uiso 1 1 calc R . . H57B H 0.4292 -0.3690 0.2720 0.062 Uiso 1 1 calc R . . H57C H 0.4400 -0.2679 0.2874 0.062 Uiso 1 1 calc R . . C58 C 0.2129(3) -0.2389(3) 0.27483(15) 0.0401(11) Uani 1 1 d . . . H58A H 0.2247 -0.2050 0.3058 0.060 Uiso 1 1 calc R . . H58B H 0.2167 -0.3064 0.2894 0.060 Uiso 1 1 calc R . . H58C H 0.1364 -0.2022 0.2578 0.060 Uiso 1 1 calc R . . C59 C -0.0100(3) 0.0307(3) 0.38271(14) 0.0244(9) Uani 1 1 d . . . C60 C -0.0490(3) 0.0174(3) 0.32472(13) 0.0297(9) Uani 1 1 d . . . H60A H 0.0125 -0.0366 0.3087 0.045 Uiso 1 1 calc R . . H60B H -0.0638 0.0792 0.2993 0.045 Uiso 1 1 calc R . . H60C H -0.1205 0.0010 0.3293 0.045 Uiso 1 1 calc R . . C61 C 0.0164(3) -0.0688(3) 0.42077(14) 0.0356(10) Uani 1 1 d . . . H61A H 0.0749 -0.1215 0.4025 0.053 Uiso 1 1 calc R . . H61B H -0.0552 -0.0847 0.4269 0.053 Uiso 1 1 calc R . . H61C H 0.0462 -0.0634 0.4571 0.053 Uiso 1 1 calc R . . C62 C -0.1116(3) 0.1116(3) 0.40843(14) 0.0352(10) Uani 1 1 d . . . H62A H -0.1785 0.0890 0.4149 0.053 Uiso 1 1 calc R . . H62B H -0.1338 0.1731 0.3823 0.053 Uiso 1 1 calc R . . H62C H -0.0869 0.1240 0.4443 0.053 Uiso 1 1 calc R . . C63 C 0.5734(3) 0.2831(3) 0.52802(15) 0.0269(9) Uani 1 1 d . . . C64 C 0.6397(3) 0.1779(3) 0.55559(17) 0.0510(12) Uani 1 1 d . . . H64A H 0.5913 0.1581 0.5852 0.077 Uiso 1 1 calc R . . H64B H 0.7120 0.1767 0.5721 0.077 Uiso 1 1 calc R . . H64C H 0.6584 0.1315 0.5271 0.077 Uiso 1 1 calc R . . C65 C 0.5493(3) 0.3549(3) 0.57287(14) 0.0354(10) Uani 1 1 d . . . H65A H 0.5097 0.4230 0.5555 0.053 Uiso 1 1 calc R . . H65B H 0.6232 0.3505 0.5892 0.053 Uiso 1 1 calc R . . H65C H 0.4997 0.3372 0.6026 0.053 Uiso 1 1 calc R . . C66 C 0.6512(3) 0.3111(3) 0.48128(14) 0.0371(10) Uani 1 1 d . . . H66A H 0.6665 0.2654 0.4526 0.056 Uiso 1 1 calc R . . H66B H 0.7252 0.3067 0.4976 0.056 Uiso 1 1 calc R . . H66C H 0.6116 0.3793 0.4639 0.056 Uiso 1 1 calc R . . C67 C 0.3705(3) 0.4098(3) 0.32352(15) 0.0316(10) Uani 1 1 d . . . C68 C 0.4695(3) 0.3152(3) 0.32110(17) 0.0473(12) Uani 1 1 d . . . H68A H 0.5431 0.3280 0.3214 0.071 Uiso 1 1 calc R . . H68B H 0.4646 0.2872 0.2865 0.071 Uiso 1 1 calc R . . H68C H 0.4663 0.2681 0.3539 0.071 Uiso 1 1 calc R . . C69 C 0.1610(3) 0.5216(3) 0.10217(14) 0.0306(10) Uani 1 1 d . . . C70 C 0.2692(3) 0.5234(3) 0.07074(15) 0.0376(10) Uani 1 1 d . . . H70A H 0.2593 0.5917 0.0548 0.056 Uiso 1 1 calc R . . H70B H 0.2836 0.4811 0.0403 0.056 Uiso 1 1 calc R . . H70C H 0.3356 0.4985 0.0966 0.056 Uiso 1 1 calc R . . C71 C 0.0466(3) 0.0997(3) 0.11115(16) 0.0291(9) Uani 1 1 d . . . C72 C -0.0057(3) 0.0841(3) 0.16755(14) 0.0397(11) Uani 1 1 d . . . H72A H -0.0850 0.1321 0.1690 0.060 Uiso 1 1 calc R . . H72B H 0.0418 0.0933 0.1968 0.060 Uiso 1 1 calc R . . H72C H -0.0081 0.0164 0.1739 0.060 Uiso 1 1 calc R . . C73 C 0.4218(3) 0.1529(3) 0.13312(16) 0.0357(10) Uani 1 1 d . . . C74 C 0.4193(3) 0.2576(3) 0.12345(16) 0.0455(11) Uani 1 1 d . . . H74A H 0.4985 0.2582 0.1157 0.068 Uiso 1 1 calc R . . H74B H 0.3885 0.2906 0.1571 0.068 Uiso 1 1 calc R . . H74C H 0.3692 0.2928 0.0912 0.068 Uiso 1 1 calc R . . C75 C 0.5142(3) 0.0365(3) 0.36619(14) 0.0260(9) Uani 1 1 d . . . C76 C 0.6189(3) 0.0667(2) 0.36791(14) 0.0306(9) Uani 1 1 d . . . H76A H 0.6883 0.0074 0.3756 0.046 Uiso 1 1 calc R . . H76B H 0.6089 0.1096 0.3978 0.046 Uiso 1 1 calc R . . H76C H 0.6281 0.1031 0.3315 0.046 Uiso 1 1 calc R . . C77 C 0.0514(6) 0.3158(5) 0.4536(3) 0.0325(17) Uiso 0.60 1 d P . . C77A C 0.0385(8) 0.3749(8) 0.4507(4) 0.032(3) Uiso 0.40 1 d P . . C78 C -0.0601(3) 0.3627(3) 0.41944(15) 0.0444(11) Uani 1 1 d . . . C79 C 0.0247(4) 0.8224(3) 0.06557(17) 0.0585(13) Uani 1 1 d . . . H79A H -0.0348 0.8538 0.0365 0.088 Uiso 1 1 calc R . . H79B H 0.0572 0.7508 0.0632 0.088 Uiso 1 1 calc R . . H79C H 0.0870 0.8508 0.0597 0.088 Uiso 1 1 calc R . . C80 C -0.0276(4) 0.8400(3) 0.1208(2) 0.0535(13) Uani 1 1 d . . . C81 C 0.7613(4) 0.0813(3) 0.06530(17) 0.0616(14) Uani 1 1 d . . . H81A H 0.8038 0.0458 0.0342 0.092 Uiso 1 1 calc R . . H81B H 0.6807 0.0823 0.0660 0.092 Uiso 1 1 calc R . . H81C H 0.7991 0.0475 0.1011 0.092 Uiso 1 1 calc R . . C82 C 0.7616(4) 0.1830(4) 0.0573(2) 0.0623(15) Uani 1 1 d . . . C83 C 0.6601(4) -0.0297(4) 0.2247(2) 0.0927(19) Uani 1 1 d . . . H83A H 0.6374 -0.0420 0.2640 0.139 Uiso 1 1 calc R . . H83B H 0.7311 -0.0839 0.2161 0.139 Uiso 1 1 calc R . . H83C H 0.5972 -0.0265 0.1998 0.139 Uiso 1 1 calc R . . C84 C 0.6811(6) 0.0609(5) 0.2162(2) 0.089(2) Uani 1 1 d . . . C52A C 0.3799(10) 0.3441(8) -0.0796(5) 0.093(4) Uiso 0.50 1 d P . . H52D H 0.4405 0.3116 -0.0512 0.139 Uiso 0.50 1 calc PR . . H52E H 0.3224 0.4029 -0.0658 0.139 Uiso 0.50 1 calc PR . . H52F H 0.4153 0.3642 -0.1145 0.139 Uiso 0.50 1 calc PR . . C53A C 0.2210(6) 0.3375(5) -0.1357(3) 0.028(2) Uiso 0.50 1 d P . . H53D H 0.2564 0.3517 -0.1719 0.042 Uiso 0.50 1 calc PR . . H53E H 0.1734 0.4001 -0.1218 0.042 Uiso 0.50 1 calc PR . . H53F H 0.1717 0.2982 -0.1407 0.042 Uiso 0.50 1 calc PR . . C54A C 0.3979(8) 0.1973(7) -0.1174(4) 0.056(3) Uiso 0.50 1 d P . . H54D H 0.4147 0.2225 -0.1556 0.084 Uiso 0.50 1 calc PR . . H54E H 0.3613 0.1472 -0.1193 0.084 Uiso 0.50 1 calc PR . . H54F H 0.4707 0.1673 -0.0961 0.084 Uiso 0.50 1 calc PR . . N1 N -0.0676(4) 0.8545(3) 0.16372(18) 0.0786(14) Uani 1 1 d . . . N2 N 0.7646(5) 0.2610(4) 0.0519(2) 0.1085(19) Uani 1 1 d . . . N3 N 0.6855(5) 0.1397(5) 0.2101(2) 0.133(2) Uani 1 1 d . . . O1 O 0.26893(19) 0.38923(16) 0.32970(9) 0.0228(6) Uani 1 1 d . . . O2 O 0.3735(2) 0.49108(19) 0.32256(12) 0.0496(8) Uani 1 1 d . . . O3 O 0.2384(2) 0.42923(18) 0.21429(9) 0.0375(7) Uani 1 1 d . . . O4 O 0.15532(18) 0.42706(16) 0.10837(9) 0.0246(6) Uani 1 1 d . . . O5 O 0.0889(2) 0.59007(18) 0.12111(10) 0.0392(7) Uani 1 1 d . . . O6 O -0.0722(2) 0.42499(18) 0.01755(9) 0.0369(7) Uani 1 1 d . . . O7 O 0.09361(19) 0.17335(16) 0.11072(9) 0.0250(6) Uani 1 1 d . . . O8 O 0.0505(2) 0.05538(18) 0.07158(10) 0.0376(7) Uani 1 1 d . . . O9 O 0.3564(2) -0.04399(17) 0.03996(9) 0.0425(7) Uani 1 1 d . . . O10 O 0.31961(19) 0.14672(16) 0.15485(9) 0.0240(6) Uani 1 1 d . . . O11 O 0.4990(2) 0.0801(2) 0.12130(13) 0.0635(9) Uani 1 1 d . . . O12 O 0.3978(2) 0.13017(18) 0.26236(9) 0.0324(6) Uani 1 1 d . . . O13 O 0.41526(18) 0.11339(16) 0.37808(8) 0.0219(6) Uani 1 1 d . . . O14 O 0.5130(2) -0.04262(18) 0.35647(10) 0.0366(7) Uani 1 1 d . . . O15 O 0.3025(2) 0.06532(18) 0.52016(10) 0.0415(7) Uani 1 1 d . . . O16 O 0.14468(18) 0.31829(16) 0.42508(9) 0.0260(6) Uani 1 1 d . . . O17 O 0.0625(3) 0.2781(3) 0.50316(17) 0.0395(11) Uiso 0.60 1 d P . . O17A O 0.0386(5) 0.4177(4) 0.4896(2) 0.0312(15) Uiso 0.40 1 d P . . O18 O 0.20499(19) 0.56478(17) 0.45462(10) 0.0345(7) 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 C1 0.018(2) 0.020(2) 0.027(2) 0.0007(17) 0.0001(17) -0.0060(17) C2 0.022(2) 0.025(2) 0.017(2) -0.0016(16) -0.0020(16) -0.0076(17) C3 0.027(2) 0.029(2) 0.021(2) -0.0090(17) 0.0009(17) -0.0070(19) C4 0.019(2) 0.028(2) 0.022(2) -0.0037(17) 0.0016(17) -0.0028(17) C5 0.024(2) 0.032(2) 0.021(2) -0.0025(18) -0.0070(17) -0.0041(18) C6 0.025(2) 0.028(2) 0.015(2) -0.0026(17) -0.0014(16) -0.0063(18) C7 0.032(2) 0.028(2) 0.020(2) 0.0021(17) -0.0009(18) -0.0075(19) C8 0.020(2) 0.025(2) 0.020(2) -0.0022(17) 0.0047(17) -0.0022(17) C9 0.022(2) 0.025(2) 0.019(2) -0.0039(17) 0.0012(17) -0.0017(17) C10 0.036(2) 0.031(2) 0.017(2) -0.0022(17) 0.0024(18) -0.002(2) C11 0.025(2) 0.026(2) 0.020(2) -0.0028(17) 0.0064(17) -0.0039(18) C12 0.026(2) 0.026(2) 0.025(2) 0.0000(17) -0.0022(18) -0.0046(18) C13 0.023(2) 0.021(2) 0.019(2) -0.0002(16) 0.0012(17) -0.0006(17) C14 0.026(2) 0.026(2) 0.022(2) -0.0019(18) -0.0021(18) -0.0090(18) C15 0.030(2) 0.030(2) 0.0119(19) -0.0030(17) -0.0007(16) -0.0155(19) C16 0.028(2) 0.026(2) 0.0124(19) -0.0022(16) 0.0006(16) -0.0072(18) C17 0.034(2) 0.022(2) 0.018(2) 0.0018(17) -0.0033(17) -0.0042(18) C18 0.032(2) 0.031(2) 0.020(2) -0.0008(18) 0.0066(18) -0.0081(19) C19 0.033(2) 0.027(2) 0.023(2) -0.0038(18) 0.0023(18) -0.0045(19) C20 0.028(2) 0.025(2) 0.0123(19) -0.0017(16) -0.0016(16) -0.0066(18) C21 0.033(2) 0.032(2) 0.015(2) -0.0009(18) -0.0034(17) -0.0104(19) C22 0.021(2) 0.019(2) 0.019(2) 0.0009(17) -0.0003(16) -0.0025(17) C23 0.022(2) 0.022(2) 0.016(2) -0.0025(16) 0.0023(16) -0.0034(17) C24 0.022(2) 0.023(2) 0.025(2) -0.0061(17) -0.0014(17) -0.0054(17) C25 0.016(2) 0.023(2) 0.020(2) -0.0008(17) 0.0017(16) -0.0027(16) C26 0.018(2) 0.030(2) 0.018(2) 0.0023(17) -0.0010(16) -0.0069(17) C27 0.017(2) 0.024(2) 0.019(2) -0.0037(17) 0.0024(16) -0.0078(17) C28 0.021(2) 0.034(2) 0.018(2) -0.0006(17) 0.0006(17) -0.0121(19) C29 0.016(2) 0.018(2) 0.026(2) -0.0027(16) 0.0002(16) -0.0089(16) C30 0.017(2) 0.025(2) 0.017(2) -0.0054(16) 0.0005(16) -0.0093(17) C31 0.023(2) 0.029(2) 0.0107(19) -0.0015(16) -0.0039(16) -0.0092(17) C32 0.020(2) 0.025(2) 0.018(2) -0.0027(16) -0.0001(16) -0.0081(17) C33 0.020(2) 0.028(2) 0.018(2) -0.0026(16) 0.0043(16) -0.0111(17) C34 0.020(2) 0.021(2) 0.019(2) 0.0008(16) -0.0013(16) -0.0089(17) C35 0.021(2) 0.029(2) 0.017(2) -0.0028(17) -0.0018(16) -0.0096(18) C36 0.019(2) 0.033(2) 0.0088(18) -0.0019(16) -0.0005(15) -0.0138(18) C37 0.024(2) 0.024(2) 0.0129(19) -0.0038(16) 0.0024(16) -0.0123(18) C38 0.024(2) 0.026(2) 0.017(2) -0.0017(16) 0.0010(16) -0.0084(18) C39 0.020(2) 0.028(2) 0.018(2) -0.0013(17) 0.0023(16) -0.0119(18) C40 0.025(2) 0.027(2) 0.021(2) -0.0054(17) 0.0044(17) -0.0143(18) C41 0.024(2) 0.025(2) 0.0107(19) -0.0021(16) 0.0022(16) -0.0091(18) C42 0.022(2) 0.033(2) 0.020(2) -0.0091(18) 0.0027(17) -0.0111(19) C43 0.021(2) 0.044(3) 0.024(2) -0.0108(19) -0.0031(18) 0.0014(19) C44 0.034(3) 0.105(4) 0.069(4) -0.004(3) 0.014(3) 0.006(3) C45 0.055(3) 0.039(3) 0.198(6) -0.051(4) -0.057(4) 0.013(3) C46 0.039(3) 0.073(3) 0.075(4) -0.034(3) -0.021(3) 0.019(3) C47 0.026(2) 0.034(2) 0.033(2) 0.001(2) 0.0087(19) -0.0072(19) C48 0.053(3) 0.085(4) 0.072(4) -0.031(3) 0.035(3) -0.024(3) C49 0.052(3) 0.070(4) 0.078(4) 0.017(3) 0.024(3) -0.020(3) C50 0.038(3) 0.158(5) 0.046(3) -0.007(3) 0.009(2) -0.049(3) C51 0.051(3) 0.030(2) 0.028(2) 0.0041(19) 0.013(2) 0.001(2) C55 0.023(2) 0.026(2) 0.021(2) 0.0001(17) 0.0022(17) -0.0087(18) C56 0.052(3) 0.032(2) 0.034(2) -0.0056(19) 0.005(2) -0.018(2) C57 0.042(3) 0.029(2) 0.048(3) 0.012(2) -0.005(2) -0.010(2) C58 0.045(3) 0.032(2) 0.044(3) -0.001(2) 0.007(2) -0.017(2) C59 0.022(2) 0.036(2) 0.019(2) -0.0030(17) 0.0002(16) -0.0142(18) C60 0.022(2) 0.045(3) 0.028(2) -0.0093(19) -0.0011(17) -0.0176(19) C61 0.034(2) 0.050(3) 0.033(2) -0.003(2) -0.0017(19) -0.027(2) C62 0.024(2) 0.054(3) 0.033(2) -0.015(2) 0.0045(18) -0.017(2) C63 0.019(2) 0.028(2) 0.036(2) -0.0024(19) -0.0032(18) -0.0095(18) C64 0.036(3) 0.043(3) 0.078(3) 0.012(2) -0.030(2) -0.022(2) C65 0.029(2) 0.049(3) 0.033(2) -0.006(2) -0.0066(18) -0.018(2) C66 0.025(2) 0.050(3) 0.041(3) -0.011(2) 0.0008(19) -0.016(2) C67 0.026(2) 0.032(3) 0.036(2) 0.002(2) 0.0062(19) -0.011(2) C68 0.023(2) 0.030(2) 0.083(3) -0.004(2) 0.011(2) -0.004(2) C69 0.037(3) 0.035(3) 0.019(2) 0.0011(19) -0.0043(19) -0.014(2) C70 0.035(2) 0.041(3) 0.037(2) 0.003(2) 0.002(2) -0.017(2) C71 0.026(2) 0.030(2) 0.029(2) 0.0038(19) -0.0023(19) -0.0088(19) C72 0.044(3) 0.049(3) 0.030(2) -0.001(2) 0.006(2) -0.022(2) C73 0.030(3) 0.034(3) 0.038(3) -0.002(2) 0.010(2) -0.008(2) C74 0.041(3) 0.029(2) 0.066(3) 0.002(2) 0.013(2) -0.015(2) C75 0.025(2) 0.031(2) 0.020(2) 0.0027(18) -0.0025(17) -0.009(2) C76 0.020(2) 0.035(2) 0.035(2) 0.0034(18) -0.0052(18) -0.0091(18) C78 0.016(2) 0.078(3) 0.042(3) 0.004(2) -0.0175(19) -0.022(2) C79 0.085(4) 0.048(3) 0.044(3) -0.006(2) -0.016(3) -0.024(3) C80 0.055(3) 0.043(3) 0.060(4) -0.002(3) -0.019(3) -0.012(3) C81 0.046(3) 0.089(4) 0.053(3) -0.012(3) -0.002(2) -0.027(3) C82 0.062(4) 0.077(4) 0.051(3) -0.015(3) 0.001(3) -0.025(3) C83 0.095(4) 0.082(4) 0.076(4) 0.001(3) -0.001(3) -0.002(4) C84 0.161(6) 0.082(5) 0.061(4) -0.008(4) 0.010(4) -0.088(5) N1 0.074(3) 0.079(3) 0.074(3) -0.013(3) 0.010(3) -0.015(3) N2 0.150(5) 0.088(4) 0.100(4) -0.027(3) -0.003(3) -0.052(4) N3 0.136(5) 0.159(6) 0.135(5) -0.024(5) -0.005(4) -0.089(5) O1 0.0192(14) 0.0232(14) 0.0231(14) -0.0033(11) 0.0007(11) -0.0038(12) O2 0.0393(18) 0.0272(17) 0.084(2) -0.0001(16) 0.0078(16) -0.0174(15) O3 0.0268(16) 0.0600(19) 0.0235(15) -0.0126(13) 0.0046(12) -0.0102(14) O4 0.0258(14) 0.0283(15) 0.0178(14) -0.0037(11) 0.0055(11) -0.0073(12) O5 0.0453(18) 0.0321(17) 0.0369(17) -0.0084(13) 0.0057(14) -0.0084(14) O6 0.0332(16) 0.0466(17) 0.0204(15) -0.0018(13) -0.0035(12) -0.0006(14) O7 0.0313(15) 0.0280(15) 0.0154(14) -0.0009(11) 0.0020(11) -0.0105(12) O8 0.0467(18) 0.0433(18) 0.0293(16) -0.0067(14) -0.0059(13) -0.0222(14) O9 0.071(2) 0.0284(16) 0.0174(15) -0.0045(12) 0.0034(14) -0.0033(15) O10 0.0278(15) 0.0226(14) 0.0213(14) -0.0006(11) 0.0004(11) -0.0091(12) O11 0.0403(19) 0.0383(19) 0.106(3) -0.0073(18) 0.0318(18) -0.0102(16) O12 0.0367(16) 0.0503(18) 0.0214(15) -0.0061(12) 0.0042(12) -0.0290(14) O13 0.0161(13) 0.0299(15) 0.0222(14) -0.0044(11) 0.0016(11) -0.0108(12) O14 0.0308(16) 0.0280(16) 0.0490(18) -0.0064(14) 0.0021(13) -0.0075(13) O15 0.069(2) 0.0463(18) 0.0210(15) 0.0075(13) -0.0148(14) -0.0375(16) O16 0.0200(14) 0.0390(16) 0.0228(14) -0.0035(12) -0.0053(11) -0.0141(12) O18 0.0315(16) 0.0337(16) 0.0381(17) -0.0129(13) -0.0084(13) -0.0068(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.384(4) . ? C1 C6 1.390(4) . ? C1 O1 1.396(3) . ? C2 C3 1.388(4) . ? C2 C42 1.504(4) . ? C3 C4 1.398(4) . ? C3 H3 0.9500 . ? C4 C5 1.397(4) . ? C4 C43 1.526(4) . ? C5 C6 1.391(4) . ? C5 H5 0.9500 . ? C6 C7 1.504(4) . ? C7 O3 1.221(4) . ? C7 C9 1.499(4) . ? C8 C13 1.378(4) . ? C8 C9 1.401(4) . ? C8 O4 1.401(4) . ? C9 C10 1.396(4) . ? C10 C11 1.395(4) . ? C10 H10 0.9500 . ? C11 C12 1.395(4) . ? C11 C47 1.528(4) . ? C12 C13 1.396(4) . ? C12 H12 0.9500 . ? C13 C14 1.503(4) . ? C14 O6 1.213(4) . ? C14 C16 1.504(4) . ? C15 C20 1.388(4) . ? C15 C16 1.392(4) . ? C15 O7 1.410(4) . ? C16 C17 1.394(4) . ? C17 C18 1.395(4) . ? C17 H17 0.9500 . ? C18 C19 1.388(4) . ? C18 C51 1.534(4) . ? C19 C20 1.399(4) . ? C19 H19 0.9500 . ? C20 C21 1.501(4) . ? C21 O9 1.217(4) . ? C21 C23 1.503(4) . ? C22 C23 1.390(4) . ? C22 C27 1.393(4) . ? C22 O10 1.401(4) . ? C23 C24 1.406(4) . ? C24 C25 1.386(4) . ? C24 H24 0.9500 . ? C25 C26 1.392(4) . ? C25 C55 1.530(4) . ? C26 C27 1.383(4) . ? C26 H26 0.9500 . ? C27 C28 1.493(4) . ? C28 O12 1.213(4) . ? C28 C30 1.496(4) . ? C29 O13 1.393(3) . ? C29 C30 1.394(4) . ? C29 C34 1.394(4) . ? C30 C31 1.405(4) . ? C31 C32 1.389(4) . ? C31 H31 0.9500 . ? C32 C33 1.395(4) . ? C32 C59 1.527(4) . ? C33 C34 1.381(4) . ? C33 H33 0.9500 . ? C34 C35 1.498(4) . ? C35 O15 1.217(3) . ? C35 C37 1.492(4) . ? C36 C37 1.384(4) . ? C36 C41 1.391(4) . ? C36 O16 1.401(3) . ? C37 C38 1.400(4) . ? C38 C39 1.386(4) . ? C38 H38 0.9500 . ? C39 C40 1.390(4) . ? C39 C63 1.538(4) . ? C40 C41 1.388(4) . ? C40 H40 0.9500 . ? C41 C42 1.500(4) . ? C42 O18 1.220(4) . ? C43 C45 1.488(5) . ? C43 C46 1.503(5) . ? C43 C44 1.543(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C50 1.492(5) . ? C47 C49 1.525(5) . ? C47 C48 1.537(5) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C54A 1.391(9) . ? C51 C52A 1.451(10) . ? C51 C53 1.462(8) . ? C51 C54 1.613(8) . ? C51 C52 1.619(8) . ? C51 C53A 1.620(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C57 1.528(4) . ? C55 C56 1.536(4) . ? C55 C58 1.538(4) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C61 1.541(4) . ? C59 C60 1.544(4) . ? C59 C62 1.546(4) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C65 1.534(4) . ? C63 C64 1.532(4) . ? C63 C66 1.540(4) . ? 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 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 O2 1.185(4) . ? C67 O1 1.371(4) . ? C67 C68 1.484(4) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 O5 1.197(4) . ? C69 O4 1.380(4) . ? C69 C70 1.496(4) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 O8 1.199(4) . ? C71 O7 1.371(4) . ? C71 C72 1.490(4) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 O11 1.199(4) . ? C73 O10 1.357(4) . ? C73 C74 1.490(5) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 O14 1.200(4) . ? C75 O13 1.377(4) . ? C75 C76 1.493(4) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 O16 1.310(6) . ? C77 O17 1.232(7) . ? C77 C78 1.522(7) . ? C77A O17A 1.181(10) . ? C77A O16 1.430(10) . ? C77A C78 1.520(10) . ? C79 C80 1.451(6) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 N1 1.129(5) . ? C81 C82 1.458(6) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 N2 1.131(6) . ? C83 C84 1.408(6) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 N3 1.149(6) . ? C52A H52D 0.9800 . ? C52A H52E 0.9800 . ? C52A H52F 0.9800 . ? C53A H53D 0.9800 . ? C53A H53E 0.9800 . ? C53A H53F 0.9800 . ? C54A H54D 0.9800 . ? C54A H54E 0.9800 . ? C54A H54F 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 C2 C1 C6 121.3(3) . . ? C2 C1 O1 120.4(3) . . ? C6 C1 O1 118.2(3) . . ? C1 C2 C3 118.6(3) . . ? C1 C2 C42 124.0(3) . . ? C3 C2 C42 117.4(3) . . ? C2 C3 C4 122.2(3) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C5 C4 C3 117.4(3) . . ? C5 C4 C43 122.5(3) . . ? C3 C4 C43 120.2(3) . . ? C6 C5 C4 121.6(3) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C1 C6 C5 118.9(3) . . ? C1 C6 C7 120.4(3) . . ? C5 C6 C7 120.7(3) . . ? O3 C7 C9 121.6(3) . . ? O3 C7 C6 120.6(3) . . ? C9 C7 C6 117.8(3) . . ? C13 C8 C9 121.3(3) . . ? C13 C8 O4 116.9(3) . . ? C9 C8 O4 121.8(3) . . ? C10 C9 C8 116.8(3) . . ? C10 C9 C7 120.4(3) . . ? C8 C9 C7 122.9(3) . . ? C11 C10 C9 124.0(3) . . ? C11 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? C10 C11 C12 116.5(3) . . ? C10 C11 C47 120.9(3) . . ? C12 C11 C47 122.5(3) . . ? C13 C12 C11 121.4(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C8 C13 C12 119.8(3) . . ? C8 C13 C14 120.9(3) . . ? C12 C13 C14 119.3(3) . . ? O6 C14 C13 120.2(3) . . ? O6 C14 C16 120.7(3) . . ? C13 C14 C16 119.1(3) . . ? C20 C15 C16 121.7(3) . . ? C20 C15 O7 121.0(3) . . ? C16 C15 O7 117.2(3) . . ? C15 C16 C17 118.6(3) . . ? C15 C16 C14 124.3(3) . . ? C17 C16 C14 117.1(3) . . ? C16 C17 C18 121.9(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 117.2(3) . . ? C19 C18 C51 121.0(3) . . ? C17 C18 C51 121.7(3) . . ? C18 C19 C20 123.0(3) . . ? C18 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C15 C20 C19 117.5(3) . . ? C15 C20 C21 125.4(3) . . ? C19 C20 C21 117.0(3) . . ? O9 C21 C23 118.5(3) . . ? O9 C21 C20 119.1(3) . . ? C23 C21 C20 122.4(3) . . ? C23 C22 C27 121.1(3) . . ? C23 C22 O10 120.7(3) . . ? C27 C22 O10 118.1(3) . . ? C22 C23 C24 118.3(3) . . ? C22 C23 C21 123.8(3) . . ? C24 C23 C21 117.5(3) . . ? C25 C24 C23 122.6(3) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C24 C25 C26 116.0(3) . . ? C24 C25 C55 123.8(3) . . ? C26 C25 C55 120.2(3) . . ? C27 C26 C25 124.2(3) . . ? C27 C26 H26 117.9 . . ? C25 C26 H26 117.9 . . ? C26 C27 C22 117.7(3) . . ? C26 C27 C28 121.4(3) . . ? C22 C27 C28 120.8(3) . . ? O12 C28 C27 121.5(3) . . ? O12 C28 C30 121.2(3) . . ? C27 C28 C30 117.3(3) . . ? O13 C29 C30 122.4(3) . . ? O13 C29 C34 116.4(3) . . ? C30 C29 C34 121.2(3) . . ? C29 C30 C31 117.1(3) . . ? C29 C30 C28 121.6(3) . . ? C31 C30 C28 121.3(3) . . ? C32 C31 C30 123.4(3) . . ? C32 C31 H31 118.3 . . ? C30 C31 H31 118.3 . . ? C31 C32 C33 116.5(3) . . ? C31 C32 C59 123.3(3) . . ? C33 C32 C59 120.2(3) . . ? C34 C33 C32 122.5(3) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C29 119.0(3) . . ? C33 C34 C35 120.9(3) . . ? C29 C34 C35 120.0(3) . . ? O15 C35 C37 121.2(3) . . ? O15 C35 C34 119.6(3) . . ? C37 C35 C34 119.2(3) . . ? C37 C36 C41 121.1(3) . . ? C37 C36 O16 119.9(3) . . ? C41 C36 O16 119.0(3) . . ? C36 C37 C38 118.5(3) . . ? C36 C37 C35 123.7(3) . . ? C38 C37 C35 117.8(3) . . ? C39 C38 C37 122.1(3) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 117.4(3) . . ? C38 C39 C63 123.1(3) . . ? C40 C39 C63 119.5(3) . . ? C41 C40 C39 122.4(3) . . ? C41 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? C40 C41 C36 118.5(3) . . ? C40 C41 C42 116.7(3) . . ? C36 C41 C42 124.8(3) . . ? O18 C42 C41 119.0(3) . . ? O18 C42 C2 118.2(3) . . ? C41 C42 C2 122.7(3) . . ? C45 C43 C46 111.7(4) . . ? C45 C43 C4 109.7(3) . . ? C46 C43 C4 112.6(3) . . ? C45 C43 C44 108.5(4) . . ? C46 C43 C44 106.0(3) . . ? C4 C43 C44 108.1(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C50 C47 C49 112.6(4) . . ? C50 C47 C11 112.1(3) . . ? C49 C47 C11 107.3(3) . . ? C50 C47 C48 107.4(3) . . ? C49 C47 C48 106.0(3) . . ? C11 C47 C48 111.3(3) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C54A C51 C52A 111.1(7) . . ? C54A C51 C53 121.1(6) . . ? C52A C51 C53 74.4(5) . . ? C54A C51 C18 116.9(5) . . ? C52A C51 C18 110.1(5) . . ? C53 C51 C18 114.7(4) . . ? C54A C51 C54 22.2(5) . . ? C52A C51 C54 131.8(6) . . ? C53 C51 C54 113.8(5) . . ? C18 C51 C54 108.2(4) . . ? C54A C51 C52 84.4(5) . . ? C52A C51 C52 34.4(5) . . ? C53 C51 C52 106.6(5) . . ? C18 C51 C52 106.3(4) . . ? C54 C51 C52 106.5(5) . . ? C54A C51 C53A 106.0(5) . . ? C52A C51 C53A 105.6(6) . . ? C53 C51 C53A 31.4(4) . . ? C18 C51 C53A 106.3(4) . . ? C54 C51 C53A 90.3(4) . . ? C52 C51 C53A 135.9(5) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C25 C55 C57 108.4(3) . . ? C25 C55 C56 112.8(3) . . ? C57 C55 C56 108.2(3) . . ? C25 C55 C58 110.3(3) . . ? C57 C55 C58 108.9(3) . . ? C56 C55 C58 108.1(3) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C32 C59 C61 108.7(3) . . ? C32 C59 C60 112.2(3) . . ? C61 C59 C60 108.0(3) . . ? C32 C59 C62 110.1(3) . . ? C61 C59 C62 109.4(3) . . ? C60 C59 C62 108.2(3) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C65 C63 C64 108.6(3) . . ? C65 C63 C39 109.8(3) . . ? C64 C63 C39 111.9(3) . . ? C65 C63 C66 109.4(3) . . ? C64 C63 C66 108.1(3) . . ? C39 C63 C66 109.1(3) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O2 C67 O1 122.9(3) . . ? O2 C67 C68 128.3(4) . . ? O1 C67 C68 108.8(3) . . ? 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 . . ? O5 C69 O4 122.9(3) . . ? O5 C69 C70 126.6(4) . . ? O4 C69 C70 110.5(3) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O8 C71 O7 123.5(3) . . ? O8 C71 C72 126.9(4) . . ? O7 C71 C72 109.5(3) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O11 C73 O10 120.8(4) . . ? O11 C73 C74 127.2(4) . . ? O10 C73 C74 111.9(3) . . ? 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 . . ? O14 C75 O13 123.2(3) . . ? O14 C75 C76 126.7(3) . . ? O13 C75 C76 110.1(3) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O16 C77 O17 118.7(6) . . ? O16 C77 C78 113.2(5) . . ? O17 C77 C78 128.1(6) . . ? O17A C77A O16 121.5(8) . . ? O17A C77A C78 131.8(9) . . ? O16 C77A C78 106.7(7) . . ? C77 C78 C77A 30.8(4) . . ? C80 C79 H79A 109.5 . . ? C80 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C80 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N1 C80 C79 179.2(6) . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N2 C82 C81 178.1(6) . . ? C84 C83 H83A 109.5 . . ? C84 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C84 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N3 C84 C83 172.6(8) . . ? C51 C52A H52D 109.5 . . ? C51 C52A H52E 109.5 . . ? H52D C52A H52E 109.5 . . ? C51 C52A H52F 109.5 . . ? H52D C52A H52F 109.5 . . ? H52E C52A H52F 109.5 . . ? C51 C53A H53D 109.5 . . ? C51 C53A H53E 109.5 . . ? H53D C53A H53E 109.5 . . ? C51 C53A H53F 109.5 . . ? H53D C53A H53F 109.5 . . ? H53E C53A H53F 109.5 . . ? C51 C54A H54D 109.5 . . ? C51 C54A H54E 109.5 . . ? H54D C54A H54E 109.5 . . ? C51 C54A H54F 109.5 . . ? H54D C54A H54F 109.5 . . ? H54E C54A H54F 109.5 . . ? C67 O1 C1 116.3(3) . . ? C69 O4 C8 116.9(3) . . ? C71 O7 C15 118.2(3) . . ? C73 O10 C22 116.9(3) . . ? C75 O13 C29 117.4(3) . . ? C77 O16 C36 122.6(4) . . ? C77 O16 C77A 33.9(4) . . ? C36 O16 C77A 117.1(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.531 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.052