# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Kaisa Helttunen' _publ_contact_author_address ; P.O. Box 35 Jyvaskyla FIN-40014 ; _publ_contact_author_email maija.nissinen@jyu.fi loop_ _publ_author_name K.Helttunen M.Nissinen # Attachment '- Octapodands.cif' data_1A _database_code_depnum_ccdc_archive 'CCDC 781919' #TrackingRef '- Octapodands.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H96 N16 O24' _chemical_formula_weight 1857.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 12.2700(3) _cell_length_b 19.6334(7) _cell_length_c 20.4221(6) _cell_angle_alpha 75.230(2) _cell_angle_beta 72.675(2) _cell_angle_gamma 75.3640(14) _cell_volume 4457.3(2) _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 block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7295 _exptl_absorpt_correction_T_max 0.8497 _exptl_absorpt_process_details 'Denzo (Otwinowski, Majewski, Borek & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 22810 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 66.98 _reflns_number_total 15349 _reflns_number_gt 10729 _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^)+(0.1210P)^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 15349 _refine_ls_number_parameters 1249 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2492 _refine_ls_wR_factor_gt 0.2233 _refine_ls_goodness_of_fit_ref 1.392 _refine_ls_restrained_S_all 1.392 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O4 O 0.3185(2) 1.14058(12) 0.11940(12) 0.0619(6) Uani 1 1 d . . . O6 O 0.6088(2) 0.92650(13) 0.15237(12) 0.0614(6) Uani 1 1 d . . . O11 O -0.14331(18) 1.18981(11) 0.29006(12) 0.0588(6) Uani 1 1 d . . . O13 O 0.1781(2) 1.31373(12) 0.19177(18) 0.0852(9) Uani 1 1 d . . . O18 O 0.2876(2) 0.80333(11) 0.25010(12) 0.0591(6) Uani 1 1 d . . . O20 O 0.0164(2) 1.02792(11) 0.20939(12) 0.0624(6) Uani 1 1 d . . . O25 O 0.77887(17) 0.81988(10) 0.29852(11) 0.0498(5) Uani 1 1 d . . . O27 O 0.45198(18) 0.69677(10) 0.39022(12) 0.0539(5) Uani 1 1 d . . . C1 C 0.5563(2) 1.00715(15) 0.22777(15) 0.0441(7) Uani 1 1 d . . . C2 C 0.4923(3) 1.07180(15) 0.24621(17) 0.0485(7) Uani 1 1 d . . . H2 H 0.5032 1.0854 0.2849 0.058 Uiso 1 1 calc R . . C3 C 0.4124(3) 1.11777(16) 0.21026(17) 0.0501(7) Uani 1 1 d . . . C4 C 0.3978(3) 1.09559(17) 0.15415(17) 0.0533(8) Uani 1 1 d . . . C5 C 0.4603(3) 1.03242(18) 0.13394(16) 0.0550(8) Uani 1 1 d . . . H5 H 0.4494 1.0184 0.0955 0.066 Uiso 1 1 calc R . . C6 C 0.5397(3) 0.98950(16) 0.17076(16) 0.0518(8) Uani 1 1 d . . . C7 C 0.3410(3) 1.18892(16) 0.22946(19) 0.0577(8) Uani 1 1 d . . . H7 H 0.3594 1.2271 0.1871 0.069 Uiso 1 1 calc R . . C8 C 0.2109(3) 1.19021(16) 0.24610(17) 0.0503(7) Uani 1 1 d . . . C9 C 0.1648(3) 1.12900(15) 0.27950(15) 0.0457(7) Uani 1 1 d . . . H9 H 0.2165 1.0860 0.2925 0.055 Uiso 1 1 calc R . . C10 C 0.0475(3) 1.12707(15) 0.29495(15) 0.0438(6) Uani 1 1 d . . . C11 C -0.0274(3) 1.19162(17) 0.27555(17) 0.0511(7) Uani 1 1 d . . . C12 C 0.0149(3) 1.25403(17) 0.24358(19) 0.0594(9) Uani 1 1 d . . . H12 H -0.0370 1.2976 0.2323 0.071 Uiso 1 1 calc R . . C13 C 0.1331(3) 1.25304(17) 0.22806(19) 0.0588(8) Uani 1 1 d . . . C14 C 0.0011(3) 1.05940(15) 0.33523(16) 0.0469(7) Uani 1 1 d . . . H14 H -0.0749 1.0634 0.3245 0.056 Uiso 1 1 calc R . . C15 C 0.0812(2) 0.99204(15) 0.31166(15) 0.0449(7) Uani 1 1 d . . . C17 C 0.2204(2) 0.87920(15) 0.33183(15) 0.0432(6) Uani 1 1 d . . . C18 C 0.2196(3) 0.86725(15) 0.26724(16) 0.0478(7) Uani 1 1 d . . . C19 C 0.1526(3) 0.91582(16) 0.22565(16) 0.0512(7) Uani 1 1 d . . . H19 H 0.1532 0.9071 0.1819 0.061 Uiso 1 1 calc R . . C20 C 0.0850(3) 0.97697(15) 0.24836(16) 0.0480(7) Uani 1 1 d . . . C21 C 0.2911(3) 0.82216(16) 0.37653(15) 0.0454(7) Uani 1 1 d . . . H21 H 0.2801 0.7746 0.3729 0.054 Uiso 1 1 calc R . . C22 C 0.4217(2) 0.82195(15) 0.35143(14) 0.0412(6) Uani 1 1 d . . . C23 C 0.4683(2) 0.88334(15) 0.32162(14) 0.0418(6) Uani 1 1 d . . . H23 H 0.4162 0.9277 0.3138 0.050 Uiso 1 1 calc R . . C24 C 0.5873(2) 0.88394(15) 0.30233(14) 0.0410(6) Uani 1 1 d . . . C25 C 0.6624(2) 0.81780(15) 0.31526(15) 0.0424(6) Uani 1 1 d . . . C16 C 0.1508(2) 0.94188(15) 0.35206(15) 0.0420(6) Uani 1 1 d . . . H16 H 0.1504 0.9512 0.3956 0.050 Uiso 1 1 calc R . . C26 C 0.6196(3) 0.75449(15) 0.34313(15) 0.0464(7) Uani 1 1 d . . . H26 H 0.6716 0.7098 0.3498 0.056 Uiso 1 1 calc R . . C27 C 0.5005(3) 0.75700(15) 0.36111(15) 0.0439(7) Uani 1 1 d . . . C28 C 0.6375(3) 0.95235(15) 0.26805(15) 0.0449(7) Uani 1 1 d . . . H28 H 0.7119 0.9386 0.2331 0.054 Uiso 1 1 calc R . . C29 C 0.3693(3) 1.2091(2) 0.2881(2) 0.0740(11) Uani 1 1 d . . . H29A H 0.3210 1.2555 0.2969 0.111 Uiso 1 1 calc R . . H29B H 0.4516 1.2125 0.2751 0.111 Uiso 1 1 calc R . . H29C H 0.3536 1.1723 0.3306 0.111 Uiso 1 1 calc R . . C30 C -0.0242(3) 1.05755(18) 0.41325(17) 0.0599(9) Uani 1 1 d . . . H30A H 0.0475 1.0576 0.4251 0.090 Uiso 1 1 calc R . . H30B H -0.0541 1.0140 0.4396 0.090 Uiso 1 1 calc R . . H30C H -0.0824 1.0999 0.4252 0.090 Uiso 1 1 calc R . . C31 C 0.2495(3) 0.82666(18) 0.45447(16) 0.0545(8) Uani 1 1 d . . . H31A H 0.2629 0.8715 0.4606 0.082 Uiso 1 1 calc R . . H31B H 0.2928 0.7858 0.4814 0.082 Uiso 1 1 calc R . . H31C H 0.1662 0.8255 0.4711 0.082 Uiso 1 1 calc R . . C32 C 0.6679(3) 0.98200(18) 0.32126(18) 0.0581(8) Uani 1 1 d . . . H32A H 0.7201 0.9444 0.3453 0.087 Uiso 1 1 calc R . . H32B H 0.5965 0.9978 0.3555 0.087 Uiso 1 1 calc R . . H32C H 0.7065 1.0228 0.2971 0.087 Uiso 1 1 calc R . . O101 O 0.3095(3) 1.31458(17) -0.03029(17) 0.0920(9) Uani 1 1 d . . . O102 O 0.2396(3) 1.42416(19) -0.0736(2) 0.1090(11) Uani 1 1 d . . . N1 N 0.1705(3) 1.22654(17) 0.04326(15) 0.0653(8) Uani 1 1 d . . . H1N H 0.241(4) 1.244(2) 0.026(2) 0.078 Uiso 1 1 d . . . N2 N 0.2243(3) 1.36481(19) -0.03728(19) 0.0800(9) Uani 1 1 d . . . C33 C 0.2576(3) 1.1074(2) 0.09086(19) 0.0664(10) Uani 1 1 d . . . H33A H 0.2414 1.0615 0.1221 0.080 Uiso 1 1 calc R . . H33B H 0.3047 1.0973 0.0445 0.080 Uiso 1 1 calc R . . C34 C 0.1466(3) 1.15817(19) 0.08400(19) 0.0656(9) Uani 1 1 d . . . H34A H 0.1042 1.1384 0.0611 0.079 Uiso 1 1 calc R . . H34B H 0.0968 1.1642 0.1310 0.079 Uiso 1 1 calc R . . C35 C 0.0869(3) 1.2847(2) 0.03264(17) 0.0643(9) Uani 1 1 d . . . C36 C -0.0309(3) 1.2801(2) 0.0577(2) 0.0725(10) Uani 1 1 d . . . H36 H -0.0507 1.2346 0.0805 0.087 Uiso 1 1 calc R . . C37 C -0.1179(4) 1.3377(3) 0.0507(2) 0.0898(13) Uani 1 1 d . . . H37 H -0.1966 1.3319 0.0687 0.108 Uiso 1 1 calc R . . C38 C -0.0926(4) 1.4052(3) 0.0173(3) 0.0945(15) Uani 1 1 d . . . H38 H -0.1534 1.4461 0.0156 0.113 Uiso 1 1 calc R . . C39 C 0.0198(4) 1.4120(2) -0.0127(2) 0.0851(12) Uani 1 1 d . . . H39 H 0.0371 1.4572 -0.0389 0.102 Uiso 1 1 calc R . . C40 C 0.1105(4) 1.3529(2) -0.0055(2) 0.0699(10) Uani 1 1 d . . . O103 O 0.9362(3) 0.8683(2) 0.0760(2) 0.1105(11) Uani 1 1 d . . . O104 O 1.0985(3) 0.8094(3) 0.0949(2) 0.1359(16) Uani 1 1 d . . . N3 N 0.7521(3) 0.80793(18) 0.11857(17) 0.0690(8) Uani 1 1 d . . . H3N H 0.793(4) 0.848(2) 0.096(2) 0.083 Uiso 1 1 d . . . N4 N 0.9977(3) 0.8121(3) 0.09777(19) 0.0898(11) Uani 1 1 d . . . C41 C 0.5657(3) 0.8873(2) 0.1200(2) 0.0682(10) Uani 1 1 d . . . H41A H 0.5825 0.9051 0.0688 0.082 Uiso 1 1 calc R . . H41B H 0.4806 0.8909 0.1389 0.082 Uiso 1 1 calc R . . C42 C 0.6284(3) 0.8110(2) 0.1371(2) 0.0713(10) Uani 1 1 d . . . H42A H 0.6018 0.7917 0.1877 0.086 Uiso 1 1 calc R . . H42B H 0.6100 0.7810 0.1110 0.086 Uiso 1 1 calc R . . C43 C 0.8284(3) 0.7497(2) 0.13946(19) 0.0658(10) Uani 1 1 d . . . C44 C 0.7911(4) 0.6835(2) 0.1740(2) 0.0807(12) Uani 1 1 d . . . H44 H 0.7117 0.6814 0.1815 0.097 Uiso 1 1 calc R . . C45 C 0.8636(5) 0.6238(3) 0.1965(3) 0.0953(15) Uani 1 1 d . . . H45 H 0.8338 0.5813 0.2194 0.114 Uiso 1 1 calc R . . C46 C 0.9804(5) 0.6232(3) 0.1870(3) 0.0967(16) Uani 1 1 d . . . H46 H 1.0304 0.5807 0.2032 0.116 Uiso 1 1 calc R . . C47 C 1.0238(4) 0.6861(3) 0.1531(2) 0.0901(14) Uani 1 1 d . . . H47 H 1.1038 0.6867 0.1457 0.108 Uiso 1 1 calc R . . O105 O -0.5956(3) 1.31488(17) 0.42168(19) 0.1162(14) Uani 1 1 d . . . O106 O -0.6996(2) 1.25710(18) 0.51211(15) 0.0890(9) Uani 1 1 d . . . N5 N -0.4111(3) 1.24602(16) 0.34446(15) 0.0633(8) Uani 1 1 d . . . H5N H -0.472(4) 1.290(2) 0.3508(19) 0.076 Uiso 1 1 d . . . N6 N -0.6101(3) 1.25917(19) 0.46523(17) 0.0723(9) Uani 1 1 d . . . C48 C 0.9484(3) 0.7480(2) 0.1303(2) 0.0710(10) Uani 1 1 d . . . C49 C -0.2171(3) 1.25243(18) 0.26223(19) 0.0578(8) Uani 1 1 d . . . H49A H -0.1849 1.2663 0.2112 0.069 Uiso 1 1 calc R . . H49B H -0.2210 1.2927 0.2842 0.069 Uiso 1 1 calc R . . C50 C -0.3353(3) 1.23762(19) 0.27601(18) 0.0598(8) Uani 1 1 d . . . H50A H -0.3733 1.2701 0.2400 0.072 Uiso 1 1 calc R . . H50B H -0.3277 1.1878 0.2705 0.072 Uiso 1 1 calc R . . C51 C -0.4267(3) 1.19101(17) 0.40066(17) 0.0543(8) Uani 1 1 d . . . C52 C -0.3472(3) 1.12588(17) 0.40158(17) 0.0553(8) Uani 1 1 d . . . H52 H -0.2815 1.1208 0.3629 0.066 Uiso 1 1 calc R . . C53 C -0.3613(3) 1.06908(19) 0.45656(19) 0.0639(9) Uani 1 1 d . . . H53 H -0.3060 1.0254 0.4552 0.077 Uiso 1 1 calc R . . C54 C -0.4550(4) 1.0748(2) 0.5139(2) 0.0739(11) Uani 1 1 d . . . H54 H -0.4632 1.0356 0.5523 0.089 Uiso 1 1 calc R . . C55 C -0.5362(3) 1.1372(2) 0.51491(19) 0.0671(10) Uani 1 1 d . . . H55 H -0.6025 1.1407 0.5534 0.081 Uiso 1 1 calc R . . C56 C -0.5219(3) 1.19504(18) 0.45988(18) 0.0570(8) Uani 1 1 d . . . O107 O 0.4695(3) 1.35470(16) 0.1790(2) 0.1008(10) Uani 1 1 d . . . O108 O 0.6287(3) 1.39287(17) 0.13351(18) 0.0954(9) Uani 1 1 d . . . N7 N 0.2738(3) 1.43258(17) 0.15290(19) 0.0759(9) Uani 1 1 d . . . H7N H 0.315(4) 1.397(3) 0.174(2) 0.091 Uiso 1 1 d . . . N8 N 0.5230(3) 1.40246(19) 0.14294(19) 0.0768(9) Uani 1 1 d . . . C57 C 0.1032(4) 1.3795(2) 0.1857(4) 0.114(2) Uani 1 1 d . . . H57A H 0.0664 1.3911 0.2328 0.137 Uiso 1 1 calc R . . H57B H 0.0408 1.3767 0.1655 0.137 Uiso 1 1 calc R . . C58 C 0.1642(4) 1.4361(2) 0.1416(4) 0.120(2) Uani 1 1 d . . . H58A H 0.1752 1.4340 0.0921 0.144 Uiso 1 1 calc R . . H58B H 0.1146 1.4830 0.1496 0.144 Uiso 1 1 calc R . . C59 C 0.3421(3) 1.48202(18) 0.11953(18) 0.0596(8) Uani 1 1 d . . . C60 C 0.2933(4) 1.5514(2) 0.0876(2) 0.0730(10) Uani 1 1 d . . . H60 H 0.2124 1.5627 0.0900 0.088 Uiso 1 1 calc R . . C61 C 0.3585(4) 1.6022(2) 0.0538(2) 0.0785(11) Uani 1 1 d . . . H61 H 0.3222 1.6483 0.0335 0.094 Uiso 1 1 calc R . . C62 C 0.4756(4) 1.5885(2) 0.0482(2) 0.0769(11) Uani 1 1 d . . . H62 H 0.5205 1.6245 0.0239 0.092 Uiso 1 1 calc R . . C63 C 0.5266(4) 1.5231(2) 0.0777(2) 0.0709(10) Uani 1 1 d . . . H63 H 0.6080 1.5130 0.0737 0.085 Uiso 1 1 calc R . . C64 C 0.4614(3) 1.47063(19) 0.11369(19) 0.0630(9) Uani 1 1 d . . . O109 O 0.1469(3) 0.60277(17) 0.29498(18) 0.0948(9) Uani 1 1 d . . . O110 O 0.1650(3) 0.48782(19) 0.3274(2) 0.1283(15) Uani 1 1 d . . . N9 N 0.3279(3) 0.65976(15) 0.22229(16) 0.0625(7) Uani 1 1 d . . . H9N H 0.247(4) 0.661(2) 0.249(2) 0.075 Uiso 1 1 d . . . N10 N 0.2081(3) 0.54185(18) 0.30201(19) 0.0783(9) Uani 1 1 d . . . C65 C 0.2988(4) 0.78914(18) 0.18411(18) 0.0651(9) Uani 1 1 d . . . H65A H 0.3291 0.8278 0.1465 0.078 Uiso 1 1 calc R . . H65B H 0.2225 0.7856 0.1793 0.078 Uiso 1 1 calc R . . C66 C 0.3832(4) 0.71844(19) 0.1799(2) 0.0735(11) Uani 1 1 d . . . H66A H 0.4110 0.7121 0.1307 0.088 Uiso 1 1 calc R . . H66B H 0.4514 0.7187 0.1962 0.088 Uiso 1 1 calc R . . C67 C 0.3872(3) 0.59202(18) 0.24205(18) 0.0591(8) Uani 1 1 d . . . C68 C 0.5105(3) 0.5760(2) 0.2227(2) 0.0667(9) Uani 1 1 d . . . H68 H 0.5518 0.6125 0.1944 0.080 Uiso 1 1 calc R . . C69 C 0.5713(4) 0.5093(2) 0.2436(2) 0.0798(12) Uani 1 1 d . . . H69 H 0.6539 0.5006 0.2292 0.096 Uiso 1 1 calc R . . C70 C 0.5162(4) 0.4544(2) 0.2849(2) 0.0790(11) Uani 1 1 d . . . H70 H 0.5601 0.4094 0.3015 0.095 Uiso 1 1 calc R . . C71 C 0.3960(4) 0.4659(2) 0.3019(2) 0.0732(11) Uani 1 1 d . . . H71 H 0.3566 0.4278 0.3277 0.088 Uiso 1 1 calc R . . C72 C 0.3329(3) 0.53377(18) 0.28107(19) 0.0623(9) Uani 1 1 d . . . O111 O -0.2083(3) 0.99709(18) 0.00497(16) 0.1081(12) Uani 1 1 d . . . O112 O -0.3485(4) 1.0485(2) -0.0447(2) 0.1371(17) Uani 1 1 d . . . N11 N -0.1726(3) 1.06151(19) 0.09371(16) 0.0740(9) Uani 1 1 d . . . H11N H -0.1449 1.0237 0.0739 0.089 Uiso 1 1 calc R . . N12 N -0.2883(4) 1.04770(19) -0.00581(17) 0.0843(11) Uani 1 1 d . . . C73 C -0.0315(3) 1.00664(19) 0.16418(19) 0.0631(9) Uani 1 1 d . . . H73A H -0.0643 0.9629 0.1876 0.076 Uiso 1 1 calc R . . H73B H 0.0282 0.9973 0.1209 0.076 Uiso 1 1 calc R . . C74 C -0.1251(4) 1.0694(2) 0.1482(2) 0.0732(10) Uani 1 1 d . . . H74A H -0.1884 1.0738 0.1912 0.088 Uiso 1 1 calc R . . H74B H -0.0929 1.1139 0.1330 0.088 Uiso 1 1 calc R . . C75 C -0.2589(3) 1.1124(2) 0.07404(18) 0.0673(10) Uani 1 1 d . . . C76 C -0.3030(4) 1.1780(2) 0.1031(2) 0.0754(11) Uani 1 1 d . . . H76 H -0.2688 1.1869 0.1354 0.091 Uiso 1 1 calc R . . C77 C -0.3925(4) 1.2250(2) 0.0831(2) 0.0810(12) Uani 1 1 d . . . H77 H -0.4188 1.2668 0.1031 0.097 Uiso 1 1 calc R . . C78 C -0.4481(4) 1.2204(2) 0.0394(2) 0.0852(12) Uani 1 1 d . . . H78 H -0.5125 1.2559 0.0287 0.102 Uiso 1 1 calc R . . C79 C -0.4076(4) 1.1620(2) 0.0108(2) 0.0802(11) Uani 1 1 d . . . H79 H -0.4439 1.1569 -0.0223 0.096 Uiso 1 1 calc R . . C80 C -0.3145(3) 1.1077(2) 0.02663(18) 0.0642(9) Uani 1 1 d . . . O113 O 0.8512(3) 0.91476(14) 0.43551(17) 0.0825(8) Uani 1 1 d . . . O114 O 0.7924(3) 0.89387(19) 0.54705(18) 0.1032(11) Uani 1 1 d . . . N13 N 0.9610(2) 0.80893(16) 0.36902(15) 0.0563(7) Uani 1 1 d . . . H13N H 0.942(3) 0.853(2) 0.3673(19) 0.068 Uiso 1 1 d . . . N14 N 0.8500(3) 0.87442(19) 0.4924(2) 0.0732(9) Uani 1 1 d . . . C81 C 0.8582(3) 0.75519(16) 0.31587(16) 0.0480(7) Uani 1 1 d . . . H81A H 0.8715 0.7232 0.2827 0.058 Uiso 1 1 calc R . . H81B H 0.8269 0.7295 0.3637 0.058 Uiso 1 1 calc R . . C82 C 0.9701(3) 0.77678(18) 0.31134(17) 0.0542(8) Uani 1 1 d . . . H82A H 1.0333 0.7339 0.3107 0.065 Uiso 1 1 calc R . . H82B H 0.9909 0.8113 0.2670 0.065 Uiso 1 1 calc R . . C83 C 0.9638(3) 0.77169(18) 0.43447(19) 0.0583(8) Uani 1 1 d . . . C84 C 1.0138(4) 0.6976(2) 0.4463(2) 0.0749(11) Uani 1 1 d . . . H84 H 1.0450 0.6740 0.4075 0.090 Uiso 1 1 calc R . . C85 C 1.0187(5) 0.6589(3) 0.5114(2) 0.0943(15) Uani 1 1 d . . . H85 H 1.0520 0.6092 0.5172 0.113 Uiso 1 1 calc R . . C86 C 0.9754(5) 0.6915(3) 0.5698(3) 0.1045(17) Uani 1 1 d . . . H86 H 0.9823 0.6646 0.6147 0.125 Uiso 1 1 calc R . . C87 C 0.9238(4) 0.7613(3) 0.5619(2) 0.0864(13) Uani 1 1 d . . . H87 H 0.8926 0.7834 0.6016 0.104 Uiso 1 1 calc R . . C88 C 0.9157(3) 0.80173(19) 0.4956(2) 0.0638(9) Uani 1 1 d . . . O115 O 0.3035(3) 0.62682(19) 0.60510(17) 0.0956(9) Uani 1 1 d . . . O116 O 0.1788(3) 0.57987(18) 0.69338(16) 0.0923(9) Uani 1 1 d . . . N15 N 0.3816(3) 0.57466(14) 0.48953(15) 0.0577(7) Uani 1 1 d D . . H15N H 0.377(3) 0.6079(16) 0.5097(18) 0.069 Uiso 1 1 d D . . N16 N 0.2377(3) 0.58345(19) 0.63254(18) 0.0743(9) Uani 1 1 d . . . C89 C 0.5258(3) 0.62849(16) 0.39422(19) 0.0571(8) Uani 1 1 d . . . H89A H 0.5731 0.6221 0.4278 0.068 Uiso 1 1 calc R . . H89B H 0.5790 0.6234 0.3478 0.068 Uiso 1 1 calc R . . C90 C 0.4486(3) 0.57368(17) 0.41825(18) 0.0579(8) Uani 1 1 d . . . H90A H 0.3953 0.5842 0.3873 0.069 Uiso 1 1 calc R . . H90B H 0.4969 0.5253 0.4151 0.069 Uiso 1 1 calc R . . C91 C 0.3002(3) 0.53365(16) 0.52269(18) 0.0542(8) Uani 1 1 d . . . C92 C 0.2842(3) 0.48326(17) 0.49020(19) 0.0582(8) Uani 1 1 d . . . H92 H 0.3320 0.4782 0.4449 0.070 Uiso 1 1 calc R . . C93 C 0.2017(4) 0.44086(19) 0.5216(2) 0.0707(10) Uani 1 1 d . . . H93 H 0.1935 0.4074 0.4978 0.085 Uiso 1 1 calc R . . C94 C 0.1306(4) 0.4467(2) 0.5877(2) 0.0776(11) Uani 1 1 d . . . H94 H 0.0726 0.4181 0.6086 0.093 Uiso 1 1 calc R . . C95 C 0.1436(4) 0.4929(2) 0.6225(2) 0.0708(10) Uani 1 1 d . . . H95 H 0.0955 0.4963 0.6681 0.085 Uiso 1 1 calc R . . C96 C 0.2282(3) 0.53587(18) 0.59146(19) 0.0618(9) 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 O4 0.0531(13) 0.0570(13) 0.0652(13) 0.0062(10) -0.0256(11) 0.0026(11) O6 0.0529(13) 0.0627(14) 0.0668(14) -0.0201(11) -0.0229(11) 0.0094(11) O11 0.0367(11) 0.0485(12) 0.0800(15) 0.0028(10) -0.0154(10) -0.0030(9) O13 0.0475(14) 0.0374(12) 0.149(2) 0.0074(14) -0.0174(15) -0.0039(10) O18 0.0680(15) 0.0449(12) 0.0723(14) -0.0205(10) -0.0364(12) 0.0067(10) O20 0.0719(15) 0.0448(12) 0.0829(15) -0.0100(11) -0.0516(13) 0.0035(11) O25 0.0388(11) 0.0391(10) 0.0681(13) -0.0018(9) -0.0191(9) -0.0033(9) O27 0.0441(12) 0.0338(10) 0.0804(14) -0.0007(9) -0.0208(10) -0.0061(9) C1 0.0371(15) 0.0401(15) 0.0505(16) 0.0011(12) -0.0123(12) -0.0077(12) C2 0.0389(16) 0.0425(15) 0.0600(18) 0.0006(13) -0.0142(13) -0.0089(13) C3 0.0360(15) 0.0428(15) 0.0639(19) 0.0007(14) -0.0095(14) -0.0087(13) C4 0.0401(17) 0.0479(17) 0.0583(18) 0.0056(14) -0.0103(14) -0.0030(13) C5 0.0499(18) 0.0610(19) 0.0458(16) -0.0025(14) -0.0136(14) -0.0020(15) C6 0.0430(17) 0.0470(16) 0.0522(17) -0.0001(13) -0.0090(13) 0.0012(13) C7 0.0440(17) 0.0372(15) 0.086(2) -0.0019(15) -0.0182(16) -0.0059(13) C8 0.0406(16) 0.0394(15) 0.0690(19) -0.0096(14) -0.0151(14) -0.0036(13) C9 0.0409(16) 0.0417(15) 0.0525(16) -0.0077(12) -0.0149(13) -0.0022(12) C10 0.0408(16) 0.0407(15) 0.0512(16) -0.0110(12) -0.0133(13) -0.0054(12) C11 0.0393(16) 0.0485(17) 0.0620(18) -0.0076(14) -0.0156(14) -0.0021(13) C12 0.0445(18) 0.0374(15) 0.085(2) -0.0002(15) -0.0172(16) 0.0013(13) C13 0.0462(18) 0.0393(16) 0.085(2) -0.0053(15) -0.0149(16) -0.0063(14) C14 0.0358(15) 0.0439(15) 0.0592(18) -0.0087(13) -0.0136(13) -0.0036(12) C15 0.0369(15) 0.0412(15) 0.0580(17) -0.0052(13) -0.0171(13) -0.0082(12) C17 0.0354(15) 0.0384(14) 0.0571(17) -0.0049(12) -0.0163(13) -0.0080(12) C18 0.0455(17) 0.0368(14) 0.0667(19) -0.0114(13) -0.0254(14) -0.0029(12) C19 0.0562(19) 0.0483(17) 0.0567(18) -0.0110(14) -0.0287(15) -0.0053(14) C20 0.0455(17) 0.0397(15) 0.0644(18) -0.0054(13) -0.0299(14) -0.0035(13) C21 0.0419(16) 0.0413(15) 0.0551(17) -0.0032(12) -0.0198(13) -0.0088(12) C22 0.0389(15) 0.0422(15) 0.0454(15) -0.0047(12) -0.0188(12) -0.0068(12) C23 0.0423(16) 0.0363(14) 0.0468(15) -0.0037(11) -0.0179(12) -0.0040(12) C24 0.0380(15) 0.0386(14) 0.0482(15) -0.0064(12) -0.0158(12) -0.0070(12) C25 0.0336(15) 0.0435(15) 0.0516(16) -0.0085(12) -0.0160(12) -0.0044(12) C16 0.0368(15) 0.0412(14) 0.0497(15) -0.0061(12) -0.0150(12) -0.0082(12) C26 0.0437(17) 0.0387(15) 0.0571(17) -0.0071(13) -0.0203(14) -0.0015(12) C27 0.0443(16) 0.0382(15) 0.0514(16) -0.0032(12) -0.0184(13) -0.0096(12) C28 0.0388(15) 0.0401(15) 0.0548(16) -0.0027(12) -0.0171(13) -0.0058(12) C29 0.056(2) 0.0507(19) 0.127(3) -0.029(2) -0.037(2) -0.0023(16) C30 0.057(2) 0.0540(19) 0.0583(19) -0.0076(15) -0.0066(16) -0.0050(16) C31 0.0449(17) 0.0569(18) 0.0547(18) -0.0013(14) -0.0134(14) -0.0061(14) C32 0.057(2) 0.0491(17) 0.075(2) -0.0029(15) -0.0310(17) -0.0147(15) O101 0.0653(18) 0.085(2) 0.121(2) -0.0127(17) -0.0292(17) -0.0060(16) O102 0.101(3) 0.076(2) 0.145(3) -0.007(2) -0.029(2) -0.0243(19) N1 0.0553(18) 0.0666(19) 0.0637(17) -0.0036(14) -0.0195(14) 0.0027(15) N2 0.075(2) 0.068(2) 0.096(2) -0.0149(19) -0.0253(19) -0.0098(19) C33 0.065(2) 0.068(2) 0.061(2) -0.0111(17) -0.0259(18) 0.0066(18) C34 0.064(2) 0.062(2) 0.065(2) -0.0052(17) -0.0277(17) 0.0037(17) C35 0.065(2) 0.066(2) 0.0531(18) -0.0061(16) -0.0224(16) 0.0061(17) C36 0.060(2) 0.070(2) 0.073(2) -0.0023(18) -0.0177(18) 0.0023(19) C37 0.064(3) 0.086(3) 0.096(3) -0.001(2) -0.018(2) 0.007(2) C38 0.075(3) 0.075(3) 0.111(3) -0.008(2) -0.027(3) 0.020(2) C39 0.084(3) 0.068(2) 0.093(3) -0.007(2) -0.026(2) 0.000(2) C40 0.063(2) 0.067(2) 0.074(2) -0.0114(18) -0.0199(19) -0.0018(18) O103 0.082(2) 0.106(3) 0.135(3) 0.011(2) -0.045(2) -0.0151(19) O104 0.070(2) 0.198(5) 0.128(3) 0.020(3) -0.043(2) -0.035(3) N3 0.0575(19) 0.0692(19) 0.079(2) -0.0231(16) -0.0253(16) 0.0082(15) N4 0.056(2) 0.131(4) 0.080(2) -0.016(2) -0.0212(18) -0.013(2) C41 0.059(2) 0.077(2) 0.072(2) -0.0286(19) -0.0274(18) 0.0081(18) C42 0.057(2) 0.068(2) 0.092(3) -0.022(2) -0.0262(19) -0.0016(18) C43 0.063(2) 0.072(2) 0.064(2) -0.0243(18) -0.0236(17) 0.0048(18) C44 0.077(3) 0.073(3) 0.100(3) -0.032(2) -0.032(2) 0.000(2) C45 0.118(4) 0.071(3) 0.104(3) -0.024(2) -0.053(3) 0.005(3) C46 0.096(4) 0.081(3) 0.114(4) -0.039(3) -0.048(3) 0.028(3) C47 0.066(3) 0.114(4) 0.094(3) -0.043(3) -0.035(2) 0.018(3) O105 0.099(2) 0.0624(18) 0.126(3) -0.0022(18) 0.022(2) 0.0160(17) O106 0.0555(16) 0.109(2) 0.0831(18) -0.0254(16) 0.0004(14) 0.0040(15) N5 0.0547(17) 0.0495(15) 0.0721(18) -0.0056(14) -0.0088(14) -0.0011(13) N6 0.059(2) 0.074(2) 0.0713(19) -0.0180(17) -0.0068(16) 0.0008(16) C48 0.056(2) 0.086(3) 0.072(2) -0.027(2) -0.0232(18) 0.007(2) C49 0.0464(18) 0.0495(17) 0.070(2) -0.0070(15) -0.0184(15) 0.0041(14) C50 0.0470(18) 0.0592(19) 0.067(2) -0.0038(16) -0.0207(16) -0.0006(15) C51 0.0514(19) 0.0515(18) 0.0596(19) -0.0099(15) -0.0157(15) -0.0081(15) C52 0.0530(19) 0.0504(18) 0.0627(19) -0.0089(15) -0.0170(15) -0.0092(15) C53 0.070(2) 0.0532(19) 0.072(2) -0.0144(17) -0.0202(19) -0.0118(17) C54 0.088(3) 0.061(2) 0.066(2) -0.0010(17) -0.016(2) -0.019(2) C55 0.064(2) 0.075(2) 0.059(2) -0.0146(18) -0.0042(17) -0.0199(19) C56 0.0516(19) 0.0579(19) 0.065(2) -0.0181(16) -0.0154(16) -0.0099(15) O107 0.091(2) 0.0576(16) 0.155(3) 0.0134(18) -0.061(2) -0.0163(16) O108 0.068(2) 0.084(2) 0.124(2) -0.0230(18) -0.0239(17) 0.0038(16) N7 0.070(2) 0.0506(17) 0.099(2) 0.0036(16) -0.0254(18) -0.0105(15) N8 0.062(2) 0.066(2) 0.103(2) -0.0183(18) -0.0313(18) 0.0014(17) C57 0.075(3) 0.051(2) 0.189(5) -0.004(3) -0.012(3) -0.008(2) C58 0.064(3) 0.047(2) 0.228(6) 0.014(3) -0.042(3) -0.008(2) C59 0.063(2) 0.0467(17) 0.067(2) -0.0098(15) -0.0165(17) -0.0075(16) C60 0.066(2) 0.054(2) 0.092(3) -0.0055(18) -0.022(2) -0.0061(18) C61 0.093(3) 0.0472(19) 0.092(3) 0.0039(18) -0.029(2) -0.016(2) C62 0.085(3) 0.071(2) 0.077(2) -0.0004(19) -0.022(2) -0.032(2) C63 0.068(2) 0.068(2) 0.077(2) -0.0163(19) -0.0138(19) -0.0168(19) C64 0.063(2) 0.057(2) 0.069(2) -0.0125(16) -0.0192(17) -0.0063(17) O109 0.0659(18) 0.0744(19) 0.126(2) -0.0112(17) -0.0131(17) -0.0024(15) O110 0.089(2) 0.078(2) 0.200(4) -0.016(2) -0.003(3) -0.0345(19) N9 0.0625(19) 0.0448(15) 0.0748(19) -0.0146(13) -0.0147(15) -0.0009(13) N10 0.072(2) 0.063(2) 0.096(2) -0.0183(17) -0.0140(18) -0.0113(18) C65 0.077(2) 0.0497(18) 0.067(2) -0.0157(16) -0.0214(18) -0.0006(17) C66 0.081(3) 0.052(2) 0.075(2) -0.0150(17) -0.010(2) -0.0014(19) C67 0.064(2) 0.0516(18) 0.0625(19) -0.0193(15) -0.0201(17) 0.0000(16) C68 0.061(2) 0.057(2) 0.081(2) -0.0191(18) -0.0188(18) -0.0034(17) C69 0.069(3) 0.066(2) 0.107(3) -0.029(2) -0.034(2) 0.010(2) C70 0.083(3) 0.053(2) 0.100(3) -0.014(2) -0.038(2) 0.008(2) C71 0.090(3) 0.051(2) 0.075(2) -0.0128(17) -0.021(2) -0.0052(19) C72 0.064(2) 0.0521(19) 0.069(2) -0.0163(16) -0.0168(17) -0.0031(17) O111 0.134(3) 0.093(2) 0.097(2) -0.0374(18) -0.065(2) 0.041(2) O112 0.199(4) 0.108(3) 0.150(3) -0.042(2) -0.135(3) 0.015(3) N11 0.071(2) 0.082(2) 0.0749(19) -0.0079(16) -0.0326(17) -0.0139(17) N12 0.113(3) 0.075(2) 0.076(2) -0.0239(17) -0.061(2) 0.016(2) C73 0.069(2) 0.0548(19) 0.073(2) -0.0093(16) -0.0415(19) -0.0001(17) C74 0.065(2) 0.071(2) 0.090(3) -0.014(2) -0.038(2) -0.0022(19) C75 0.066(2) 0.078(2) 0.056(2) 0.0032(17) -0.0179(17) -0.0242(19) C76 0.070(3) 0.088(3) 0.071(2) -0.017(2) -0.023(2) -0.010(2) C77 0.074(3) 0.059(2) 0.101(3) 0.002(2) -0.029(2) -0.006(2) C78 0.075(3) 0.075(3) 0.092(3) 0.005(2) -0.023(2) -0.009(2) C79 0.077(3) 0.062(2) 0.092(3) -0.003(2) -0.022(2) -0.008(2) C80 0.072(2) 0.064(2) 0.0568(19) -0.0082(16) -0.0192(17) -0.0130(18) O113 0.096(2) 0.0561(15) 0.099(2) -0.0158(15) -0.0372(17) -0.0036(14) O114 0.113(3) 0.099(2) 0.102(2) -0.0457(19) -0.042(2) 0.018(2) N13 0.0532(16) 0.0470(14) 0.0732(18) -0.0057(14) -0.0272(14) -0.0101(13) N14 0.072(2) 0.070(2) 0.090(2) -0.0306(19) -0.0344(19) -0.0034(17) C81 0.0397(16) 0.0439(16) 0.0572(17) -0.0097(13) -0.0149(13) 0.0009(13) C82 0.0395(16) 0.0534(18) 0.0637(19) -0.0079(15) -0.0122(14) -0.0028(14) C83 0.0476(18) 0.0559(19) 0.079(2) -0.0075(17) -0.0331(17) -0.0085(15) C84 0.073(3) 0.063(2) 0.090(3) -0.016(2) -0.041(2) 0.0095(19) C85 0.106(4) 0.076(3) 0.098(3) -0.006(2) -0.058(3) 0.016(3) C86 0.124(4) 0.100(4) 0.081(3) -0.009(3) -0.053(3) 0.016(3) C87 0.087(3) 0.092(3) 0.083(3) -0.022(2) -0.040(2) 0.005(2) C88 0.059(2) 0.060(2) 0.081(2) -0.0197(18) -0.0339(18) -0.0006(17) O115 0.112(3) 0.100(2) 0.093(2) -0.0327(17) -0.0230(19) -0.041(2) O116 0.094(2) 0.103(2) 0.0745(19) -0.0253(16) -0.0154(17) -0.0085(18) N15 0.0608(17) 0.0446(15) 0.0687(18) -0.0052(12) -0.0207(14) -0.0123(13) N16 0.075(2) 0.076(2) 0.075(2) -0.0150(17) -0.0286(18) -0.0077(18) C89 0.0523(19) 0.0401(16) 0.076(2) -0.0036(15) -0.0205(16) -0.0062(14) C90 0.058(2) 0.0414(16) 0.075(2) -0.0063(15) -0.0217(17) -0.0099(14) C91 0.0511(18) 0.0417(16) 0.069(2) -0.0015(14) -0.0236(16) -0.0071(14) C92 0.059(2) 0.0459(17) 0.072(2) -0.0067(15) -0.0207(17) -0.0121(15) C93 0.070(2) 0.0508(19) 0.094(3) -0.0098(18) -0.024(2) -0.0165(18) C94 0.067(2) 0.057(2) 0.101(3) 0.001(2) -0.015(2) -0.0214(19) C95 0.066(2) 0.061(2) 0.074(2) -0.0011(18) -0.0138(19) -0.0091(18) C96 0.063(2) 0.0504(18) 0.071(2) -0.0061(16) -0.0248(18) -0.0054(16) _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 O4 C4 1.373(4) . ? O4 C33 1.422(5) . ? O6 C6 1.381(4) . ? O6 C41 1.408(4) . ? O11 C11 1.372(4) . ? O11 C49 1.429(4) . ? O13 C57 1.382(5) . ? O13 C13 1.383(4) . ? O18 C18 1.384(3) . ? O18 C65 1.405(4) . ? O20 C20 1.382(3) . ? O20 C73 1.420(4) . ? O25 C25 1.376(3) . ? O25 C81 1.427(3) . ? O27 C27 1.376(3) . ? O27 C89 1.414(4) . ? C1 C6 1.379(5) . ? C1 C2 1.391(4) . ? C1 C28 1.524(4) . ? C2 C3 1.399(4) . ? C3 C4 1.397(5) . ? C3 C7 1.526(4) . ? C4 C5 1.375(5) . ? C5 C6 1.386(4) . ? C7 C29 1.507(5) . ? C7 C8 1.525(4) . ? C8 C9 1.387(4) . ? C8 C13 1.397(4) . ? C9 C10 1.387(4) . ? C10 C11 1.407(4) . ? C10 C14 1.520(4) . ? C11 C12 1.382(5) . ? C12 C13 1.385(5) . ? C14 C30 1.522(4) . ? C14 C15 1.527(4) . ? C15 C20 1.383(4) . ? C15 C16 1.400(4) . ? C17 C16 1.390(4) . ? C17 C18 1.401(4) . ? C17 C21 1.517(4) . ? C18 C19 1.383(4) . ? C19 C20 1.377(4) . ? C21 C22 1.529(4) . ? C21 C31 1.538(4) . ? C22 C23 1.385(4) . ? C22 C27 1.401(4) . ? C23 C24 1.397(4) . ? C24 C25 1.403(4) . ? C24 C28 1.534(4) . ? C25 C26 1.391(4) . ? C26 C27 1.387(4) . ? C28 C32 1.527(4) . ? O101 N2 1.258(4) . ? O102 N2 1.237(5) . ? N1 C35 1.348(4) . ? N1 C34 1.437(5) . ? N2 C40 1.405(5) . ? C33 C34 1.492(5) . ? C35 C36 1.400(6) . ? C35 C40 1.419(6) . ? C36 C37 1.355(5) . ? C37 C38 1.392(7) . ? C38 C39 1.358(7) . ? C39 C40 1.401(6) . ? O103 N4 1.231(5) . ? O104 N4 1.209(5) . ? N3 C43 1.347(5) . ? N3 C42 1.440(5) . ? N4 C48 1.453(6) . ? C41 C42 1.505(5) . ? C43 C48 1.419(6) . ? C43 C44 1.428(6) . ? C44 C45 1.347(6) . ? C45 C46 1.385(7) . ? C46 C47 1.403(8) . ? C47 C48 1.395(6) . ? O105 N6 1.236(4) . ? O106 N6 1.225(4) . ? N5 C51 1.364(4) . ? N5 C50 1.453(4) . ? N6 C56 1.443(5) . ? C49 C50 1.482(5) . ? C51 C52 1.398(5) . ? C51 C56 1.412(5) . ? C52 C53 1.370(5) . ? C53 C54 1.380(5) . ? C54 C55 1.370(6) . ? C55 C56 1.385(5) . ? O107 N8 1.234(4) . ? O108 N8 1.225(4) . ? N7 C59 1.358(5) . ? N7 C58 1.412(6) . ? N8 C64 1.439(5) . ? C57 C58 1.455(6) . ? C59 C64 1.396(5) . ? C59 C60 1.417(5) . ? C60 C61 1.355(6) . ? C61 C62 1.369(6) . ? C62 C63 1.353(6) . ? C63 C64 1.386(5) . ? O109 N10 1.240(4) . ? O110 N10 1.230(5) . ? N9 C67 1.368(4) . ? N9 C66 1.440(5) . ? N10 C72 1.440(5) . ? C65 C66 1.513(5) . ? C67 C72 1.411(5) . ? C67 C68 1.419(5) . ? C68 C69 1.364(5) . ? C69 C70 1.377(6) . ? C70 C71 1.384(6) . ? C71 C72 1.393(5) . ? O111 N12 1.234(4) . ? O112 N12 1.231(4) . ? N11 C75 1.340(5) . ? N11 C74 1.457(5) . ? N12 C80 1.418(5) . ? C73 C74 1.499(5) . ? C75 C80 1.371(5) . ? C75 C76 1.467(6) . ? C76 C77 1.336(6) . ? C77 C78 1.307(6) . ? C78 C79 1.335(6) . ? C79 C80 1.406(5) . ? O113 N14 1.227(4) . ? O114 N14 1.225(4) . ? N13 C83 1.356(4) . ? N13 C82 1.437(4) . ? N14 C88 1.447(5) . ? C81 C82 1.508(5) . ? C83 C84 1.418(5) . ? C83 C88 1.419(5) . ? C84 C85 1.363(6) . ? C85 C86 1.398(7) . ? C86 C87 1.349(7) . ? C87 C88 1.401(6) . ? O115 N16 1.235(4) . ? O116 N16 1.232(4) . ? N15 C91 1.352(4) . ? N15 C90 1.445(4) . ? N16 C96 1.450(5) . ? C89 C90 1.505(5) . ? C91 C92 1.403(5) . ? C91 C96 1.424(5) . ? C92 C93 1.376(5) . ? C93 C94 1.388(6) . ? C94 C95 1.349(6) . ? C95 C96 1.404(5) . ? 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 C4 O4 C33 116.5(3) . . ? C6 O6 C41 118.4(3) . . ? C11 O11 C49 117.4(2) . . ? C57 O13 C13 119.0(3) . . ? C18 O18 C65 118.9(2) . . ? C20 O20 C73 119.7(2) . . ? C25 O25 C81 118.5(2) . . ? C27 O27 C89 119.0(2) . . ? C6 C1 C2 117.2(3) . . ? C6 C1 C28 117.5(3) . . ? C2 C1 C28 125.3(3) . . ? C1 C2 C3 122.9(3) . . ? C4 C3 C2 116.8(3) . . ? C4 C3 C7 119.2(3) . . ? C2 C3 C7 123.9(3) . . ? O4 C4 C5 121.4(3) . . ? O4 C4 C3 116.7(3) . . ? C5 C4 C3 121.9(3) . . ? C4 C5 C6 118.8(3) . . ? C1 C6 O6 115.2(3) . . ? C1 C6 C5 122.4(3) . . ? O6 C6 C5 122.4(3) . . ? C29 C7 C8 110.0(3) . . ? C29 C7 C3 114.3(3) . . ? C8 C7 C3 111.3(3) . . ? C9 C8 C13 117.2(3) . . ? C9 C8 C7 121.4(3) . . ? C13 C8 C7 121.4(3) . . ? C10 C9 C8 123.7(3) . . ? C9 C10 C11 117.0(3) . . ? C9 C10 C14 121.3(3) . . ? C11 C10 C14 121.6(3) . . ? O11 C11 C12 121.8(3) . . ? O11 C11 C10 117.2(3) . . ? C12 C11 C10 121.0(3) . . ? C11 C12 C13 119.9(3) . . ? O13 C13 C12 120.8(3) . . ? O13 C13 C8 118.0(3) . . ? C12 C13 C8 121.1(3) . . ? C10 C14 C30 109.0(3) . . ? C10 C14 C15 112.0(2) . . ? C30 C14 C15 114.2(3) . . ? C20 C15 C16 116.6(3) . . ? C20 C15 C14 120.0(3) . . ? C16 C15 C14 123.4(3) . . ? C16 C17 C18 116.9(3) . . ? C16 C17 C21 124.3(3) . . ? C18 C17 C21 118.7(3) . . ? C19 C18 O18 123.7(3) . . ? C19 C18 C17 121.3(3) . . ? O18 C18 C17 114.9(3) . . ? C20 C19 C18 119.3(3) . . ? C19 C20 O20 122.4(3) . . ? C19 C20 C15 122.4(3) . . ? O20 C20 C15 115.1(3) . . ? C17 C21 C22 113.4(2) . . ? C17 C21 C31 113.0(2) . . ? C22 C21 C31 109.2(2) . . ? C23 C22 C27 116.8(3) . . ? C23 C22 C21 123.8(2) . . ? C27 C22 C21 119.3(2) . . ? C22 C23 C24 124.0(3) . . ? C23 C24 C25 116.9(3) . . ? C23 C24 C28 123.2(2) . . ? C25 C24 C28 119.9(2) . . ? O25 C25 C26 122.9(2) . . ? O25 C25 C24 116.0(2) . . ? C26 C25 C24 121.1(3) . . ? C17 C16 C15 123.4(3) . . ? C27 C26 C25 119.6(3) . . ? O27 C27 C26 122.7(3) . . ? O27 C27 C22 115.7(3) . . ? C26 C27 C22 121.6(3) . . ? C1 C28 C32 113.3(2) . . ? C1 C28 C24 110.5(2) . . ? C32 C28 C24 111.5(2) . . ? C35 N1 C34 123.4(3) . . ? O102 N2 O101 120.6(4) . . ? O102 N2 C40 119.5(4) . . ? O101 N2 C40 119.9(4) . . ? O4 C33 C34 107.3(3) . . ? N1 C34 C33 110.0(3) . . ? N1 C35 C36 120.8(4) . . ? N1 C35 C40 123.5(4) . . ? C36 C35 C40 115.7(3) . . ? C37 C36 C35 122.8(4) . . ? C36 C37 C38 120.4(4) . . ? C39 C38 C37 119.4(4) . . ? C38 C39 C40 120.5(4) . . ? C39 C40 N2 116.9(4) . . ? C39 C40 C35 120.9(4) . . ? N2 C40 C35 122.3(3) . . ? C43 N3 C42 123.4(4) . . ? O104 N4 O103 121.3(5) . . ? O104 N4 C48 118.6(4) . . ? O103 N4 C48 120.1(4) . . ? O6 C41 C42 104.9(3) . . ? N3 C42 C41 110.2(3) . . ? N3 C43 C48 124.8(4) . . ? N3 C43 C44 120.4(4) . . ? C48 C43 C44 114.8(4) . . ? C45 C44 C43 122.9(5) . . ? C44 C45 C46 121.5(5) . . ? C45 C46 C47 119.0(4) . . ? C48 C47 C46 119.4(4) . . ? C51 N5 C50 124.2(3) . . ? O106 N6 O105 121.0(3) . . ? O106 N6 C56 119.3(3) . . ? O105 N6 C56 119.6(3) . . ? C47 C48 C43 122.4(4) . . ? C47 C48 N4 116.7(4) . . ? C43 C48 N4 120.8(4) . . ? O11 C49 C50 109.6(3) . . ? N5 C50 C49 115.5(3) . . ? N5 C51 C52 120.4(3) . . ? N5 C51 C56 123.5(3) . . ? C52 C51 C56 116.1(3) . . ? C53 C52 C51 122.0(3) . . ? C52 C53 C54 120.6(3) . . ? C55 C54 C53 119.6(3) . . ? C54 C55 C56 120.1(3) . . ? C55 C56 C51 121.6(3) . . ? C55 C56 N6 116.8(3) . . ? C51 C56 N6 121.6(3) . . ? C59 N7 C58 124.0(4) . . ? O108 N8 O107 120.2(4) . . ? O108 N8 C64 119.5(4) . . ? O107 N8 C64 120.3(3) . . ? O13 C57 C58 111.3(4) . . ? N7 C58 C57 114.7(5) . . ? N7 C59 C64 124.9(3) . . ? N7 C59 C60 120.2(4) . . ? C64 C59 C60 114.9(3) . . ? C61 C60 C59 122.0(4) . . ? C60 C61 C62 121.3(4) . . ? C63 C62 C61 119.1(4) . . ? C62 C63 C64 120.7(4) . . ? C63 C64 C59 122.0(3) . . ? C63 C64 N8 116.9(4) . . ? C59 C64 N8 121.1(3) . . ? C67 N9 C66 123.9(3) . . ? O110 N10 O109 121.7(4) . . ? O110 N10 C72 118.8(3) . . ? O109 N10 C72 119.5(3) . . ? O18 C65 C66 106.1(3) . . ? N9 C66 C65 110.5(3) . . ? N9 C67 C72 123.9(3) . . ? N9 C67 C68 120.7(3) . . ? C72 C67 C68 115.4(3) . . ? C69 C68 C67 121.6(4) . . ? C68 C69 C70 121.8(4) . . ? C69 C70 C71 118.9(4) . . ? C70 C71 C72 119.7(4) . . ? C71 C72 C67 122.3(4) . . ? C71 C72 N10 116.4(4) . . ? C67 C72 N10 121.3(3) . . ? C75 N11 C74 119.4(3) . . ? O112 N12 O111 122.0(4) . . ? O112 N12 C80 117.2(3) . . ? O111 N12 C80 120.8(3) . . ? O20 C73 C74 104.1(3) . . ? N11 C74 C73 111.7(3) . . ? N11 C75 C80 123.8(4) . . ? N11 C75 C76 121.9(4) . . ? C80 C75 C76 114.4(4) . . ? C77 C76 C75 118.5(4) . . ? C78 C77 C76 127.8(5) . . ? C77 C78 C79 114.8(5) . . ? C78 C79 C80 124.0(5) . . ? C75 C80 C79 120.5(4) . . ? C75 C80 N12 123.5(4) . . ? C79 C80 N12 115.9(4) . . ? C83 N13 C82 124.3(3) . . ? O114 N14 O113 121.4(3) . . ? O114 N14 C88 118.8(4) . . ? O113 N14 C88 119.7(3) . . ? O25 C81 C82 106.6(2) . . ? N13 C82 C81 111.9(3) . . ? N13 C83 C84 120.9(3) . . ? N13 C83 C88 124.0(3) . . ? C84 C83 C88 115.0(3) . . ? C85 C84 C83 122.2(4) . . ? C84 C85 C86 120.9(4) . . ? C87 C86 C85 119.4(4) . . ? C86 C87 C88 120.6(4) . . ? C87 C88 C83 121.7(3) . . ? C87 C88 N14 117.1(3) . . ? C83 C88 N14 121.1(3) . . ? C91 N15 C90 122.8(3) . . ? O116 N16 O115 122.2(4) . . ? O116 N16 C96 118.9(4) . . ? O115 N16 C96 118.9(3) . . ? O27 C89 C90 106.9(3) . . ? N15 C90 C89 110.6(3) . . ? N15 C91 C92 120.2(3) . . ? N15 C91 C96 124.5(3) . . ? C92 C91 C96 115.3(3) . . ? C93 C92 C91 122.3(3) . . ? C92 C93 C94 120.4(4) . . ? C95 C94 C93 120.2(4) . . ? C94 C95 C96 120.0(4) . . ? C95 C96 C91 121.8(3) . . ? C95 C96 N16 116.7(3) . . ? C91 C96 N16 121.6(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 C6 C1 C2 C3 0.9(4) . . . . ? C28 C1 C2 C3 -175.1(3) . . . . ? C1 C2 C3 C4 0.7(4) . . . . ? C1 C2 C3 C7 179.9(3) . . . . ? C33 O4 C4 C5 33.2(4) . . . . ? C33 O4 C4 C3 -147.6(3) . . . . ? C2 C3 C4 O4 179.4(3) . . . . ? C7 C3 C4 O4 0.2(4) . . . . ? C2 C3 C4 C5 -1.4(5) . . . . ? C7 C3 C4 C5 179.4(3) . . . . ? O4 C4 C5 C6 179.5(3) . . . . ? C3 C4 C5 C6 0.4(5) . . . . ? C2 C1 C6 O6 177.2(3) . . . . ? C28 C1 C6 O6 -6.5(4) . . . . ? C2 C1 C6 C5 -2.0(5) . . . . ? C28 C1 C6 C5 174.4(3) . . . . ? C41 O6 C6 C1 150.7(3) . . . . ? C41 O6 C6 C5 -30.2(4) . . . . ? C4 C5 C6 C1 1.4(5) . . . . ? C4 C5 C6 O6 -177.7(3) . . . . ? C4 C3 C7 C29 -176.7(3) . . . . ? C2 C3 C7 C29 4.1(4) . . . . ? C4 C3 C7 C8 57.9(4) . . . . ? C2 C3 C7 C8 -121.3(3) . . . . ? C29 C7 C8 C9 -92.5(4) . . . . ? C3 C7 C8 C9 35.3(4) . . . . ? C29 C7 C8 C13 87.8(4) . . . . ? C3 C7 C8 C13 -144.4(3) . . . . ? C13 C8 C9 C10 0.7(5) . . . . ? C7 C8 C9 C10 -179.1(3) . . . . ? C8 C9 C10 C11 -0.4(4) . . . . ? C8 C9 C10 C14 -176.6(3) . . . . ? C49 O11 C11 C12 8.6(5) . . . . ? C49 O11 C11 C10 -171.8(3) . . . . ? C9 C10 C11 O11 179.3(3) . . . . ? C14 C10 C11 O11 -4.5(4) . . . . ? C9 C10 C11 C12 -1.0(5) . . . . ? C14 C10 C11 C12 175.1(3) . . . . ? O11 C11 C12 C13 -178.1(3) . . . . ? C10 C11 C12 C13 2.2(5) . . . . ? C57 O13 C13 C12 15.5(6) . . . . ? C57 O13 C13 C8 -166.9(4) . . . . ? C11 C12 C13 O13 175.5(3) . . . . ? C11 C12 C13 C8 -2.0(6) . . . . ? C9 C8 C13 O13 -177.0(3) . . . . ? C7 C8 C13 O13 2.8(5) . . . . ? C9 C8 C13 C12 0.6(5) . . . . ? C7 C8 C13 C12 -179.7(3) . . . . ? C9 C10 C14 C30 86.0(3) . . . . ? C11 C10 C14 C30 -90.0(3) . . . . ? C9 C10 C14 C15 -41.3(4) . . . . ? C11 C10 C14 C15 142.8(3) . . . . ? C10 C14 C15 C20 -74.3(4) . . . . ? C30 C14 C15 C20 161.3(3) . . . . ? C10 C14 C15 C16 107.7(3) . . . . ? C30 C14 C15 C16 -16.7(4) . . . . ? C65 O18 C18 C19 6.2(5) . . . . ? C65 O18 C18 C17 -175.5(3) . . . . ? C16 C17 C18 C19 0.1(4) . . . . ? C21 C17 C18 C19 177.0(3) . . . . ? C16 C17 C18 O18 -178.3(3) . . . . ? C21 C17 C18 O18 -1.4(4) . . . . ? O18 C18 C19 C20 178.0(3) . . . . ? C17 C18 C19 C20 -0.3(5) . . . . ? C18 C19 C20 O20 179.7(3) . . . . ? C18 C19 C20 C15 0.0(5) . . . . ? C73 O20 C20 C19 30.4(5) . . . . ? C73 O20 C20 C15 -149.9(3) . . . . ? C16 C15 C20 C19 0.4(5) . . . . ? C14 C15 C20 C19 -177.8(3) . . . . ? C16 C15 C20 O20 -179.3(3) . . . . ? C14 C15 C20 O20 2.6(4) . . . . ? C16 C17 C21 C22 -106.0(3) . . . . ? C18 C17 C21 C22 77.3(3) . . . . ? C16 C17 C21 C31 19.0(4) . . . . ? C18 C17 C21 C31 -157.7(3) . . . . ? C17 C21 C22 C23 34.7(4) . . . . ? C31 C21 C22 C23 -92.4(3) . . . . ? C17 C21 C22 C27 -148.0(3) . . . . ? C31 C21 C22 C27 84.9(3) . . . . ? C27 C22 C23 C24 -1.2(4) . . . . ? C21 C22 C23 C24 176.1(3) . . . . ? C22 C23 C24 C25 -0.8(4) . . . . ? C22 C23 C24 C28 178.8(3) . . . . ? C81 O25 C25 C26 -5.3(4) . . . . ? C81 O25 C25 C24 174.9(2) . . . . ? C23 C24 C25 O25 -177.5(2) . . . . ? C28 C24 C25 O25 2.9(4) . . . . ? C23 C24 C25 C26 2.8(4) . . . . ? C28 C24 C25 C26 -176.8(3) . . . . ? C18 C17 C16 C15 0.3(4) . . . . ? C21 C17 C16 C15 -176.4(3) . . . . ? C20 C15 C16 C17 -0.6(4) . . . . ? C14 C15 C16 C17 177.5(3) . . . . ? O25 C25 C26 C27 177.6(3) . . . . ? C24 C25 C26 C27 -2.6(4) . . . . ? C89 O27 C27 C26 -8.1(4) . . . . ? C89 O27 C27 C22 172.8(3) . . . . ? C25 C26 C27 O27 -178.6(3) . . . . ? C25 C26 C27 C22 0.5(4) . . . . ? C23 C22 C27 O27 -179.4(2) . . . . ? C21 C22 C27 O27 3.1(4) . . . . ? C23 C22 C27 C26 1.4(4) . . . . ? C21 C22 C27 C26 -176.1(3) . . . . ? C6 C1 C28 C32 169.3(3) . . . . ? C2 C1 C28 C32 -14.7(4) . . . . ? C6 C1 C28 C24 -64.8(3) . . . . ? C2 C1 C28 C24 111.3(3) . . . . ? C23 C24 C28 C1 -27.1(4) . . . . ? C25 C24 C28 C1 152.5(3) . . . . ? C23 C24 C28 C32 99.9(3) . . . . ? C25 C24 C28 C32 -80.5(3) . . . . ? C4 O4 C33 C34 156.1(3) . . . . ? C35 N1 C34 C33 -174.9(3) . . . . ? O4 C33 C34 N1 55.3(4) . . . . ? C34 N1 C35 C36 -4.3(6) . . . . ? C34 N1 C35 C40 177.7(3) . . . . ? N1 C35 C36 C37 177.3(4) . . . . ? C40 C35 C36 C37 -4.5(6) . . . . ? C35 C36 C37 C38 0.3(7) . . . . ? C36 C37 C38 C39 4.7(8) . . . . ? C37 C38 C39 C40 -5.1(7) . . . . ? C38 C39 C40 N2 -179.1(4) . . . . ? C38 C39 C40 C35 0.7(7) . . . . ? O102 N2 C40 C39 -4.9(6) . . . . ? O101 N2 C40 C39 177.2(4) . . . . ? O102 N2 C40 C35 175.4(4) . . . . ? O101 N2 C40 C35 -2.5(6) . . . . ? N1 C35 C40 C39 -177.8(4) . . . . ? C36 C35 C40 C39 4.0(6) . . . . ? N1 C35 C40 N2 1.9(6) . . . . ? C36 C35 C40 N2 -176.2(4) . . . . ? C6 O6 C41 C42 -154.4(3) . . . . ? C43 N3 C42 C41 167.1(3) . . . . ? O6 C41 C42 N3 -52.1(4) . . . . ? C42 N3 C43 C48 -171.1(4) . . . . ? C42 N3 C43 C44 8.6(5) . . . . ? N3 C43 C44 C45 -179.4(4) . . . . ? C48 C43 C44 C45 0.2(6) . . . . ? C43 C44 C45 C46 -0.3(7) . . . . ? C44 C45 C46 C47 -0.1(7) . . . . ? C45 C46 C47 C48 0.5(7) . . . . ? C46 C47 C48 C43 -0.6(6) . . . . ? C46 C47 C48 N4 177.9(4) . . . . ? N3 C43 C48 C47 179.9(4) . . . . ? C44 C43 C48 C47 0.3(5) . . . . ? N3 C43 C48 N4 1.5(6) . . . . ? C44 C43 C48 N4 -178.2(3) . . . . ? O104 N4 C48 C47 -3.1(6) . . . . ? O103 N4 C48 C47 179.4(4) . . . . ? O104 N4 C48 C43 175.4(4) . . . . ? O103 N4 C48 C43 -2.1(6) . . . . ? C11 O11 C49 C50 173.3(3) . . . . ? C51 N5 C50 C49 -96.1(4) . . . . ? O11 C49 C50 N5 84.1(4) . . . . ? C50 N5 C51 C52 17.4(5) . . . . ? C50 N5 C51 C56 -161.7(3) . . . . ? N5 C51 C52 C53 -178.8(3) . . . . ? C56 C51 C52 C53 0.4(5) . . . . ? C51 C52 C53 C54 -0.6(6) . . . . ? C52 C53 C54 C55 1.6(6) . . . . ? C53 C54 C55 C56 -2.4(6) . . . . ? C54 C55 C56 C51 2.2(6) . . . . ? C54 C55 C56 N6 -179.2(4) . . . . ? N5 C51 C56 C55 178.0(3) . . . . ? C52 C51 C56 C55 -1.1(5) . . . . ? N5 C51 C56 N6 -0.6(5) . . . . ? C52 C51 C56 N6 -179.8(3) . . . . ? O106 N6 C56 C55 -9.5(5) . . . . ? O105 N6 C56 C55 172.0(4) . . . . ? O106 N6 C56 C51 169.2(4) . . . . ? O105 N6 C56 C51 -9.3(6) . . . . ? C13 O13 C57 C58 -175.7(5) . . . . ? C59 N7 C58 C57 -176.9(4) . . . . ? O13 C57 C58 N7 -42.0(8) . . . . ? C58 N7 C59 C64 -160.5(5) . . . . ? C58 N7 C59 C60 19.8(6) . . . . ? N7 C59 C60 C61 -179.9(4) . . . . ? C64 C59 C60 C61 0.4(6) . . . . ? C59 C60 C61 C62 0.7(7) . . . . ? C60 C61 C62 C63 -0.6(7) . . . . ? C61 C62 C63 C64 -0.5(6) . . . . ? C62 C63 C64 C59 1.7(6) . . . . ? C62 C63 C64 N8 179.5(3) . . . . ? N7 C59 C64 C63 178.8(4) . . . . ? C60 C59 C64 C63 -1.6(5) . . . . ? N7 C59 C64 N8 1.0(6) . . . . ? C60 C59 C64 N8 -179.3(3) . . . . ? O108 N8 C64 C63 -2.0(5) . . . . ? O107 N8 C64 C63 175.9(4) . . . . ? O108 N8 C64 C59 175.9(4) . . . . ? O107 N8 C64 C59 -6.3(6) . . . . ? C18 O18 C65 C66 176.6(3) . . . . ? C67 N9 C66 C65 -164.3(3) . . . . ? O18 C65 C66 N9 74.5(4) . . . . ? C66 N9 C67 C72 -177.1(3) . . . . ? C66 N9 C67 C68 1.7(5) . . . . ? N9 C67 C68 C69 178.0(3) . . . . ? C72 C67 C68 C69 -3.0(5) . . . . ? C67 C68 C69 C70 -0.5(6) . . . . ? C68 C69 C70 C71 4.2(7) . . . . ? C69 C70 C71 C72 -4.3(6) . . . . ? C70 C71 C72 C67 0.7(6) . . . . ? C70 C71 C72 N10 -178.7(4) . . . . ? N9 C67 C72 C71 -178.2(3) . . . . ? C68 C67 C72 C71 2.9(5) . . . . ? N9 C67 C72 N10 1.2(5) . . . . ? C68 C67 C72 N10 -177.7(3) . . . . ? O110 N10 C72 C71 -10.5(6) . . . . ? O109 N10 C72 C71 168.6(4) . . . . ? O110 N10 C72 C67 170.1(4) . . . . ? O109 N10 C72 C67 -10.8(6) . . . . ? C20 O20 C73 C74 163.9(3) . . . . ? C75 N11 C74 C73 178.8(3) . . . . ? O20 C73 C74 N11 171.3(3) . . . . ? C74 N11 C75 C80 -175.6(4) . . . . ? C74 N11 C75 C76 3.4(6) . . . . ? N11 C75 C76 C77 -177.3(4) . . . . ? C80 C75 C76 C77 1.8(5) . . . . ? C75 C76 C77 C78 -0.2(7) . . . . ? C76 C77 C78 C79 -1.5(7) . . . . ? C77 C78 C79 C80 1.6(6) . . . . ? N11 C75 C80 C79 177.3(4) . . . . ? C76 C75 C80 C79 -1.7(5) . . . . ? N11 C75 C80 N12 1.4(6) . . . . ? C76 C75 C80 N12 -177.7(4) . . . . ? C78 C79 C80 C75 0.1(6) . . . . ? C78 C79 C80 N12 176.3(4) . . . . ? O112 N12 C80 C75 176.3(4) . . . . ? O111 N12 C80 C75 -3.6(6) . . . . ? O112 N12 C80 C79 0.2(6) . . . . ? O111 N12 C80 C79 -179.7(4) . . . . ? C25 O25 C81 C82 -164.0(2) . . . . ? C83 N13 C82 C81 76.7(4) . . . . ? O25 C81 C82 N13 73.6(3) . . . . ? C82 N13 C83 C84 21.3(5) . . . . ? C82 N13 C83 C88 -156.9(3) . . . . ? N13 C83 C84 C85 179.4(4) . . . . ? C88 C83 C84 C85 -2.2(6) . . . . ? C83 C84 C85 C86 -0.9(8) . . . . ? C84 C85 C86 C87 2.8(9) . . . . ? C85 C86 C87 C88 -1.4(9) . . . . ? C86 C87 C88 C83 -1.8(7) . . . . ? C86 C87 C88 N14 174.6(5) . . . . ? N13 C83 C88 C87 -178.2(4) . . . . ? C84 C83 C88 C87 3.5(5) . . . . ? N13 C83 C88 N14 5.6(5) . . . . ? C84 C83 C88 N14 -172.8(4) . . . . ? O114 N14 C88 C87 -9.7(6) . . . . ? O113 N14 C88 C87 171.6(4) . . . . ? O114 N14 C88 C83 166.8(4) . . . . ? O113 N14 C88 C83 -11.9(5) . . . . ? C27 O27 C89 C90 -172.0(3) . . . . ? C91 N15 C90 C89 176.0(3) . . . . ? O27 C89 C90 N15 -67.4(3) . . . . ? C90 N15 C91 C92 5.3(5) . . . . ? C90 N15 C91 C96 -176.6(3) . . . . ? N15 C91 C92 C93 -179.3(3) . . . . ? C96 C91 C92 C93 2.3(5) . . . . ? C91 C92 C93 C94 -0.1(6) . . . . ? C92 C93 C94 C95 -1.6(6) . . . . ? C93 C94 C95 C96 0.9(6) . . . . ? C94 C95 C96 C91 1.5(6) . . . . ? C94 C95 C96 N16 -179.3(3) . . . . ? N15 C91 C96 C95 178.7(3) . . . . ? C92 C91 C96 C95 -3.0(5) . . . . ? N15 C91 C96 N16 -0.4(5) . . . . ? C92 C91 C96 N16 177.8(3) . . . . ? O116 N16 C96 C95 5.6(5) . . . . ? O115 N16 C96 C95 -173.6(4) . . . . ? O116 N16 C96 C91 -175.3(3) . . . . ? O115 N16 C96 C91 5.6(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 N1 H1N O101 0.95(4) 1.78(4) 2.607(5) 144(4) . N1 H1N N2 0.95(4) 2.39(4) 2.914(5) 115(3) . N3 H3N O103 0.98(4) 1.81(4) 2.632(5) 140(4) . N3 H3N N4 0.98(4) 2.44(4) 2.935(5) 111(3) . N5 H5N O105 1.00(4) 1.82(4) 2.618(4) 135(3) . N7 H7N O107 0.86(5) 1.89(5) 2.623(5) 142(4) . N7 H7N N8 0.86(5) 2.47(5) 2.918(5) 113(4) . N9 H9N O109 0.98(4) 1.78(4) 2.614(4) 140(3) . N9 H9N N10 0.98(4) 2.42(4) 2.923(5) 111(3) . N11 H11N O111 0.88 2.02 2.645(5) 126.7 . N13 H13N O113 0.84(4) 1.97(4) 2.629(4) 135(3) . N15 H15N O115 0.840(19) 1.98(3) 2.632(4) 134(3) . _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 66.98 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.721 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.057 #===end data_1B _database_code_depnum_ccdc_archive 'CCDC 781920' #TrackingRef '- Octapodands.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H102 N16 O25' _chemical_formula_weight 1915.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 11.8003(4) _cell_length_b 20.6248(7) _cell_length_c 21.2868(8) _cell_angle_alpha 110.363(2) _cell_angle_beta 97.492(2) _cell_angle_gamma 99.820(2) _cell_volume 4683.8(3) _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 plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8523 _exptl_absorpt_correction_T_max 0.9369 _exptl_absorpt_process_details 'Denzo (Otwinowski, Majewski, Borek & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 23802 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 66.98 _reflns_number_total 15647 _reflns_number_gt 9268 _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^)+(0.0915P)^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 SHELXL _refine_ls_extinction_coef 0.00050(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15647 _refine_ls_number_parameters 1284 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2343 _refine_ls_wR_factor_gt 0.2032 _refine_ls_goodness_of_fit_ref 1.370 _refine_ls_restrained_S_all 1.374 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O4 O 0.1918(2) 0.03938(13) 0.27701(13) 0.0455(7) Uani 1 1 d . . . O6 O 0.4920(2) 0.23047(13) 0.27619(13) 0.0426(6) Uani 1 1 d . . . O11 O 0.2446(2) -0.25601(13) 0.11661(16) 0.0534(7) Uani 1 1 d . . . O13 O -0.0551(2) -0.12048(17) 0.1414(2) 0.0830(11) Uani 1 1 d . . . O18 O 0.7718(2) 0.10270(13) 0.25052(13) 0.0457(7) Uani 1 1 d . . . O20 O 0.4786(2) -0.09718(14) 0.24461(12) 0.0473(7) Uani 1 1 d . . . O25 O 0.5789(2) 0.32316(13) 0.15440(14) 0.0494(7) Uani 1 1 d . . . O27 O 0.8775(2) 0.18802(14) 0.12691(15) 0.0498(7) Uani 1 1 d . . . C1 C 0.3479(3) 0.16138(18) 0.17673(18) 0.0334(8) Uani 1 1 d . . . C2 C 0.2485(3) 0.10500(18) 0.14504(18) 0.0349(8) Uani 1 1 d . . . H2 H 0.2145 0.0944 0.0986 0.042 Uiso 1 1 calc R . . C3 C 0.1972(3) 0.06387(18) 0.17795(18) 0.0332(8) Uani 1 1 d . . . C4 C 0.2475(3) 0.08036(19) 0.24605(19) 0.0380(9) Uani 1 1 d . . . C5 C 0.3461(3) 0.1352(2) 0.27971(19) 0.0410(9) Uani 1 1 d . . . H5 H 0.3801 0.1458 0.3262 0.049 Uiso 1 1 calc R . . C6 C 0.3944(3) 0.17442(18) 0.24446(18) 0.0369(9) Uani 1 1 d . . . C7 C 0.0958(3) -0.00023(18) 0.14390(18) 0.0349(8) Uani 1 1 d . . . H7 H 0.0391 0.0038 0.1754 0.042 Uiso 1 1 calc R . . C8 C 0.1368(3) -0.06899(19) 0.13566(18) 0.0368(9) Uani 1 1 d . . . C9 C 0.2485(3) -0.07641(18) 0.12771(17) 0.0322(8) Uani 1 1 d . . . H9 H 0.3026 -0.0371 0.1269 0.039 Uiso 1 1 calc R . . C10 C 0.2865(3) -0.13877(18) 0.12081(17) 0.0344(8) Uani 1 1 d . . . C11 C 0.2052(3) -0.19498(19) 0.1224(2) 0.0427(9) Uani 1 1 d . . . C12 C 0.0916(4) -0.1903(2) 0.1296(3) 0.0597(12) Uani 1 1 d . . . H12 H 0.0372 -0.2297 0.1301 0.072 Uiso 1 1 calc R . . C13 C 0.0579(3) -0.1274(2) 0.1359(2) 0.0531(11) Uani 1 1 d . . . C14 C 0.4075(3) -0.14749(18) 0.10865(17) 0.0324(8) Uani 1 1 d . . . H14 H 0.4272 -0.1822 0.1289 0.039 Uiso 1 1 calc R . . C15 C 0.5037(3) -0.07994(17) 0.14479(17) 0.0307(8) Uani 1 1 d . . . C16 C 0.5615(3) -0.04164(17) 0.11158(18) 0.0310(8) Uani 1 1 d . . . H16 H 0.5379 -0.0572 0.0633 0.037 Uiso 1 1 calc R . . C17 C 0.6526(3) 0.01867(18) 0.14568(18) 0.0324(8) Uani 1 1 d . . . C18 C 0.6845(3) 0.04055(18) 0.21608(19) 0.0378(9) Uani 1 1 d . . . C19 C 0.6285(3) 0.00383(18) 0.25206(19) 0.0372(9) Uani 1 1 d . . . H19 H 0.6516 0.0198 0.3004 0.045 Uiso 1 1 calc R . . C20 C 0.5388(3) -0.05624(19) 0.21602(18) 0.0365(9) Uani 1 1 d . . . C21 C 0.7156(3) 0.06154(18) 0.11009(18) 0.0354(8) Uani 1 1 d . E . H21 H 0.8014 0.0723 0.1300 0.042 Uiso 1 1 calc R . . C22 C 0.6822(3) 0.13276(18) 0.12487(17) 0.0337(8) Uani 1 1 d . . . C23 C 0.5683(3) 0.13952(18) 0.13003(17) 0.0324(8) Uani 1 1 d . E . H23 H 0.5119 0.0989 0.1265 0.039 Uiso 1 1 calc R . . C24 C 0.5326(3) 0.20266(19) 0.14012(18) 0.0353(8) Uani 1 1 d . . . C25 C 0.6170(3) 0.26123(18) 0.14568(18) 0.0375(9) Uani 1 1 d . E . C26 C 0.7319(3) 0.25772(19) 0.14292(19) 0.0401(9) Uani 1 1 d . . . H26 H 0.7891 0.2989 0.1488 0.048 Uiso 1 1 calc R E . C27 C 0.7634(3) 0.19295(19) 0.13145(19) 0.0379(9) Uani 1 1 d . E . C28 C 0.4060(3) 0.20711(19) 0.14183(18) 0.0379(9) Uani 1 1 d . E . H28 H 0.4076 0.2575 0.1702 0.045 Uiso 1 1 calc R . . C29 C 0.0291(3) -0.0052(2) 0.0759(2) 0.0439(10) Uani 1 1 d . . . H29A H 0.0818 -0.0094 0.0435 0.066 Uiso 1 1 calc R . . H29B H -0.0010 0.0377 0.0825 0.066 Uiso 1 1 calc R . . H29C H -0.0368 -0.0471 0.0577 0.066 Uiso 1 1 calc R . . C30 C 0.4031(3) -0.18244(19) 0.03172(18) 0.0418(9) Uani 1 1 d . . . H30A H 0.3471 -0.2288 0.0129 0.063 Uiso 1 1 calc R . . H30B H 0.4813 -0.1889 0.0243 0.063 Uiso 1 1 calc R . . H30C H 0.3780 -0.1520 0.0088 0.063 Uiso 1 1 calc R . . C31 C 0.7000(3) 0.0218(2) 0.03298(19) 0.0433(9) Uani 1 1 d . . . H31A H 0.7238 -0.0233 0.0242 0.065 Uiso 1 1 calc R E . H31B H 0.7489 0.0509 0.0143 0.065 Uiso 1 1 calc R . . H31C H 0.6174 0.0123 0.0110 0.065 Uiso 1 1 calc R . . C32 C 0.3407(3) 0.1920(2) 0.06932(19) 0.0448(10) Uani 1 1 d . . . H32A H 0.3767 0.2283 0.0534 0.067 Uiso 1 1 calc R E . H32B H 0.2581 0.1931 0.0697 0.067 Uiso 1 1 calc R . . H32C H 0.3457 0.1450 0.0385 0.067 Uiso 1 1 calc R . . O101 O -0.1504(3) -0.04109(19) 0.34834(18) 0.0727(10) Uani 1 1 d . . . O102 O -0.2420(3) 0.0162(2) 0.4234(2) 0.0933(12) Uani 1 1 d . . . N1 N 0.0816(4) -0.0078(2) 0.3718(2) 0.0620(10) Uani 1 1 d D . . H1N H 0.008(2) -0.032(2) 0.343(2) 0.074 Uiso 1 1 d D . . N2 N -0.1515(4) 0.0058(2) 0.4049(2) 0.0635(10) Uani 1 1 d . . . C33 C 0.2593(4) 0.0371(2) 0.3369(2) 0.0554(11) Uani 1 1 d . . . H33A H 0.2733 0.0833 0.3757 0.067 Uiso 1 1 calc R . . H33B H 0.3363 0.0273 0.3283 0.067 Uiso 1 1 calc R . . C34 C 0.1908(4) -0.0210(3) 0.3534(3) 0.0659(13) Uani 1 1 d . . . H34A H 0.1744 -0.0662 0.3132 0.079 Uiso 1 1 calc R . . H34B H 0.2395 -0.0267 0.3918 0.079 Uiso 1 1 calc R . . C35 C 0.0686(4) 0.0383(2) 0.4321(2) 0.0560(12) Uani 1 1 d . . . C36 C 0.1707(4) 0.0822(3) 0.4835(3) 0.0681(14) Uani 1 1 d . . . H36 H 0.2468 0.0785 0.4751 0.082 Uiso 1 1 calc R . . C37 C 0.1587(5) 0.1293(3) 0.5448(3) 0.0778(16) Uani 1 1 d . . . H37 H 0.2276 0.1580 0.5777 0.093 Uiso 1 1 calc R . . C38 C 0.0516(6) 0.1367(3) 0.5604(3) 0.0779(15) Uani 1 1 d . . . H38 H 0.0464 0.1699 0.6034 0.094 Uiso 1 1 calc R . . C39 C -0.0493(5) 0.0951(3) 0.5123(3) 0.0686(14) Uani 1 1 d . . . H39 H -0.1244 0.0995 0.5224 0.082 Uiso 1 1 calc R . . C40 C -0.0407(4) 0.0476(2) 0.4504(2) 0.0580(12) Uani 1 1 d . . . O103 O 0.6353(5) 0.4490(2) 0.3187(3) 0.1207(17) Uani 1 1 d . . . O104 O 0.6043(6) 0.5367(3) 0.3998(3) 0.167(3) Uani 1 1 d . . . N3 N 0.6939(3) 0.34081(19) 0.34264(18) 0.0547(9) Uani 1 1 d D . . H3N H 0.660(4) 0.358(2) 0.3125(19) 0.066 Uiso 1 1 d D . . N4 N 0.6361(5) 0.4803(3) 0.3800(4) 0.1084(19) Uani 1 1 d . . . C41 C 0.5830(3) 0.2195(2) 0.32000(19) 0.0431(9) Uani 1 1 d . . . H41A H 0.5874 0.1689 0.3025 0.052 Uiso 1 1 calc R . . H41B H 0.5672 0.2322 0.3668 0.052 Uiso 1 1 calc R . . C42 C 0.6962(4) 0.2661(2) 0.3209(2) 0.0501(10) Uani 1 1 d . . . H42A H 0.7606 0.2607 0.3521 0.060 Uiso 1 1 calc R . . H42B H 0.7136 0.2499 0.2744 0.060 Uiso 1 1 calc R . . C43 C 0.6983(4) 0.3840(2) 0.4085(2) 0.0531(11) Uani 1 1 d . . . C44 C 0.7357(4) 0.3626(3) 0.4620(2) 0.0643(13) Uani 1 1 d . . . H44 H 0.7549 0.3176 0.4510 0.077 Uiso 1 1 calc R . . C45 C 0.7457(6) 0.4043(3) 0.5295(3) 0.0889(18) Uani 1 1 d . . . H45 H 0.7737 0.3883 0.5641 0.107 Uiso 1 1 calc R . . C46 C 0.7155(7) 0.4690(3) 0.5479(3) 0.108(2) Uani 1 1 d . . . H46 H 0.7202 0.4971 0.5946 0.130 Uiso 1 1 calc R . . C47 C 0.6783(6) 0.4923(3) 0.4973(3) 0.095(2) Uani 1 1 d . . . H47 H 0.6570 0.5368 0.5091 0.114 Uiso 1 1 calc R . . C48 C 0.6717(4) 0.4510(2) 0.4288(3) 0.0684(14) Uani 1 1 d . . . O105 O -0.0239(3) -0.55237(17) 0.03717(17) 0.0724(10) Uani 1 1 d . . . O106 O -0.1009(3) -0.61508(17) 0.09029(18) 0.0732(9) Uani 1 1 d . . . N5 N 0.1424(3) -0.43870(17) 0.10136(18) 0.0482(8) Uani 1 1 d D . . H5N H 0.090(3) -0.4680(19) 0.0614(14) 0.058 Uiso 1 1 d D . . N6 N -0.0336(3) -0.56224(19) 0.0903(2) 0.0547(9) Uani 1 1 d . . . C49 C 0.1615(3) -0.3154(2) 0.1150(2) 0.0515(11) Uani 1 1 d . . . H49A H 0.0918 -0.3278 0.0780 0.062 Uiso 1 1 calc R . . H49B H 0.1354 -0.3045 0.1592 0.062 Uiso 1 1 calc R . . C50 C 0.2218(3) -0.3760(2) 0.1022(2) 0.0503(10) Uani 1 1 d . . . H50A H 0.2467 -0.3868 0.0578 0.060 Uiso 1 1 calc R . . H50B H 0.2927 -0.3624 0.1386 0.060 Uiso 1 1 calc R . . C51 C 0.1201(4) -0.4515(2) 0.1574(2) 0.0456(10) Uani 1 1 d . . . C52 C 0.1857(5) -0.4057(3) 0.2231(3) 0.0736(15) Uani 1 1 d . . . H52 H 0.2432 -0.3651 0.2277 0.088 Uiso 1 1 calc R . . C53 C 0.1677(6) -0.4188(3) 0.2799(3) 0.095(2) Uani 1 1 d . . . H53 H 0.2133 -0.3872 0.3234 0.114 Uiso 1 1 calc R . . C54 C 0.0843(6) -0.4773(3) 0.2761(3) 0.0934(19) Uani 1 1 d . . . H54 H 0.0728 -0.4852 0.3164 0.112 Uiso 1 1 calc R . . C55 C 0.0189(5) -0.5233(3) 0.2132(3) 0.0707(14) Uani 1 1 d . . . H55 H -0.0381 -0.5636 0.2096 0.085 Uiso 1 1 calc R . . C56 C 0.0364(4) -0.5105(2) 0.1548(2) 0.0488(10) Uani 1 1 d . . . C57 C -0.1251(5) -0.1647(4) 0.1593(5) 0.123(3) Uani 1 1 d . B . H57A H -0.0868 -0.1652 0.2033 0.148 Uiso 1 1 calc R . . H57B H -0.1406 -0.2134 0.1241 0.148 Uiso 1 1 calc R . . C58 C -0.2394(4) -0.1424(3) 0.1665(4) 0.093(2) Uani 1 1 d D . . H58A H -0.2801 -0.1445 0.1219 0.112 Uiso 1 1 calc R A 1 H58B H -0.2238 -0.0928 0.1999 0.112 Uiso 1 1 calc R A 1 O109 O 0.9499(3) 0.3361(2) 0.2895(2) 0.0829(11) Uani 1 1 d . . . O110 O 0.9737(4) 0.43586(19) 0.3746(2) 0.1002(13) Uani 1 1 d . . . N9 N 0.9791(3) 0.2213(2) 0.3107(2) 0.0602(10) Uani 1 1 d D . . H9N H 0.947(4) 0.238(2) 0.281(2) 0.072 Uiso 1 1 d D . . N10 N 0.9779(4) 0.3727(2) 0.3519(3) 0.0742(12) Uani 1 1 d . . . C65 C 0.8713(3) 0.0991(2) 0.2936(2) 0.0547(11) Uani 1 1 d . . . H65A H 0.8798 0.0495 0.2797 0.066 Uiso 1 1 calc R . . H65B H 0.8615 0.1158 0.3417 0.066 Uiso 1 1 calc R . . C66 C 0.9794(4) 0.1460(2) 0.2870(3) 0.0685(14) Uani 1 1 d . . . H66A H 1.0498 0.1402 0.3134 0.082 Uiso 1 1 calc R . . H66B H 0.9860 0.1294 0.2383 0.082 Uiso 1 1 calc R . . C67 C 1.0171(4) 0.2676(3) 0.3771(3) 0.0603(12) Uani 1 1 d . . . C68 C 1.0599(4) 0.2451(3) 0.4293(3) 0.0731(15) Uani 1 1 d . . . H68 H 1.0617 0.1964 0.4175 0.088 Uiso 1 1 calc R . . C69 C 1.0991(5) 0.2912(3) 0.4967(3) 0.0853(17) Uani 1 1 d . . . H69 H 1.1283 0.2738 0.5300 0.102 Uiso 1 1 calc R . . C70 C 1.0966(5) 0.3616(4) 0.5164(3) 0.0876(18) Uani 1 1 d . . . H70 H 1.1230 0.3930 0.5630 0.105 Uiso 1 1 calc R . . C71 C 1.0551(5) 0.3858(3) 0.4674(3) 0.0790(16) Uani 1 1 d . . . H71 H 1.0529 0.4345 0.4805 0.095 Uiso 1 1 calc R . . C72 C 1.0163(4) 0.3406(2) 0.3989(3) 0.0594(12) Uani 1 1 d . . . O111 O 0.5228(3) -0.05986(16) 0.52928(14) 0.0627(9) Uani 1 1 d . . . O112 O 0.4550(3) -0.09702(16) 0.60277(14) 0.0647(9) Uani 1 1 d . . . N11 N 0.4256(3) -0.12345(18) 0.39802(16) 0.0516(9) Uani 1 1 d D . . H11N H 0.487(3) -0.0909(19) 0.4280(18) 0.062 Uiso 1 1 d D . . N12 N 0.4502(3) -0.10036(18) 0.54339(17) 0.0510(9) Uani 1 1 d . . . C73 C 0.5064(4) -0.0817(2) 0.31561(18) 0.0433(9) Uani 1 1 d . . . H73A H 0.5026 -0.0323 0.3423 0.052 Uiso 1 1 calc R . . H73B H 0.5859 -0.0881 0.3293 0.052 Uiso 1 1 calc R . . C74 C 0.4134(4) -0.1347(2) 0.32608(19) 0.0483(10) Uani 1 1 d . . . H74A H 0.3347 -0.1298 0.3085 0.058 Uiso 1 1 calc R . . H74B H 0.4203 -0.1835 0.2999 0.058 Uiso 1 1 calc R . . C75 C 0.3480(4) -0.1602(2) 0.4212(2) 0.0456(10) Uani 1 1 d . . . C76 C 0.2496(4) -0.2128(2) 0.3751(2) 0.0559(11) Uani 1 1 d . . . H76 H 0.2400 -0.2220 0.3276 0.067 Uiso 1 1 calc R . . C77 C 0.1686(4) -0.2506(3) 0.3973(3) 0.0639(13) Uani 1 1 d . . . H77 H 0.1036 -0.2848 0.3648 0.077 Uiso 1 1 calc R . . C78 C 0.1787(4) -0.2403(3) 0.4658(3) 0.0649(13) Uani 1 1 d . . . H78 H 0.1217 -0.2671 0.4804 0.078 Uiso 1 1 calc R . . C79 C 0.2727(4) -0.1908(2) 0.5119(2) 0.0547(11) Uani 1 1 d . . . H79 H 0.2813 -0.1832 0.5591 0.066 Uiso 1 1 calc R . . C80 C 0.3556(4) -0.1515(2) 0.49056(19) 0.0442(10) Uani 1 1 d . . . O57A O -0.3840(7) -0.2280(5) 0.2876(4) 0.082(3) Uani 0.479(6) 1 d P B 1 O58A O -0.5094(9) -0.3245(6) 0.2619(5) 0.129(4) Uani 0.479(6) 1 d P B 1 N7A N -0.3163(6) -0.1915(4) 0.1908(6) 0.063(3) Uani 0.479(6) 1 d PD B 1 H7A H -0.3250 -0.1758 0.2335 0.076 Uiso 0.479(6) 1 calc PR B 1 N8A N -0.4402(8) -0.2862(6) 0.2468(5) 0.073(3) Uani 0.479(6) 1 d P B 1 O57B O -0.4359(16) -0.3208(6) 0.0262(5) 0.188(7) Uani 0.521(6) 1 d P B 2 O58B O -0.5317(10) -0.4154(6) 0.0383(5) 0.147(5) Uani 0.521(6) 1 d P B 2 N7B N -0.3264(9) -0.2114(5) 0.1303(6) 0.098(4) Uani 0.521(6) 1 d PD B 2 H7B H -0.3538 -0.2267 0.0859 0.118 Uiso 0.521(6) 1 calc PR B 2 N8B N -0.4725(13) -0.3565(7) 0.0597(6) 0.105(4) Uani 0.521(6) 1 d P B 2 C59A C -0.3739(6) -0.2609(3) 0.1473(4) 0.042(3) Uiso 0.479(6) 1 d PG B 1 C60A C -0.3715(7) -0.2855(4) 0.0780(4) 0.067(3) Uiso 0.479(6) 1 d PG B 1 H60A H -0.3338 -0.2543 0.0592 0.081 Uiso 0.479(6) 1 calc PR B 1 C61A C -0.4243(8) -0.3558(5) 0.0362(3) 0.094(6) Uiso 0.479(6) 1 d PG B 1 H61A H -0.4227 -0.3726 -0.0112 0.112 Uiso 0.479(6) 1 calc PR B 1 C62A C -0.4795(8) -0.4015(3) 0.0637(4) 0.084(5) Uiso 0.479(6) 1 d PG B 1 H62A H -0.5156 -0.4496 0.0352 0.101 Uiso 0.479(6) 1 calc PR B 1 C63A C -0.4819(6) -0.3769(3) 0.1331(4) 0.063(3) Uiso 0.479(6) 1 d PG B 1 H63A H -0.5197 -0.4082 0.1519 0.075 Uiso 0.479(6) 1 calc PR B 1 C64A C -0.4291(6) -0.3066(3) 0.1749(3) 0.048(2) Uiso 0.479(6) 1 d PG B 1 C59B C -0.3640(5) -0.2519(3) 0.1677(3) 0.047(3) Uiso 0.521(6) 1 d PG B 2 C60B C -0.3309(6) -0.2237(3) 0.2387(3) 0.065(3) Uiso 0.521(6) 1 d PG B 2 H60B H -0.2826 -0.1771 0.2618 0.078 Uiso 0.521(6) 1 calc PR B 2 C61B C -0.3683(7) -0.2639(4) 0.2759(2) 0.068(4) Uiso 0.521(6) 1 d PG B 2 H61B H -0.3457 -0.2447 0.3244 0.082 Uiso 0.521(6) 1 calc PR B 2 C62B C -0.4389(7) -0.3321(4) 0.2421(3) 0.082(4) Uiso 0.521(6) 1 d PG B 2 H62B H -0.4645 -0.3596 0.2676 0.098 Uiso 0.521(6) 1 calc PR B 2 C63B C -0.4721(5) -0.3603(3) 0.1711(3) 0.055(2) Uiso 0.521(6) 1 d PG B 2 H63B H -0.5203 -0.4069 0.1481 0.067 Uiso 0.521(6) 1 calc PR B 2 C64B C -0.4346(5) -0.3201(3) 0.1339(2) 0.047(2) Uiso 0.521(6) 1 d PG B 2 C81 C 0.6636(4) 0.3834(2) 0.1585(3) 0.0651(13) Uani 1 1 d . D . H81A H 0.6969 0.3727 0.1166 0.078 Uiso 1 1 calc R . . H81B H 0.7284 0.3980 0.1987 0.078 Uiso 1 1 calc R . . C82 C 0.5971(5) 0.4412(3) 0.1653(4) 0.118(3) Uani 1 1 d D . . H82A H 0.5318 0.4344 0.1889 0.142 Uiso 1 1 calc R C 1 H82B H 0.5635 0.4393 0.1194 0.142 Uiso 1 1 calc R C 1 N14A N 0.8486(9) 0.6544(8) 0.2711(5) 0.099(4) Uani 0.683(5) 1 d P D 1 O54A O 0.9151(7) 0.7122(4) 0.2944(4) 0.139(3) Uani 0.683(5) 1 d P D 1 O53A O 0.8056(10) 0.6270(5) 0.3120(4) 0.146(4) Uani 0.683(5) 1 d P D 1 N13A N 0.6841(6) 0.5149(3) 0.2075(3) 0.0715(19) Uani 0.683(5) 1 d PD D 1 H13A H 0.6971 0.5342 0.2525 0.086 Uiso 0.683(5) 1 calc PR D 1 O54B O 0.8624(10) 0.6387(6) 0.0657(6) 0.078(4) Uiso 0.317(5) 1 d P D 2 O53B O 0.7558(12) 0.5324(7) 0.0325(8) 0.082(4) Uiso 0.317(5) 1 d P D 2 N14B N 0.8133(16) 0.5911(11) 0.0806(8) 0.069(4) Uiso 0.317(5) 1 d P D 2 N13B N 0.6635(9) 0.4847(5) 0.1224(5) 0.043(3) Uani 0.317(5) 1 d PD D 2 H13B H 0.6547 0.4698 0.0776 0.051 Uiso 0.317(5) 1 calc PR D 2 C83A C 0.7386(3) 0.5469(2) 0.16954(18) 0.030(2) Uiso 0.683(5) 1 d PG D 1 C84A C 0.7148(4) 0.5128(2) 0.09870(19) 0.064(2) Uiso 0.683(5) 1 d PG D 1 H84A H 0.6629 0.4670 0.0773 0.076 Uiso 0.683(5) 1 calc PR D 1 C85A C 0.7668(6) 0.5455(3) 0.05910(18) 0.068(3) Uiso 0.683(5) 1 d PG D 1 H85A H 0.7506 0.5221 0.0107 0.082 Uiso 0.683(5) 1 calc PR D 1 C86A C 0.8427(6) 0.6123(4) 0.0903(3) 0.103(5) Uiso 0.683(5) 1 d PG D 1 H86A H 0.8783 0.6347 0.0633 0.123 Uiso 0.683(5) 1 calc PR D 1 C87A C 0.8665(4) 0.6465(2) 0.1612(3) 0.076(2) Uiso 0.683(5) 1 d PG D 1 H87A H 0.9184 0.6922 0.1825 0.091 Uiso 0.683(5) 1 calc PR D 1 C88A C 0.8144(4) 0.6138(2) 0.20078(19) 0.0577(19) Uiso 0.683(5) 1 d PG D 1 C83B C 0.7376(11) 0.5504(5) 0.1709(6) 0.136(16) Uiso 0.317(5) 1 d PG D 2 C84B C 0.7333(11) 0.5671(7) 0.2396(6) 0.064(4) Uiso 0.317(5) 1 d PG D 2 H84B H 0.6872 0.5338 0.2532 0.077 Uiso 0.317(5) 1 calc PR D 2 C85B C 0.7964(15) 0.6325(9) 0.2883(4) 0.075(9) Uiso 0.317(5) 1 d PG D 2 H85B H 0.7934 0.6439 0.3352 0.090 Uiso 0.317(5) 1 calc PR D 2 C86B C 0.8638(15) 0.6812(7) 0.2684(5) 0.15(3) Uiso 0.317(5) 1 d PG D 2 H86B H 0.9069 0.7259 0.3017 0.182 Uiso 0.317(5) 1 calc PR D 2 C87B C 0.8682(10) 0.6644(5) 0.1998(6) 0.058(4) Uiso 0.317(5) 1 d PG D 2 H87B H 0.9142 0.6977 0.1862 0.069 Uiso 0.317(5) 1 calc PR D 2 C88B C 0.8051(9) 0.5990(5) 0.1510(4) 0.041(3) Uiso 0.317(5) 1 d PG D 2 C89A C 0.9179(6) 0.2052(4) 0.0714(4) 0.046(3) Uiso 0.584(15) 1 d P E 1 H89A H 0.9038 0.2518 0.0735 0.055 Uiso 0.584(15) 1 calc PR E 1 H89B H 0.8751 0.1685 0.0265 0.055 Uiso 0.584(15) 1 calc PR E 1 C90A C 1.0443(6) 0.2074(3) 0.0801(3) 0.0973(19) Uiso 0.584(15) 1 d PD E 1 H90A H 1.0531 0.1580 0.0685 0.117 Uiso 0.584(15) 1 calc PR E 1 H90B H 1.0740 0.2240 0.0455 0.117 Uiso 0.584(15) 1 calc PR E 1 C89B C 0.9462(12) 0.2429(9) 0.1171(9) 0.079(5) Uiso 0.416(15) 1 d P E 2 H89C H 0.9832 0.2826 0.1613 0.095 Uiso 0.416(15) 1 calc PR E 2 H89D H 0.8996 0.2609 0.0875 0.095 Uiso 0.416(15) 1 calc PR E 2 C90B C 1.0443(6) 0.2074(3) 0.0801(3) 0.0973(19) Uiso 0.416(15) 1 d PD E 2 H90C H 1.0757 0.1756 0.0999 0.117 Uiso 0.416(15) 1 calc PR E 2 H90D H 1.0204 0.1845 0.0296 0.117 Uiso 0.416(15) 1 calc PR E 2 O55A O 1.2187(7) 0.2851(5) 0.2746(4) 0.079(3) Uani 0.489(6) 1 d P E 1 O56A O 1.3272(10) 0.3855(5) 0.3326(6) 0.121(4) Uani 0.489(6) 1 d P E 1 N15A N 1.1208(7) 0.2502(4) 0.1455(4) 0.067(3) Uani 0.489(6) 1 d PD E 1 H15A H 1.1291 0.2340 0.1786 0.080 Uiso 0.489(6) 1 calc PR E 1 N16A N 1.2674(16) 0.3444(11) 0.2753(9) 0.124(12) Uani 0.489(6) 1 d P E 1 O55B O 1.2128(8) 0.3887(4) 0.0687(5) 0.095(3) Uani 0.511(6) 1 d P E 2 O56B O 1.3462(8) 0.4777(5) 0.1365(9) 0.206(8) Uani 0.511(6) 1 d P E 2 N15B N 1.1257(8) 0.2863(4) 0.1073(5) 0.090(3) Uani 0.511(6) 1 d PD E 2 H15B H 1.1246 0.3061 0.0768 0.108 Uiso 0.511(6) 1 calc PR E 2 N16B N 1.2754(15) 0.4218(6) 0.1278(10) 0.095(6) Uani 0.511(6) 1 d P E 2 C91A C 1.1828(6) 0.3198(3) 0.1549(4) 0.045(3) Uiso 0.489(6) 1 d PGD E 1 C92A C 1.1804(7) 0.3451(4) 0.1023(3) 0.070(3) Uiso 0.489(6) 1 d PG E 1 H92A H 1.1340 0.3163 0.0581 0.084 Uiso 0.489(6) 1 calc PR E 1 C93A C 1.2459(9) 0.4125(5) 0.1143(4) 0.093(10) Uiso 0.489(6) 1 d PG E 1 H93A H 1.2442 0.4298 0.0783 0.112 Uiso 0.489(6) 1 calc PR E 1 C94A C 1.3138(9) 0.4547(4) 0.1789(5) 0.074(4) Uiso 0.489(6) 1 d PG E 1 H94A H 1.3586 0.5008 0.1870 0.089 Uiso 0.489(6) 1 calc PR E 1 C95A C 1.3162(8) 0.4294(4) 0.2315(4) 0.133(9) Uiso 0.489(6) 1 d PG E 1 H95A H 1.3626 0.4582 0.2757 0.159 Uiso 0.489(6) 1 calc PR E 1 C96A C 1.2507(7) 0.3620(4) 0.2195(3) 0.061(3) Uiso 0.489(6) 1 d PG E 1 C91B C 1.1970(10) 0.3285(6) 0.1699(6) 0.112(7) Uiso 0.511(6) 1 d PGD E 2 C92B C 1.1998(13) 0.3086(7) 0.2261(9) 0.196(10) Uiso 0.511(6) 1 d PG E 2 H92B H 1.1515 0.2648 0.2218 0.236 Uiso 0.511(6) 1 calc PR E 2 C93B C 1.2734(15) 0.3527(9) 0.2884(7) 0.131(16) Uiso 0.511(6) 1 d PG E 2 H93B H 1.2753 0.3391 0.3267 0.157 Uiso 0.511(6) 1 calc PR E 2 C94B C 1.3441(13) 0.4168(8) 0.2946(5) 0.182(9) Uiso 0.511(6) 1 d PG E 2 H94B H 1.3943 0.4469 0.3372 0.218 Uiso 0.511(6) 1 calc PR E 2 C95B C 1.3412(11) 0.4367(5) 0.2385(6) 0.135(9) Uiso 0.511(6) 1 d PG E 2 H95B H 1.3895 0.4804 0.2427 0.163 Uiso 0.511(6) 1 calc PR E 2 C96B C 1.2676(10) 0.3925(7) 0.1762(5) 0.102(4) Uiso 0.511(6) 1 d PG E 2 O200 O 0.4059(4) 0.2047(2) 0.4650(2) 0.1111(15) Uani 1 1 d . . . C201 C 0.4197(5) 0.2673(3) 0.4920(3) 0.0723(14) Uani 1 1 d . . . C202 C 0.3968(5) 0.3124(3) 0.4524(3) 0.0867(17) Uani 1 1 d . . . H20A H 0.4663 0.3511 0.4634 0.130 Uiso 1 1 calc R . . H20B H 0.3294 0.3325 0.4646 0.130 Uiso 1 1 calc R . . H20C H 0.3795 0.2834 0.4033 0.130 Uiso 1 1 calc R . . C200 C 0.4612(7) 0.3028(3) 0.5674(3) 0.115(2) Uani 1 1 d . . . H20D H 0.4007 0.3250 0.5877 0.173 Uiso 1 1 calc R . . H20E H 0.5335 0.3394 0.5778 0.173 Uiso 1 1 calc R . . H20F H 0.4769 0.2676 0.5865 0.173 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 O4 0.0492(16) 0.0491(16) 0.0467(16) 0.0289(13) 0.0176(12) 0.0050(12) O6 0.0442(15) 0.0361(14) 0.0444(15) 0.0172(12) 0.0044(12) 0.0006(12) O11 0.0366(15) 0.0344(15) 0.098(2) 0.0336(15) 0.0231(14) 0.0071(12) O13 0.0357(16) 0.075(2) 0.181(4) 0.086(2) 0.046(2) 0.0217(15) O18 0.0447(15) 0.0355(15) 0.0502(16) 0.0195(13) -0.0048(12) -0.0038(12) O20 0.0562(17) 0.0477(16) 0.0335(14) 0.0199(12) 0.0070(12) -0.0076(13) O25 0.0496(16) 0.0310(14) 0.0734(19) 0.0243(13) 0.0215(14) 0.0074(12) O27 0.0354(15) 0.0430(16) 0.077(2) 0.0309(14) 0.0158(13) 0.0039(12) C1 0.035(2) 0.0288(19) 0.041(2) 0.0161(16) 0.0151(16) 0.0084(16) C2 0.040(2) 0.034(2) 0.038(2) 0.0186(17) 0.0149(16) 0.0124(17) C3 0.0327(19) 0.036(2) 0.038(2) 0.0180(17) 0.0129(16) 0.0141(16) C4 0.044(2) 0.040(2) 0.041(2) 0.0231(18) 0.0196(18) 0.0129(18) C5 0.046(2) 0.041(2) 0.038(2) 0.0186(18) 0.0117(17) 0.0054(18) C6 0.041(2) 0.032(2) 0.041(2) 0.0152(17) 0.0144(17) 0.0076(17) C7 0.0331(19) 0.035(2) 0.044(2) 0.0213(17) 0.0148(16) 0.0087(16) C8 0.032(2) 0.036(2) 0.045(2) 0.0196(17) 0.0069(16) 0.0026(16) C9 0.0317(19) 0.0293(19) 0.035(2) 0.0148(16) 0.0057(15) 0.0014(15) C10 0.034(2) 0.033(2) 0.035(2) 0.0145(16) 0.0081(15) -0.0006(16) C11 0.034(2) 0.033(2) 0.068(3) 0.0264(19) 0.0148(18) 0.0083(16) C12 0.037(2) 0.047(3) 0.110(4) 0.046(3) 0.025(2) 0.0045(19) C13 0.033(2) 0.052(3) 0.089(3) 0.042(2) 0.018(2) 0.0114(19) C14 0.0284(18) 0.0330(19) 0.039(2) 0.0168(16) 0.0095(15) 0.0063(15) C15 0.0270(18) 0.0307(19) 0.037(2) 0.0154(16) 0.0082(15) 0.0061(15) C16 0.0301(18) 0.0305(19) 0.036(2) 0.0158(16) 0.0078(15) 0.0073(15) C17 0.0309(19) 0.0313(19) 0.039(2) 0.0175(16) 0.0074(15) 0.0081(15) C18 0.032(2) 0.031(2) 0.048(2) 0.0172(18) 0.0037(17) 0.0020(16) C19 0.039(2) 0.033(2) 0.034(2) 0.0099(16) 0.0030(16) 0.0034(17) C20 0.035(2) 0.037(2) 0.042(2) 0.0209(18) 0.0090(17) 0.0047(16) C21 0.0311(19) 0.034(2) 0.043(2) 0.0179(17) 0.0109(16) 0.0044(15) C22 0.036(2) 0.0304(19) 0.036(2) 0.0157(16) 0.0082(16) 0.0049(16) C23 0.035(2) 0.0278(19) 0.034(2) 0.0123(16) 0.0103(15) 0.0008(15) C24 0.035(2) 0.037(2) 0.036(2) 0.0185(17) 0.0095(16) 0.0024(16) C25 0.046(2) 0.029(2) 0.039(2) 0.0162(17) 0.0094(17) 0.0042(17) C26 0.042(2) 0.030(2) 0.045(2) 0.0138(17) 0.0086(17) -0.0003(16) C27 0.033(2) 0.037(2) 0.045(2) 0.0186(18) 0.0094(16) 0.0024(16) C28 0.044(2) 0.030(2) 0.042(2) 0.0150(17) 0.0132(17) 0.0084(16) C29 0.030(2) 0.045(2) 0.057(2) 0.026(2) 0.0013(17) 0.0028(17) C30 0.047(2) 0.037(2) 0.039(2) 0.0134(18) 0.0137(17) 0.0013(17) C31 0.048(2) 0.037(2) 0.050(2) 0.0192(19) 0.0217(18) 0.0073(17) C32 0.043(2) 0.056(3) 0.048(2) 0.034(2) 0.0128(18) 0.0123(19) O101 0.073(2) 0.071(2) 0.063(2) 0.027(2) -0.0054(17) 0.0011(18) O102 0.059(2) 0.095(3) 0.120(3) 0.031(2) 0.014(2) 0.027(2) N1 0.063(3) 0.063(3) 0.058(3) 0.030(2) 0.0093(19) -0.002(2) N2 0.065(3) 0.055(3) 0.070(3) 0.033(2) 0.001(2) 0.006(2) C33 0.062(3) 0.061(3) 0.054(3) 0.035(2) 0.015(2) 0.010(2) C34 0.075(3) 0.063(3) 0.070(3) 0.038(3) 0.019(3) 0.012(2) C35 0.057(3) 0.057(3) 0.053(3) 0.028(2) 0.006(2) 0.001(2) C36 0.064(3) 0.071(3) 0.067(3) 0.035(3) 0.007(3) -0.004(3) C37 0.086(4) 0.061(3) 0.071(4) 0.024(3) 0.004(3) -0.013(3) C38 0.101(4) 0.054(3) 0.071(4) 0.020(3) 0.014(3) 0.009(3) C39 0.082(4) 0.062(3) 0.063(3) 0.026(3) 0.000(3) 0.025(3) C40 0.062(3) 0.056(3) 0.059(3) 0.032(2) -0.001(2) 0.007(2) O103 0.191(5) 0.087(3) 0.096(3) 0.053(3) 0.007(3) 0.038(3) O104 0.250(7) 0.073(3) 0.158(5) 0.030(3) -0.023(4) 0.070(4) N3 0.064(2) 0.044(2) 0.047(2) 0.0172(18) 0.0002(18) -0.0035(17) N4 0.143(5) 0.056(3) 0.115(5) 0.034(3) -0.015(4) 0.019(3) C41 0.047(2) 0.042(2) 0.042(2) 0.0197(19) 0.0092(18) 0.0058(18) C42 0.049(2) 0.051(3) 0.044(2) 0.015(2) 0.0089(19) 0.002(2) C43 0.056(3) 0.038(2) 0.053(3) 0.014(2) 0.001(2) -0.005(2) C44 0.082(3) 0.051(3) 0.049(3) 0.014(2) 0.005(2) 0.007(2) C45 0.131(5) 0.072(4) 0.051(3) 0.016(3) 0.006(3) 0.016(4) C46 0.153(7) 0.068(4) 0.074(4) -0.003(3) 0.015(4) 0.020(4) C47 0.116(5) 0.044(3) 0.101(5) 0.000(3) 0.013(4) 0.019(3) C48 0.077(3) 0.041(3) 0.072(3) 0.013(3) -0.002(3) 0.004(2) O105 0.083(2) 0.062(2) 0.064(2) 0.0335(17) -0.0018(17) -0.0134(17) O106 0.064(2) 0.0533(19) 0.103(3) 0.0402(18) 0.0204(18) -0.0088(16) N5 0.050(2) 0.0361(19) 0.058(2) 0.0238(17) 0.0061(17) -0.0010(15) N6 0.045(2) 0.046(2) 0.079(3) 0.033(2) 0.0145(19) 0.0068(17) C49 0.035(2) 0.035(2) 0.089(3) 0.032(2) 0.013(2) 0.0009(17) C50 0.040(2) 0.042(2) 0.071(3) 0.028(2) 0.011(2) 0.0024(18) C51 0.050(2) 0.039(2) 0.050(3) 0.018(2) 0.011(2) 0.0112(19) C52 0.090(4) 0.056(3) 0.064(3) 0.020(3) 0.005(3) 0.004(3) C53 0.139(6) 0.072(4) 0.056(3) 0.020(3) 0.011(3) -0.003(4) C54 0.140(6) 0.099(5) 0.055(3) 0.041(3) 0.030(4) 0.029(4) C55 0.085(4) 0.069(3) 0.075(4) 0.042(3) 0.029(3) 0.018(3) C56 0.055(3) 0.041(2) 0.054(3) 0.024(2) 0.010(2) 0.009(2) C57 0.053(3) 0.159(6) 0.248(9) 0.155(6) 0.081(4) 0.054(4) C58 0.044(3) 0.070(4) 0.205(7) 0.086(4) 0.055(3) 0.023(2) O109 0.088(3) 0.069(2) 0.089(3) 0.035(2) 0.006(2) 0.0074(19) O110 0.112(3) 0.048(2) 0.132(3) 0.035(2) 0.006(3) 0.006(2) N9 0.050(2) 0.046(2) 0.080(3) 0.022(2) 0.013(2) 0.0031(17) N10 0.064(3) 0.048(3) 0.101(4) 0.026(3) 0.008(2) -0.001(2) C65 0.044(2) 0.047(3) 0.065(3) 0.021(2) -0.007(2) 0.0036(19) C66 0.046(3) 0.052(3) 0.095(4) 0.019(3) 0.011(2) 0.003(2) C67 0.037(2) 0.054(3) 0.082(4) 0.026(3) 0.009(2) -0.006(2) C68 0.045(3) 0.063(3) 0.107(4) 0.042(3) -0.002(3) -0.006(2) C69 0.059(3) 0.087(4) 0.095(4) 0.041(4) -0.007(3) -0.018(3) C70 0.073(4) 0.092(5) 0.076(4) 0.026(4) 0.005(3) -0.014(3) C71 0.070(3) 0.059(3) 0.091(4) 0.020(3) 0.010(3) -0.008(3) C72 0.053(3) 0.051(3) 0.071(3) 0.026(3) 0.008(2) 0.000(2) O111 0.084(2) 0.0517(18) 0.0450(17) 0.0235(15) 0.0013(15) -0.0056(16) O112 0.099(2) 0.064(2) 0.0385(17) 0.0262(15) 0.0162(16) 0.0212(17) N11 0.062(2) 0.051(2) 0.0368(19) 0.0196(17) 0.0098(16) -0.0052(17) N12 0.072(2) 0.042(2) 0.043(2) 0.0216(17) 0.0132(18) 0.0110(18) C73 0.053(2) 0.042(2) 0.033(2) 0.0175(18) 0.0068(18) 0.0036(18) C74 0.057(3) 0.049(2) 0.035(2) 0.0195(19) 0.0075(18) -0.003(2) C75 0.053(2) 0.041(2) 0.045(2) 0.0195(19) 0.0121(19) 0.0060(19) C76 0.061(3) 0.052(3) 0.047(3) 0.018(2) 0.008(2) -0.002(2) C77 0.055(3) 0.060(3) 0.075(3) 0.033(3) 0.008(2) -0.002(2) C78 0.059(3) 0.075(3) 0.078(3) 0.047(3) 0.027(3) 0.013(3) C79 0.064(3) 0.057(3) 0.057(3) 0.033(2) 0.019(2) 0.020(2) C80 0.053(2) 0.040(2) 0.042(2) 0.0185(19) 0.0112(19) 0.0086(19) O57A 0.074(5) 0.082(6) 0.095(6) 0.043(5) 0.018(4) 0.012(5) O58A 0.096(7) 0.157(10) 0.142(8) 0.088(8) 0.026(6) -0.018(7) N7A 0.036(4) 0.056(5) 0.105(8) 0.032(5) 0.031(5) 0.014(4) N8A 0.058(6) 0.069(7) 0.093(7) 0.036(6) 0.032(5) -0.005(5) O57B 0.39(2) 0.116(9) 0.059(6) 0.017(6) 0.018(9) 0.117(11) O58B 0.128(8) 0.116(8) 0.118(8) -0.040(7) -0.027(7) 0.047(7) N7B 0.127(9) 0.077(7) 0.144(10) 0.072(7) 0.080(8) 0.056(6) N8B 0.131(10) 0.082(9) 0.075(8) 0.002(7) -0.019(8) 0.044(7) C81 0.049(3) 0.039(2) 0.118(4) 0.040(3) 0.030(3) 0.004(2) C82 0.063(4) 0.057(4) 0.263(9) 0.089(5) 0.045(4) 0.015(3) N14A 0.078(7) 0.078(6) 0.084(7) -0.016(5) -0.048(5) 0.019(5) O54A 0.120(6) 0.073(5) 0.157(7) 0.003(4) -0.052(5) 0.003(4) O53A 0.229(10) 0.092(6) 0.073(5) 0.011(4) -0.040(5) 0.025(6) N13A 0.093(5) 0.057(4) 0.062(4) 0.019(3) 0.013(3) 0.022(3) N13B 0.059(7) 0.021(5) 0.051(6) 0.016(4) 0.032(5) -0.003(4) O55A 0.082(5) 0.077(6) 0.073(5) 0.018(5) 0.023(4) 0.021(4) O56A 0.151(9) 0.057(5) 0.121(8) 0.015(6) 0.001(7) 0.000(5) N15A 0.077(6) 0.056(5) 0.090(6) 0.042(5) 0.040(5) 0.024(4) N16A 0.143(19) 0.16(2) 0.073(9) 0.002(10) 0.042(9) 0.118(17) O55B 0.098(6) 0.077(6) 0.127(8) 0.064(5) 0.031(6) 0.002(5) O56B 0.071(6) 0.067(6) 0.47(2) 0.086(10) 0.062(9) 0.013(5) N15B 0.087(7) 0.047(5) 0.158(10) 0.052(6) 0.053(6) 0.019(5) N16B 0.062(6) 0.055(7) 0.182(16) 0.051(9) 0.041(8) 0.028(5) O200 0.160(4) 0.060(3) 0.097(3) 0.013(2) 0.008(3) 0.033(3) C201 0.077(3) 0.054(3) 0.084(4) 0.017(3) 0.028(3) 0.022(3) C202 0.097(4) 0.070(4) 0.107(4) 0.036(3) 0.047(3) 0.032(3) C200 0.181(7) 0.086(5) 0.074(4) 0.020(4) 0.034(4) 0.033(5) _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 O4 C4 1.375(4) . ? O4 C33 1.432(5) . ? O6 C6 1.386(4) . ? O6 C41 1.430(4) . ? O11 C11 1.386(4) . ? O11 C49 1.420(4) . ? O13 C57 1.313(6) . ? O13 C13 1.381(5) . ? O18 C18 1.393(4) . ? O18 C65 1.421(4) . ? O20 C20 1.361(4) . ? O20 C73 1.412(4) . ? O25 C25 1.386(4) . ? O25 C81 1.425(5) . ? O27 C89B 1.371(14) . ? O27 C27 1.381(4) . ? O27 C89A 1.460(8) . ? C1 C6 1.388(5) . ? C1 C2 1.402(5) . ? C1 C28 1.520(5) . ? C2 C3 1.388(5) . ? C3 C4 1.390(5) . ? C3 C7 1.508(5) . ? C4 C5 1.385(5) . ? C5 C6 1.384(5) . ? C7 C29 1.516(5) . ? C7 C8 1.536(5) . ? C8 C9 1.377(5) . ? C8 C13 1.394(5) . ? C9 C10 1.400(5) . ? C10 C11 1.386(5) . ? C10 C14 1.513(5) . ? C11 C12 1.385(5) . ? C12 C13 1.387(6) . ? C14 C15 1.519(5) . ? C14 C30 1.532(5) . ? C15 C16 1.385(5) . ? C15 C20 1.400(5) . ? C16 C17 1.393(5) . ? C17 C18 1.384(5) . ? C17 C21 1.516(5) . ? C18 C19 1.401(5) . ? C19 C20 1.387(5) . ? C21 C22 1.523(5) . ? C21 C31 1.528(5) . ? C22 C27 1.385(5) . ? C22 C23 1.389(5) . ? C23 C24 1.391(5) . ? C24 C25 1.388(5) . ? C24 C28 1.517(5) . ? C25 C26 1.378(5) . ? C26 C27 1.396(5) . ? C28 C32 1.532(5) . ? O101 N2 1.258(5) . ? O102 N2 1.213(5) . ? N1 C35 1.351(6) . ? N1 C34 1.437(6) . ? N2 C40 1.447(6) . ? C33 C34 1.499(6) . ? C35 C40 1.420(7) . ? C35 C36 1.436(6) . ? C36 C37 1.370(7) . ? C37 C38 1.368(8) . ? C38 C39 1.387(7) . ? C39 C40 1.371(7) . ? O103 N4 1.237(7) . ? O104 N4 1.233(7) . ? N3 C43 1.363(5) . ? N3 C42 1.453(5) . ? N4 C48 1.425(7) . ? C41 C42 1.500(5) . ? C43 C48 1.401(6) . ? C43 C44 1.403(6) . ? C44 C45 1.370(7) . ? C45 C46 1.378(8) . ? C46 C47 1.375(9) . ? C47 C48 1.392(8) . ? O105 N6 1.233(4) . ? O106 N6 1.234(4) . ? N5 C51 1.356(5) . ? N5 C50 1.454(5) . ? N6 C56 1.445(5) . ? C49 C50 1.504(5) . ? C51 C56 1.410(5) . ? C51 C52 1.413(6) . ? C52 C53 1.362(7) . ? C53 C54 1.390(8) . ? C54 C55 1.374(7) . ? C55 C56 1.390(6) . ? C57 C58 1.507(7) . ? C58 N7B 1.485(10) . ? C58 N7A 1.512(9) . ? O109 N10 1.243(5) . ? O110 N10 1.234(5) . ? N9 C67 1.364(6) . ? N9 C66 1.457(6) . ? N10 C72 1.445(6) . ? C65 C66 1.517(6) . ? C67 C68 1.413(7) . ? C67 C72 1.414(6) . ? C68 C69 1.381(8) . ? C69 C70 1.371(8) . ? C70 C71 1.375(8) . ? C71 C72 1.393(7) . ? O111 N12 1.233(4) . ? O112 N12 1.235(4) . ? N11 C75 1.340(5) . ? N11 C74 1.450(5) . ? N12 C80 1.438(5) . ? C73 C74 1.507(5) . ? C75 C80 1.413(5) . ? C75 C76 1.421(6) . ? C76 C77 1.364(6) . ? C77 C78 1.385(7) . ? C78 C79 1.367(6) . ? C79 C80 1.386(6) . ? O57A N8A 1.220(11) . ? O58A N8A 1.192(11) . ? N7A C59A 1.396(10) . ? N8A C64A 1.470(11) . ? O57B N8B 1.257(19) . ? O58B N8B 1.189(15) . ? N7B C59B 1.398(10) . ? N8B C64B 1.461(12) . ? C59A C60A 1.3900 . ? C59A C64A 1.3900 . ? C60A C61A 1.3900 . ? C61A C62A 1.3900 . ? C62A C63A 1.3900 . ? C63A C64A 1.3900 . ? C59B C60B 1.3900 . ? C59B C64B 1.3900 . ? C60B C61B 1.3900 . ? C61B C62B 1.3900 . ? C62B C63B 1.3900 . ? C63B C64B 1.3900 . ? C81 C82 1.514(6) . ? C82 N13A 1.564(8) . ? C82 N13B 1.664(10) . ? N14A O54A 1.204(18) . ? N14A O53A 1.303(19) . ? N14A C88A 1.400(8) . ? N13A C83A 1.366(7) . ? O54B N14B 1.21(2) . ? O53B N14B 1.29(2) . ? N14B C88B 1.467(16) . ? N13B C83B 1.434(12) . ? C83A C84A 1.3900 . ? C83A C88A 1.3900 . ? C84A C85A 1.3900 . ? C85A C86A 1.3900 . ? C86A C87A 1.3900 . ? C87A C88A 1.3900 . ? C83B C84B 1.3900 . ? C83B C88B 1.3900 . ? C84B C85B 1.3900 . ? C85B C86B 1.3900 . ? C86B C87B 1.3900 . ? C87B C88B 1.3900 . ? C89A C90A 1.470(9) . ? C90A N15A 1.442(9) . ? O55A N16A 1.255(19) . ? O56A N16A 1.25(2) . ? N15A C91A 1.427(9) . ? N16A C96A 1.356(18) . ? O55B N16B 1.26(2) . ? O56B N16B 1.243(14) . ? N15B C91B 1.375(11) . ? N16B C96B 1.368(15) . ? C91A C92A 1.3900 . ? C91A C96A 1.3900 . ? C92A C93A 1.3900 . ? C93A C94A 1.3900 . ? C94A C95A 1.3900 . ? C95A C96A 1.3900 . ? C91B C92B 1.3900 . ? C91B C96B 1.3900 . ? C92B C93B 1.3900 . ? C93B C94B 1.3900 . ? C94B C95B 1.3900 . ? C95B C96B 1.3900 . ? O200 C201 1.188(6) . ? C201 C200 1.485(8) . ? C201 C202 1.490(7) . ? 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 C4 O4 C33 117.0(3) . . ? C6 O6 C41 116.4(3) . . ? C11 O11 C49 117.1(3) . . ? C57 O13 C13 120.7(4) . . ? C18 O18 C65 117.6(3) . . ? C20 O20 C73 121.1(3) . . ? C25 O25 C81 116.8(3) . . ? C89B O27 C27 116.0(6) . . ? C27 O27 C89A 114.3(4) . . ? C6 C1 C2 115.9(3) . . ? C6 C1 C28 119.5(3) . . ? C2 C1 C28 124.5(3) . . ? C3 C2 C1 123.4(3) . . ? C2 C3 C4 117.6(3) . . ? C2 C3 C7 124.6(3) . . ? C4 C3 C7 117.7(3) . . ? O4 C4 C5 123.2(3) . . ? O4 C4 C3 115.5(3) . . ? C5 C4 C3 121.3(3) . . ? C6 C5 C4 118.8(3) . . ? C5 C6 O6 121.0(3) . . ? C5 C6 C1 122.9(3) . . ? O6 C6 C1 116.2(3) . . ? C3 C7 C29 114.2(3) . . ? C3 C7 C8 110.8(3) . . ? C29 C7 C8 110.4(3) . . ? C9 C8 C13 117.6(3) . . ? C9 C8 C7 123.4(3) . . ? C13 C8 C7 119.1(3) . . ? C8 C9 C10 123.5(3) . . ? C11 C10 C9 116.7(3) . . ? C11 C10 C14 120.3(3) . . ? C9 C10 C14 123.0(3) . . ? C12 C11 O11 122.1(3) . . ? C12 C11 C10 121.9(3) . . ? O11 C11 C10 116.1(3) . . ? C11 C12 C13 119.3(4) . . ? O13 C13 C12 121.7(3) . . ? O13 C13 C8 117.3(3) . . ? C12 C13 C8 121.1(4) . . ? C10 C14 C15 114.0(3) . . ? C10 C14 C30 109.9(3) . . ? C15 C14 C30 113.7(3) . . ? C16 C15 C20 117.9(3) . . ? C16 C15 C14 124.2(3) . . ? C20 C15 C14 117.8(3) . . ? C15 C16 C17 123.1(3) . . ? C18 C17 C16 117.3(3) . . ? C18 C17 C21 119.1(3) . . ? C16 C17 C21 123.6(3) . . ? C17 C18 O18 117.2(3) . . ? C17 C18 C19 121.8(3) . . ? O18 C18 C19 120.9(3) . . ? C20 C19 C18 119.0(3) . . ? O20 C20 C19 124.8(3) . . ? O20 C20 C15 114.3(3) . . ? C19 C20 C15 120.9(3) . . ? C17 C21 C22 111.9(3) . . ? C17 C21 C31 114.1(3) . . ? C22 C21 C31 110.2(3) . . ? C27 C22 C23 117.3(3) . . ? C27 C22 C21 121.2(3) . . ? C23 C22 C21 121.5(3) . . ? C22 C23 C24 123.4(3) . . ? C25 C24 C23 117.1(3) . . ? C25 C24 C28 120.9(3) . . ? C23 C24 C28 121.9(3) . . ? C26 C25 O25 122.3(3) . . ? C26 C25 C24 121.7(3) . . ? O25 C25 C24 116.0(3) . . ? C25 C26 C27 119.3(3) . . ? O27 C27 C22 118.6(3) . . ? O27 C27 C26 120.1(3) . . ? C22 C27 C26 121.3(3) . . ? C24 C28 C1 112.2(3) . . ? C24 C28 C32 109.0(3) . . ? C1 C28 C32 114.8(3) . . ? C35 N1 C34 126.2(4) . . ? O102 N2 O101 122.4(4) . . ? O102 N2 C40 118.7(5) . . ? O101 N2 C40 118.9(4) . . ? O4 C33 C34 107.7(4) . . ? N1 C34 C33 113.5(4) . . ? N1 C35 C40 125.1(4) . . ? N1 C35 C36 119.8(5) . . ? C40 C35 C36 115.1(5) . . ? C37 C36 C35 120.3(5) . . ? C38 C37 C36 122.8(5) . . ? C37 C38 C39 118.8(5) . . ? C40 C39 C38 120.1(5) . . ? C39 C40 C35 122.9(4) . . ? C39 C40 N2 115.3(5) . . ? C35 C40 N2 121.8(4) . . ? C43 N3 C42 124.3(4) . . ? O104 N4 O103 120.6(6) . . ? O104 N4 C48 118.9(7) . . ? O103 N4 C48 120.5(5) . . ? O6 C41 C42 107.2(3) . . ? N3 C42 C41 113.3(4) . . ? N3 C43 C48 125.3(4) . . ? N3 C43 C44 119.4(4) . . ? C48 C43 C44 115.3(4) . . ? C45 C44 C43 122.5(5) . . ? C44 C45 C46 120.9(6) . . ? C47 C46 C45 118.8(6) . . ? C46 C47 C48 120.3(5) . . ? C47 C48 C43 122.1(5) . . ? C47 C48 N4 116.5(5) . . ? C43 C48 N4 121.4(5) . . ? C51 N5 C50 125.5(3) . . ? O105 N6 O106 122.2(4) . . ? O105 N6 C56 119.1(3) . . ? O106 N6 C56 118.7(4) . . ? O11 C49 C50 106.9(3) . . ? N5 C50 C49 110.1(3) . . ? N5 C51 C56 123.9(4) . . ? N5 C51 C52 119.9(4) . . ? C56 C51 C52 116.1(4) . . ? C53 C52 C51 121.0(5) . . ? C52 C53 C54 121.9(5) . . ? C55 C54 C53 119.0(5) . . ? C54 C55 C56 119.7(5) . . ? C55 C56 C51 122.3(4) . . ? C55 C56 N6 116.5(4) . . ? C51 C56 N6 121.2(4) . . ? O13 C57 C58 110.1(5) . . ? N7B C58 C57 101.5(6) . . ? N7B C58 N7A 46.8(5) . . ? C57 C58 N7A 109.4(5) . . ? C67 N9 C66 124.2(4) . . ? O110 N10 O109 121.3(5) . . ? O110 N10 C72 119.4(5) . . ? O109 N10 C72 119.3(4) . . ? O18 C65 C66 108.3(4) . . ? N9 C66 C65 114.3(4) . . ? N9 C67 C68 121.5(5) . . ? N9 C67 C72 123.1(5) . . ? C68 C67 C72 115.4(5) . . ? C69 C68 C67 122.3(5) . . ? C70 C69 C68 121.0(6) . . ? C69 C70 C71 118.6(6) . . ? C70 C71 C72 121.5(5) . . ? C71 C72 C67 121.1(5) . . ? C71 C72 N10 116.3(5) . . ? C67 C72 N10 122.5(4) . . ? C75 N11 C74 122.4(3) . . ? O111 N12 O112 121.3(3) . . ? O111 N12 C80 120.0(3) . . ? O112 N12 C80 118.7(4) . . ? O20 C73 C74 103.7(3) . . ? N11 C74 C73 110.9(3) . . ? N11 C75 C80 124.7(4) . . ? N11 C75 C76 120.6(4) . . ? C80 C75 C76 114.7(4) . . ? C77 C76 C75 121.9(4) . . ? C76 C77 C78 121.7(4) . . ? C79 C78 C77 118.4(4) . . ? C78 C79 C80 120.8(4) . . ? C79 C80 C75 122.4(4) . . ? C79 C80 N12 116.1(4) . . ? C75 C80 N12 121.4(4) . . ? C59A N7A C58 122.0(8) . . ? O58A N8A O57A 122.8(11) . . ? O58A N8A C64A 118.9(10) . . ? O57A N8A C64A 118.0(8) . . ? C59B N7B C58 119.0(9) . . ? O58B N8B O57B 127.9(13) . . ? O58B N8B C64B 117.7(14) . . ? O57B N8B C64B 114.4(12) . . ? C60A C59A C64A 120.0 . . ? C60A C59A N7A 120.8(6) . . ? C64A C59A N7A 119.1(6) . . ? C59A C60A C61A 120.0 . . ? C62A C61A C60A 120.0 . . ? C61A C62A C63A 120.0 . . ? C64A C63A C62A 120.0 . . ? C63A C64A C59A 120.0 . . ? C63A C64A N8A 115.1(5) . . ? C59A C64A N8A 124.9(5) . . ? C60B C59B C64B 120.0 . . ? C60B C59B N7B 120.0(6) . . ? C64B C59B N7B 120.0(6) . . ? C59B C60B C61B 120.0 . . ? C62B C61B C60B 120.0 . . ? C61B C62B C63B 120.0 . . ? C64B C63B C62B 120.0 . . ? C63B C64B C59B 120.0 . . ? C63B C64B N8B 114.6(8) . . ? C59B C64B N8B 125.4(8) . . ? O25 C81 C82 105.1(4) . . ? C81 C82 N13A 108.5(4) . . ? C81 C82 N13B 101.6(5) . . ? N13A C82 N13B 62.1(4) . . ? O54A N14A O53A 119.9(9) . . ? O54A N14A C88A 123.0(16) . . ? O53A N14A C88A 117.1(12) . . ? C83A N13A C82 115.2(5) . . ? O54B N14B O53B 119.1(14) . . ? O54B N14B C88B 123.5(16) . . ? O53B N14B C88B 117.1(17) . . ? C83B N13B C82 108.3(8) . . ? N13A C83A C84A 119.2(4) . . ? N13A C83A C88A 120.8(4) . . ? C84A C83A C88A 120.0 . . ? C85A C84A C83A 120.0 . . ? C84A C85A C86A 120.0 . . ? C85A C86A C87A 120.0 . . ? C88A C87A C86A 120.0 . . ? C87A C88A C83A 120.0 . . ? C87A C88A N14A 113.1(9) . . ? C83A C88A N14A 126.8(9) . . ? C84B C83B C88B 120.0 . . ? C84B C83B N13B 117.5(8) . . ? C88B C83B N13B 122.3(8) . . ? C85B C84B C83B 120.0 . . ? C86B C85B C84B 120.0 . . ? C85B C86B C87B 120.0 . . ? C88B C87B C86B 120.0 . . ? C87B C88B C83B 120.0 . . ? C87B C88B N14B 113.4(11) . . ? C83B C88B N14B 126.5(11) . . ? O27 C89A C90A 107.0(5) . . ? N15A C90A C89A 119.4(6) . . ? C91A N15A C90A 117.9(7) . . ? O56A N16A O55A 113.0(16) . . ? O56A N16A C96A 124.5(19) . . ? O55A N16A C96A 122.3(18) . . ? O56B N16B O55B 116.3(16) . . ? O56B N16B C96B 124(2) . . ? O55B N16B C96B 119.1(12) . . ? C92A C91A C96A 120.0 . . ? C92A C91A N15A 122.8(6) . . ? C96A C91A N15A 117.1(6) . . ? C91A C92A C93A 120.0 . . ? C92A C93A C94A 120.0 . . ? C95A C94A C93A 120.0 . . ? C94A C95A C96A 120.0 . . ? N16A C96A C95A 112.3(11) . . ? N16A C96A C91A 127.6(11) . . ? C95A C96A C91A 120.0 . . ? N15B C91B C92B 121.9(11) . . ? N15B C91B C96B 118.1(11) . . ? C92B C91B C96B 120.0 . . ? C93B C92B C91B 120.0 . . ? C92B C93B C94B 120.0 . . ? C95B C94B C93B 120.0 . . ? C94B C95B C96B 120.0 . . ? N16B C96B C95B 111.4(13) . . ? N16B C96B C91B 128.6(13) . . ? C95B C96B C91B 120.0 . . ? O200 C201 C200 120.0(6) . . ? O200 C201 C202 122.0(5) . . ? C200 C201 C202 118.1(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 0.3(5) . . . . ? C28 C1 C2 C3 179.8(3) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C1 C2 C3 C7 -175.5(3) . . . . ? C33 O4 C4 C5 -21.6(5) . . . . ? C33 O4 C4 C3 159.3(3) . . . . ? C2 C3 C4 O4 178.4(3) . . . . ? C7 C3 C4 O4 -5.5(5) . . . . ? C2 C3 C4 C5 -0.8(5) . . . . ? C7 C3 C4 C5 175.4(3) . . . . ? O4 C4 C5 C6 -178.7(3) . . . . ? C3 C4 C5 C6 0.4(6) . . . . ? C4 C5 C6 O6 179.1(3) . . . . ? C4 C5 C6 C1 0.3(6) . . . . ? C41 O6 C6 C5 41.6(5) . . . . ? C41 O6 C6 C1 -139.6(3) . . . . ? C2 C1 C6 C5 -0.7(5) . . . . ? C28 C1 C6 C5 179.8(3) . . . . ? C2 C1 C6 O6 -179.5(3) . . . . ? C28 C1 C6 O6 0.9(5) . . . . ? C2 C3 C7 C29 -17.0(5) . . . . ? C4 C3 C7 C29 167.1(3) . . . . ? C2 C3 C7 C8 108.4(4) . . . . ? C4 C3 C7 C8 -67.5(4) . . . . ? C3 C7 C8 C9 -29.6(5) . . . . ? C29 C7 C8 C9 97.9(4) . . . . ? C3 C7 C8 C13 150.6(4) . . . . ? C29 C7 C8 C13 -81.9(4) . . . . ? C13 C8 C9 C10 -0.8(5) . . . . ? C7 C8 C9 C10 179.4(3) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? C8 C9 C10 C14 176.9(3) . . . . ? C49 O11 C11 C12 2.9(6) . . . . ? C49 O11 C11 C10 -177.2(4) . . . . ? C9 C10 C11 C12 0.8(6) . . . . ? C14 C10 C11 C12 -176.3(4) . . . . ? C9 C10 C11 O11 -179.0(3) . . . . ? C14 C10 C11 O11 3.8(5) . . . . ? O11 C11 C12 C13 179.2(4) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C57 O13 C13 C12 18.6(8) . . . . ? C57 O13 C13 C8 -162.7(6) . . . . ? C11 C12 C13 O13 178.3(4) . . . . ? C11 C12 C13 C8 -0.3(7) . . . . ? C9 C8 C13 O13 -177.7(4) . . . . ? C7 C8 C13 O13 2.1(6) . . . . ? C9 C8 C13 C12 1.0(6) . . . . ? C7 C8 C13 C12 -179.2(4) . . . . ? C11 C10 C14 C15 -147.9(3) . . . . ? C9 C10 C14 C15 35.1(5) . . . . ? C11 C10 C14 C30 83.0(4) . . . . ? C9 C10 C14 C30 -93.9(4) . . . . ? C10 C14 C15 C16 -110.2(4) . . . . ? C30 C14 C15 C16 16.9(5) . . . . ? C10 C14 C15 C20 72.1(4) . . . . ? C30 C14 C15 C20 -160.9(3) . . . . ? C20 C15 C16 C17 0.3(5) . . . . ? C14 C15 C16 C17 -177.4(3) . . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C15 C16 C17 C21 -179.3(3) . . . . ? C16 C17 C18 O18 -177.1(3) . . . . ? C21 C17 C18 O18 1.7(5) . . . . ? C16 C17 C18 C19 0.3(5) . . . . ? C21 C17 C18 C19 179.1(3) . . . . ? C65 O18 C18 C17 -125.5(4) . . . . ? C65 O18 C18 C19 57.2(5) . . . . ? C17 C18 C19 C20 0.2(5) . . . . ? O18 C18 C19 C20 177.4(3) . . . . ? C73 O20 C20 C19 -1.6(6) . . . . ? C73 O20 C20 C15 177.8(3) . . . . ? C18 C19 C20 O20 179.0(3) . . . . ? C18 C19 C20 C15 -0.4(5) . . . . ? C16 C15 C20 O20 -179.3(3) . . . . ? C14 C15 C20 O20 -1.4(5) . . . . ? C16 C15 C20 C19 0.2(5) . . . . ? C14 C15 C20 C19 178.1(3) . . . . ? C18 C17 C21 C22 -71.2(4) . . . . ? C16 C17 C21 C22 107.5(4) . . . . ? C18 C17 C21 C31 162.8(3) . . . . ? C16 C17 C21 C31 -18.5(5) . . . . ? C17 C21 C22 C27 144.9(3) . . . . ? C31 C21 C22 C27 -87.1(4) . . . . ? C17 C21 C22 C23 -37.3(5) . . . . ? C31 C21 C22 C23 90.7(4) . . . . ? C27 C22 C23 C24 1.2(5) . . . . ? C21 C22 C23 C24 -176.8(3) . . . . ? C22 C23 C24 C25 -0.5(5) . . . . ? C22 C23 C24 C28 176.8(3) . . . . ? C81 O25 C25 C26 1.8(5) . . . . ? C81 O25 C25 C24 -178.4(4) . . . . ? C23 C24 C25 C26 -1.4(5) . . . . ? C28 C24 C25 C26 -178.7(3) . . . . ? C23 C24 C25 O25 178.8(3) . . . . ? C28 C24 C25 O25 1.5(5) . . . . ? O25 C25 C26 C27 -177.6(3) . . . . ? C24 C25 C26 C27 2.7(6) . . . . ? C89B O27 C27 C22 164.7(9) . . . . ? C89A O27 C27 C22 119.9(5) . . . . ? C89B O27 C27 C26 -15.7(10) . . . . ? C89A O27 C27 C26 -60.5(6) . . . . ? C23 C22 C27 O27 179.7(3) . . . . ? C21 C22 C27 O27 -2.4(5) . . . . ? C23 C22 C27 C26 0.1(5) . . . . ? C21 C22 C27 C26 178.0(3) . . . . ? C25 C26 C27 O27 178.5(3) . . . . ? C25 C26 C27 C22 -2.0(6) . . . . ? C25 C24 C28 C1 -145.6(3) . . . . ? C23 C24 C28 C1 37.2(5) . . . . ? C25 C24 C28 C32 86.2(4) . . . . ? C23 C24 C28 C32 -91.0(4) . . . . ? C6 C1 C28 C24 60.1(4) . . . . ? C2 C1 C28 C24 -119.5(4) . . . . ? C6 C1 C28 C32 -174.9(3) . . . . ? C2 C1 C28 C32 5.6(5) . . . . ? C4 O4 C33 C34 -168.8(3) . . . . ? C35 N1 C34 C33 -75.4(6) . . . . ? O4 C33 C34 N1 -64.4(5) . . . . ? C34 N1 C35 C40 -176.4(4) . . . . ? C34 N1 C35 C36 3.1(7) . . . . ? N1 C35 C36 C37 179.7(5) . . . . ? C40 C35 C36 C37 -0.7(7) . . . . ? C35 C36 C37 C38 0.6(8) . . . . ? C36 C37 C38 C39 -0.2(8) . . . . ? C37 C38 C39 C40 -0.2(8) . . . . ? C38 C39 C40 C35 0.0(7) . . . . ? C38 C39 C40 N2 178.7(4) . . . . ? N1 C35 C40 C39 179.9(4) . . . . ? C36 C35 C40 C39 0.4(6) . . . . ? N1 C35 C40 N2 1.4(7) . . . . ? C36 C35 C40 N2 -178.2(4) . . . . ? O102 N2 C40 C39 1.3(6) . . . . ? O101 N2 C40 C39 -176.8(4) . . . . ? O102 N2 C40 C35 179.9(4) . . . . ? O101 N2 C40 C35 1.8(6) . . . . ? C6 O6 C41 C42 152.9(3) . . . . ? C43 N3 C42 C41 73.7(5) . . . . ? O6 C41 C42 N3 56.8(4) . . . . ? C42 N3 C43 C48 -165.8(4) . . . . ? C42 N3 C43 C44 16.5(6) . . . . ? N3 C43 C44 C45 178.0(5) . . . . ? C48 C43 C44 C45 0.0(7) . . . . ? C43 C44 C45 C46 2.0(9) . . . . ? C44 C45 C46 C47 -1.9(11) . . . . ? C45 C46 C47 C48 -0.1(11) . . . . ? C46 C47 C48 C43 2.2(9) . . . . ? C46 C47 C48 N4 -177.9(6) . . . . ? N3 C43 C48 C47 -179.9(5) . . . . ? C44 C43 C48 C47 -2.1(7) . . . . ? N3 C43 C48 N4 0.2(8) . . . . ? C44 C43 C48 N4 178.0(5) . . . . ? O104 N4 C48 C47 -5.9(9) . . . . ? O103 N4 C48 C47 175.4(6) . . . . ? O104 N4 C48 C43 174.0(6) . . . . ? O103 N4 C48 C43 -4.7(9) . . . . ? C11 O11 C49 C50 175.0(3) . . . . ? C51 N5 C50 C49 -81.2(5) . . . . ? O11 C49 C50 N5 178.8(3) . . . . ? C50 N5 C51 C56 175.4(4) . . . . ? C50 N5 C51 C52 -7.0(6) . . . . ? N5 C51 C52 C53 -177.7(5) . . . . ? C56 C51 C52 C53 0.0(7) . . . . ? C51 C52 C53 C54 -0.2(10) . . . . ? C52 C53 C54 C55 0.4(10) . . . . ? C53 C54 C55 C56 -0.4(9) . . . . ? C54 C55 C56 C51 0.1(7) . . . . ? C54 C55 C56 N6 178.5(5) . . . . ? N5 C51 C56 C55 177.7(4) . . . . ? C52 C51 C56 C55 0.1(6) . . . . ? N5 C51 C56 N6 -0.6(6) . . . . ? C52 C51 C56 N6 -178.2(4) . . . . ? O105 N6 C56 C55 178.0(4) . . . . ? O106 N6 C56 C55 -2.5(6) . . . . ? O105 N6 C56 C51 -3.7(6) . . . . ? O106 N6 C56 C51 175.9(4) . . . . ? C13 O13 C57 C58 175.8(5) . . . . ? O13 C57 C58 N7B 135.1(7) . . . . ? O13 C57 C58 N7A -176.9(7) . . . . ? C18 O18 C65 C66 142.3(4) . . . . ? C67 N9 C66 C65 85.6(5) . . . . ? O18 C65 C66 N9 63.7(5) . . . . ? C66 N9 C67 C68 -0.5(7) . . . . ? C66 N9 C67 C72 179.8(4) . . . . ? N9 C67 C68 C69 179.8(4) . . . . ? C72 C67 C68 C69 -0.5(7) . . . . ? C67 C68 C69 C70 1.0(8) . . . . ? C68 C69 C70 C71 -0.6(9) . . . . ? C69 C70 C71 C72 -0.1(8) . . . . ? C70 C71 C72 C67 0.5(8) . . . . ? C70 C71 C72 N10 -178.2(5) . . . . ? N9 C67 C72 C71 179.5(4) . . . . ? C68 C67 C72 C71 -0.2(7) . . . . ? N9 C67 C72 N10 -1.8(7) . . . . ? C68 C67 C72 N10 178.5(4) . . . . ? O110 N10 C72 C71 -4.9(7) . . . . ? O109 N10 C72 C71 175.1(4) . . . . ? O110 N10 C72 C67 176.4(4) . . . . ? O109 N10 C72 C67 -3.7(7) . . . . ? C20 O20 C73 C74 175.0(3) . . . . ? C75 N11 C74 C73 174.8(4) . . . . ? O20 C73 C74 N11 -177.0(3) . . . . ? C74 N11 C75 C80 -180.0(4) . . . . ? C74 N11 C75 C76 0.4(6) . . . . ? N11 C75 C76 C77 -179.3(4) . . . . ? C80 C75 C76 C77 1.0(7) . . . . ? C75 C76 C77 C78 -0.9(8) . . . . ? C76 C77 C78 C79 0.2(7) . . . . ? C77 C78 C79 C80 0.3(7) . . . . ? C78 C79 C80 C75 -0.1(7) . . . . ? C78 C79 C80 N12 179.4(4) . . . . ? N11 C75 C80 C79 179.8(4) . . . . ? C76 C75 C80 C79 -0.6(6) . . . . ? N11 C75 C80 N12 0.3(6) . . . . ? C76 C75 C80 N12 179.9(4) . . . . ? O111 N12 C80 C79 -174.9(4) . . . . ? O112 N12 C80 C79 3.4(5) . . . . ? O111 N12 C80 C75 4.7(6) . . . . ? O112 N12 C80 C75 -177.0(4) . . . . ? N7B C58 N7A C59A 13.4(7) . . . . ? C57 C58 N7A C59A -74.3(9) . . . . ? C57 C58 N7B C59B 91.4(8) . . . . ? N7A C58 N7B C59B -14.5(6) . . . . ? C58 N7A C59A C60A -6.1(9) . . . . ? C58 N7A C59A C64A 170.7(5) . . . . ? C64A C59A C60A C61A 0.0 . . . . ? N7A C59A C60A C61A 176.7(7) . . . . ? C59A C60A C61A C62A 0.0 . . . . ? C60A C61A C62A C63A 0.0 . . . . ? C61A C62A C63A C64A 0.0 . . . . ? C62A C63A C64A C59A 0.0 . . . . ? C62A C63A C64A N8A 178.3(7) . . . . ? C60A C59A C64A C63A 0.0 . . . . ? N7A C59A C64A C63A -176.8(7) . . . . ? C60A C59A C64A N8A -178.2(8) . . . . ? N7A C59A C64A N8A 5.0(8) . . . . ? O58A N8A C64A C63A -14.0(12) . . . . ? O57A N8A C64A C63A 171.3(8) . . . . ? O58A N8A C64A C59A 164.3(9) . . . . ? O57A N8A C64A C59A -10.4(12) . . . . ? C58 N7B C59B C60B 7.5(10) . . . . ? C58 N7B C59B C64B -172.6(5) . . . . ? C64B C59B C60B C61B 0.0 . . . . ? N7B C59B C60B C61B 179.9(7) . . . . ? C59B C60B C61B C62B 0.0 . . . . ? C60B C61B C62B C63B 0.0 . . . . ? C61B C62B C63B C64B 0.0 . . . . ? C62B C63B C64B C59B 0.0 . . . . ? C62B C63B C64B N8B 178.2(7) . . . . ? C60B C59B C64B C63B 0.0 . . . . ? N7B C59B C64B C63B -179.9(7) . . . . ? C60B C59B C64B N8B -178.0(8) . . . . ? N7B C59B C64B N8B 2.0(9) . . . . ? O58B N8B C64B C63B 0.9(14) . . . . ? O57B N8B C64B C63B -178.2(11) . . . . ? O58B N8B C64B C59B 179.0(9) . . . . ? O57B N8B C64B C59B -0.1(16) . . . . ? C25 O25 C81 C82 178.1(4) . . . . ? O25 C81 C82 N13A 150.1(5) . . . . ? O25 C81 C82 N13B -145.7(5) . . . . ? C81 C82 N13A C83A 91.7(6) . . . . ? N13B C82 N13A C83A -1.9(6) . . . . ? C81 C82 N13B C83B -105.5(9) . . . . ? N13A C82 N13B C83B -0.5(8) . . . . ? C82 N13A C83A C84A -0.8(6) . . . . ? C82 N13A C83A C88A 177.4(4) . . . . ? N13A C83A C84A C85A 178.2(5) . . . . ? C88A C83A C84A C85A 0.0 . . . . ? C83A C84A C85A C86A 0.0 . . . . ? C84A C85A C86A C87A 0.0 . . . . ? C85A C86A C87A C88A 0.0 . . . . ? C86A C87A C88A C83A 0.0 . . . . ? C86A C87A C88A N14A 179.0(6) . . . . ? N13A C83A C88A C87A -178.2(5) . . . . ? C84A C83A C88A C87A 0.0 . . . . ? N13A C83A C88A N14A 2.9(7) . . . . ? C84A C83A C88A N14A -178.9(6) . . . . ? O54A N14A C88A C87A 1.0(10) . . . . ? O53A N14A C88A C87A -178.7(7) . . . . ? O54A N14A C88A C83A 179.9(6) . . . . ? O53A N14A C88A C83A 0.3(11) . . . . ? C82 N13B C83B C84B -4.8(11) . . . . ? C82 N13B C83B C88B -179.8(7) . . . . ? C88B C83B C84B C85B 0.0 . . . . ? N13B C83B C84B C85B -175.1(13) . . . . ? C83B C84B C85B C86B 0.0 . . . . ? C84B C85B C86B C87B 0.0 . . . . ? C85B C86B C87B C88B 0.0 . . . . ? C86B C87B C88B C83B 0.0 . . . . ? C86B C87B C88B N14B 176.6(11) . . . . ? C84B C83B C88B C87B 0.0 . . . . ? N13B C83B C88B C87B 174.9(14) . . . . ? C84B C83B C88B N14B -176.2(13) . . . . ? N13B C83B C88B N14B -1.3(13) . . . . ? O54B N14B C88B C87B -5.4(19) . . . . ? O53B N14B C88B C87B -179.0(11) . . . . ? O54B N14B C88B C83B 171.0(12) . . . . ? O53B N14B C88B C83B -2.6(16) . . . . ? C89B O27 C89A C90A 69.8(10) . . . . ? C27 O27 C89A C90A 172.0(5) . . . . ? O27 C89A C90A N15A -51.6(8) . . . . ? C89A C90A N15A C91A -96.7(8) . . . . ? C90A N15A C91A C92A -5.9(10) . . . . ? C90A N15A C91A C96A 176.3(6) . . . . ? C96A C91A C92A C93A 0.0 . . . . ? N15A C91A C92A C93A -177.8(8) . . . . ? C91A C92A C93A C94A 0.0 . . . . ? C92A C93A C94A C95A 0.0 . . . . ? C93A C94A C95A C96A 0.0 . . . . ? O56A N16A C96A C95A 5.2(15) . . . . ? O55A N16A C96A C95A -178.1(10) . . . . ? O56A N16A C96A C91A -178.0(10) . . . . ? O55A N16A C96A C91A -1.3(17) . . . . ? C94A C95A C96A N16A 177.1(9) . . . . ? C94A C95A C96A C91A 0.0 . . . . ? C92A C91A C96A N16A -176.6(10) . . . . ? N15A C91A C96A N16A 1.3(11) . . . . ? C92A C91A C96A C95A 0.0 . . . . ? N15A C91A C96A C95A 177.9(7) . . . . ? N15B C91B C92B C93B 179.8(12) . . . . ? C96B C91B C92B C93B 0.0 . . . . ? C91B C92B C93B C94B 0.0 . . . . ? C92B C93B C94B C95B 0.0 . . . . ? C93B C94B C95B C96B 0.0 . . . . ? O56B N16B C96B C95B 5.7(15) . . . . ? O55B N16B C96B C95B -179.0(9) . . . . ? O56B N16B C96B C91B -175.7(10) . . . . ? O55B N16B C96B C91B -0.4(16) . . . . ? C94B C95B C96B N16B 178.8(11) . . . . ? C94B C95B C96B C91B 0.0 . . . . ? N15B C91B C96B N16B 1.6(14) . . . . ? C92B C91B C96B N16B -178.5(13) . . . . ? N15B C91B C96B C95B -179.8(11) . . . . ? C92B C91B C96B C95B 0.0 . . . . ? 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 N1 H1N O101 0.939(19) 1.87(4) 2.642(5) 138(4) . N3 H3N O103 0.908(19) 1.92(3) 2.636(6) 134(4) . N5 H5N O105 0.922(19) 1.87(3) 2.591(4) 134(4) . N5 H5N O105 0.922(19) 2.34(3) 3.024(5) 131(3) 2_545 N9 H9N O109 0.891(19) 1.97(4) 2.629(5) 130(4) . N11 H11N O111 0.894(19) 1.99(4) 2.635(4) 128(4) . N13A H13A O53A 0.88 1.99 2.610(10) 126.4 . N13B H13B O53B 0.88 2.16 2.703(17) 119.8 . N13B H13B O58B 0.88 2.46 3.257(14) 151.7 2 N15A H15A O55A 0.88 1.99 2.630(11) 128.4 . N15B H15B O55B 0.88 1.91 2.623(11) 136.6 . N7A H7A O57A 0.88 1.94 2.599(12) 130.0 . N7B H7B O57B 0.88 1.91 2.539(16) 127.2 . _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 66.98 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.620 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.059 #===end data_2A _database_code_depnum_ccdc_archive 'CCDC 781921' #TrackingRef '- Octapodands.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C103 H110 N16 O25' _chemical_formula_weight 1972.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 11.1398(3) _cell_length_b 22.0112(6) _cell_length_c 22.5117(6) _cell_angle_alpha 113.189(2) _cell_angle_beta 100.4270(16) _cell_angle_gamma 99.9650(11) _cell_volume 4804.5(2) _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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8800 _exptl_absorpt_correction_T_max 0.9838 _exptl_absorpt_process_details 'Denzo (Otwinowski, Majewski, Borek & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 23754 _diffrn_reflns_av_R_equivalents 0.1092 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 66.84 _reflns_number_total 16232 _reflns_number_gt 9865 _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^)+(0.1497P)^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 16232 _refine_ls_number_parameters 1297 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1549 _refine_ls_R_factor_gt 0.0979 _refine_ls_wR_factor_ref 0.3077 _refine_ls_wR_factor_gt 0.2643 _refine_ls_goodness_of_fit_ref 1.323 _refine_ls_restrained_S_all 1.323 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O4 O 0.3865(3) 0.10638(16) 0.25365(15) 0.0410(8) Uani 1 1 d . . . O6 O 0.4741(3) -0.10092(16) 0.25802(15) 0.0416(8) Uani 1 1 d . . . O11 O 0.8181(3) 0.29948(16) 0.20435(17) 0.0417(8) Uani 1 1 d . . . O13 O 0.3678(3) 0.20024(16) 0.15363(16) 0.0397(8) Uani 1 1 d . . . O18 O 0.9496(3) 0.02373(16) 0.33244(15) 0.0372(8) Uani 1 1 d . . . O20 O 0.8926(3) 0.22816(15) 0.31231(15) 0.0374(8) Uani 1 1 d . . . O25 O 0.5424(3) -0.24614(17) 0.18010(18) 0.0460(8) Uani 1 1 d . . . O27 O 0.9913(3) -0.13607(17) 0.25857(17) 0.0467(9) Uani 1 1 d . . . C1 C 0.4658(4) -0.0814(2) 0.1626(2) 0.0317(10) Uani 1 1 d . . . C2 C 0.4506(4) -0.0394(2) 0.1309(2) 0.0323(10) Uani 1 1 d . . . H2 H 0.4583 -0.0546 0.0864 0.039 Uiso 1 1 calc R . . C3 C 0.4246(4) 0.0236(2) 0.1604(2) 0.0304(10) Uani 1 1 d . . . C4 C 0.4161(4) 0.0446(2) 0.2265(2) 0.0336(10) Uani 1 1 d . . . C5 C 0.4326(5) 0.0053(2) 0.2608(2) 0.0371(11) Uani 1 1 d . . . H5 H 0.4266 0.0208 0.3056 0.044 Uiso 1 1 calc R . . C6 C 0.4580(5) -0.0571(2) 0.2284(2) 0.0348(11) Uani 1 1 d . . . C7 C 0.3993(4) 0.0672(2) 0.1241(2) 0.0310(10) Uani 1 1 d . . . H7 H 0.3253 0.0842 0.1361 0.037 Uiso 1 1 calc R . . C8 C 0.5098(4) 0.1303(2) 0.1482(2) 0.0312(10) Uani 1 1 d . . . C9 C 0.6336(4) 0.1263(2) 0.1558(2) 0.0299(10) Uani 1 1 d . . . H9 H 0.6483 0.0829 0.1482 0.036 Uiso 1 1 calc R . . C10 C 0.7383(4) 0.1808(2) 0.1737(2) 0.0310(10) Uani 1 1 d . . . C11 C 0.7155(4) 0.2446(2) 0.1863(2) 0.0342(10) Uani 1 1 d . . . C12 C 0.5927(4) 0.2515(2) 0.1797(2) 0.0380(11) Uani 1 1 d . . . H12 H 0.5782 0.2950 0.1879 0.046 Uiso 1 1 calc R . . C13 C 0.4906(4) 0.1949(2) 0.1613(2) 0.0339(10) Uani 1 1 d . . . C14 C 0.8712(4) 0.1707(2) 0.1774(2) 0.0310(10) Uani 1 1 d . . . H14 H 0.9323 0.2174 0.2018 0.037 Uiso 1 1 calc R . . C15 C 0.8983(4) 0.1321(2) 0.2195(2) 0.0293(10) Uani 1 1 d . . . C16 C 0.9184(4) 0.0669(2) 0.1934(2) 0.0313(10) Uani 1 1 d . . . H16 H 0.9181 0.0463 0.1475 0.038 Uiso 1 1 calc R . . C17 C 0.9388(4) 0.0306(2) 0.2306(2) 0.0293(10) Uani 1 1 d . . . C18 C 0.9334(4) 0.0613(2) 0.2972(2) 0.0298(10) Uani 1 1 d . . . C19 C 0.9146(4) 0.1259(2) 0.3255(2) 0.0342(10) Uani 1 1 d . . . H19 H 0.9116 0.1458 0.3709 0.041 Uiso 1 1 calc R . . C20 C 0.9001(4) 0.1615(2) 0.2868(2) 0.0311(10) Uani 1 1 d . . . C21 C 0.9621(5) -0.0405(2) 0.2026(2) 0.0356(11) Uani 1 1 d . A . H21 H 1.0387 -0.0386 0.2350 0.043 Uiso 1 1 calc R . . C22 C 0.8522(5) -0.0949(2) 0.1993(2) 0.0344(10) Uani 1 1 d . . . C23 C 0.7263(5) -0.1007(2) 0.1690(2) 0.0336(10) Uani 1 1 d . . . H23 H 0.7111 -0.0683 0.1524 0.040 Uiso 1 1 calc R . . C24 C 0.6242(5) -0.1498(2) 0.1621(2) 0.0330(10) Uani 1 1 d . . . C25 C 0.6470(5) -0.1967(2) 0.1870(2) 0.0373(11) Uani 1 1 d . . . C26 C 0.7695(5) -0.1928(2) 0.2184(2) 0.0396(11) Uani 1 1 d . . . H26 H 0.7837 -0.2244 0.2360 0.048 Uiso 1 1 calc R . . C27 C 0.8704(5) -0.1427(2) 0.2238(2) 0.0359(11) Uani 1 1 d . . . C28 C 0.4901(5) -0.1516(2) 0.1293(2) 0.0363(11) Uani 1 1 d . . . H28 H 0.4300 -0.1843 0.1381 0.044 Uiso 1 1 calc R . . C29 C 0.3609(5) 0.0262(2) 0.0473(2) 0.0395(11) Uani 1 1 d . . . H29A H 0.4356 0.0137 0.0329 0.047 Uiso 1 1 calc R . . H29B H 0.2954 -0.0169 0.0341 0.047 Uiso 1 1 calc R . . C30 C 0.3096(6) 0.0655(3) 0.0107(3) 0.0616(16) Uani 1 1 d . . . H30A H 0.2876 0.0372 -0.0380 0.092 Uiso 1 1 calc R . . H30B H 0.3744 0.1080 0.0230 0.092 Uiso 1 1 calc R . . H30C H 0.2339 0.0768 0.0234 0.092 Uiso 1 1 calc R . . C31 C 0.8900(5) 0.1383(2) 0.1076(2) 0.0348(10) Uani 1 1 d . . . H31A H 0.8301 0.0919 0.0820 0.042 Uiso 1 1 calc R . . H31B H 0.9771 0.1328 0.1119 0.042 Uiso 1 1 calc R . . C32 C 0.8702(5) 0.1799(3) 0.0677(3) 0.0485(13) Uani 1 1 d . . . H32A H 0.8847 0.1564 0.0236 0.073 Uiso 1 1 calc R . . H32B H 0.9301 0.2257 0.0922 0.073 Uiso 1 1 calc R . . H32C H 0.7833 0.1842 0.0617 0.073 Uiso 1 1 calc R . . C33 C 0.9888(6) -0.0628(3) 0.1353(3) 0.0577(16) Uani 1 1 d . . . H33A H 0.9829 -0.1124 0.1174 0.069 Uiso 0.701(11) 1 calc PR A 1 H33B H 0.9199 -0.0574 0.1047 0.069 Uiso 0.701(11) 1 calc PR A 1 H33C H 0.9822 -0.1125 0.1175 0.069 Uiso 0.299(11) 1 d PR A 2 H33D H 0.9204 -0.0571 0.1047 0.069 Uiso 0.299(11) 1 d PR A 2 C34A C 1.1051(7) -0.0297(4) 0.1311(4) 0.051(2) Uani 0.701(11) 1 d P A 1 H34A H 1.1117 -0.0519 0.0850 0.077 Uiso 0.701(11) 1 calc PR A 1 H34B H 1.1753 -0.0328 0.1619 0.077 Uiso 0.701(11) 1 calc PR A 1 H34C H 1.1092 0.0187 0.1433 0.077 Uiso 0.701(11) 1 calc PR A 1 C34B C 1.0798(17) -0.1093(9) 0.1260(8) 0.041(5) Uani 0.299(11) 1 d P A 2 H34D H 1.0933 -0.1227 0.0813 0.061 Uiso 0.299(11) 1 calc PR A 2 H34E H 1.0426 -0.1505 0.1305 0.061 Uiso 0.299(11) 1 calc PR A 2 H34F H 1.1611 -0.0843 0.1603 0.061 Uiso 0.299(11) 1 calc PR A 2 C35 C 0.4637(5) -0.1795(3) 0.0527(2) 0.0431(12) Uani 1 1 d . . . H35A H 0.3804 -0.1744 0.0342 0.052 Uiso 1 1 calc R . . H35B H 0.5291 -0.1517 0.0424 0.052 Uiso 1 1 calc R . . C36 C 0.4632(6) -0.2545(3) 0.0183(3) 0.0546(14) Uani 1 1 d . . . H36A H 0.4448 -0.2696 -0.0303 0.082 Uiso 1 1 calc R . . H36B H 0.3981 -0.2825 0.0280 0.082 Uiso 1 1 calc R . . H36C H 0.5464 -0.2597 0.0352 0.082 Uiso 1 1 calc R . . O101 O 0.5849(4) 0.3115(2) 0.3644(3) 0.0880(16) Uani 1 1 d . . . O102 O 0.6254(4) 0.4063(2) 0.3561(3) 0.0850(14) Uani 1 1 d . . . N1 N 0.3526(4) 0.2363(2) 0.3285(2) 0.0398(10) Uani 1 1 d D . . H1N H 0.436(3) 0.242(3) 0.336(3) 0.048 Uiso 1 1 d D . . N2 N 0.5496(5) 0.3572(3) 0.3533(2) 0.0600(13) Uani 1 1 d . . . C37 C 0.3181(5) 0.1157(2) 0.3030(2) 0.0384(11) Uani 1 1 d . . . H37A H 0.3766 0.1284 0.3473 0.046 Uiso 1 1 calc R . . H37B H 0.2530 0.0726 0.2903 0.046 Uiso 1 1 calc R . . C38 C 0.2563(5) 0.1721(2) 0.3062(3) 0.0414(12) Uani 1 1 d . . . H38A H 0.2008 0.1597 0.2612 0.050 Uiso 1 1 calc R . . H38B H 0.2032 0.1777 0.3378 0.050 Uiso 1 1 calc R . . C39 C 0.3250(5) 0.2922(2) 0.3250(2) 0.0369(11) Uani 1 1 d . . . C40 C 0.1959(5) 0.2931(3) 0.3079(2) 0.0431(12) Uani 1 1 d . . . H40 H 0.1310 0.2551 0.3018 0.052 Uiso 1 1 calc R . . C41 C 0.1632(5) 0.3474(3) 0.3002(2) 0.0484(13) Uani 1 1 d . . . H41 H 0.0762 0.3455 0.2866 0.058 Uiso 1 1 calc R . . C42 C 0.2547(6) 0.4046(3) 0.3119(3) 0.0564(15) Uani 1 1 d . . . H42 H 0.2306 0.4419 0.3065 0.068 Uiso 1 1 calc R . . C43 C 0.3799(6) 0.4080(3) 0.3311(3) 0.0547(14) Uani 1 1 d . . . H43 H 0.4429 0.4481 0.3403 0.066 Uiso 1 1 calc R . . C44 C 0.4156(5) 0.3517(3) 0.3372(2) 0.0460(12) Uani 1 1 d . . . O103 O 0.4481(5) -0.0517(2) 0.52264(19) 0.0775(14) Uani 1 1 d . . . O104 O 0.3939(5) -0.1016(2) 0.5841(2) 0.0780(13) Uani 1 1 d . . . N3 N 0.4948(5) -0.1231(2) 0.4090(2) 0.0511(12) Uani 1 1 d . . . H3N H 0.4915 -0.0819 0.4357 0.061 Uiso 1 1 calc R . . N4 N 0.4302(5) -0.1028(3) 0.5352(2) 0.0608(13) Uani 1 1 d . . . C45 C 0.4917(6) -0.0761(3) 0.3280(2) 0.0450(13) Uani 1 1 d . . . H45A H 0.4168 -0.0619 0.3406 0.054 Uiso 1 1 calc R . . H45B H 0.5675 -0.0363 0.3529 0.054 Uiso 1 1 calc R . . C46 C 0.5092(5) -0.1359(3) 0.3428(2) 0.0442(12) Uani 1 1 d . . . H46A H 0.4455 -0.1786 0.3086 0.053 Uiso 1 1 calc R . . H46B H 0.5946 -0.1420 0.3407 0.053 Uiso 1 1 calc R . . C47 C 0.4861(5) -0.1723(3) 0.4320(2) 0.0455(13) Uani 1 1 d . . . C48 C 0.5074(5) -0.2363(3) 0.3942(3) 0.0474(13) Uani 1 1 d . . . H48 H 0.5240 -0.2448 0.3521 0.057 Uiso 1 1 calc R . . C49 C 0.5048(5) -0.2859(3) 0.4161(3) 0.0550(15) Uani 1 1 d . . . H49 H 0.5214 -0.3276 0.3894 0.066 Uiso 1 1 calc R . . C50 C 0.4782(5) -0.2768(3) 0.4770(3) 0.0601(16) Uani 1 1 d . . . H50 H 0.4773 -0.3115 0.4921 0.072 Uiso 1 1 calc R . . C51 C 0.4537(5) -0.2169(3) 0.5140(3) 0.0546(15) Uani 1 1 d . . . H51 H 0.4339 -0.2101 0.5551 0.066 Uiso 1 1 calc R . . C52 C 0.4569(5) -0.1649(3) 0.4927(2) 0.0464(13) Uani 1 1 d . . . O105 O 0.8866(5) 0.5532(2) 0.1500(2) 0.0704(13) Uani 1 1 d . . . O106 O 0.8452(5) 0.6499(2) 0.1979(2) 0.0772(14) Uani 1 1 d . . . N5 N 0.8953(4) 0.4706(2) 0.2091(2) 0.0401(10) Uani 1 1 d . . . H5N H 0.9075 0.4765 0.1740 0.048 Uiso 1 1 calc R . . N6 N 0.8581(5) 0.5947(2) 0.1967(2) 0.0543(13) Uani 1 1 d . . . C53 C 0.7922(5) 0.3561(2) 0.1937(3) 0.0419(12) Uani 1 1 d . . . H53A H 0.7361 0.3761 0.2210 0.050 Uiso 1 1 calc R . . H53B H 0.7487 0.3407 0.1458 0.050 Uiso 1 1 calc R . . C54 C 0.9163(5) 0.4092(2) 0.2140(3) 0.0405(11) Uani 1 1 d . . . H54A H 0.9624 0.4214 0.2608 0.049 Uiso 1 1 calc R . . H54B H 0.9694 0.3898 0.1845 0.049 Uiso 1 1 calc R . . C55 C 0.8583(5) 0.5190(2) 0.2551(2) 0.0401(12) Uani 1 1 d . . . C56 C 0.8331(6) 0.5115(3) 0.3115(3) 0.0603(16) Uani 1 1 d . . . H56 H 0.8413 0.4710 0.3157 0.072 Uiso 1 1 calc R . . C57 C 0.7979(8) 0.5592(3) 0.3600(3) 0.075(2) Uani 1 1 d . . . H57 H 0.7833 0.5515 0.3971 0.090 Uiso 1 1 calc R . . C58 C 0.7829(7) 0.6196(3) 0.3561(3) 0.0707(18) Uani 1 1 d . . . H58 H 0.7593 0.6531 0.3904 0.085 Uiso 1 1 calc R . . C59 C 0.8027(5) 0.6289(3) 0.3027(3) 0.0565(15) Uani 1 1 d . . . H59 H 0.7920 0.6693 0.2992 0.068 Uiso 1 1 calc R . . C60 C 0.8393(5) 0.5794(2) 0.2515(3) 0.0446(13) Uani 1 1 d . . . O107 O 0.1824(4) 0.44304(19) 0.17251(19) 0.0548(10) Uani 1 1 d . . . O108 O 0.1824(5) 0.4967(2) 0.1107(2) 0.0799(14) Uani 1 1 d . . . N7 N 0.1838(4) 0.3133(2) 0.1241(2) 0.0395(9) Uani 1 1 d D . . H7N H 0.191(5) 0.352(2) 0.160(2) 0.047 Uiso 1 1 d D . . N8 N 0.1868(4) 0.4450(2) 0.1188(2) 0.0501(11) Uani 1 1 d . . . C61 C 0.3479(4) 0.2616(2) 0.1514(2) 0.0370(11) Uani 1 1 d . . . H61A H 0.3848 0.2697 0.1174 0.044 Uiso 1 1 calc R . . H61B H 0.3896 0.3013 0.1957 0.044 Uiso 1 1 calc R . . C62 C 0.2076(4) 0.2537(3) 0.1332(2) 0.0384(11) Uani 1 1 d . . . H62A H 0.1652 0.2113 0.0912 0.046 Uiso 1 1 calc R . . H62B H 0.1724 0.2499 0.1693 0.046 Uiso 1 1 calc R . . C63 C 0.1943(4) 0.3227(3) 0.0683(2) 0.0366(11) Uani 1 1 d . . . C64 C 0.2018(5) 0.2685(3) 0.0107(2) 0.0446(12) Uani 1 1 d . . . H64 H 0.2015 0.2256 0.0114 0.054 Uiso 1 1 calc R . . C65 C 0.2096(5) 0.2755(3) -0.0470(3) 0.0549(15) Uani 1 1 d . . . H65 H 0.2151 0.2377 -0.0850 0.066 Uiso 1 1 calc R . . C66 C 0.2093(6) 0.3368(4) -0.0499(3) 0.0607(16) Uani 1 1 d . . . H66 H 0.2145 0.3413 -0.0897 0.073 Uiso 1 1 calc R . . C68 C 0.1933(5) 0.3847(3) 0.0634(2) 0.0402(11) Uani 1 1 d . . . O109 O 0.7751(4) 0.0372(2) 0.5649(2) 0.0662(12) Uani 1 1 d . . . O110 O 0.7226(5) -0.0181(3) 0.6207(2) 0.0768(14) Uani 1 1 d . . . N9 N 0.8367(5) -0.0255(2) 0.4523(2) 0.0492(11) Uani 1 1 d D . . H9N H 0.825(5) 0.014(2) 0.480(2) 0.059 Uiso 1 1 d D . . N10 N 0.7611(4) -0.0158(3) 0.5732(2) 0.0536(12) Uani 1 1 d . . . C69 C 0.8884(5) 0.0339(3) 0.3855(2) 0.0411(12) Uani 1 1 d . . . H69A H 0.8031 0.0400 0.3726 0.049 Uiso 1 1 calc R . . H69B H 0.9396 0.0745 0.4275 0.049 Uiso 1 1 calc R . . C67 C 0.2015(5) 0.3912(3) 0.0048(3) 0.0520(14) Uani 1 1 d . . . H67 H 0.2017 0.4336 0.0030 0.062 Uiso 1 1 calc R . . C70 C 0.8799(5) -0.0300(3) 0.3938(3) 0.0463(12) Uani 1 1 d . . . H70A H 0.8203 -0.0689 0.3530 0.056 Uiso 1 1 calc R . . H70B H 0.9642 -0.0391 0.3986 0.056 Uiso 1 1 calc R . . C71 C 0.8294(5) -0.0763(3) 0.4715(2) 0.0421(12) Uani 1 1 d . . . C72 C 0.8608(5) -0.1377(3) 0.4330(3) 0.0519(14) Uani 1 1 d . . . H72 H 0.8859 -0.1426 0.3936 0.062 Uiso 1 1 calc R . . C73 C 0.8550(5) -0.1893(3) 0.4527(3) 0.0522(14) Uani 1 1 d . . . H73 H 0.8768 -0.2294 0.4263 0.063 Uiso 1 1 calc R . . C74 C 0.8191(5) -0.1855(3) 0.5086(3) 0.0588(16) Uani 1 1 d . . . H74 H 0.8162 -0.2220 0.5213 0.071 Uiso 1 1 calc R . . C75 C 0.7879(5) -0.1290(3) 0.5452(3) 0.0501(13) Uani 1 1 d . . . H75 H 0.7609 -0.1264 0.5836 0.060 Uiso 1 1 calc R . . C76 C 0.7936(5) -0.0739(3) 0.5289(3) 0.0438(12) Uani 1 1 d . . . O111 O 1.2318(4) 0.3375(2) 0.4777(2) 0.0609(11) Uani 1 1 d . . . O112 O 1.4070(4) 0.4138(3) 0.5064(3) 0.0825(14) Uani 1 1 d . . . N11 N 1.0149(4) 0.3562(2) 0.4300(2) 0.0413(10) Uani 1 1 d D . . H11N H 1.050(5) 0.323(2) 0.431(3) 0.050 Uiso 1 1 d D . . N12 N 1.2915(5) 0.3945(2) 0.4857(2) 0.0522(11) Uani 1 1 d . . . C77 C 0.8406(5) 0.2545(2) 0.3671(3) 0.0444(12) Uani 1 1 d . . . H77A H 0.8721 0.2398 0.4018 0.053 Uiso 1 1 calc R . . H77B H 0.7470 0.2378 0.3518 0.053 Uiso 1 1 calc R . . C78 C 0.8821(5) 0.3312(2) 0.3948(3) 0.0429(12) Uani 1 1 d . . . H78A H 0.8664 0.3448 0.3577 0.051 Uiso 1 1 calc R . . H78B H 0.8324 0.3518 0.4259 0.051 Uiso 1 1 calc R . . C79 C 1.0898(5) 0.4177(2) 0.4426(2) 0.0386(11) Uani 1 1 d . . . C80 C 1.0360(5) 0.4657(2) 0.4290(2) 0.0441(12) Uani 1 1 d . . . H80 H 0.9466 0.4544 0.4116 0.053 Uiso 1 1 calc R . . C81 C 1.1089(6) 0.5286(3) 0.4402(3) 0.0540(14) Uani 1 1 d . . . H81 H 1.0694 0.5596 0.4301 0.065 Uiso 1 1 calc R . . C82 C 1.2402(6) 0.5469(3) 0.4663(3) 0.0593(15) Uani 1 1 d . . . H82 H 1.2899 0.5902 0.4737 0.071 Uiso 1 1 calc R . . C83 C 1.2970(6) 0.5026(3) 0.4812(3) 0.0536(14) Uani 1 1 d . . . H83 H 1.3864 0.5152 0.4992 0.064 Uiso 1 1 calc R . . C84 C 1.2236(5) 0.4383(3) 0.4701(2) 0.0454(12) Uani 1 1 d . . . O113 O 0.4633(7) -0.4792(4) 0.2639(3) 0.114(2) Uani 1 1 d . . . O114 O 0.5091(8) -0.5771(4) 0.2257(4) 0.157(3) Uani 1 1 d . . . N13 N 0.4666(6) -0.4060(3) 0.2004(3) 0.0882(18) Uani 1 1 d . . . H13N H 0.4546 -0.4081 0.2372 0.106 Uiso 1 1 calc R . . N14 N 0.4993(7) -0.5264(4) 0.2194(4) 0.103(2) Uani 1 1 d . . . C85 C 0.5658(6) -0.2961(3) 0.2017(4) 0.0648(17) Uani 1 1 d . . . H85A H 0.6062 -0.2741 0.2508 0.078 Uiso 1 1 calc R . . H85B H 0.6236 -0.3198 0.1787 0.078 Uiso 1 1 calc R . . C86 C 0.4439(7) -0.3456(4) 0.1855(4) 0.081(2) Uani 1 1 d . . . H86A H 0.3989 -0.3630 0.1374 0.098 Uiso 1 1 calc R . . H86B H 0.3902 -0.3227 0.2126 0.098 Uiso 1 1 calc R . . C87 C 0.5073(5) -0.4581(2) 0.1538(2) 0.0609(16) Uani 1 1 d G . . C88 C 0.5406(7) -0.4517(3) 0.0996(3) 0.136(4) Uani 1 1 d G . . H88 H 0.5341 -0.4125 0.0923 0.163 Uiso 1 1 calc R . . C89 C 0.5836(8) -0.5024(4) 0.0560(3) 0.150(5) Uani 1 1 d G . . H89 H 0.6063 -0.4980 0.0189 0.180 Uiso 1 1 calc R . . C90 C 0.5932(7) -0.5597(3) 0.0667(3) 0.122(4) Uani 1 1 d G . . H90 H 0.6225 -0.5944 0.0369 0.146 Uiso 1 1 calc R . . C91 C 0.5599(5) -0.5661(2) 0.1209(3) 0.116(4) Uani 1 1 d G . . H91 H 0.5665 -0.6052 0.1282 0.139 Uiso 1 1 calc R . . C92 C 0.5170(5) -0.5153(2) 0.1645(3) 0.087(3) Uani 1 1 d G . . O115 O 1.1616(5) -0.1602(3) 0.4537(3) 0.0908(15) Uani 1 1 d . . . O116 O 1.1276(6) -0.2424(4) 0.4827(4) 0.138(3) Uani 1 1 d . . . N16 N 1.1480(5) -0.2195(3) 0.4479(3) 0.0728(16) Uani 1 1 d . . . N15 N 1.1696(5) -0.1901(3) 0.3308(3) 0.0708(15) Uani 1 1 d . . . H15N H 1.1707 -0.1575 0.3695 0.085 Uiso 1 1 calc R . . C93 C 1.0509(6) -0.1865(4) 0.2280(3) 0.0718(18) Uani 1 1 d . . . H93A H 1.0638 -0.1857 0.1859 0.086 Uiso 1 1 calc R . . H93B H 0.9972 -0.2325 0.2168 0.086 Uiso 1 1 calc R . . C94 C 1.1761(6) -0.1723(4) 0.2759(4) 0.0747(19) Uani 1 1 d . . . H94A H 1.2290 -0.1979 0.2503 0.090 Uiso 1 1 calc R . . H94B H 1.2194 -0.1227 0.2950 0.090 Uiso 1 1 calc R . . C95 C 1.1614(4) -0.25766(17) 0.3261(2) 0.0586(15) Uani 1 1 d G . . C96 C 1.1661(4) -0.3081(2) 0.26594(17) 0.0557(15) Uani 1 1 d G . . H96 H 1.1669 -0.2984 0.2285 0.067 Uiso 1 1 calc R . . C97 C 1.1697(4) -0.37283(18) 0.2606(2) 0.081(2) Uani 1 1 d G . . H97 H 1.1730 -0.4073 0.2195 0.097 Uiso 1 1 calc R . . C98 C 1.1686(4) -0.3871(2) 0.3154(3) 0.113(4) Uani 1 1 d G . . H98 H 1.1711 -0.4313 0.3118 0.135 Uiso 1 1 calc R . . C99 C 1.1639(4) -0.3367(3) 0.3756(3) 0.101(3) Uani 1 1 d G . . H99 H 1.1632 -0.3464 0.4131 0.122 Uiso 1 1 calc R . . C100 C 1.1603(4) -0.2719(3) 0.38095(17) 0.076(2) Uani 1 1 d G . . O200 O 0.8901(5) 0.3754(3) 0.0620(3) 0.1015(18) Uani 1 1 d . . . C200 C 0.8757(6) 0.3614(4) 0.0015(4) 0.078(2) Uani 1 1 d . . . C201 C 0.8658(8) 0.2920(5) -0.0463(4) 0.111(3) Uani 1 1 d . . . H20A H 0.8192 0.2591 -0.0335 0.166 Uiso 1 1 calc R . . H20B H 0.9510 0.2859 -0.0461 0.166 Uiso 1 1 calc R . . H20C H 0.8206 0.2840 -0.0914 0.166 Uiso 1 1 calc R . . C202 C 0.8762(9) 0.4194(5) -0.0146(5) 0.122(4) Uani 1 1 d . . . H20D H 0.8168 0.4437 0.0049 0.184 Uiso 1 1 calc R . . H20E H 0.8505 0.4028 -0.0635 0.184 Uiso 1 1 calc R . . H20F H 0.9618 0.4508 0.0039 0.184 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 O4 0.069(2) 0.0323(18) 0.0373(18) 0.0211(15) 0.0252(16) 0.0258(17) O6 0.070(2) 0.0326(18) 0.0343(18) 0.0207(14) 0.0190(16) 0.0240(17) O11 0.0392(19) 0.0275(17) 0.062(2) 0.0268(16) 0.0057(16) 0.0097(15) O13 0.0356(18) 0.0362(18) 0.058(2) 0.0291(16) 0.0138(15) 0.0153(15) O18 0.048(2) 0.0365(18) 0.0360(17) 0.0218(15) 0.0142(14) 0.0156(15) O20 0.052(2) 0.0256(16) 0.0366(17) 0.0130(14) 0.0132(15) 0.0150(15) O25 0.048(2) 0.0319(18) 0.068(2) 0.0295(17) 0.0176(17) 0.0141(16) O27 0.051(2) 0.0332(19) 0.059(2) 0.0246(16) 0.0061(17) 0.0190(16) C1 0.034(2) 0.029(2) 0.031(2) 0.0137(19) 0.0034(18) 0.010(2) C2 0.034(2) 0.034(3) 0.028(2) 0.014(2) 0.0076(18) 0.008(2) C3 0.034(2) 0.028(2) 0.028(2) 0.0119(19) 0.0042(18) 0.0087(19) C4 0.046(3) 0.021(2) 0.036(3) 0.0141(19) 0.010(2) 0.011(2) C5 0.057(3) 0.028(2) 0.033(2) 0.015(2) 0.016(2) 0.018(2) C6 0.048(3) 0.026(2) 0.035(3) 0.017(2) 0.008(2) 0.014(2) C7 0.036(2) 0.029(2) 0.033(2) 0.018(2) 0.0096(19) 0.011(2) C8 0.037(3) 0.032(2) 0.029(2) 0.0174(19) 0.0091(19) 0.009(2) C9 0.034(2) 0.028(2) 0.032(2) 0.0184(19) 0.0065(18) 0.0109(19) C10 0.034(2) 0.025(2) 0.035(2) 0.0160(19) 0.0064(19) 0.0081(19) C11 0.035(3) 0.027(2) 0.040(3) 0.017(2) 0.006(2) 0.007(2) C12 0.039(3) 0.030(2) 0.053(3) 0.024(2) 0.010(2) 0.014(2) C13 0.036(3) 0.034(3) 0.039(3) 0.021(2) 0.011(2) 0.013(2) C14 0.031(2) 0.025(2) 0.036(2) 0.0160(19) 0.0044(19) 0.0069(19) C15 0.027(2) 0.027(2) 0.035(2) 0.017(2) 0.0048(18) 0.0067(19) C16 0.034(2) 0.032(2) 0.033(2) 0.018(2) 0.0094(19) 0.012(2) C17 0.030(2) 0.026(2) 0.035(2) 0.0151(19) 0.0091(18) 0.0081(19) C18 0.030(2) 0.028(2) 0.035(2) 0.020(2) 0.0065(18) 0.0075(19) C19 0.043(3) 0.033(3) 0.030(2) 0.017(2) 0.0098(19) 0.011(2) C20 0.035(2) 0.025(2) 0.034(2) 0.0140(19) 0.0064(19) 0.0094(19) C21 0.043(3) 0.037(3) 0.035(3) 0.020(2) 0.012(2) 0.021(2) C22 0.047(3) 0.025(2) 0.030(2) 0.0110(19) 0.006(2) 0.014(2) C23 0.047(3) 0.027(2) 0.030(2) 0.0129(19) 0.010(2) 0.017(2) C24 0.050(3) 0.022(2) 0.028(2) 0.0092(18) 0.013(2) 0.016(2) C25 0.055(3) 0.024(2) 0.032(2) 0.0078(19) 0.017(2) 0.016(2) C26 0.056(3) 0.027(2) 0.046(3) 0.022(2) 0.015(2) 0.020(2) C27 0.044(3) 0.027(2) 0.036(2) 0.014(2) 0.004(2) 0.015(2) C28 0.046(3) 0.027(2) 0.032(2) 0.011(2) 0.005(2) 0.011(2) C29 0.043(3) 0.039(3) 0.036(3) 0.020(2) 0.005(2) 0.008(2) C30 0.083(4) 0.057(4) 0.043(3) 0.030(3) 0.000(3) 0.013(3) C31 0.043(3) 0.030(2) 0.034(2) 0.017(2) 0.009(2) 0.009(2) C32 0.058(3) 0.055(3) 0.047(3) 0.033(3) 0.017(3) 0.020(3) C33 0.089(5) 0.061(4) 0.061(4) 0.041(3) 0.044(3) 0.054(4) C34A 0.049(5) 0.053(5) 0.052(5) 0.023(4) 0.019(4) 0.012(4) C34B 0.056(11) 0.041(10) 0.035(9) 0.016(7) 0.020(7) 0.031(8) C35 0.050(3) 0.041(3) 0.034(3) 0.013(2) 0.009(2) 0.015(2) C36 0.057(3) 0.042(3) 0.043(3) -0.001(2) 0.006(2) 0.017(3) O101 0.047(3) 0.054(3) 0.148(4) 0.041(3) 0.000(3) 0.012(2) O102 0.062(3) 0.068(3) 0.119(4) 0.051(3) 0.011(3) -0.006(2) N1 0.038(2) 0.030(2) 0.050(2) 0.0163(18) 0.0044(19) 0.0147(19) N2 0.055(3) 0.047(3) 0.072(3) 0.025(3) 0.008(2) 0.009(3) C37 0.050(3) 0.036(3) 0.039(3) 0.021(2) 0.015(2) 0.019(2) C38 0.041(3) 0.035(3) 0.053(3) 0.022(2) 0.011(2) 0.017(2) C39 0.047(3) 0.031(3) 0.034(3) 0.015(2) 0.009(2) 0.015(2) C40 0.048(3) 0.042(3) 0.045(3) 0.020(2) 0.012(2) 0.022(2) C41 0.058(3) 0.049(3) 0.045(3) 0.022(3) 0.011(2) 0.030(3) C42 0.085(5) 0.044(3) 0.058(3) 0.031(3) 0.023(3) 0.035(3) C43 0.073(4) 0.038(3) 0.055(3) 0.022(3) 0.019(3) 0.015(3) C44 0.052(3) 0.041(3) 0.040(3) 0.013(2) 0.012(2) 0.015(3) O103 0.131(4) 0.057(3) 0.048(2) 0.026(2) 0.020(2) 0.030(3) O104 0.092(3) 0.087(3) 0.043(2) 0.021(2) 0.017(2) 0.012(3) N3 0.074(3) 0.046(3) 0.040(2) 0.026(2) 0.010(2) 0.022(2) N4 0.074(4) 0.058(3) 0.034(3) 0.012(2) 0.003(2) 0.010(3) C45 0.069(4) 0.036(3) 0.031(3) 0.017(2) 0.007(2) 0.018(3) C46 0.057(3) 0.040(3) 0.037(3) 0.019(2) 0.006(2) 0.019(3) C47 0.048(3) 0.043(3) 0.044(3) 0.023(2) 0.000(2) 0.012(2) C48 0.045(3) 0.044(3) 0.059(3) 0.031(3) 0.006(2) 0.015(2) C49 0.049(3) 0.044(3) 0.075(4) 0.033(3) 0.007(3) 0.016(3) C50 0.051(3) 0.061(4) 0.076(4) 0.048(3) 0.002(3) 0.003(3) C51 0.052(3) 0.064(4) 0.046(3) 0.036(3) -0.002(3) 0.000(3) C52 0.048(3) 0.048(3) 0.036(3) 0.020(2) -0.004(2) 0.009(3) O105 0.114(4) 0.047(2) 0.051(2) 0.029(2) 0.013(2) 0.016(2) O106 0.102(4) 0.049(2) 0.089(3) 0.049(2) 0.001(3) 0.019(2) N5 0.048(2) 0.031(2) 0.048(2) 0.0257(19) 0.0108(19) 0.0087(19) N6 0.065(3) 0.032(2) 0.059(3) 0.029(2) -0.009(2) 0.004(2) C53 0.044(3) 0.028(2) 0.060(3) 0.026(2) 0.011(2) 0.012(2) C54 0.038(3) 0.034(3) 0.055(3) 0.027(2) 0.009(2) 0.009(2) C55 0.039(3) 0.029(3) 0.047(3) 0.017(2) 0.001(2) 0.004(2) C56 0.090(5) 0.040(3) 0.061(4) 0.031(3) 0.020(3) 0.020(3) C57 0.117(6) 0.056(4) 0.069(4) 0.032(3) 0.044(4) 0.033(4) C58 0.094(5) 0.043(4) 0.081(5) 0.023(3) 0.038(4) 0.028(3) C59 0.054(3) 0.034(3) 0.073(4) 0.022(3) 0.003(3) 0.014(3) C60 0.040(3) 0.031(3) 0.058(3) 0.026(2) -0.006(2) 0.005(2) O107 0.063(3) 0.052(2) 0.052(2) 0.0204(19) 0.0140(18) 0.028(2) O108 0.114(4) 0.046(3) 0.091(3) 0.041(2) 0.021(3) 0.031(3) N7 0.048(2) 0.041(2) 0.039(2) 0.0205(19) 0.0149(19) 0.023(2) N8 0.047(3) 0.044(3) 0.064(3) 0.029(2) 0.009(2) 0.014(2) C61 0.040(3) 0.038(3) 0.043(3) 0.025(2) 0.011(2) 0.018(2) C62 0.038(3) 0.043(3) 0.048(3) 0.029(2) 0.015(2) 0.018(2) C63 0.033(3) 0.045(3) 0.039(3) 0.024(2) 0.010(2) 0.015(2) C64 0.044(3) 0.050(3) 0.042(3) 0.021(2) 0.011(2) 0.019(3) C65 0.055(3) 0.074(4) 0.046(3) 0.029(3) 0.019(3) 0.029(3) C66 0.061(4) 0.089(5) 0.043(3) 0.038(3) 0.016(3) 0.021(3) C68 0.036(3) 0.044(3) 0.043(3) 0.022(2) 0.008(2) 0.012(2) O109 0.105(3) 0.062(3) 0.066(3) 0.045(2) 0.044(2) 0.044(3) O110 0.098(3) 0.106(4) 0.087(3) 0.071(3) 0.068(3) 0.060(3) N9 0.065(3) 0.049(3) 0.050(3) 0.030(2) 0.029(2) 0.022(2) N10 0.060(3) 0.063(3) 0.067(3) 0.045(3) 0.034(2) 0.030(3) C69 0.051(3) 0.046(3) 0.036(3) 0.023(2) 0.021(2) 0.015(2) C67 0.049(3) 0.060(4) 0.062(4) 0.045(3) 0.011(3) 0.015(3) C70 0.050(3) 0.049(3) 0.051(3) 0.028(3) 0.020(2) 0.017(3) C71 0.047(3) 0.033(3) 0.049(3) 0.021(2) 0.013(2) 0.007(2) C72 0.053(3) 0.056(4) 0.050(3) 0.026(3) 0.017(3) 0.015(3) C73 0.054(3) 0.032(3) 0.068(4) 0.025(3) 0.007(3) 0.008(3) C74 0.050(3) 0.049(4) 0.077(4) 0.037(3) 0.004(3) 0.004(3) C75 0.044(3) 0.052(3) 0.067(4) 0.035(3) 0.022(3) 0.014(3) C76 0.041(3) 0.046(3) 0.059(3) 0.033(3) 0.021(2) 0.015(2) O111 0.062(3) 0.053(2) 0.077(3) 0.040(2) 0.011(2) 0.017(2) O112 0.045(3) 0.081(3) 0.121(4) 0.056(3) 0.000(2) 0.010(2) N11 0.045(2) 0.032(2) 0.043(2) 0.0149(19) 0.0080(19) 0.0098(19) N12 0.049(3) 0.050(3) 0.056(3) 0.025(2) 0.009(2) 0.012(2) C77 0.046(3) 0.034(3) 0.052(3) 0.014(2) 0.023(2) 0.012(2) C78 0.040(3) 0.034(3) 0.049(3) 0.012(2) 0.013(2) 0.010(2) C79 0.046(3) 0.031(3) 0.035(3) 0.011(2) 0.013(2) 0.008(2) C80 0.057(3) 0.033(3) 0.041(3) 0.014(2) 0.014(2) 0.012(2) C81 0.068(4) 0.031(3) 0.067(4) 0.024(3) 0.026(3) 0.013(3) C82 0.067(4) 0.035(3) 0.068(4) 0.018(3) 0.021(3) 0.001(3) C83 0.059(4) 0.044(3) 0.048(3) 0.016(3) 0.012(3) 0.006(3) C84 0.047(3) 0.041(3) 0.044(3) 0.016(2) 0.009(2) 0.010(2) O113 0.122(5) 0.087(4) 0.132(5) 0.058(4) 0.020(4) 0.022(4) O114 0.182(8) 0.116(6) 0.212(8) 0.111(6) 0.045(6) 0.052(5) N13 0.092(5) 0.076(4) 0.092(4) 0.034(3) 0.021(4) 0.023(4) N14 0.109(6) 0.068(4) 0.148(7) 0.080(5) 0.014(5) 0.004(4) C85 0.061(4) 0.044(3) 0.113(5) 0.048(4) 0.036(4) 0.021(3) C86 0.086(5) 0.057(4) 0.106(6) 0.042(4) 0.027(4) 0.016(4) C87 0.063(4) 0.046(3) 0.079(4) 0.036(3) 0.013(3) 0.015(3) C88 0.213(13) 0.071(6) 0.121(8) 0.039(6) 0.072(8) 0.009(7) C89 0.237(14) 0.120(9) 0.181(11) 0.097(9) 0.142(11) 0.098(10) C90 0.154(10) 0.076(6) 0.117(7) 0.024(5) 0.065(7) 0.004(6) C91 0.058(5) 0.058(5) 0.208(11) 0.042(6) 0.015(6) 0.021(4) C92 0.051(4) 0.045(4) 0.155(7) 0.053(5) -0.007(4) 0.001(3) O115 0.085(4) 0.103(4) 0.091(4) 0.046(3) 0.025(3) 0.031(3) O116 0.088(4) 0.201(8) 0.162(6) 0.142(6) 0.009(4) 0.002(5) N16 0.058(3) 0.072(4) 0.100(5) 0.055(4) 0.012(3) 0.016(3) N15 0.062(3) 0.046(3) 0.082(4) 0.008(3) 0.012(3) 0.017(3) C93 0.066(4) 0.069(4) 0.081(4) 0.033(4) 0.018(3) 0.024(4) C94 0.060(4) 0.064(4) 0.094(5) 0.039(4) -0.005(3) 0.019(3) C95 0.035(3) 0.069(4) 0.066(4) 0.029(3) -0.001(3) 0.016(3) C96 0.051(3) 0.047(3) 0.059(4) 0.016(3) 0.004(3) 0.018(3) C97 0.044(4) 0.043(4) 0.125(6) 0.016(4) -0.003(4) 0.013(3) C98 0.051(4) 0.071(5) 0.211(10) 0.097(7) -0.031(6) -0.010(4) C99 0.049(4) 0.118(7) 0.125(7) 0.084(6) -0.028(4) -0.025(5) C100 0.041(3) 0.090(5) 0.089(5) 0.042(4) 0.005(3) 0.007(3) O200 0.089(4) 0.149(6) 0.074(3) 0.052(3) 0.025(3) 0.040(4) C200 0.051(4) 0.102(6) 0.101(6) 0.060(5) 0.030(4) 0.022(4) C201 0.071(5) 0.113(7) 0.105(6) 0.008(5) 0.041(5) -0.006(5) C202 0.108(7) 0.136(9) 0.127(8) 0.084(7) -0.006(6) 0.016(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 O4 C4 1.380(5) . ? O4 C37 1.426(5) . ? O6 C6 1.389(5) . ? O6 C45 1.411(5) . ? O11 C11 1.377(5) . ? O11 C53 1.424(5) . ? O13 C13 1.378(5) . ? O13 C61 1.424(5) . ? O18 C18 1.364(5) . ? O18 C69 1.443(5) . ? O20 C20 1.374(5) . ? O20 C77 1.415(6) . ? O25 C25 1.389(6) . ? O25 C85 1.410(6) . ? O27 C27 1.381(6) . ? O27 C93 1.402(7) . ? C1 C2 1.386(6) . ? C1 C6 1.390(6) . ? C1 C28 1.524(6) . ? C2 C3 1.390(6) . ? C3 C4 1.400(6) . ? C3 C7 1.515(6) . ? C4 C5 1.382(6) . ? C5 C6 1.385(6) . ? C7 C8 1.520(6) . ? C7 C29 1.536(6) . ? C8 C9 1.382(6) . ? C8 C13 1.398(6) . ? C9 C10 1.388(6) . ? C10 C11 1.398(6) . ? C10 C14 1.527(6) . ? C11 C12 1.391(6) . ? C12 C13 1.397(6) . ? C14 C31 1.521(6) . ? C14 C15 1.527(6) . ? C15 C20 1.387(6) . ? C15 C16 1.396(6) . ? C16 C17 1.384(6) . ? C17 C18 1.398(6) . ? C17 C21 1.529(6) . ? C18 C19 1.384(6) . ? C19 C20 1.389(6) . ? C21 C33 1.501(7) . ? C21 C22 1.525(7) . ? C22 C27 1.395(6) . ? C22 C23 1.404(6) . ? C23 C24 1.365(7) . ? C24 C25 1.391(6) . ? C24 C28 1.529(6) . ? C25 C26 1.389(7) . ? C26 C27 1.381(7) . ? C28 C35 1.535(6) . ? C29 C30 1.522(7) . ? C31 C32 1.530(6) . ? C33 C34A 1.412(9) . ? C33 C34B 1.546(15) . ? C35 C36 1.521(7) . ? O101 N2 1.236(6) . ? O102 N2 1.224(6) . ? N1 C39 1.347(6) . ? N1 C38 1.457(6) . ? N2 C44 1.443(7) . ? C37 C38 1.504(6) . ? C39 C44 1.403(7) . ? C39 C40 1.425(7) . ? C40 C41 1.373(7) . ? C41 C42 1.376(8) . ? C42 C43 1.363(8) . ? C43 C44 1.414(7) . ? O103 N4 1.257(6) . ? O104 N4 1.234(6) . ? N3 C47 1.370(6) . ? N3 C46 1.450(6) . ? N4 C52 1.445(7) . ? C45 C46 1.515(6) . ? C47 C52 1.414(7) . ? C47 C48 1.417(7) . ? C48 C49 1.361(7) . ? C49 C50 1.402(8) . ? C50 C51 1.360(9) . ? C51 C52 1.402(7) . ? O105 N6 1.227(6) . ? O106 N6 1.240(6) . ? N5 C55 1.348(6) . ? N5 C54 1.453(6) . ? N6 C60 1.439(7) . ? C53 C54 1.509(7) . ? C55 C56 1.411(7) . ? C55 C60 1.413(6) . ? C56 C57 1.358(9) . ? C57 C58 1.403(8) . ? C58 C59 1.345(8) . ? C59 C60 1.420(8) . ? O107 N8 1.236(5) . ? O108 N8 1.228(5) . ? N7 C63 1.373(6) . ? N7 C62 1.465(6) . ? N8 C68 1.444(7) . ? C61 C62 1.503(6) . ? C63 C64 1.403(7) . ? C63 C68 1.413(7) . ? C64 C65 1.384(7) . ? C65 C66 1.376(8) . ? C66 C67 1.368(8) . ? C68 C67 1.399(7) . ? O109 N10 1.241(5) . ? O110 N10 1.237(5) . ? N9 C71 1.343(6) . ? N9 C70 1.456(6) . ? N10 C76 1.430(7) . ? C69 C70 1.479(7) . ? C71 C76 1.405(7) . ? C71 C72 1.432(7) . ? C72 C73 1.369(7) . ? C73 C74 1.366(8) . ? C74 C75 1.338(8) . ? C75 C76 1.392(7) . ? O111 N12 1.241(6) . ? O112 N12 1.221(6) . ? N11 C79 1.354(6) . ? N11 C78 1.439(6) . ? N12 C84 1.430(7) . ? C77 C78 1.500(7) . ? C79 C80 1.404(7) . ? C79 C84 1.423(7) . ? C80 C81 1.379(7) . ? C81 C82 1.395(8) . ? C82 C83 1.363(8) . ? C83 C84 1.408(7) . ? O113 N14 1.309(10) . ? O114 N14 1.200(8) . ? N13 C87 1.424(7) . ? N13 C86 1.543(9) . ? N14 C92 1.391(8) . ? C85 C86 1.470(9) . ? C87 C88 1.3900 . ? C87 C92 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C90 C91 1.3900 . ? C91 C92 1.3900 . ? O115 N16 1.237(7) . ? O116 N16 1.122(7) . ? N16 C100 1.543(8) . ? N15 C95 1.433(6) . ? N15 C94 1.447(9) . ? C93 C94 1.498(9) . ? C95 C96 1.3900 . ? C95 C100 1.3900 . ? C96 C97 1.3900 . ? C97 C98 1.3900 . ? C98 C99 1.3900 . ? C99 C100 1.3900 . ? O200 C200 1.246(8) . ? C200 C201 1.453(11) . ? C200 C202 1.457(11) . ? 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 C4 O4 C37 117.4(3) . . ? C6 O6 C45 119.1(3) . . ? C11 O11 C53 116.6(3) . . ? C13 O13 C61 116.3(3) . . ? C18 O18 C69 117.6(3) . . ? C20 O20 C77 120.9(3) . . ? C25 O25 C85 117.2(4) . . ? C27 O27 C93 117.4(4) . . ? C2 C1 C6 116.9(4) . . ? C2 C1 C28 123.9(4) . . ? C6 C1 C28 119.2(4) . . ? C1 C2 C3 124.0(4) . . ? C2 C3 C4 116.2(4) . . ? C2 C3 C7 123.8(4) . . ? C4 C3 C7 119.9(4) . . ? O4 C4 C5 122.9(4) . . ? O4 C4 C3 114.8(4) . . ? C5 C4 C3 122.2(4) . . ? C4 C5 C6 118.7(4) . . ? C5 C6 O6 123.2(4) . . ? C5 C6 C1 121.9(4) . . ? O6 C6 C1 114.8(4) . . ? C3 C7 C8 111.8(3) . . ? C3 C7 C29 112.9(4) . . ? C8 C7 C29 111.5(4) . . ? C9 C8 C13 116.6(4) . . ? C9 C8 C7 121.8(4) . . ? C13 C8 C7 121.5(4) . . ? C8 C9 C10 125.0(4) . . ? C9 C10 C11 116.8(4) . . ? C9 C10 C14 121.3(4) . . ? C11 C10 C14 121.8(4) . . ? O11 C11 C12 121.7(4) . . ? O11 C11 C10 117.8(4) . . ? C12 C11 C10 120.5(4) . . ? C11 C12 C13 120.4(4) . . ? O13 C13 C12 121.5(4) . . ? O13 C13 C8 117.8(4) . . ? C12 C13 C8 120.7(4) . . ? C31 C14 C10 111.0(3) . . ? C31 C14 C15 114.5(4) . . ? C10 C14 C15 110.0(3) . . ? C20 C15 C16 117.3(4) . . ? C20 C15 C14 119.4(4) . . ? C16 C15 C14 123.3(4) . . ? C17 C16 C15 123.7(4) . . ? C16 C17 C18 116.5(4) . . ? C16 C17 C21 124.0(4) . . ? C18 C17 C21 119.5(4) . . ? O18 C18 C19 122.4(4) . . ? O18 C18 C17 115.7(4) . . ? C19 C18 C17 122.0(4) . . ? C18 C19 C20 119.2(4) . . ? O20 C20 C15 115.5(4) . . ? O20 C20 C19 123.1(4) . . ? C15 C20 C19 121.3(4) . . ? C33 C21 C22 109.6(4) . . ? C33 C21 C17 114.5(4) . . ? C22 C21 C17 111.3(4) . . ? C27 C22 C23 116.3(4) . . ? C27 C22 C21 122.5(4) . . ? C23 C22 C21 121.2(4) . . ? C24 C23 C22 124.0(4) . . ? C23 C24 C25 117.7(4) . . ? C23 C24 C28 120.4(4) . . ? C25 C24 C28 121.9(4) . . ? O25 C25 C26 122.0(4) . . ? O25 C25 C24 117.2(4) . . ? C26 C25 C24 120.8(5) . . ? C27 C26 C25 119.8(4) . . ? O27 C27 C26 119.9(4) . . ? O27 C27 C22 118.6(4) . . ? C26 C27 C22 121.4(4) . . ? C1 C28 C24 110.5(4) . . ? C1 C28 C35 113.3(4) . . ? C24 C28 C35 111.6(4) . . ? C30 C29 C7 113.1(4) . . ? C14 C31 C32 113.8(4) . . ? C34A C33 C21 118.9(6) . . ? C34A C33 C34B 69.1(8) . . ? C21 C33 C34B 112.7(7) . . ? C36 C35 C28 113.1(4) . . ? C39 N1 C38 122.8(4) . . ? O102 N2 O101 121.6(5) . . ? O102 N2 C44 120.1(5) . . ? O101 N2 C44 118.3(5) . . ? O4 C37 C38 107.5(4) . . ? N1 C38 C37 110.1(4) . . ? N1 C39 C44 124.5(5) . . ? N1 C39 C40 119.6(5) . . ? C44 C39 C40 115.9(4) . . ? C41 C40 C39 121.5(5) . . ? C40 C41 C42 120.9(5) . . ? C43 C42 C41 120.2(5) . . ? C42 C43 C44 119.8(5) . . ? C39 C44 C43 121.6(5) . . ? C39 C44 N2 121.7(5) . . ? C43 C44 N2 116.7(5) . . ? C47 N3 C46 122.8(4) . . ? O104 N4 O103 122.3(5) . . ? O104 N4 C52 117.9(5) . . ? O103 N4 C52 119.7(5) . . ? O6 C45 C46 104.8(4) . . ? N3 C46 C45 109.8(4) . . ? N3 C47 C52 124.9(5) . . ? N3 C47 C48 119.9(5) . . ? C52 C47 C48 115.2(5) . . ? C49 C48 C47 122.2(5) . . ? C48 C49 C50 121.5(6) . . ? C51 C50 C49 118.1(5) . . ? C50 C51 C52 121.2(5) . . ? C51 C52 C47 121.6(5) . . ? C51 C52 N4 117.6(5) . . ? C47 C52 N4 120.8(5) . . ? C55 N5 C54 123.8(4) . . ? O105 N6 O106 121.3(5) . . ? O105 N6 C60 119.8(4) . . ? O106 N6 C60 118.9(5) . . ? O11 C53 C54 108.4(4) . . ? N5 C54 C53 110.9(4) . . ? N5 C55 C56 120.9(4) . . ? N5 C55 C60 124.5(5) . . ? C56 C55 C60 114.6(5) . . ? C57 C56 C55 123.4(5) . . ? C56 C57 C58 120.8(6) . . ? C59 C58 C57 118.5(6) . . ? C58 C59 C60 121.3(5) . . ? C55 C60 C59 121.3(5) . . ? C55 C60 N6 122.0(5) . . ? C59 C60 N6 116.6(5) . . ? C63 N7 C62 122.9(4) . . ? O108 N8 O107 121.5(5) . . ? O108 N8 C68 118.9(5) . . ? O107 N8 C68 119.6(4) . . ? O13 C61 C62 108.4(4) . . ? N7 C62 C61 109.6(4) . . ? N7 C63 C64 120.3(4) . . ? N7 C63 C68 123.7(4) . . ? C64 C63 C68 115.9(4) . . ? C65 C64 C63 122.1(5) . . ? C66 C65 C64 120.5(5) . . ? C67 C66 C65 119.6(5) . . ? C67 C68 C63 121.4(5) . . ? C67 C68 N8 116.5(5) . . ? C63 C68 N8 122.1(4) . . ? C71 N9 C70 121.7(4) . . ? O110 N10 O109 120.3(5) . . ? O110 N10 C76 119.8(4) . . ? O109 N10 C76 119.9(4) . . ? O18 C69 C70 103.4(4) . . ? C66 C67 C68 120.4(5) . . ? N9 C70 C69 111.7(4) . . ? N9 C71 C76 124.5(5) . . ? N9 C71 C72 120.1(5) . . ? C76 C71 C72 115.5(4) . . ? C73 C72 C71 120.5(5) . . ? C74 C73 C72 122.6(5) . . ? C75 C74 C73 118.3(5) . . ? C74 C75 C76 122.4(5) . . ? C75 C76 C71 120.8(5) . . ? C75 C76 N10 116.8(5) . . ? C71 C76 N10 122.4(4) . . ? C79 N11 C78 124.2(4) . . ? O112 N12 O111 121.2(5) . . ? O112 N12 C84 119.5(5) . . ? O111 N12 C84 119.3(5) . . ? O20 C77 C78 106.6(4) . . ? N11 C78 C77 109.9(4) . . ? N11 C79 C80 120.1(5) . . ? N11 C79 C84 123.6(4) . . ? C80 C79 C84 116.3(5) . . ? C81 C80 C79 122.0(5) . . ? C80 C81 C82 120.4(5) . . ? C83 C82 C81 119.9(5) . . ? C82 C83 C84 120.2(6) . . ? C83 C84 C79 121.1(5) . . ? C83 C84 N12 116.3(5) . . ? C79 C84 N12 122.5(5) . . ? C87 N13 C86 119.0(6) . . ? O114 N14 O113 120.0(9) . . ? O114 N14 C92 123.8(9) . . ? O113 N14 C92 116.1(6) . . ? O25 C85 C86 108.1(5) . . ? C85 C86 N13 109.8(6) . . ? C88 C87 C92 120.0 . . ? C88 C87 N13 121.2(4) . . ? C92 C87 N13 118.7(4) . . ? C87 C88 C89 120.0 . . ? C90 C89 C88 120.0 . . ? C91 C90 C89 120.0 . . ? C90 C91 C92 120.0 . . ? C91 C92 C87 120.0 . . ? C91 C92 N14 112.7(5) . . ? C87 C92 N14 127.0(5) . . ? O116 N16 O115 131.4(8) . . ? O116 N16 C100 113.4(7) . . ? O115 N16 C100 115.2(6) . . ? C95 N15 C94 124.0(5) . . ? O27 C93 C94 108.5(5) . . ? N15 C94 C93 115.2(6) . . ? C96 C95 C100 120.0 . . ? C96 C95 N15 117.7(4) . . ? C100 C95 N15 122.1(4) . . ? C97 C96 C95 120.0 . . ? C98 C97 C96 120.0 . . ? C97 C98 C99 120.0 . . ? C100 C99 C98 120.0 . . ? C99 C100 C95 120.0 . . ? C99 C100 N16 117.4(4) . . ? C95 C100 N16 122.5(4) . . ? O200 C200 C201 119.6(8) . . ? O200 C200 C202 115.1(8) . . ? C201 C200 C202 125.3(8) . . ? 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 -2.0(7) . . . . ? C28 C1 C2 C3 177.9(4) . . . . ? C1 C2 C3 C4 1.1(7) . . . . ? C1 C2 C3 C7 -175.8(4) . . . . ? C37 O4 C4 C5 -27.8(6) . . . . ? C37 O4 C4 C3 150.3(4) . . . . ? C2 C3 C4 O4 -178.2(4) . . . . ? C7 C3 C4 O4 -1.2(6) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? C7 C3 C4 C5 177.0(4) . . . . ? O4 C4 C5 C6 177.9(4) . . . . ? C3 C4 C5 C6 -0.2(7) . . . . ? C4 C5 C6 O6 -178.9(4) . . . . ? C4 C5 C6 C1 -0.8(7) . . . . ? C45 O6 C6 C5 -13.6(7) . . . . ? C45 O6 C6 C1 168.2(4) . . . . ? C2 C1 C6 C5 1.8(7) . . . . ? C28 C1 C6 C5 -178.1(5) . . . . ? C2 C1 C6 O6 -179.9(4) . . . . ? C28 C1 C6 O6 0.2(6) . . . . ? C2 C3 C7 C8 -107.4(5) . . . . ? C4 C3 C7 C8 75.9(5) . . . . ? C2 C3 C7 C29 19.4(6) . . . . ? C4 C3 C7 C29 -157.3(4) . . . . ? C3 C7 C8 C9 46.4(5) . . . . ? C29 C7 C8 C9 -81.1(5) . . . . ? C3 C7 C8 C13 -136.1(4) . . . . ? C29 C7 C8 C13 96.4(5) . . . . ? C13 C8 C9 C10 -1.6(6) . . . . ? C7 C8 C9 C10 176.0(4) . . . . ? C8 C9 C10 C11 1.4(6) . . . . ? C8 C9 C10 C14 -176.8(4) . . . . ? C53 O11 C11 C12 -21.0(6) . . . . ? C53 O11 C11 C10 158.3(4) . . . . ? C9 C10 C11 O11 179.8(4) . . . . ? C14 C10 C11 O11 -2.0(6) . . . . ? C9 C10 C11 C12 -0.9(6) . . . . ? C14 C10 C11 C12 177.3(4) . . . . ? O11 C11 C12 C13 180.0(4) . . . . ? C10 C11 C12 C13 0.7(7) . . . . ? C61 O13 C13 C12 12.9(6) . . . . ? C61 O13 C13 C8 -165.4(4) . . . . ? C11 C12 C13 O13 -179.2(4) . . . . ? C11 C12 C13 C8 -0.9(7) . . . . ? C9 C8 C13 O13 179.6(4) . . . . ? C7 C8 C13 O13 2.0(6) . . . . ? C9 C8 C13 C12 1.2(6) . . . . ? C7 C8 C13 C12 -176.4(4) . . . . ? C9 C10 C14 C31 77.4(5) . . . . ? C11 C10 C14 C31 -100.7(5) . . . . ? C9 C10 C14 C15 -50.3(5) . . . . ? C11 C10 C14 C15 131.6(4) . . . . ? C31 C14 C15 C20 171.8(4) . . . . ? C10 C14 C15 C20 -62.4(5) . . . . ? C31 C14 C15 C16 -10.1(6) . . . . ? C10 C14 C15 C16 115.7(5) . . . . ? C20 C15 C16 C17 0.4(7) . . . . ? C14 C15 C16 C17 -177.7(4) . . . . ? C15 C16 C17 C18 2.6(7) . . . . ? C15 C16 C17 C21 -179.4(4) . . . . ? C69 O18 C18 C19 29.9(6) . . . . ? C69 O18 C18 C17 -151.0(4) . . . . ? C16 C17 C18 O18 177.9(4) . . . . ? C21 C17 C18 O18 -0.1(6) . . . . ? C16 C17 C18 C19 -2.9(6) . . . . ? C21 C17 C18 C19 179.0(4) . . . . ? O18 C18 C19 C20 179.3(4) . . . . ? C17 C18 C19 C20 0.3(7) . . . . ? C77 O20 C20 C15 152.9(4) . . . . ? C77 O20 C20 C19 -30.1(7) . . . . ? C16 C15 C20 O20 173.8(4) . . . . ? C14 C15 C20 O20 -8.0(6) . . . . ? C16 C15 C20 C19 -3.3(6) . . . . ? C14 C15 C20 C19 174.9(4) . . . . ? C18 C19 C20 O20 -173.9(4) . . . . ? C18 C19 C20 C15 3.0(7) . . . . ? C16 C17 C21 C33 12.4(7) . . . . ? C18 C17 C21 C33 -169.7(4) . . . . ? C16 C17 C21 C22 -112.6(5) . . . . ? C18 C17 C21 C22 65.3(5) . . . . ? C33 C21 C22 C27 100.7(5) . . . . ? C17 C21 C22 C27 -131.6(4) . . . . ? C33 C21 C22 C23 -77.3(5) . . . . ? C17 C21 C22 C23 50.4(5) . . . . ? C27 C22 C23 C24 -0.8(7) . . . . ? C21 C22 C23 C24 177.3(4) . . . . ? C22 C23 C24 C25 0.5(7) . . . . ? C22 C23 C24 C28 179.1(4) . . . . ? C85 O25 C25 C26 -4.8(7) . . . . ? C85 O25 C25 C24 176.4(5) . . . . ? C23 C24 C25 O25 179.5(4) . . . . ? C28 C24 C25 O25 0.8(6) . . . . ? C23 C24 C25 C26 0.6(6) . . . . ? C28 C24 C25 C26 -178.0(4) . . . . ? O25 C25 C26 C27 179.9(4) . . . . ? C24 C25 C26 C27 -1.3(7) . . . . ? C93 O27 C27 C26 72.9(6) . . . . ? C93 O27 C27 C22 -111.9(5) . . . . ? C25 C26 C27 O27 176.1(4) . . . . ? C25 C26 C27 C22 1.0(7) . . . . ? C23 C22 C27 O27 -175.1(4) . . . . ? C21 C22 C27 O27 6.8(6) . . . . ? C23 C22 C27 C26 0.1(7) . . . . ? C21 C22 C27 C26 -178.0(4) . . . . ? C2 C1 C28 C24 111.8(5) . . . . ? C6 C1 C28 C24 -68.3(5) . . . . ? C2 C1 C28 C35 -14.3(7) . . . . ? C6 C1 C28 C35 165.6(4) . . . . ? C23 C24 C28 C1 -51.9(5) . . . . ? C25 C24 C28 C1 126.7(4) . . . . ? C23 C24 C28 C35 75.1(5) . . . . ? C25 C24 C28 C35 -106.3(5) . . . . ? C3 C7 C29 C30 168.3(4) . . . . ? C8 C7 C29 C30 -64.8(6) . . . . ? C10 C14 C31 C32 58.3(5) . . . . ? C15 C14 C31 C32 -176.5(4) . . . . ? C22 C21 C33 C34A -164.0(5) . . . . ? C17 C21 C33 C34A 70.2(7) . . . . ? C22 C21 C33 C34B -86.1(9) . . . . ? C17 C21 C33 C34B 148.0(8) . . . . ? C1 C28 C35 C36 -168.9(4) . . . . ? C24 C28 C35 C36 65.6(6) . . . . ? C4 O4 C37 C38 -159.5(4) . . . . ? C39 N1 C38 C37 168.3(4) . . . . ? O4 C37 C38 N1 -63.1(5) . . . . ? C38 N1 C39 C44 -170.8(5) . . . . ? C38 N1 C39 C40 9.2(7) . . . . ? N1 C39 C40 C41 -176.4(4) . . . . ? C44 C39 C40 C41 3.6(7) . . . . ? C39 C40 C41 C42 -3.2(8) . . . . ? C40 C41 C42 C43 0.3(8) . . . . ? C41 C42 C43 C44 1.8(8) . . . . ? N1 C39 C44 C43 178.5(5) . . . . ? C40 C39 C44 C43 -1.5(7) . . . . ? N1 C39 C44 N2 1.6(8) . . . . ? C40 C39 C44 N2 -178.5(4) . . . . ? C42 C43 C44 C39 -1.1(8) . . . . ? C42 C43 C44 N2 176.0(5) . . . . ? O102 N2 C44 C39 171.6(5) . . . . ? O101 N2 C44 C39 -8.7(8) . . . . ? O102 N2 C44 C43 -5.5(8) . . . . ? O101 N2 C44 C43 174.2(5) . . . . ? C6 O6 C45 C46 -178.6(4) . . . . ? C47 N3 C46 C45 169.6(5) . . . . ? O6 C45 C46 N3 -165.0(4) . . . . ? C46 N3 C47 C52 -172.0(5) . . . . ? C46 N3 C47 C48 8.1(8) . . . . ? N3 C47 C48 C49 177.3(5) . . . . ? C52 C47 C48 C49 -2.5(8) . . . . ? C47 C48 C49 C50 1.3(8) . . . . ? C48 C49 C50 C51 0.5(8) . . . . ? C49 C50 C51 C52 -1.1(8) . . . . ? C50 C51 C52 C47 -0.2(8) . . . . ? C50 C51 C52 N4 -179.7(5) . . . . ? N3 C47 C52 C51 -177.9(5) . . . . ? C48 C47 C52 C51 1.9(7) . . . . ? N3 C47 C52 N4 1.6(8) . . . . ? C48 C47 C52 N4 -178.5(5) . . . . ? O104 N4 C52 C51 -7.0(7) . . . . ? O103 N4 C52 C51 170.8(5) . . . . ? O104 N4 C52 C47 173.4(5) . . . . ? O103 N4 C52 C47 -8.8(8) . . . . ? C11 O11 C53 C54 -177.8(4) . . . . ? C55 N5 C54 C53 78.2(6) . . . . ? O11 C53 C54 N5 -175.7(4) . . . . ? C54 N5 C55 C56 -2.1(7) . . . . ? C54 N5 C55 C60 179.0(4) . . . . ? N5 C55 C56 C57 178.7(6) . . . . ? C60 C55 C56 C57 -2.3(9) . . . . ? C55 C56 C57 C58 0.8(11) . . . . ? C56 C57 C58 C59 0.8(11) . . . . ? C57 C58 C59 C60 -0.7(10) . . . . ? N5 C55 C60 C59 -178.7(5) . . . . ? C56 C55 C60 C59 2.4(7) . . . . ? N5 C55 C60 N6 0.2(7) . . . . ? C56 C55 C60 N6 -178.8(5) . . . . ? C58 C59 C60 C55 -1.0(8) . . . . ? C58 C59 C60 N6 -179.9(5) . . . . ? O105 N6 C60 C55 3.0(7) . . . . ? O106 N6 C60 C55 -176.9(5) . . . . ? O105 N6 C60 C59 -178.1(5) . . . . ? O106 N6 C60 C59 2.0(7) . . . . ? C13 O13 C61 C62 172.1(4) . . . . ? C63 N7 C62 C61 75.1(6) . . . . ? O13 C61 C62 N7 -174.5(4) . . . . ? C62 N7 C63 C64 13.9(7) . . . . ? C62 N7 C63 C68 -168.8(4) . . . . ? N7 C63 C64 C65 178.5(5) . . . . ? C68 C63 C64 C65 0.9(7) . . . . ? C63 C64 C65 C66 -0.5(8) . . . . ? C64 C65 C66 C67 0.1(9) . . . . ? N7 C63 C68 C67 -178.6(5) . . . . ? C64 C63 C68 C67 -1.1(7) . . . . ? N7 C63 C68 N8 2.9(7) . . . . ? C64 C63 C68 N8 -179.6(4) . . . . ? O108 N8 C68 C67 3.6(7) . . . . ? O107 N8 C68 C67 -178.3(4) . . . . ? O108 N8 C68 C63 -177.8(5) . . . . ? O107 N8 C68 C63 0.2(7) . . . . ? C18 O18 C69 C70 158.0(4) . . . . ? C65 C66 C67 C68 -0.3(9) . . . . ? C63 C68 C67 C66 0.8(8) . . . . ? N8 C68 C67 C66 179.4(5) . . . . ? C71 N9 C70 C69 -176.0(5) . . . . ? O18 C69 C70 N9 171.7(4) . . . . ? C70 N9 C71 C76 177.3(5) . . . . ? C70 N9 C71 C72 -1.9(8) . . . . ? N9 C71 C72 C73 179.3(5) . . . . ? C76 C71 C72 C73 0.0(8) . . . . ? C71 C72 C73 C74 0.3(8) . . . . ? C72 C73 C74 C75 0.3(8) . . . . ? C73 C74 C75 C76 -1.4(8) . . . . ? C74 C75 C76 C71 1.8(8) . . . . ? C74 C75 C76 N10 -178.3(5) . . . . ? N9 C71 C76 C75 179.7(5) . . . . ? C72 C71 C76 C75 -1.1(7) . . . . ? N9 C71 C76 N10 -0.1(8) . . . . ? C72 C71 C76 N10 179.1(5) . . . . ? O110 N10 C76 C75 -4.4(8) . . . . ? O109 N10 C76 C75 173.7(5) . . . . ? O110 N10 C76 C71 175.5(5) . . . . ? O109 N10 C76 C71 -6.5(8) . . . . ? C20 O20 C77 C78 163.2(4) . . . . ? C79 N11 C78 C77 158.7(4) . . . . ? O20 C77 C78 N11 -72.7(5) . . . . ? C78 N11 C79 C80 8.5(7) . . . . ? C78 N11 C79 C84 -172.1(5) . . . . ? N11 C79 C80 C81 -179.1(5) . . . . ? C84 C79 C80 C81 1.5(7) . . . . ? C79 C80 C81 C82 -0.6(8) . . . . ? C80 C81 C82 C83 -0.3(9) . . . . ? C81 C82 C83 C84 0.3(8) . . . . ? C82 C83 C84 C79 0.7(8) . . . . ? C82 C83 C84 N12 178.6(5) . . . . ? N11 C79 C84 C83 179.1(5) . . . . ? C80 C79 C84 C83 -1.5(7) . . . . ? N11 C79 C84 N12 1.3(8) . . . . ? C80 C79 C84 N12 -179.3(4) . . . . ? O112 N12 C84 C83 -1.1(7) . . . . ? O111 N12 C84 C83 179.1(5) . . . . ? O112 N12 C84 C79 176.8(5) . . . . ? O111 N12 C84 C79 -3.0(7) . . . . ? C25 O25 C85 C86 -176.0(5) . . . . ? O25 C85 C86 N13 173.2(5) . . . . ? C87 N13 C86 C85 -78.2(8) . . . . ? C86 N13 C87 C88 7.4(8) . . . . ? C86 N13 C87 C92 -174.4(5) . . . . ? C92 C87 C88 C89 0.0 . . . . ? N13 C87 C88 C89 178.1(5) . . . . ? C87 C88 C89 C90 0.0 . . . . ? C88 C89 C90 C91 0.0 . . . . ? C89 C90 C91 C92 0.0 . . . . ? C90 C91 C92 C87 0.0 . . . . ? C90 C91 C92 N14 -174.2(5) . . . . ? C88 C87 C92 C91 0.0 . . . . ? N13 C87 C92 C91 -178.2(5) . . . . ? C88 C87 C92 N14 173.3(6) . . . . ? N13 C87 C92 N14 -4.8(7) . . . . ? O114 N14 C92 C91 -6.2(10) . . . . ? O113 N14 C92 C91 177.6(6) . . . . ? O114 N14 C92 C87 -179.9(7) . . . . ? O113 N14 C92 C87 3.9(9) . . . . ? C27 O27 C93 C94 -176.1(5) . . . . ? C95 N15 C94 C93 84.0(7) . . . . ? O27 C93 C94 N15 75.8(7) . . . . ? C94 N15 C95 C96 3.2(7) . . . . ? C94 N15 C95 C100 177.4(4) . . . . ? C100 C95 C96 C97 0.0 . . . . ? N15 C95 C96 C97 174.4(4) . . . . ? C95 C96 C97 C98 0.0 . . . . ? C96 C97 C98 C99 0.0 . . . . ? C97 C98 C99 C100 0.0 . . . . ? C98 C99 C100 C95 0.0 . . . . ? C98 C99 C100 N16 176.8(4) . . . . ? C96 C95 C100 C99 0.0 . . . . ? N15 C95 C100 C99 -174.1(4) . . . . ? C96 C95 C100 N16 -176.7(4) . . . . ? N15 C95 C100 N16 9.2(5) . . . . ? O116 N16 C100 C99 -9.3(7) . . . . ? O115 N16 C100 C99 171.0(4) . . . . ? O116 N16 C100 C95 167.5(5) . . . . ? O115 N16 C100 C95 -12.2(6) . . . . ? 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 N1 H1N O101 0.89(3) 1.86(4) 2.607(6) 141(5) . N1 H1N N2 0.89(3) 2.46(5) 2.928(7) 113(4) . N3 H3N O103 0.88 1.98 2.623(6) 128.4 . N3 H3N O103 0.88 2.62 3.421(6) 151.1 2_656 N5 H5N O105 0.88 2.00 2.645(5) 129.2 . N5 H5N O200 0.88 2.57 3.127(7) 122.2 . N7 H7N O107 0.89(3) 1.92(4) 2.630(5) 135(4) . N9 H9N O109 0.89(3) 1.99(5) 2.647(6) 129(5) . N11 H11N O111 0.89(3) 2.01(5) 2.629(6) 125(4) . N13 H13N O113 0.88 1.90 2.542(9) 128.9 . N15 H15N O115 0.88 1.94 2.601(8) 130.8 . N15 H15N O109 0.88 2.37 3.125(7) 144.2 2_756 _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 66.84 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.268 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.084 #===end data_2B _database_code_depnum_ccdc_archive 'CCDC 781922' #TrackingRef '- Octapodands.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C103 H110 N16 O25' _chemical_formula_weight 1972.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 11.8347(3) _cell_length_b 20.5903(5) _cell_length_c 22.5132(7) _cell_angle_alpha 113.258(2) _cell_angle_beta 95.992(2) _cell_angle_gamma 100.282(2) _cell_volume 4865.6(2) _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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8548 _exptl_absorpt_correction_T_max 0.9840 _exptl_absorpt_process_details 'Denzo (Otwinowski, Majewski, Borek & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 22141 _diffrn_reflns_av_R_equivalents 0.1285 _diffrn_reflns_av_sigmaI/netI 0.1165 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 66.86 _reflns_number_total 15235 _reflns_number_gt 8353 _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^)+(0.1160P)^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 SHELXL _refine_ls_extinction_coef 0.00097(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15235 _refine_ls_number_parameters 1272 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1702 _refine_ls_R_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.2682 _refine_ls_wR_factor_gt 0.2234 _refine_ls_goodness_of_fit_ref 1.217 _refine_ls_restrained_S_all 1.217 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O4 O 0.1816(3) 0.54858(18) 0.29267(17) 0.0408(9) Uani 1 1 d . . . O6 O 0.4864(3) 0.74452(18) 0.30471(16) 0.0400(8) Uani 1 1 d . . . O11 O 0.2487(3) 0.25689(18) 0.15115(18) 0.0438(9) Uani 1 1 d . . . O13 O -0.0433(3) 0.39827(19) 0.1903(2) 0.0499(10) Uani 1 1 d . . . O18 O 0.7728(3) 0.60764(18) 0.27339(17) 0.0403(8) Uani 1 1 d . . . O20 O 0.4681(3) 0.40327(19) 0.25178(17) 0.0429(9) Uani 1 1 d . . . O25 O 0.5905(3) 0.84996(19) 0.2222(2) 0.0514(10) Uani 1 1 d . . . O27 O 0.8860(3) 0.71147(18) 0.19574(18) 0.0434(9) Uani 1 1 d . . . C1 C 0.3458(4) 0.6743(2) 0.2045(2) 0.0310(11) Uani 1 1 d . . . C2 C 0.2479(4) 0.6160(3) 0.1715(3) 0.0341(11) Uani 1 1 d . . . H2 H 0.2174 0.6049 0.1269 0.041 Uiso 1 1 calc R . . C3 C 0.1922(4) 0.5732(3) 0.1996(2) 0.0325(11) Uani 1 1 d . . . C4 C 0.2386(4) 0.5909(3) 0.2654(2) 0.0329(11) Uani 1 1 d . . . C5 C 0.3366(4) 0.6470(3) 0.2994(3) 0.0364(12) Uani 1 1 d . . . H5 H 0.3676 0.6581 0.3439 0.044 Uiso 1 1 calc R . . C6 C 0.3896(4) 0.6871(3) 0.2688(3) 0.0349(12) Uani 1 1 d . . . C7 C 0.0914(4) 0.5073(3) 0.1636(2) 0.0337(11) Uani 1 1 d . . . H7 H 0.0296 0.5130 0.1910 0.040 Uiso 1 1 calc R . . C8 C 0.1308(4) 0.4387(3) 0.1590(2) 0.0332(11) Uani 1 1 d . . . C9 C 0.2381(4) 0.4281(3) 0.1433(2) 0.0321(11) Uani 1 1 d . . . H9 H 0.2860 0.4641 0.1345 0.039 Uiso 1 1 calc R . . C10 C 0.2801(4) 0.3681(3) 0.1397(2) 0.0333(11) Uani 1 1 d . . . C11 C 0.2088(4) 0.3166(3) 0.1542(2) 0.0352(12) Uani 1 1 d . . . C12 C 0.1019(4) 0.3262(3) 0.1719(2) 0.0378(12) Uani 1 1 d . . . H12 H 0.0553 0.2916 0.1830 0.045 Uiso 1 1 calc R . . C13 C 0.0637(4) 0.3868(3) 0.1732(2) 0.0361(12) Uani 1 1 d . . . C14 C 0.3979(4) 0.3583(3) 0.1203(2) 0.0346(12) Uani 1 1 d . . . H14 H 0.4172 0.3186 0.1315 0.042 Uiso 1 1 calc R . . C15 C 0.4958(4) 0.4266(3) 0.1610(2) 0.0311(11) Uani 1 1 d . . . C16 C 0.5551(4) 0.4700(3) 0.1338(2) 0.0322(11) Uani 1 1 d . . . H16 H 0.5300 0.4583 0.0885 0.039 Uiso 1 1 calc R . . C17 C 0.6489(4) 0.5293(3) 0.1700(2) 0.0320(11) Uani 1 1 d . . . C18 C 0.6804(4) 0.5469(2) 0.2368(2) 0.0316(11) Uani 1 1 d . . . C19 C 0.6223(4) 0.5072(3) 0.2664(3) 0.0351(12) Uani 1 1 d . . . H19 H 0.6447 0.5205 0.3122 0.042 Uiso 1 1 calc R . . C20 C 0.5311(4) 0.4477(3) 0.2281(3) 0.0338(12) Uani 1 1 d . . . C21 C 0.7150(4) 0.5759(3) 0.1400(2) 0.0322(11) Uani 1 1 d . . . H21 H 0.8005 0.5847 0.1568 0.039 Uiso 1 1 calc R . . C22 C 0.6851(4) 0.6502(3) 0.1634(2) 0.0327(11) Uani 1 1 d . . . C23 C 0.5694(4) 0.6557(3) 0.1584(2) 0.0335(11) Uani 1 1 d . . . H23 H 0.5098 0.6119 0.1406 0.040 Uiso 1 1 calc R . . C26 C 0.7399(4) 0.7822(3) 0.2077(3) 0.0438(13) Uani 1 1 d . . . H26 H 0.7996 0.8260 0.2247 0.053 Uiso 1 1 calc R . . C24 C 0.5353(4) 0.7205(3) 0.1776(2) 0.0349(12) Uani 1 1 d . . . C25 C 0.6236(4) 0.7844(3) 0.2018(3) 0.0399(13) Uani 1 1 d . . . C27 C 0.7693(4) 0.7152(3) 0.1884(2) 0.0368(12) Uani 1 1 d . . . C28 C 0.4053(4) 0.7196(3) 0.1718(2) 0.0337(11) Uani 1 1 d . . . H28 H 0.3997 0.7708 0.1972 0.040 Uiso 1 1 calc R . . C29 C 0.0360(4) 0.5003(3) 0.0961(3) 0.0421(13) Uani 1 1 d . . . H29A H 0.0152 0.5465 0.1015 0.051 Uiso 1 1 calc R . . H29B H 0.0946 0.4926 0.0672 0.051 Uiso 1 1 calc R . . C30 C -0.0734(5) 0.4380(3) 0.0623(3) 0.0610(17) Uani 1 1 d . . . H30A H -0.1039 0.4362 0.0193 0.092 Uiso 1 1 calc R . . H30B H -0.1330 0.4459 0.0898 0.092 Uiso 1 1 calc R . . H30C H -0.0534 0.3918 0.0560 0.092 Uiso 1 1 calc R . . C31 C 0.3919(5) 0.3328(3) 0.0466(2) 0.0451(14) Uani 1 1 d . . . H31A H 0.3700 0.3702 0.0336 0.054 Uiso 1 1 calc R . . H31B H 0.4706 0.3285 0.0369 0.054 Uiso 1 1 calc R . . C32 C 0.3057(5) 0.2608(3) 0.0055(3) 0.0623(18) Uani 1 1 d . . . H32A H 0.3045 0.2485 -0.0413 0.093 Uiso 1 1 calc R . . H32B H 0.2275 0.2643 0.0149 0.093 Uiso 1 1 calc R . . H32C H 0.3292 0.2228 0.0162 0.093 Uiso 1 1 calc R . . C33 C 0.6951(4) 0.5399(3) 0.0650(3) 0.0424(13) Uani 1 1 d . . . H33A H 0.6139 0.5374 0.0467 0.051 Uiso 1 1 calc R . . H33B H 0.7047 0.4894 0.0503 0.051 Uiso 1 1 calc R . . C34 C 0.7801(5) 0.5813(4) 0.0382(3) 0.0590(17) Uani 1 1 d . . . H34A H 0.7647 0.5563 -0.0100 0.089 Uiso 1 1 calc R . . H34B H 0.8607 0.5832 0.0557 0.089 Uiso 1 1 calc R . . H34C H 0.7696 0.6309 0.0517 0.089 Uiso 1 1 calc R . . C35 C 0.3489(5) 0.6968(3) 0.1004(3) 0.0459(14) Uani 1 1 d . . . H35A H 0.2643 0.6953 0.0977 0.055 Uiso 1 1 calc R . . H35B H 0.3565 0.6470 0.0735 0.055 Uiso 1 1 calc R . . C36 C 0.4037(5) 0.7482(4) 0.0718(3) 0.0581(17) Uani 1 1 d . . . H36A H 0.3655 0.7306 0.0257 0.087 Uiso 1 1 calc R . . H36B H 0.4874 0.7499 0.0743 0.087 Uiso 1 1 calc R . . H36C H 0.3934 0.7972 0.0971 0.087 Uiso 1 1 calc R . . O101 O -0.1636(3) 0.4589(2) 0.3568(2) 0.0542(10) Uani 1 1 d . . . O102 O -0.2574(4) 0.5120(2) 0.4316(2) 0.0694(12) Uani 1 1 d . . . N1 N 0.0666(4) 0.4974(3) 0.3794(2) 0.0485(12) Uani 1 1 d . . . H1N H 0.0032 0.4734 0.3487 0.058 Uiso 1 1 calc R . . N2 N -0.1644(4) 0.5047(3) 0.4133(3) 0.0483(12) Uani 1 1 d . . . C37 C 0.2475(5) 0.5461(3) 0.3482(3) 0.0491(14) Uani 1 1 d . . . H37A H 0.2613 0.5934 0.3870 0.059 Uiso 1 1 calc R . . H37B H 0.3242 0.5365 0.3388 0.059 Uiso 1 1 calc R . . C38 C 0.1790(5) 0.4863(3) 0.3617(3) 0.0498(14) Uani 1 1 d . . . H38A H 0.1651 0.4398 0.3220 0.060 Uiso 1 1 calc R . . H38B H 0.2268 0.4817 0.3980 0.060 Uiso 1 1 calc R . . C39 C 0.0536(5) 0.5419(3) 0.4394(3) 0.0439(14) Uani 1 1 d . . . C40 C 0.1531(5) 0.5869(3) 0.4897(3) 0.0490(15) Uani 1 1 d . . . H40 H 0.2291 0.5845 0.4804 0.059 Uiso 1 1 calc R . . C41 C 0.1426(5) 0.6330(3) 0.5504(3) 0.0556(16) Uani 1 1 d . . . H41 H 0.2112 0.6616 0.5827 0.067 Uiso 1 1 calc R . . C42 C 0.0335(6) 0.6393(3) 0.5665(3) 0.0548(15) Uani 1 1 d . . . H42 H 0.0276 0.6725 0.6090 0.066 Uiso 1 1 calc R . . C43 C -0.0648(5) 0.5971(3) 0.5204(3) 0.0496(14) Uani 1 1 d . . . H43 H -0.1397 0.6007 0.5311 0.060 Uiso 1 1 calc R . . C44 C -0.0563(4) 0.5489(3) 0.4579(3) 0.0421(13) Uani 1 1 d . . . O103 O 0.4247(5) 0.7420(4) 0.4905(3) 0.0993(19) Uani 1 1 d . . . O104 O 0.4018(6) 0.8054(6) 0.5874(3) 0.182(4) Uani 1 1 d . . . N3 N 0.5898(4) 0.7928(3) 0.4402(2) 0.0555(13) Uani 1 1 d D . . H3N H 0.529(4) 0.752(2) 0.434(3) 0.067 Uiso 1 1 d D . . N4 N 0.4538(7) 0.7937(6) 0.5424(4) 0.104(3) Uani 1 1 d . . . C45 C 0.5891(4) 0.7247(3) 0.3261(3) 0.0441(13) Uani 1 1 d . . . H45A H 0.6379 0.7144 0.2918 0.053 Uiso 1 1 calc R . . H45B H 0.5659 0.6804 0.3337 0.053 Uiso 1 1 calc R . . C46 C 0.6560(5) 0.7864(3) 0.3880(3) 0.0538(15) Uani 1 1 d . . . H46A H 0.7332 0.7780 0.3999 0.065 Uiso 1 1 calc R . . H46B H 0.6691 0.8321 0.3819 0.065 Uiso 1 1 calc R . . C47 C 0.6234(6) 0.8469(4) 0.5020(3) 0.0643(18) Uani 1 1 d . . . C48 C 0.7241(7) 0.9034(4) 0.5195(4) 0.078(2) Uani 1 1 d . . . H48 H 0.7701 0.9018 0.4870 0.093 Uiso 1 1 calc R . . C49 C 0.7597(9) 0.9599(5) 0.5798(5) 0.108(3) Uani 1 1 d . . . H49 H 0.8262 0.9981 0.5885 0.130 Uiso 1 1 calc R . . C50 C 0.6948(13) 0.9607(6) 0.6299(5) 0.131(5) Uani 1 1 d . . . H50 H 0.7195 0.9992 0.6729 0.157 Uiso 1 1 calc R . . C51 C 0.5947(11) 0.9052(7) 0.6162(5) 0.120(4) Uani 1 1 d . . . H51 H 0.5511 0.9054 0.6493 0.144 Uiso 1 1 calc R . . C52 C 0.5615(8) 0.8504(5) 0.5533(4) 0.085(2) Uani 1 1 d . . . O105 O -0.0185(5) -0.0522(3) 0.0252(3) 0.0829(14) Uani 1 1 d . . . O106 O -0.1177(5) -0.1250(3) 0.0588(3) 0.1069(19) Uani 1 1 d . . . N5 N 0.1378(4) 0.0632(3) 0.1076(3) 0.0591(14) Uani 1 1 d D . . H5N H 0.094(5) 0.033(3) 0.0637(18) 0.071 Uiso 1 1 d D . . N6 N -0.0443(5) -0.0687(3) 0.0711(3) 0.0727(16) Uani 1 1 d . . . C53 C 0.1635(5) 0.1933(3) 0.1414(3) 0.0492(15) Uani 1 1 d . . . H53A H 0.0971 0.1833 0.1059 0.059 Uiso 1 1 calc R . . H53B H 0.1333 0.2006 0.1823 0.059 Uiso 1 1 calc R . . C54 C 0.2204(5) 0.1312(3) 0.1230(4) 0.0642(18) Uani 1 1 d . . . H54A H 0.2562 0.1272 0.0842 0.077 Uiso 1 1 calc R . . H54B H 0.2837 0.1406 0.1599 0.077 Uiso 1 1 calc R . . C55 C 0.0994(5) 0.0416(3) 0.1544(3) 0.0558(16) Uani 1 1 d . . . C56 C 0.1458(6) 0.0820(4) 0.2218(4) 0.0711(19) Uani 1 1 d . . . H56 H 0.2041 0.1260 0.2359 0.085 Uiso 1 1 calc R . . C57 C 0.1094(8) 0.0597(5) 0.2674(4) 0.090(2) Uani 1 1 d . . . H57 H 0.1442 0.0881 0.3125 0.108 Uiso 1 1 calc R . . C58 C 0.0224(8) -0.0038(5) 0.2500(5) 0.089(2) Uani 1 1 d . . . H58 H -0.0031 -0.0182 0.2825 0.107 Uiso 1 1 calc R . . C59 C -0.0241(6) -0.0439(4) 0.1856(5) 0.075(2) Uani 1 1 d . . . H59 H -0.0824 -0.0877 0.1727 0.089 Uiso 1 1 calc R . . C60 C 0.0112(5) -0.0226(3) 0.1371(3) 0.0581(17) Uani 1 1 d . . . O109 O 0.9122(4) 0.8367(2) 0.3401(2) 0.0668(12) Uani 1 1 d . . . O110 O 0.9517(7) 0.9381(3) 0.4227(3) 0.137(3) Uani 1 1 d . . . N9 N 0.9744(4) 0.7239(2) 0.3460(2) 0.0483(12) Uani 1 1 d . . . H9N H 0.9431 0.7423 0.3209 0.058 Uiso 1 1 calc R . . N10 N 0.9564(5) 0.8740(3) 0.3984(3) 0.0618(14) Uani 1 1 d . . . C69 C 0.8658(5) 0.5977(3) 0.3108(3) 0.0511(15) Uani 1 1 d . . . H69A H 0.8723 0.5466 0.2900 0.061 Uiso 1 1 calc R . . H69B H 0.8508 0.6082 0.3557 0.061 Uiso 1 1 calc R . . C70 C 0.9753(5) 0.6472(3) 0.3144(3) 0.0558(16) Uani 1 1 d . . . H70A H 1.0409 0.6386 0.3391 0.067 Uiso 1 1 calc R . . H70B H 0.9897 0.6355 0.2692 0.067 Uiso 1 1 calc R . . C71 C 1.0165(4) 0.7691(3) 0.4093(3) 0.0446(14) Uani 1 1 d . . . C72 C 1.0723(5) 0.7478(3) 0.4547(3) 0.0551(16) Uani 1 1 d . . . H72 H 1.0773 0.6985 0.4397 0.066 Uiso 1 1 calc R . . C73 C 1.1190(6) 0.7936(4) 0.5180(3) 0.0638(18) Uani 1 1 d . . . H73 H 1.1575 0.7760 0.5456 0.077 Uiso 1 1 calc R . . C74 C 1.1121(6) 0.8669(4) 0.5442(3) 0.0711(19) Uani 1 1 d . . . H74 H 1.1445 0.8988 0.5891 0.085 Uiso 1 1 calc R . . C75 C 1.0576(6) 0.8901(3) 0.5033(3) 0.0630(17) Uani 1 1 d . . . H75 H 1.0514 0.9393 0.5199 0.076 Uiso 1 1 calc R . . C76 C 1.0101(5) 0.8435(3) 0.4373(3) 0.0490(14) Uani 1 1 d . . . O111 O 0.5309(4) 0.4312(2) 0.5187(2) 0.0689(13) Uani 1 1 d . . . O112 O 0.4674(4) 0.3923(2) 0.5885(2) 0.0640(12) Uani 1 1 d . . . N11 N 0.4181(4) 0.3738(3) 0.3953(2) 0.0510(12) Uani 1 1 d D . . H11N H 0.474(4) 0.412(3) 0.431(2) 0.061 Uiso 1 1 d D . . N12 N 0.4572(4) 0.3906(3) 0.5324(2) 0.0499(12) Uani 1 1 d . . . C77 C 0.4931(5) 0.4202(3) 0.3203(3) 0.0422(13) Uani 1 1 d . . . H77A H 0.4859 0.4700 0.3474 0.051 Uiso 1 1 calc R . . H77B H 0.5729 0.4159 0.3336 0.051 Uiso 1 1 calc R . . C78 C 0.4011(5) 0.3636(3) 0.3270(3) 0.0451(14) Uani 1 1 d . . . H78A H 0.3221 0.3687 0.3133 0.054 Uiso 1 1 calc R . . H78B H 0.4076 0.3142 0.2982 0.054 Uiso 1 1 calc R . . C79 C 0.3437(5) 0.3343(3) 0.4171(3) 0.0420(13) Uani 1 1 d . . . C80 C 0.2421(5) 0.2831(3) 0.3743(3) 0.0497(14) Uani 1 1 d . . . H80 H 0.2284 0.2757 0.3295 0.060 Uiso 1 1 calc R . . C81 C 0.1620(5) 0.2435(3) 0.3950(3) 0.0539(15) Uani 1 1 d . . . H81 H 0.0942 0.2100 0.3646 0.065 Uiso 1 1 calc R . . C82 C 0.1800(5) 0.2522(3) 0.4603(3) 0.0551(16) Uani 1 1 d . . . H82 H 0.1257 0.2241 0.4743 0.066 Uiso 1 1 calc R . . C83 C 0.2768(5) 0.3019(3) 0.5039(3) 0.0513(15) Uani 1 1 d . . . H83 H 0.2888 0.3091 0.5486 0.062 Uiso 1 1 calc R . . C84 C 0.3572(5) 0.3416(3) 0.4829(3) 0.0442(13) Uani 1 1 d . . . O113 O 0.8482(5) 1.1689(3) 0.3130(2) 0.0835(15) Uani 1 1 d . . . O114 O 0.9391(4) 1.2139(3) 0.2549(3) 0.0838(15) Uani 1 1 d . . . N13 N 0.7011(4) 1.0404(3) 0.2570(3) 0.0591(14) Uani 1 1 d D . . H13N H 0.741(5) 1.083(3) 0.296(2) 0.071 Uiso 1 1 d D . . N14 N 0.8666(4) 1.1646(3) 0.2585(3) 0.0600(14) Uani 1 1 d . . . C85 C 0.6799(5) 0.9146(3) 0.2457(4) 0.0623(18) Uani 1 1 d . . . H85A H 0.7297 0.9120 0.2126 0.075 Uiso 1 1 calc R . . H85B H 0.7298 0.9212 0.2868 0.075 Uiso 1 1 calc R . . C86 C 0.6216(6) 0.9784(3) 0.2589(4) 0.075(2) Uani 1 1 d . . . H86A H 0.5495 0.9628 0.2253 0.090 Uiso 1 1 calc R . . H86B H 0.5992 0.9931 0.3027 0.090 Uiso 1 1 calc R . . C87 C 0.7273(5) 1.0428(3) 0.2001(3) 0.0530(15) Uani 1 1 d . . . C88 C 0.6747(6) 0.9852(4) 0.1390(4) 0.072(2) Uani 1 1 d . . . H88 H 0.6191 0.9445 0.1370 0.087 Uiso 1 1 calc R . . C89 C 0.7029(8) 0.9868(6) 0.0814(5) 0.105(3) Uani 1 1 d . . . H89 H 0.6673 0.9471 0.0402 0.126 Uiso 1 1 calc R . . C90 C 0.7849(8) 1.0476(5) 0.0835(4) 0.090(2) Uani 1 1 d . . . H90 H 0.8040 1.0484 0.0438 0.108 Uiso 1 1 calc R . . C91 C 0.8341(6) 1.1024(4) 0.1400(4) 0.0701(19) Uani 1 1 d . . . H91 H 0.8886 1.1428 0.1408 0.084 Uiso 1 1 calc R . . C92 C 0.8078(5) 1.1028(3) 0.1998(3) 0.0519(15) Uani 1 1 d . . . O115 O 1.3223(4) 0.9266(2) 0.2202(3) 0.0699(13) Uani 1 1 d . . . O116 O 1.3623(5) 0.9796(3) 0.1568(3) 0.115(2) Uani 1 1 d . . . N15 N 1.1633(3) 0.8042(2) 0.1759(2) 0.0401(11) Uani 1 1 d D . . H15N H 1.212(4) 0.842(2) 0.2146(19) 0.048 Uiso 1 1 d D . . N16 N 1.3061(4) 0.9284(3) 0.1653(3) 0.0651(15) Uani 1 1 d . . . C93 C 0.9683(4) 0.7713(3) 0.1947(3) 0.0448(13) Uani 1 1 d . . . H93A H 0.9804 0.8151 0.2367 0.054 Uiso 1 1 calc R . . H93B H 0.9389 0.7828 0.1582 0.054 Uiso 1 1 calc R . . C94 C 1.0821(4) 0.7481(3) 0.1852(3) 0.0411(13) Uani 1 1 d . . . H94A H 1.1159 0.7421 0.2243 0.049 Uiso 1 1 calc R . . H94B H 1.0677 0.7009 0.1462 0.049 Uiso 1 1 calc R . . C95 C 1.1533(4) 0.8132(3) 0.1192(3) 0.0387(13) Uani 1 1 d . . . C96 C 1.0734(5) 0.7617(3) 0.0621(3) 0.0547(15) Uani 1 1 d . . . H96 H 1.0231 0.7215 0.0642 0.066 Uiso 1 1 calc R . . C97 C 1.0663(6) 0.7680(4) 0.0044(4) 0.0727(19) Uani 1 1 d . . . H97 H 1.0113 0.7320 -0.0329 0.087 Uiso 1 1 calc R . . C98 C 1.1359(7) 0.8248(5) -0.0021(4) 0.078(2) Uani 1 1 d . . . H98 H 1.1291 0.8280 -0.0432 0.094 Uiso 1 1 calc R . . C99 C 1.2151(7) 0.8765(5) 0.0515(4) 0.075(2) Uani 1 1 d . . . H99 H 1.2649 0.9157 0.0476 0.090 Uiso 1 1 calc R . . C100 C 1.2231(5) 0.8720(3) 0.1118(3) 0.0511(15) Uani 1 1 d . . . C61 C -0.1275(4) 0.3382(3) 0.1858(3) 0.0557(17) Uani 1 1 d . B . H61A H -0.1081 0.3270 0.2240 0.067 Uiso 1 1 calc R . . H61B H -0.1301 0.2948 0.1450 0.067 Uiso 1 1 calc R . . C62 C -0.2445(5) 0.3584(3) 0.1850(4) 0.077(2) Uani 1 1 d . . . H62A H -0.2463 0.3918 0.1634 0.092 Uiso 1 1 calc R A 1 H62B H -0.2561 0.3836 0.2308 0.092 Uiso 1 1 calc R A 1 N7A N -0.3420(7) 0.2890(5) 0.1475(4) 0.060(2) Uiso 0.599(6) 1 d P B 1 H7A H -0.3760 0.2765 0.1066 0.072 Uiso 0.599(6) 1 calc PR B 1 N8A N -0.4545(19) 0.1324(9) 0.0759(10) 0.193(11) Uiso 0.599(6) 1 d PD B 1 O50A O -0.4535(8) 0.1687(6) 0.0435(5) 0.100(3) Uiso 0.599(6) 1 d PD B 1 O51A O -0.5309(9) 0.0748(6) 0.0579(5) 0.104(3) Uiso 0.599(6) 1 d PD B 1 N7B N -0.3165(9) 0.3147(6) 0.2195(5) 0.044(3) Uiso 0.401(6) 1 d P B 2 H7B H -0.3176 0.3348 0.2619 0.053 Uiso 0.401(6) 1 calc PR B 2 N8B N -0.4538(12) 0.2237(7) 0.2675(6) 0.068(4) Uiso 0.401(6) 1 d PD B 2 O50B O -0.3911(9) 0.2821(6) 0.3113(5) 0.067(3) Uiso 0.401(6) 1 d PD B 2 O51B O -0.5313(11) 0.1894(7) 0.2844(6) 0.090(4) Uiso 0.401(6) 1 d PD B 2 C63 C -0.3745(3) 0.24682(19) 0.18103(18) 0.0456(13) Uiso 1 1 d G . . C64A C -0.3502(3) 0.2780(2) 0.24952(18) 0.057(3) Uiso 0.599(6) 1 d PG B 1 H64A H -0.3051 0.3267 0.2733 0.068 Uiso 0.599(6) 1 calc PR B 1 C65A C -0.3918(3) 0.2378(3) 0.28327(17) 0.068(3) Uiso 0.599(6) 1 d PG B 1 H65A H -0.3752 0.2591 0.3301 0.082 Uiso 0.599(6) 1 calc PR B 1 C66A C -0.4578(3) 0.1665(3) 0.2485(2) 0.069(3) Uiso 0.599(6) 1 d PG B 1 H66A H -0.4862 0.1391 0.2716 0.082 Uiso 0.599(6) 1 calc PR B 1 C67A C -0.4821(3) 0.1354(2) 0.1801(2) 0.065(15) Uiso 0.599(6) 1 d PG B 1 H67A H -0.5272 0.0867 0.1563 0.078 Uiso 0.599(6) 1 calc PR B 1 C68A C -0.4405(3) 0.1755(2) 0.14629(17) 0.049(3) Uiso 0.599(6) 1 d PG B 1 C64B C -0.3675(3) 0.2187(3) 0.11202(17) 0.056(4) Uiso 0.401(6) 1 d PG B 2 H64B H -0.3168 0.2409 0.0917 0.067 Uiso 0.401(6) 1 calc PR B 2 C65B C -0.4659(4) 0.1402(3) 0.07578(17) 0.057(6) Uiso 0.401(6) 1 d PR B 2 H65B H -0.5117 0.1256 0.0334 0.068 Uiso 0.401(6) 1 calc PR B 2 C66B C -0.4788(3) 0.0992(2) 0.1067(2) 0.094(6) Uiso 0.401(6) 1 d PR B 2 H66B H -0.4859 0.0483 0.0847 0.112 Uiso 0.401(6) 1 calc PR B 2 C67B C -0.4821(3) 0.1354(2) 0.1800(2) 0.10(3) Uiso 0.401(6) 1 d PR B 2 H67B H -0.5179 0.1132 0.2055 0.120 Uiso 0.401(6) 1 calc PR B 2 C68B C -0.4316(3) 0.19577(19) 0.19817(17) 0.049(4) Uiso 0.401(6) 1 d PR B 2 O200 O 1.2539(6) 0.8516(3) 0.3242(3) 0.115(2) Uani 1 1 d . B . C200 C 1.3379(8) 0.8724(4) 0.3650(4) 0.078(2) Uani 1 1 d . . . C201 C 1.4556(8) 0.9107(5) 0.3641(5) 0.115(3) Uani 1 1 d . B . H20A H 1.4513 0.9234 0.3264 0.172 Uiso 1 1 calc R . . H20B H 1.5096 0.8789 0.3603 0.172 Uiso 1 1 calc R . . H20C H 1.4839 0.9553 0.4050 0.172 Uiso 1 1 calc R . . C202 C 1.3223(4) 0.8596(6) 0.4227(5) 0.169(6) Uani 1 1 d G B . H20D H 1.2405 0.8564 0.4277 0.253 Uiso 1 1 calc R . . H20E H 1.3732 0.8998 0.4619 0.253 Uiso 1 1 calc R . . H20F H 1.3426 0.8138 0.4176 0.253 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 O4 0.042(2) 0.043(2) 0.049(2) 0.0327(18) 0.0139(17) 0.0043(16) O6 0.0352(19) 0.0354(19) 0.048(2) 0.0195(17) 0.0072(16) 0.0015(16) O11 0.0277(18) 0.034(2) 0.073(3) 0.0281(19) 0.0063(17) 0.0063(15) O13 0.0314(19) 0.037(2) 0.091(3) 0.034(2) 0.0231(19) 0.0086(16) O18 0.0365(19) 0.0349(19) 0.049(2) 0.0240(17) -0.0001(16) -0.0037(15) O20 0.042(2) 0.043(2) 0.040(2) 0.0224(17) 0.0051(16) -0.0087(16) O25 0.037(2) 0.036(2) 0.093(3) 0.038(2) 0.0223(19) 0.0072(17) O27 0.0277(18) 0.045(2) 0.074(3) 0.041(2) 0.0193(17) 0.0075(16) C1 0.030(3) 0.029(3) 0.040(3) 0.018(2) 0.013(2) 0.009(2) C2 0.033(3) 0.036(3) 0.044(3) 0.024(2) 0.013(2) 0.012(2) C3 0.029(3) 0.032(3) 0.044(3) 0.020(2) 0.016(2) 0.011(2) C4 0.031(3) 0.032(3) 0.042(3) 0.021(2) 0.016(2) 0.007(2) C5 0.036(3) 0.039(3) 0.040(3) 0.024(3) 0.010(2) 0.004(2) C6 0.033(3) 0.029(3) 0.045(3) 0.016(2) 0.014(2) 0.006(2) C7 0.030(3) 0.037(3) 0.042(3) 0.023(2) 0.011(2) 0.011(2) C8 0.027(3) 0.033(3) 0.040(3) 0.019(2) 0.003(2) 0.002(2) C9 0.026(3) 0.032(3) 0.039(3) 0.017(2) 0.007(2) 0.006(2) C10 0.027(3) 0.033(3) 0.036(3) 0.013(2) 0.005(2) 0.004(2) C11 0.031(3) 0.029(3) 0.045(3) 0.016(2) 0.003(2) 0.007(2) C12 0.035(3) 0.031(3) 0.050(3) 0.020(2) 0.008(2) 0.005(2) C13 0.025(3) 0.034(3) 0.048(3) 0.016(2) 0.009(2) 0.006(2) C14 0.029(3) 0.030(3) 0.045(3) 0.016(2) 0.009(2) 0.008(2) C15 0.024(2) 0.035(3) 0.037(3) 0.015(2) 0.008(2) 0.009(2) C16 0.033(3) 0.032(3) 0.038(3) 0.019(2) 0.004(2) 0.013(2) C17 0.029(3) 0.034(3) 0.037(3) 0.019(2) 0.007(2) 0.008(2) C18 0.029(3) 0.025(2) 0.040(3) 0.014(2) 0.007(2) 0.003(2) C19 0.033(3) 0.034(3) 0.039(3) 0.020(2) 0.005(2) 0.002(2) C20 0.029(3) 0.032(3) 0.049(3) 0.023(3) 0.018(2) 0.010(2) C21 0.026(2) 0.041(3) 0.038(3) 0.024(2) 0.012(2) 0.011(2) C22 0.033(3) 0.036(3) 0.041(3) 0.026(2) 0.013(2) 0.009(2) C23 0.030(3) 0.039(3) 0.035(3) 0.020(2) 0.009(2) 0.005(2) C26 0.037(3) 0.037(3) 0.070(4) 0.035(3) 0.017(3) 0.004(2) C24 0.038(3) 0.034(3) 0.046(3) 0.028(2) 0.017(2) 0.008(2) C25 0.041(3) 0.038(3) 0.063(4) 0.037(3) 0.023(3) 0.017(2) C27 0.034(3) 0.043(3) 0.048(3) 0.029(3) 0.023(2) 0.013(2) C28 0.033(3) 0.034(3) 0.046(3) 0.024(2) 0.017(2) 0.014(2) C29 0.035(3) 0.039(3) 0.056(4) 0.024(3) 0.008(2) 0.010(2) C30 0.059(4) 0.043(3) 0.073(4) 0.029(3) -0.014(3) -0.002(3) C31 0.041(3) 0.044(3) 0.039(3) 0.007(3) 0.010(2) 0.009(3) C32 0.051(4) 0.048(4) 0.060(4) 0.002(3) 0.011(3) -0.006(3) C33 0.037(3) 0.053(3) 0.048(4) 0.027(3) 0.017(2) 0.018(3) C34 0.065(4) 0.085(5) 0.056(4) 0.047(4) 0.034(3) 0.035(4) C35 0.043(3) 0.056(4) 0.057(4) 0.036(3) 0.020(3) 0.021(3) C36 0.055(4) 0.078(4) 0.074(4) 0.058(4) 0.029(3) 0.025(3) O101 0.054(2) 0.056(3) 0.049(3) 0.026(2) 0.0016(19) 0.001(2) O102 0.042(2) 0.073(3) 0.084(3) 0.026(3) 0.008(2) 0.012(2) N1 0.047(3) 0.053(3) 0.049(3) 0.032(3) 0.006(2) -0.002(2) N2 0.050(3) 0.050(3) 0.054(3) 0.034(3) 0.008(2) 0.009(2) C37 0.044(3) 0.062(4) 0.051(4) 0.038(3) 0.008(3) 0.004(3) C38 0.045(3) 0.052(4) 0.067(4) 0.039(3) 0.016(3) 0.010(3) C39 0.050(3) 0.040(3) 0.044(4) 0.028(3) 0.004(3) -0.006(3) C40 0.045(3) 0.055(4) 0.054(4) 0.039(3) 0.004(3) -0.004(3) C41 0.055(4) 0.047(4) 0.062(4) 0.031(3) -0.006(3) -0.004(3) C42 0.073(4) 0.039(3) 0.051(4) 0.021(3) 0.007(3) 0.006(3) C43 0.062(4) 0.039(3) 0.055(4) 0.029(3) 0.008(3) 0.007(3) C44 0.033(3) 0.044(3) 0.048(4) 0.026(3) -0.001(2) -0.003(2) O103 0.084(4) 0.150(6) 0.096(5) 0.075(4) 0.045(4) 0.037(4) O104 0.134(6) 0.368(14) 0.089(5) 0.126(7) 0.062(5) 0.077(7) N3 0.053(3) 0.063(3) 0.045(3) 0.020(3) 0.012(2) 0.008(3) N4 0.106(6) 0.181(9) 0.064(5) 0.071(6) 0.038(5) 0.071(6) C45 0.039(3) 0.043(3) 0.048(3) 0.020(3) 0.005(2) 0.005(2) C46 0.050(3) 0.050(4) 0.060(4) 0.024(3) 0.010(3) 0.006(3) C47 0.072(4) 0.075(5) 0.047(4) 0.020(4) 0.006(3) 0.037(4) C48 0.093(5) 0.049(4) 0.066(5) 0.007(4) -0.012(4) 0.013(4) C49 0.143(8) 0.078(6) 0.079(7) 0.013(5) -0.027(6) 0.042(6) C50 0.194(12) 0.109(9) 0.060(7) -0.005(6) -0.028(8) 0.093(9) C51 0.146(9) 0.161(11) 0.060(7) 0.024(7) 0.017(6) 0.110(9) C52 0.094(6) 0.118(7) 0.060(5) 0.034(5) 0.019(4) 0.073(6) O105 0.104(4) 0.057(3) 0.078(4) 0.028(3) 0.002(3) 0.006(3) O106 0.086(4) 0.055(3) 0.145(5) 0.029(3) 0.009(3) -0.027(3) N5 0.053(3) 0.033(3) 0.090(4) 0.030(3) 0.005(3) 0.002(2) N6 0.056(3) 0.039(3) 0.103(5) 0.021(3) 0.000(3) -0.004(3) C53 0.038(3) 0.027(3) 0.078(4) 0.022(3) 0.006(3) 0.002(2) C54 0.045(3) 0.044(4) 0.111(6) 0.041(4) 0.015(3) 0.008(3) C55 0.045(3) 0.037(3) 0.087(5) 0.029(3) 0.004(3) 0.012(3) C56 0.076(5) 0.046(4) 0.086(6) 0.032(4) -0.012(4) 0.007(3) C57 0.133(7) 0.077(6) 0.064(5) 0.029(4) -0.003(5) 0.046(6) C58 0.104(6) 0.081(6) 0.106(7) 0.054(6) 0.028(5) 0.040(5) C59 0.071(5) 0.058(4) 0.119(7) 0.054(5) 0.034(5) 0.024(4) C60 0.048(3) 0.034(3) 0.086(5) 0.021(3) 0.011(3) 0.008(3) O109 0.081(3) 0.058(3) 0.061(3) 0.025(3) 0.003(2) 0.021(2) O110 0.244(8) 0.053(3) 0.087(4) 0.006(3) -0.034(4) 0.065(4) N9 0.047(3) 0.035(3) 0.057(3) 0.015(2) 0.009(2) 0.008(2) N10 0.082(4) 0.036(3) 0.058(4) 0.011(3) 0.007(3) 0.016(3) C69 0.042(3) 0.040(3) 0.066(4) 0.024(3) -0.004(3) 0.001(3) C70 0.043(3) 0.039(3) 0.074(4) 0.015(3) 0.009(3) 0.006(3) C71 0.037(3) 0.043(3) 0.056(4) 0.024(3) 0.012(3) 0.006(3) C72 0.056(4) 0.043(3) 0.070(5) 0.029(3) 0.013(3) 0.007(3) C73 0.064(4) 0.068(5) 0.068(5) 0.045(4) 0.007(3) 0.002(3) C74 0.089(5) 0.057(4) 0.057(4) 0.022(4) -0.001(4) 0.005(4) C75 0.083(5) 0.043(4) 0.056(4) 0.014(3) 0.012(3) 0.015(3) C76 0.055(3) 0.043(3) 0.050(4) 0.023(3) 0.008(3) 0.008(3) O111 0.062(3) 0.074(3) 0.062(3) 0.039(2) -0.005(2) -0.020(2) O112 0.080(3) 0.072(3) 0.047(3) 0.036(2) 0.007(2) 0.011(2) N11 0.051(3) 0.057(3) 0.043(3) 0.030(3) 0.003(2) -0.012(2) N12 0.056(3) 0.046(3) 0.048(3) 0.023(2) 0.009(2) 0.006(2) C77 0.045(3) 0.044(3) 0.039(3) 0.025(3) 0.003(2) 0.000(3) C78 0.043(3) 0.051(3) 0.044(3) 0.027(3) 0.010(2) -0.003(3) C79 0.046(3) 0.044(3) 0.043(3) 0.026(3) 0.011(3) 0.008(3) C80 0.052(3) 0.046(3) 0.048(4) 0.022(3) 0.012(3) 0.001(3) C81 0.047(3) 0.048(4) 0.060(4) 0.022(3) 0.011(3) -0.002(3) C82 0.050(4) 0.061(4) 0.071(5) 0.042(4) 0.027(3) 0.012(3) C83 0.055(4) 0.060(4) 0.061(4) 0.042(3) 0.024(3) 0.020(3) C84 0.046(3) 0.042(3) 0.047(4) 0.023(3) 0.009(3) 0.008(3) O113 0.106(4) 0.063(3) 0.064(3) 0.024(3) 0.016(3) -0.015(3) O114 0.077(3) 0.061(3) 0.113(4) 0.047(3) 0.016(3) -0.008(3) N13 0.053(3) 0.038(3) 0.086(4) 0.029(3) 0.022(3) 0.000(2) N14 0.058(3) 0.039(3) 0.079(4) 0.028(3) 0.008(3) -0.001(3) C85 0.047(3) 0.040(3) 0.110(5) 0.041(4) 0.021(3) 0.007(3) C86 0.053(4) 0.039(3) 0.145(7) 0.045(4) 0.041(4) 0.011(3) C87 0.045(3) 0.041(3) 0.076(5) 0.030(3) 0.004(3) 0.009(3) C88 0.055(4) 0.049(4) 0.094(6) 0.020(4) -0.008(4) 0.006(3) C89 0.112(7) 0.104(8) 0.072(6) 0.020(5) -0.025(5) 0.032(6) C90 0.118(7) 0.089(6) 0.070(6) 0.044(5) 0.004(5) 0.026(6) C91 0.069(4) 0.067(5) 0.075(5) 0.035(4) 0.001(4) 0.016(4) C92 0.045(3) 0.053(4) 0.063(4) 0.031(3) 0.010(3) 0.009(3) O115 0.058(3) 0.057(3) 0.078(3) 0.021(3) 0.013(2) -0.007(2) O116 0.086(4) 0.087(4) 0.185(6) 0.096(4) 0.008(4) -0.023(3) N15 0.031(2) 0.039(3) 0.050(3) 0.021(2) 0.009(2) 0.0024(19) N16 0.046(3) 0.054(3) 0.105(5) 0.043(4) 0.024(3) 0.005(3) C93 0.033(3) 0.043(3) 0.063(4) 0.029(3) 0.014(3) 0.003(2) C94 0.032(3) 0.042(3) 0.059(4) 0.029(3) 0.019(2) 0.007(2) C95 0.028(3) 0.045(3) 0.053(4) 0.028(3) 0.014(2) 0.010(2) C96 0.054(4) 0.057(4) 0.056(4) 0.027(3) 0.010(3) 0.015(3) C97 0.083(5) 0.072(5) 0.060(5) 0.024(4) 0.010(4) 0.026(4) C98 0.093(6) 0.100(6) 0.077(6) 0.061(5) 0.038(5) 0.040(5) C99 0.080(5) 0.092(6) 0.097(6) 0.071(5) 0.047(5) 0.037(5) C100 0.040(3) 0.047(3) 0.076(4) 0.034(3) 0.023(3) 0.010(3) C61 0.033(3) 0.038(3) 0.108(5) 0.040(3) 0.029(3) 0.006(3) C62 0.039(3) 0.049(4) 0.164(7) 0.062(5) 0.040(4) 0.009(3) O200 0.118(5) 0.083(4) 0.100(5) 0.025(4) -0.038(4) -0.015(4) C200 0.094(6) 0.058(4) 0.085(6) 0.032(4) 0.019(5) 0.019(4) C201 0.118(7) 0.092(6) 0.179(10) 0.080(7) 0.084(7) 0.043(6) C202 0.105(7) 0.322(18) 0.229(13) 0.237(14) 0.090(8) 0.091(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 O4 C4 1.375(5) . ? O4 C37 1.425(6) . ? O6 C6 1.389(6) . ? O6 C45 1.444(6) . ? O11 C11 1.374(6) . ? O11 C53 1.426(6) . ? O13 C13 1.393(6) . ? O13 C61 1.405(6) . ? O18 C18 1.396(5) . ? O18 C69 1.409(6) . ? O20 C20 1.379(5) . ? O20 C77 1.426(6) . ? O25 C25 1.387(6) . ? O25 C85 1.412(6) . ? O27 C27 1.393(6) . ? O27 C93 1.437(6) . ? C1 C6 1.387(7) . ? C1 C2 1.398(7) . ? C1 C28 1.525(6) . ? C2 C3 1.391(6) . ? C3 C4 1.399(7) . ? C3 C7 1.507(7) . ? C4 C5 1.380(7) . ? C5 C6 1.381(6) . ? C7 C29 1.531(7) . ? C7 C8 1.535(7) . ? C8 C13 1.377(6) . ? C8 C9 1.384(6) . ? C9 C10 1.388(7) . ? C10 C11 1.399(6) . ? C10 C14 1.528(6) . ? C11 C12 1.388(7) . ? C12 C13 1.391(7) . ? C14 C31 1.519(7) . ? C14 C15 1.530(7) . ? C15 C20 1.389(7) . ? C15 C16 1.402(6) . ? C16 C17 1.389(7) . ? C17 C18 1.390(7) . ? C17 C21 1.532(6) . ? C18 C19 1.383(6) . ? C19 C20 1.382(7) . ? C21 C33 1.523(7) . ? C21 C22 1.531(7) . ? C22 C27 1.383(7) . ? C22 C23 1.390(7) . ? C23 C24 1.380(7) . ? C26 C25 1.379(7) . ? C26 C27 1.395(7) . ? C24 C25 1.394(7) . ? C24 C28 1.527(7) . ? C28 C35 1.522(7) . ? C29 C30 1.526(7) . ? C31 C32 1.508(7) . ? C33 C34 1.527(7) . ? C35 C36 1.530(7) . ? O101 N2 1.252(6) . ? O102 N2 1.228(6) . ? N1 C39 1.343(7) . ? N1 C38 1.459(7) . ? N2 C44 1.438(7) . ? C37 C38 1.503(7) . ? C39 C44 1.421(7) . ? C39 C40 1.425(8) . ? C40 C41 1.355(8) . ? C41 C42 1.391(8) . ? C42 C43 1.364(8) . ? C43 C44 1.392(8) . ? O103 N4 1.193(9) . ? O104 N4 1.206(8) . ? N3 C47 1.355(8) . ? N3 C46 1.457(7) . ? N4 C52 1.491(12) . ? C45 C46 1.482(8) . ? C47 C48 1.405(10) . ? C47 C52 1.416(10) . ? C48 C49 1.353(11) . ? C49 C50 1.426(15) . ? C50 C51 1.402(15) . ? C51 C52 1.377(12) . ? O105 N6 1.259(7) . ? O106 N6 1.229(6) . ? N5 C55 1.383(8) . ? N5 C54 1.448(7) . ? N6 C60 1.415(9) . ? C53 C54 1.485(8) . ? C55 C56 1.399(9) . ? C55 C60 1.417(8) . ? C56 C57 1.358(10) . ? C57 C58 1.398(12) . ? C58 C59 1.345(11) . ? C59 C60 1.402(9) . ? O109 N10 1.224(6) . ? O110 N10 1.227(7) . ? N9 C71 1.336(7) . ? N9 C70 1.456(7) . ? N10 C76 1.424(8) . ? C69 C70 1.472(7) . ? C71 C72 1.410(8) . ? C71 C76 1.428(8) . ? C72 C73 1.347(9) . ? C73 C74 1.408(9) . ? C74 C75 1.352(9) . ? C75 C76 1.398(8) . ? O111 N12 1.246(6) . ? O112 N12 1.242(6) . ? N11 C79 1.351(6) . ? N11 C78 1.454(7) . ? N12 C84 1.440(7) . ? C77 C78 1.511(7) . ? C79 C80 1.410(8) . ? C79 C84 1.418(7) . ? C80 C81 1.378(7) . ? C81 C82 1.397(8) . ? C82 C83 1.370(8) . ? C83 C84 1.385(7) . ? O113 N14 1.239(6) . ? O114 N14 1.242(6) . ? N13 C87 1.366(8) . ? N13 C86 1.464(7) . ? N14 C92 1.419(8) . ? C85 C86 1.532(8) . ? C87 C88 1.399(9) . ? C87 C92 1.422(8) . ? C88 C89 1.383(11) . ? C89 C90 1.422(12) . ? C90 C91 1.306(10) . ? C91 C92 1.412(9) . ? O115 N16 1.246(7) . ? O116 N16 1.236(6) . ? N15 C95 1.358(6) . ? N15 C94 1.463(6) . ? N16 C100 1.416(8) . ? C93 C94 1.516(7) . ? C95 C96 1.408(8) . ? C95 C100 1.415(7) . ? C96 C97 1.352(9) . ? C97 C98 1.371(10) . ? C98 C99 1.364(11) . ? C99 C100 1.392(9) . ? C61 C62 1.515(8) . ? C62 N7A 1.530(10) . ? C62 N7B 1.597(12) . ? N7A C63 1.390(9) . ? N8A O50A 1.231(14) . ? N8A O51A 1.246(13) . ? N8A C68A 1.45(2) . ? N7B C63 1.324(11) . ? N8B O51B 1.242(12) . ? N8B O50B 1.250(12) . ? N8B C68B 1.505(14) . ? C63 C68B 1.3534 . ? C63 C64A 1.3900 . ? C63 C68A 1.3900 . ? C63 C64B 1.4455 . ? C64A C65A 1.3900 . ? C65A C66A 1.3900 . ? C66A C67A 1.3900 . ? C67A C68A 1.3900 . ? C64B C65B 1.6507 . ? C65B C66B 1.2876 . ? C66B C67B 1.5287 . ? C67B C68B 1.1628 . ? O200 C200 1.168(9) . ? C200 C202 1.448(11) . ? C200 C201 1.479(11) . ? 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 C4 O4 C37 116.7(4) . . ? C6 O6 C45 115.7(4) . . ? C11 O11 C53 117.3(4) . . ? C13 O13 C61 117.9(4) . . ? C18 O18 C69 117.1(4) . . ? C20 O20 C77 119.4(4) . . ? C25 O25 C85 117.7(4) . . ? C27 O27 C93 115.6(4) . . ? C6 C1 C2 116.0(4) . . ? C6 C1 C28 121.2(4) . . ? C2 C1 C28 122.8(4) . . ? C3 C2 C1 124.2(5) . . ? C2 C3 C4 116.7(4) . . ? C2 C3 C7 124.8(5) . . ? C4 C3 C7 118.4(4) . . ? O4 C4 C5 123.1(4) . . ? O4 C4 C3 115.9(4) . . ? C5 C4 C3 121.0(4) . . ? C4 C5 C6 119.9(5) . . ? C5 C6 C1 122.1(5) . . ? C5 C6 O6 118.7(5) . . ? C1 C6 O6 119.1(4) . . ? C3 C7 C29 113.5(4) . . ? C3 C7 C8 109.5(4) . . ? C29 C7 C8 112.1(4) . . ? C13 C8 C9 117.2(4) . . ? C13 C8 C7 121.6(4) . . ? C9 C8 C7 121.2(4) . . ? C8 C9 C10 124.2(4) . . ? C9 C10 C11 116.6(4) . . ? C9 C10 C14 121.9(4) . . ? C11 C10 C14 121.4(4) . . ? O11 C11 C12 121.3(4) . . ? O11 C11 C10 117.7(4) . . ? C12 C11 C10 121.0(4) . . ? C11 C12 C13 119.5(4) . . ? C8 C13 C12 121.4(4) . . ? C8 C13 O13 117.1(4) . . ? C12 C13 O13 121.4(4) . . ? C31 C14 C10 112.1(4) . . ? C31 C14 C15 112.7(4) . . ? C10 C14 C15 111.5(4) . . ? C20 C15 C16 116.8(4) . . ? C20 C15 C14 120.1(4) . . ? C16 C15 C14 123.1(4) . . ? C17 C16 C15 122.9(5) . . ? C16 C17 C18 117.2(4) . . ? C16 C17 C21 122.9(4) . . ? C18 C17 C21 119.9(4) . . ? C19 C18 C17 122.0(4) . . ? C19 C18 O18 120.9(4) . . ? C17 C18 O18 117.0(4) . . ? C20 C19 C18 118.7(5) . . ? O20 C20 C19 124.1(5) . . ? O20 C20 C15 113.7(4) . . ? C19 C20 C15 122.2(4) . . ? C33 C21 C22 110.0(4) . . ? C33 C21 C17 114.1(4) . . ? C22 C21 C17 110.5(4) . . ? C27 C22 C23 116.0(4) . . ? C27 C22 C21 122.9(4) . . ? C23 C22 C21 121.0(4) . . ? C24 C23 C22 124.5(5) . . ? C25 C26 C27 119.5(5) . . ? C23 C24 C25 117.2(4) . . ? C23 C24 C28 119.6(4) . . ? C25 C24 C28 123.2(4) . . ? C26 C25 O25 121.4(5) . . ? C26 C25 C24 120.8(5) . . ? O25 C25 C24 117.7(4) . . ? C22 C27 O27 117.3(4) . . ? C22 C27 C26 121.9(4) . . ? O27 C27 C26 120.7(4) . . ? C35 C28 C1 114.6(4) . . ? C35 C28 C24 110.4(4) . . ? C1 C28 C24 110.4(4) . . ? C30 C29 C7 113.7(4) . . ? C32 C31 C14 113.8(5) . . ? C21 C33 C34 112.0(5) . . ? C28 C35 C36 112.8(5) . . ? C39 N1 C38 124.3(5) . . ? O102 N2 O101 120.4(5) . . ? O102 N2 C44 119.2(5) . . ? O101 N2 C44 120.4(5) . . ? O4 C37 C38 108.2(4) . . ? N1 C38 C37 114.2(5) . . ? N1 C39 C44 124.3(5) . . ? N1 C39 C40 120.7(5) . . ? C44 C39 C40 115.0(5) . . ? C41 C40 C39 122.0(5) . . ? C40 C41 C42 121.4(6) . . ? C43 C42 C41 119.1(6) . . ? C42 C43 C44 120.6(6) . . ? C43 C44 C39 121.9(5) . . ? C43 C44 N2 116.7(5) . . ? C39 C44 N2 121.3(5) . . ? C47 N3 C46 123.6(5) . . ? O103 N4 O104 125.4(10) . . ? O103 N4 C52 118.5(7) . . ? O104 N4 C52 116.1(10) . . ? O6 C45 C46 108.0(4) . . ? N3 C46 C45 108.9(4) . . ? N3 C47 C48 121.5(6) . . ? N3 C47 C52 123.1(7) . . ? C48 C47 C52 115.4(7) . . ? C49 C48 C47 124.0(8) . . ? C48 C49 C50 118.4(10) . . ? C51 C50 C49 120.5(9) . . ? C52 C51 C50 118.1(10) . . ? C51 C52 C47 123.5(10) . . ? C51 C52 N4 114.9(9) . . ? C47 C52 N4 121.6(7) . . ? C55 N5 C54 124.1(6) . . ? O106 N6 O105 120.2(6) . . ? O106 N6 C60 119.7(7) . . ? O105 N6 C60 120.1(5) . . ? O11 C53 C54 108.2(4) . . ? N5 C54 C53 111.8(5) . . ? N5 C55 C56 121.9(6) . . ? N5 C55 C60 122.0(6) . . ? C56 C55 C60 116.1(6) . . ? C57 C56 C55 121.5(7) . . ? C56 C57 C58 122.1(8) . . ? C59 C58 C57 117.8(8) . . ? C58 C59 C60 121.7(7) . . ? C59 C60 N6 116.8(6) . . ? C59 C60 C55 120.7(7) . . ? N6 C60 C55 122.5(6) . . ? C71 N9 C70 126.4(5) . . ? O109 N10 O110 118.4(6) . . ? O109 N10 C76 120.9(5) . . ? O110 N10 C76 120.7(6) . . ? O18 C69 C70 109.1(5) . . ? N9 C70 C69 113.6(5) . . ? N9 C71 C72 123.0(5) . . ? N9 C71 C76 123.3(5) . . ? C72 C71 C76 113.7(5) . . ? C73 C72 C71 123.5(6) . . ? C72 C73 C74 121.6(6) . . ? C75 C74 C73 117.6(6) . . ? C74 C75 C76 121.5(6) . . ? C75 C76 N10 116.8(5) . . ? C75 C76 C71 122.1(6) . . ? N10 C76 C71 121.0(5) . . ? C79 N11 C78 122.4(5) . . ? O112 N12 O111 121.2(5) . . ? O112 N12 C84 119.0(4) . . ? O111 N12 C84 119.8(5) . . ? O20 C77 C78 103.2(4) . . ? N11 C78 C77 109.0(4) . . ? N11 C79 C80 120.6(5) . . ? N11 C79 C84 124.5(5) . . ? C80 C79 C84 114.8(4) . . ? C81 C80 C79 122.5(5) . . ? C80 C81 C82 120.4(6) . . ? C83 C82 C81 119.2(5) . . ? C82 C83 C84 120.2(6) . . ? C83 C84 C79 122.8(5) . . ? C83 C84 N12 115.5(5) . . ? C79 C84 N12 121.7(5) . . ? C87 N13 C86 123.5(6) . . ? O113 N14 O114 120.1(5) . . ? O113 N14 C92 120.7(5) . . ? O114 N14 C92 119.2(6) . . ? O25 C85 C86 107.9(5) . . ? N13 C86 C85 110.7(5) . . ? N13 C87 C88 120.6(6) . . ? N13 C87 C92 122.4(6) . . ? C88 C87 C92 117.1(6) . . ? C89 C88 C87 120.6(7) . . ? C88 C89 C90 120.4(8) . . ? C91 C90 C89 120.0(8) . . ? C90 C91 C92 121.3(7) . . ? C91 C92 N14 116.9(5) . . ? C91 C92 C87 120.5(6) . . ? N14 C92 C87 122.6(5) . . ? C95 N15 C94 123.1(4) . . ? O116 N16 O115 120.4(6) . . ? O116 N16 C100 119.0(6) . . ? O115 N16 C100 120.7(5) . . ? O27 C93 C94 107.1(4) . . ? N15 C94 C93 108.4(4) . . ? N15 C95 C96 120.8(5) . . ? N15 C95 C100 123.7(5) . . ? C96 C95 C100 115.4(5) . . ? C97 C96 C95 121.6(6) . . ? C96 C97 C98 122.3(7) . . ? C99 C98 C97 118.9(7) . . ? C98 C99 C100 120.1(7) . . ? C99 C100 C95 121.7(6) . . ? C99 C100 N16 116.7(6) . . ? C95 C100 N16 121.5(6) . . ? O13 C61 C62 107.1(4) . . ? C61 C62 N7A 109.1(5) . . ? C61 C62 N7B 104.7(6) . . ? N7A C62 N7B 56.0(5) . . ? C63 N7A C62 116.9(7) . . ? O50A N8A O51A 120.1(19) . . ? O50A N8A C68A 113.6(15) . . ? O51A N8A C68A 110.2(14) . . ? C63 N7B C62 116.6(8) . . ? O51B N8B O50B 116.9(13) . . ? O51B N8B C68B 122.4(11) . . ? O50B N8B C68B 120.6(10) . . ? N7B C63 C68B 128.8(5) . . ? N7B C63 C64A 54.4(5) . . ? C68B C63 C64A 74.7 . . ? N7B C63 C68A 174.0(5) . . ? C68B C63 C68A 45.4 . . ? C64A C63 C68A 120.0 . . ? N7B C63 N7A 65.5(6) . . ? C68B C63 N7A 163.3(4) . . ? C64A C63 N7A 119.8(4) . . ? C68A C63 N7A 119.9(4) . . ? N7B C63 C64B 117.6(5) . . ? C68B C63 C64B 113.2 . . ? C64A C63 C64B 165.3 . . ? C68A C63 C64B 68.3 . . ? N7A C63 C64B 54.8(4) . . ? C63 C64A C65A 120.0 . . ? C66A C65A C64A 120.0 . . ? C67A C66A C65A 120.0 . . ? C66A C67A C68A 120.0 . . ? C67A C68A C63 120.0 . . ? C67A C68A N8A 113.7(6) . . ? C63 C68A N8A 125.4(6) . . ? C63 C64B C65B 105.8 . . ? C66B C65B C64B 118.0 . . ? C65B C66B C67B 117.7 . . ? C68B C67B C66B 105.4 . . ? C67B C68B C63 146.1 . . ? C67B C68B N8B 98.1(5) . . ? C63 C68B N8B 115.5(5) . . ? O200 C200 C202 115.1(7) . . ? O200 C200 C201 127.2(8) . . ? C202 C200 C201 117.8(8) . . ? 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 2.0(7) . . . . ? C28 C1 C2 C3 179.4(4) . . . . ? C1 C2 C3 C4 0.3(7) . . . . ? C1 C2 C3 C7 -176.0(4) . . . . ? C37 O4 C4 C5 -21.8(7) . . . . ? C37 O4 C4 C3 157.3(4) . . . . ? C2 C3 C4 O4 179.2(4) . . . . ? C7 C3 C4 O4 -4.2(6) . . . . ? C2 C3 C4 C5 -1.7(7) . . . . ? C7 C3 C4 C5 174.9(4) . . . . ? O4 C4 C5 C6 179.7(4) . . . . ? C3 C4 C5 C6 0.7(7) . . . . ? C4 C5 C6 C1 1.7(7) . . . . ? C4 C5 C6 O6 178.4(4) . . . . ? C2 C1 C6 C5 -3.0(7) . . . . ? C28 C1 C6 C5 179.5(4) . . . . ? C2 C1 C6 O6 -179.6(4) . . . . ? C28 C1 C6 O6 2.9(7) . . . . ? C45 O6 C6 C5 64.9(6) . . . . ? C45 O6 C6 C1 -118.3(5) . . . . ? C2 C3 C7 C29 -12.8(7) . . . . ? C4 C3 C7 C29 170.9(4) . . . . ? C2 C3 C7 C8 113.3(5) . . . . ? C4 C3 C7 C8 -62.9(5) . . . . ? C3 C7 C8 C13 133.8(5) . . . . ? C29 C7 C8 C13 -99.2(5) . . . . ? C3 C7 C8 C9 -43.1(6) . . . . ? C29 C7 C8 C9 83.8(5) . . . . ? C13 C8 C9 C10 1.5(7) . . . . ? C7 C8 C9 C10 178.6(5) . . . . ? C8 C9 C10 C11 -1.2(7) . . . . ? C8 C9 C10 C14 178.3(4) . . . . ? C53 O11 C11 C12 23.6(7) . . . . ? C53 O11 C11 C10 -157.2(5) . . . . ? C9 C10 C11 O11 -179.8(4) . . . . ? C14 C10 C11 O11 0.7(7) . . . . ? C9 C10 C11 C12 -0.6(7) . . . . ? C14 C10 C11 C12 179.9(5) . . . . ? O11 C11 C12 C13 -178.8(5) . . . . ? C10 C11 C12 C13 2.0(8) . . . . ? C9 C8 C13 C12 -0.1(7) . . . . ? C7 C8 C13 C12 -177.1(5) . . . . ? C9 C8 C13 O13 178.8(4) . . . . ? C7 C8 C13 O13 1.7(7) . . . . ? C11 C12 C13 C8 -1.6(8) . . . . ? C11 C12 C13 O13 179.6(5) . . . . ? C61 O13 C13 C8 161.4(5) . . . . ? C61 O13 C13 C12 -19.8(7) . . . . ? C9 C10 C14 C31 -76.7(6) . . . . ? C11 C10 C14 C31 102.8(5) . . . . ? C9 C10 C14 C15 50.7(6) . . . . ? C11 C10 C14 C15 -129.8(5) . . . . ? C31 C14 C15 C20 -165.4(4) . . . . ? C10 C14 C15 C20 67.5(6) . . . . ? C31 C14 C15 C16 13.6(6) . . . . ? C10 C14 C15 C16 -113.5(5) . . . . ? C20 C15 C16 C17 3.3(7) . . . . ? C14 C15 C16 C17 -175.7(4) . . . . ? C15 C16 C17 C18 -2.7(7) . . . . ? C15 C16 C17 C21 178.9(4) . . . . ? C16 C17 C18 C19 0.6(7) . . . . ? C21 C17 C18 C19 179.0(4) . . . . ? C16 C17 C18 O18 -178.4(4) . . . . ? C21 C17 C18 O18 0.1(6) . . . . ? C69 O18 C18 C19 54.0(6) . . . . ? C69 O18 C18 C17 -127.0(5) . . . . ? C17 C18 C19 C20 0.7(7) . . . . ? O18 C18 C19 C20 179.7(4) . . . . ? C77 O20 C20 C19 2.9(7) . . . . ? C77 O20 C20 C15 -178.1(4) . . . . ? C18 C19 C20 O20 178.8(4) . . . . ? C18 C19 C20 C15 -0.1(7) . . . . ? C16 C15 C20 O20 179.1(4) . . . . ? C14 C15 C20 O20 -1.8(6) . . . . ? C16 C15 C20 C19 -1.9(7) . . . . ? C14 C15 C20 C19 177.2(4) . . . . ? C16 C17 C21 C33 -17.4(6) . . . . ? C18 C17 C21 C33 164.2(4) . . . . ? C16 C17 C21 C22 107.3(5) . . . . ? C18 C17 C21 C22 -71.1(6) . . . . ? C33 C21 C22 C27 -102.3(5) . . . . ? C17 C21 C22 C27 130.8(5) . . . . ? C33 C21 C22 C23 75.6(5) . . . . ? C17 C21 C22 C23 -51.3(6) . . . . ? C27 C22 C23 C24 -1.1(7) . . . . ? C21 C22 C23 C24 -179.2(4) . . . . ? C22 C23 C24 C25 1.9(7) . . . . ? C22 C23 C24 C28 -178.0(4) . . . . ? C27 C26 C25 O25 178.0(5) . . . . ? C27 C26 C25 C24 0.7(8) . . . . ? C85 O25 C25 C26 3.7(8) . . . . ? C85 O25 C25 C24 -179.0(5) . . . . ? C23 C24 C25 C26 -1.7(7) . . . . ? C28 C24 C25 C26 178.2(5) . . . . ? C23 C24 C25 O25 -179.0(4) . . . . ? C28 C24 C25 O25 0.8(7) . . . . ? C23 C22 C27 O27 178.2(4) . . . . ? C21 C22 C27 O27 -3.8(7) . . . . ? C23 C22 C27 C26 0.1(7) . . . . ? C21 C22 C27 C26 178.1(4) . . . . ? C93 O27 C27 C22 155.0(4) . . . . ? C93 O27 C27 C26 -26.9(6) . . . . ? C25 C26 C27 C22 0.1(8) . . . . ? C25 C26 C27 O27 -178.0(4) . . . . ? C6 C1 C28 C35 177.9(4) . . . . ? C2 C1 C28 C35 0.6(6) . . . . ? C6 C1 C28 C24 52.4(6) . . . . ? C2 C1 C28 C24 -124.9(5) . . . . ? C23 C24 C28 C35 -76.5(5) . . . . ? C25 C24 C28 C35 103.6(6) . . . . ? C23 C24 C28 C1 51.3(6) . . . . ? C25 C24 C28 C1 -128.5(5) . . . . ? C3 C7 C29 C30 -174.4(4) . . . . ? C8 C7 C29 C30 60.9(6) . . . . ? C10 C14 C31 C32 -60.0(6) . . . . ? C15 C14 C31 C32 173.3(5) . . . . ? C22 C21 C33 C34 66.2(5) . . . . ? C17 C21 C33 C34 -168.8(4) . . . . ? C1 C28 C35 C36 174.3(4) . . . . ? C24 C28 C35 C36 -60.2(6) . . . . ? C4 O4 C37 C38 -168.7(4) . . . . ? C39 N1 C38 C37 -78.8(6) . . . . ? O4 C37 C38 N1 -62.7(6) . . . . ? C38 N1 C39 C44 -175.4(5) . . . . ? C38 N1 C39 C40 5.1(8) . . . . ? N1 C39 C40 C41 179.1(5) . . . . ? C44 C39 C40 C41 -0.4(8) . . . . ? C39 C40 C41 C42 -0.7(9) . . . . ? C40 C41 C42 C43 1.2(8) . . . . ? C41 C42 C43 C44 -0.6(8) . . . . ? C42 C43 C44 C39 -0.5(8) . . . . ? C42 C43 C44 N2 177.9(5) . . . . ? N1 C39 C44 C43 -178.5(5) . . . . ? C40 C39 C44 C43 1.0(7) . . . . ? N1 C39 C44 N2 3.2(8) . . . . ? C40 C39 C44 N2 -177.3(5) . . . . ? O102 N2 C44 C43 0.9(7) . . . . ? O101 N2 C44 C43 -178.2(5) . . . . ? O102 N2 C44 C39 179.3(5) . . . . ? O101 N2 C44 C39 0.2(7) . . . . ? C6 O6 C45 C46 -151.0(4) . . . . ? C47 N3 C46 C45 -175.5(6) . . . . ? O6 C45 C46 N3 68.9(6) . . . . ? C46 N3 C47 C48 2.6(10) . . . . ? C46 N3 C47 C52 -176.6(6) . . . . ? N3 C47 C48 C49 177.9(7) . . . . ? C52 C47 C48 C49 -2.9(11) . . . . ? C47 C48 C49 C50 3.3(12) . . . . ? C48 C49 C50 C51 -1.8(14) . . . . ? C49 C50 C51 C52 0.0(15) . . . . ? C50 C51 C52 C47 0.3(13) . . . . ? C50 C51 C52 N4 -179.5(8) . . . . ? N3 C47 C52 C51 -179.8(7) . . . . ? C48 C47 C52 C51 1.0(11) . . . . ? N3 C47 C52 N4 0.0(10) . . . . ? C48 C47 C52 N4 -179.2(7) . . . . ? O103 N4 C52 C51 -174.8(8) . . . . ? O104 N4 C52 C51 6.6(11) . . . . ? O103 N4 C52 C47 5.4(11) . . . . ? O104 N4 C52 C47 -173.3(8) . . . . ? C11 O11 C53 C54 166.0(5) . . . . ? C55 N5 C54 C53 -79.5(7) . . . . ? O11 C53 C54 N5 -175.9(5) . . . . ? C54 N5 C55 C56 -5.6(9) . . . . ? C54 N5 C55 C60 174.7(5) . . . . ? N5 C55 C56 C57 -178.6(6) . . . . ? C60 C55 C56 C57 1.2(9) . . . . ? C55 C56 C57 C58 -1.2(11) . . . . ? C56 C57 C58 C59 1.1(12) . . . . ? C57 C58 C59 C60 -1.1(11) . . . . ? C58 C59 C60 N6 -179.6(6) . . . . ? C58 C59 C60 C55 1.2(10) . . . . ? O106 N6 C60 C59 -1.4(9) . . . . ? O105 N6 C60 C59 178.6(6) . . . . ? O106 N6 C60 C55 177.8(6) . . . . ? O105 N6 C60 C55 -2.2(9) . . . . ? N5 C55 C60 C59 178.6(5) . . . . ? C56 C55 C60 C59 -1.2(8) . . . . ? N5 C55 C60 N6 -0.6(9) . . . . ? C56 C55 C60 N6 179.6(6) . . . . ? C18 O18 C69 C70 148.4(4) . . . . ? C71 N9 C70 C69 95.4(7) . . . . ? O18 C69 C70 N9 60.9(7) . . . . ? C70 N9 C71 C72 2.1(8) . . . . ? C70 N9 C71 C76 -178.5(5) . . . . ? N9 C71 C72 C73 177.4(5) . . . . ? C76 C71 C72 C73 -2.1(8) . . . . ? C71 C72 C73 C74 1.9(9) . . . . ? C72 C73 C74 C75 -0.6(10) . . . . ? C73 C74 C75 C76 -0.3(10) . . . . ? C74 C75 C76 N10 -179.0(6) . . . . ? C74 C75 C76 C71 -0.1(9) . . . . ? O109 N10 C76 C75 -179.6(5) . . . . ? O110 N10 C76 C75 -0.8(9) . . . . ? O109 N10 C76 C71 1.5(8) . . . . ? O110 N10 C76 C71 -179.7(7) . . . . ? N9 C71 C76 C75 -178.3(5) . . . . ? C72 C71 C76 C75 1.2(8) . . . . ? N9 C71 C76 N10 0.5(8) . . . . ? C72 C71 C76 N10 -179.9(5) . . . . ? C20 O20 C77 C78 175.6(4) . . . . ? C79 N11 C78 C77 175.3(5) . . . . ? O20 C77 C78 N11 178.9(4) . . . . ? C78 N11 C79 C80 -2.9(8) . . . . ? C78 N11 C79 C84 179.2(5) . . . . ? N11 C79 C80 C81 -177.8(6) . . . . ? C84 C79 C80 C81 0.3(8) . . . . ? C79 C80 C81 C82 -0.8(9) . . . . ? C80 C81 C82 C83 1.5(9) . . . . ? C81 C82 C83 C84 -1.6(9) . . . . ? C82 C83 C84 C79 1.0(9) . . . . ? C82 C83 C84 N12 -178.3(5) . . . . ? N11 C79 C84 C83 177.6(5) . . . . ? C80 C79 C84 C83 -0.4(8) . . . . ? N11 C79 C84 N12 -3.1(8) . . . . ? C80 C79 C84 N12 178.9(5) . . . . ? O112 N12 C84 C83 2.7(7) . . . . ? O111 N12 C84 C83 -176.4(5) . . . . ? O112 N12 C84 C79 -176.6(5) . . . . ? O111 N12 C84 C79 4.3(8) . . . . ? C25 O25 C85 C86 174.7(5) . . . . ? C87 N13 C86 C85 74.1(8) . . . . ? O25 C85 C86 N13 -156.9(6) . . . . ? C86 N13 C87 C88 2.1(9) . . . . ? C86 N13 C87 C92 -178.0(5) . . . . ? N13 C87 C88 C89 -178.7(7) . . . . ? C92 C87 C88 C89 1.4(10) . . . . ? C87 C88 C89 C90 -0.8(12) . . . . ? C88 C89 C90 C91 -0.1(13) . . . . ? C89 C90 C91 C92 0.2(12) . . . . ? C90 C91 C92 N14 179.5(7) . . . . ? C90 C91 C92 C87 0.6(10) . . . . ? O113 N14 C92 C91 -179.9(6) . . . . ? O114 N14 C92 C91 -1.5(8) . . . . ? O113 N14 C92 C87 -1.0(9) . . . . ? O114 N14 C92 C87 177.4(6) . . . . ? N13 C87 C92 C91 178.7(6) . . . . ? C88 C87 C92 C91 -1.3(9) . . . . ? N13 C87 C92 N14 -0.1(9) . . . . ? C88 C87 C92 N14 179.8(5) . . . . ? C27 O27 C93 C94 -165.4(4) . . . . ? C95 N15 C94 C93 -74.6(6) . . . . ? O27 C93 C94 N15 173.2(4) . . . . ? C94 N15 C95 C96 -9.5(7) . . . . ? C94 N15 C95 C100 172.8(5) . . . . ? N15 C95 C96 C97 -176.7(5) . . . . ? C100 C95 C96 C97 1.1(8) . . . . ? C95 C96 C97 C98 -0.2(10) . . . . ? C96 C97 C98 C99 0.1(11) . . . . ? C97 C98 C99 C100 -1.1(11) . . . . ? C98 C99 C100 C95 2.2(10) . . . . ? C98 C99 C100 N16 -179.0(6) . . . . ? N15 C95 C100 C99 175.7(5) . . . . ? C96 C95 C100 C99 -2.1(8) . . . . ? N15 C95 C100 N16 -3.1(8) . . . . ? C96 C95 C100 N16 179.2(5) . . . . ? O116 N16 C100 C99 3.4(8) . . . . ? O115 N16 C100 C99 -176.8(5) . . . . ? O116 N16 C100 C95 -177.8(6) . . . . ? O115 N16 C100 C95 2.0(8) . . . . ? C13 O13 C61 C62 -162.1(5) . . . . ? O13 C61 C62 N7A 152.1(6) . . . . ? O13 C61 C62 N7B -149.3(6) . . . . ? C61 C62 N7A C63 78.3(8) . . . . ? N7B C62 N7A C63 -16.9(6) . . . . ? C61 C62 N7B C63 -85.7(9) . . . . ? N7A C62 N7B C63 17.7(7) . . . . ? C62 N7B C63 C68B 172.3(4) . . . . ? C62 N7B C63 C64A 165.3(10) . . . . ? C62 N7B C63 N7A -17.8(7) . . . . ? C62 N7B C63 C64B -0.1(10) . . . . ? C62 N7A C63 N7B 18.6(7) . . . . ? C62 N7A C63 C68B 170.1(9) . . . . ? C62 N7A C63 C64A 21.5(8) . . . . ? C62 N7A C63 C68A -164.3(4) . . . . ? C62 N7A C63 C64B -142.2(8) . . . . ? N7B C63 C64A C65A 177.4(6) . . . . ? C68B C63 C64A C65A 3.1 . . . . ? C68A C63 C64A C65A 0.0 . . . . ? N7A C63 C64A C65A 174.2(4) . . . . ? C64B C63 C64A C65A -121.4 . . . . ? C63 C64A C65A C66A 0.0 . . . . ? C64A C65A C66A C67A 0.0 . . . . ? C65A C66A C67A C68A 0.0 . . . . ? C66A C67A C68A C63 0.0 . . . . ? C66A C67A C68A N8A 169.6(11) . . . . ? C68B C63 C68A C67A -4.2 . . . . ? C64A C63 C68A C67A 0.0 . . . . ? N7A C63 C68A C67A -174.2(4) . . . . ? C64B C63 C68A C67A 166.5 . . . . ? C68B C63 C68A N8A -172.5(12) . . . . ? C64A C63 C68A N8A -168.3(12) . . . . ? N7A C63 C68A N8A 17.5(12) . . . . ? C64B C63 C68A N8A -1.8(12) . . . . ? O50A N8A C68A C67A 158.2(13) . . . . ? O51A N8A C68A C67A 20(2) . . . . ? O50A N8A C68A C63 -33(2) . . . . ? O51A N8A C68A C63 -170.9(10) . . . . ? N7B C63 C64B C65B -170.1(5) . . . . ? C68B C63 C64B C65B 16.3 . . . . ? C64A C63 C64B C65B 136.4 . . . . ? C68A C63 C64B C65B 9.1 . . . . ? N7A C63 C64B C65B -150.3(5) . . . . ? C63 C64B C65B C66B -38.5 . . . . ? C64B C65B C66B C67B 43.8 . . . . ? C65B C66B C67B C68B -24.8 . . . . ? C66B C67B C68B C63 2.5 . . . . ? C66B C67B C68B N8B 174.7(6) . . . . ? N7B C63 C68B C67B -174.4(6) . . . . ? C64A C63 C68B C67B -168.5 . . . . ? C68A C63 C68B C67B 7.7 . . . . ? N7A C63 C68B C67B 39.4(14) . . . . ? C64B C63 C68B C67B -1.7 . . . . ? N7B C63 C68B N8B 14.1(9) . . . . ? C64A C63 C68B N8B 20.0(6) . . . . ? C68A C63 C68B N8B -163.7(6) . . . . ? N7A C63 C68B N8B -132.1(15) . . . . ? C64B C63 C68B N8B -173.2(6) . . . . ? O51B N8B C68B C67B -16.3(15) . . . . ? O50B N8B C68B C67B 161.2(12) . . . . ? O51B N8B C68B C63 158.9(12) . . . . ? O50B N8B C68B C63 -23.5(15) . . . . ? 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 N1 H1N O101 0.88 1.98 2.633(6) 129.8 . N3 H3N O103 0.96(3) 1.90(5) 2.620(7) 130(5) . N5 H5N O105 0.96(3) 1.82(5) 2.596(7) 136(5) . N5 H5N O105 0.96(3) 2.31(5) 3.073(8) 135(5) 2 N7A H7A O50A 0.88 2.07 2.640(13) 121.4 . N7B H7B O50B 0.88 2.00 2.602(15) 124.8 . N9 H9N O109 0.88 1.93 2.606(6) 132.4 . N11 H11N O111 0.95(3) 1.87(5) 2.639(6) 136(5) . N13 H13N O113 0.96(3) 1.86(5) 2.624(6) 134(5) . N15 H15N O115 0.95(3) 1.94(5) 2.612(6) 126(4) . N15 H15N O200 0.95(3) 2.38(4) 3.091(8) 131(4) . _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 66.86 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.774 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.084 #===end data_2C _database_code_depnum_ccdc_archive 'CCDC 781923' #TrackingRef '- Octapodands.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H104 N16 O24' _chemical_formula_weight 1913.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 11.9965(3) _cell_length_b 20.2594(5) _cell_length_c 22.8564(5) _cell_angle_alpha 114.6950(10) _cell_angle_beta 96.9670(9) _cell_angle_gamma 99.770(2) _cell_volume 4857.9(2) _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 needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8335 _exptl_absorpt_correction_T_max 0.9692 _exptl_absorpt_process_details 'Denzo (Otwinowski, Majewski, Borek & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 24820 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 66.98 _reflns_number_total 16339 _reflns_number_gt 9752 _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^)+(0.0808P)^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 16339 _refine_ls_number_parameters 1289 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1812 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.500 0.500 1.000 266 87 ' ' _platon_squeeze_details ; ; 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 O4 O 0.83385(16) 0.95142(12) 0.19778(11) 0.0391(5) Uani 1 1 d . . . O6 O 0.53489(16) 0.76008(12) 0.19743(10) 0.0374(5) Uani 1 1 d . . . O11 O 0.77975(15) 1.25431(11) 0.33126(11) 0.0351(5) Uani 1 1 d . . . O13 O 1.06578(16) 1.10791(12) 0.29277(12) 0.0424(6) Uani 1 1 d . . . O18 O 0.26155(16) 0.90834(11) 0.23561(10) 0.0343(5) Uani 1 1 d . . . O20 O 0.55528(16) 1.11266(12) 0.24781(10) 0.0382(5) Uani 1 1 d . . . O25 O 0.44392(18) 0.66491(12) 0.28492(13) 0.0505(7) Uani 1 1 d . . . O27 O 0.16029(16) 0.81383(12) 0.32637(11) 0.0391(5) Uani 1 1 d . . . C1 C 0.6832(2) 0.83642(16) 0.29461(15) 0.0309(7) Uani 1 1 d . . . C2 C 0.7832(2) 0.89553(17) 0.32480(16) 0.0315(7) Uani 1 1 d . . . H2 H 0.8182 0.9098 0.3693 0.038 Uiso 1 1 calc R . . C3 C 0.8336(2) 0.93417(17) 0.29295(15) 0.0307(7) Uani 1 1 d . . . C4 C 0.7807(2) 0.91284(17) 0.22807(16) 0.0333(7) Uani 1 1 d . . . C5 C 0.6808(2) 0.85554(18) 0.19684(16) 0.0366(8) Uani 1 1 d . . . H5 H 0.6455 0.8412 0.1524 0.044 Uiso 1 1 calc R . . C6 C 0.6329(2) 0.81936(17) 0.23084(16) 0.0332(7) Uani 1 1 d . . . C7 C 0.9365(2) 1.00210(17) 0.32754(16) 0.0335(7) Uani 1 1 d . . . H7 H 0.9959 0.9929 0.2998 0.040 Uiso 1 1 calc R . . C8 C 0.8984(2) 1.07082(17) 0.32855(15) 0.0319(7) Uani 1 1 d . . . C9 C 0.7951(2) 1.08472(16) 0.34687(15) 0.0305(7) Uani 1 1 d . . . H9 H 0.7501 1.0506 0.3585 0.037 Uiso 1 1 calc R . . C10 C 0.7540(2) 1.14590(16) 0.34908(14) 0.0281(7) Uani 1 1 d . . . C11 C 0.8201(2) 1.19362(16) 0.32987(15) 0.0290(7) Uani 1 1 d . . . C12 C 0.9224(2) 1.18113(17) 0.31024(16) 0.0347(8) Uani 1 1 d . . . H12 H 0.9655 1.2137 0.2963 0.042 Uiso 1 1 calc R . . C13 C 0.9620(2) 1.12074(17) 0.31092(16) 0.0353(8) Uani 1 1 d . . . C14 C 0.6469(2) 1.16157(16) 0.37622(15) 0.0288(7) Uani 1 1 d . . . H14 H 0.6263 1.2028 0.3674 0.035 Uiso 1 1 calc R . . C15 C 0.5438(2) 1.09335(16) 0.34048(14) 0.0265(7) Uani 1 1 d . . . C16 C 0.4901(2) 1.05325(16) 0.36973(15) 0.0276(7) Uani 1 1 d . . . H16 H 0.5194 1.0682 0.4151 0.033 Uiso 1 1 calc R . . C17 C 0.3940(2) 0.99146(16) 0.33596(15) 0.0271(7) Uani 1 1 d . . . C18 C 0.3547(2) 0.97060(16) 0.27001(15) 0.0281(7) Uani 1 1 d . . . C19 C 0.4067(2) 1.00809(17) 0.23747(15) 0.0308(7) Uani 1 1 d . . . H19 H 0.3794 0.9918 0.1917 0.037 Uiso 1 1 calc R . . C20 C 0.4997(2) 1.06997(16) 0.27385(15) 0.0287(7) Uani 1 1 d . . . C21 C 0.3324(2) 0.94953(16) 0.36932(15) 0.0279(7) Uani 1 1 d . . . H21 H 0.2475 0.9404 0.3529 0.034 Uiso 1 1 calc R . . C22 C 0.3590(2) 0.87262(16) 0.34826(14) 0.0279(7) Uani 1 1 d . . . C23 C 0.4723(2) 0.86539(16) 0.34872(14) 0.0297(7) Uani 1 1 d . . . H23 H 0.5323 0.9096 0.3636 0.036 Uiso 1 1 calc R . . C24 C 0.5030(2) 0.79710(17) 0.32868(15) 0.0316(7) Uani 1 1 d . . . C25 C 0.4141(3) 0.73340(17) 0.30707(16) 0.0342(7) Uani 1 1 d . . . C26 C 0.3000(3) 0.73798(17) 0.30725(16) 0.0369(8) Uani 1 1 d . . . H26 H 0.2401 0.6940 0.2936 0.044 Uiso 1 1 calc R . . C27 C 0.2742(2) 0.80753(17) 0.32764(15) 0.0307(7) Uani 1 1 d . . . C28 C 0.6293(2) 0.79368(17) 0.32916(15) 0.0317(7) Uani 1 1 d . . . H28 H 0.6296 0.7399 0.3030 0.038 Uiso 1 1 calc R . . C29 C 0.9942(3) 1.01541(18) 0.39562(17) 0.0416(8) Uani 1 1 d . . . H29A H 1.0106 0.9681 0.3930 0.050 Uiso 1 1 calc R . . H29B H 0.9397 1.0294 0.4254 0.050 Uiso 1 1 calc R . . C30 C 1.1068(3) 1.07666(19) 0.42533(19) 0.0521(10) Uani 1 1 d . . . H30A H 1.1629 1.0621 0.3974 0.078 Uiso 1 1 calc R . . H30B H 1.1385 1.0835 0.4696 0.078 Uiso 1 1 calc R . . H30C H 1.0915 1.1237 0.4280 0.078 Uiso 1 1 calc R . . C31 C 0.6777(2) 1.19096(18) 0.45098(15) 0.0347(7) Uani 1 1 d . . . H31A H 0.6858 1.1486 0.4608 0.042 Uiso 1 1 calc R . . H31B H 0.7540 1.2275 0.4682 0.042 Uiso 1 1 calc R . . C32 C 0.5925(3) 1.2277(2) 0.48726(19) 0.0571(11) Uani 1 1 d . . . H32A H 0.5892 1.2728 0.4817 0.086 Uiso 1 1 calc R . . H32B H 0.6166 1.2415 0.5342 0.086 Uiso 1 1 calc R . . H32C H 0.5157 1.1928 0.4696 0.086 Uiso 1 1 calc R . . C33 C 0.3564(2) 0.99363(18) 0.44460(15) 0.0340(7) Uani 1 1 d . . . H33A H 0.4390 1.0005 0.4628 0.041 Uiso 1 1 calc R . . H33B H 0.3423 1.0439 0.4563 0.041 Uiso 1 1 calc R . . C34 C 0.2823(3) 0.9558(2) 0.47653(17) 0.0442(9) Uani 1 1 d . . . H34A H 0.2005 0.9522 0.4613 0.066 Uiso 1 1 calc R . . H34B H 0.3043 0.9854 0.5246 0.066 Uiso 1 1 calc R . . H34C H 0.2942 0.9054 0.4643 0.066 Uiso 1 1 calc R . . C35 C 0.6950(3) 0.81881(18) 0.39975(16) 0.0360(8) Uani 1 1 d . . . H35A H 0.7774 0.8184 0.3995 0.043 Uiso 1 1 calc R . . H35B H 0.6918 0.8710 0.4275 0.043 Uiso 1 1 calc R . . C36 C 0.6467(3) 0.7695(2) 0.43017(19) 0.0497(9) Uani 1 1 d . . . H36A H 0.5683 0.7744 0.4357 0.074 Uiso 1 1 calc R . . H36B H 0.6965 0.7850 0.4733 0.074 Uiso 1 1 calc R . . H36C H 0.6441 0.7172 0.4012 0.074 Uiso 1 1 calc R . . O101 O 1.1697(2) 1.04458(15) 0.14260(13) 0.0551(7) Uani 1 1 d . . . O102 O 1.2683(2) 0.99499(17) 0.06993(15) 0.0734(9) Uani 1 1 d . . . N1 N 0.9423(2) 1.00137(18) 0.11377(16) 0.0495(8) Uani 1 1 d D . . H1N H 1.009(2) 1.0313(19) 0.1442(15) 0.059 Uiso 1 1 d D . . N2 N 1.1750(3) 0.99885(17) 0.08672(16) 0.0483(8) Uani 1 1 d . . . C37 C 0.7654(3) 0.9492(2) 0.14124(18) 0.0484(9) Uani 1 1 d . . . H37A H 0.6887 0.9575 0.1495 0.058 Uiso 1 1 calc R . . H37B H 0.7537 0.8998 0.1028 0.058 Uiso 1 1 calc R . . C38 C 0.8299(3) 1.0102(2) 0.1282(2) 0.0530(10) Uani 1 1 d . . . H38A H 0.7822 1.0117 0.0904 0.064 Uiso 1 1 calc R . . H38B H 0.8404 1.0589 0.1672 0.064 Uiso 1 1 calc R . . C39 C 0.9600(3) 0.95420(19) 0.05507(18) 0.0419(9) Uani 1 1 d . . . C40 C 0.8649(3) 0.9048(2) 0.00234(19) 0.0516(10) Uani 1 1 d . . . H40 H 0.7882 0.9053 0.0088 0.062 Uiso 1 1 calc R . . C41 C 0.8810(4) 0.8573(2) -0.0567(2) 0.0621(12) Uani 1 1 d . . . H41 H 0.8149 0.8254 -0.0905 0.075 Uiso 1 1 calc R . . C42 C 0.9906(4) 0.8531(2) -0.0702(2) 0.0570(10) Uani 1 1 d . . . H42 H 0.9997 0.8191 -0.1120 0.068 Uiso 1 1 calc R . . C43 C 1.0841(3) 0.8998(2) -0.02109(19) 0.0523(10) Uani 1 1 d . . . H43 H 1.1599 0.8981 -0.0288 0.063 Uiso 1 1 calc R . . C44 C 1.0705(3) 0.94992(19) 0.04027(17) 0.0427(9) Uani 1 1 d . . . O103 O 0.5866(3) 0.7419(2) 0.01258(18) 0.0991(12) Uani 1 1 d . . . O104 O 0.5977(4) 0.6690(3) -0.0861(2) 0.151(2) Uani 1 1 d . . . N3 N 0.4202(2) 0.70041(18) 0.06407(14) 0.0503(8) Uani 1 1 d D . . H3N H 0.489(2) 0.7346(18) 0.0717(18) 0.060 Uiso 1 1 d D . . N4 N 0.5442(4) 0.6853(3) -0.0407(2) 0.0962(15) Uani 1 1 d . . . C45 C 0.4311(2) 0.77972(19) 0.17854(16) 0.0410(8) Uani 1 1 d . . . H45A H 0.4508 0.8235 0.1694 0.049 Uiso 1 1 calc R . . H45B H 0.3877 0.7925 0.2143 0.049 Uiso 1 1 calc R . . C46 C 0.3595(3) 0.71251(19) 0.11738(16) 0.0412(8) Uani 1 1 d . . . H46A H 0.3468 0.6677 0.1255 0.049 Uiso 1 1 calc R . . H46B H 0.2830 0.7212 0.1055 0.049 Uiso 1 1 calc R . . C47 C 0.3767(3) 0.6457(2) 0.00109(18) 0.0527(10) Uani 1 1 d . . . C48 C 0.2712(3) 0.5936(2) -0.0142(2) 0.0611(11) Uani 1 1 d . . . H48 H 0.2310 0.5964 0.0198 0.073 Uiso 1 1 calc R . . C49 C 0.2249(4) 0.5384(3) -0.0774(2) 0.0808(15) Uani 1 1 d . . . H49 H 0.1523 0.5048 -0.0866 0.097 Uiso 1 1 calc R . . C50 C 0.2821(5) 0.5311(3) -0.1278(2) 0.0875(16) Uani 1 1 d . . . H50 H 0.2488 0.4930 -0.1713 0.105 Uiso 1 1 calc R . . C51 C 0.3855(5) 0.5784(3) -0.1149(2) 0.0865(15) Uani 1 1 d . . . H51 H 0.4259 0.5728 -0.1493 0.104 Uiso 1 1 calc R . . C52 C 0.4344(4) 0.6364(3) -0.0504(2) 0.0660(12) Uani 1 1 d . . . O105 O 1.0677(3) 1.55425(17) 0.48221(15) 0.0791(9) Uani 1 1 d . . . O106 O 1.1876(3) 1.63317(16) 0.46572(17) 0.0916(11) Uani 1 1 d . . . N5 N 0.8985(2) 1.45356(16) 0.38716(17) 0.0526(8) Uani 1 1 d D . . H5N H 0.931(3) 1.475(2) 0.4318(10) 0.063 Uiso 1 1 d D . . N6 N 1.1035(3) 1.57883(17) 0.44513(19) 0.0645(10) Uani 1 1 d . . . C53 C 0.8653(2) 1.31835(17) 0.34214(18) 0.0398(8) Uani 1 1 d . . . H53A H 0.8936 1.3101 0.3013 0.048 Uiso 1 1 calc R . . H53B H 0.9318 1.3281 0.3773 0.048 Uiso 1 1 calc R . . C54 C 0.8108(3) 1.38382(18) 0.36232(19) 0.0466(9) Uani 1 1 d . . . H54A H 0.7549 1.3782 0.3239 0.056 Uiso 1 1 calc R . . H54B H 0.7679 1.3849 0.3969 0.056 Uiso 1 1 calc R . . C55 C 0.9510(3) 1.48031(19) 0.3493(2) 0.0512(10) Uani 1 1 d . . . C56 C 0.9092(3) 1.4493(2) 0.2807(2) 0.0586(11) Uani 1 1 d . . . H56 H 0.8455 1.4066 0.2599 0.070 Uiso 1 1 calc R . . C57 C 0.9574(4) 1.4789(3) 0.2433(2) 0.0684(12) Uani 1 1 d . . . H57 H 0.9265 1.4562 0.1971 0.082 Uiso 1 1 calc R . . C58 C 1.0505(4) 1.5411(2) 0.2706(3) 0.0677(12) Uani 1 1 d . . . H58 H 1.0819 1.5615 0.2438 0.081 Uiso 1 1 calc R . . C59 C 1.0957(3) 1.5725(2) 0.3361(3) 0.0621(12) Uani 1 1 d . . . H59 H 1.1607 1.6144 0.3553 0.074 Uiso 1 1 calc R . . C60 C 1.0473(3) 1.54345(19) 0.3758(2) 0.0529(10) Uani 1 1 d . . . O107 O 1.4745(3) 1.35163(19) 0.44170(15) 0.0871(10) Uani 1 1 d . . . O108 O 1.5821(2) 1.43742(15) 0.42768(15) 0.0771(9) Uani 1 1 d . . . N7 N 1.3617(2) 1.22509(18) 0.34131(18) 0.0552(9) Uani 1 1 d D . . H7N H 1.383(3) 1.2607(19) 0.3865(11) 0.066 Uiso 1 1 d D . . N8 N 1.5132(3) 1.37677(19) 0.40515(18) 0.0620(9) Uani 1 1 d . . . C61 C 1.1532(3) 1.17406(19) 0.3089(2) 0.0492(10) Uani 1 1 d . . . H61A H 1.1494 1.2148 0.3514 0.059 Uiso 1 1 calc R . . H61B H 1.1413 1.1910 0.2743 0.059 Uiso 1 1 calc R . . C62 C 1.2709(3) 1.1553(2) 0.3139(2) 0.0542(10) Uani 1 1 d . . . H62A H 1.2772 1.1303 0.3428 0.065 Uiso 1 1 calc R . . H62B H 1.2797 1.1209 0.2697 0.065 Uiso 1 1 calc R . . C63 C 1.3964(2) 1.26131(18) 0.30646(18) 0.0407(8) Uani 1 1 d . . . C64 C 1.3612(3) 1.2276(2) 0.2366(2) 0.0535(10) Uani 1 1 d . . . H64 H 1.3062 1.1806 0.2147 0.064 Uiso 1 1 calc R . . C65 C 1.4036(3) 1.2605(3) 0.2001(2) 0.0616(11) Uani 1 1 d . . . H65 H 1.3821 1.2347 0.1534 0.074 Uiso 1 1 calc R . . C66 C 1.4782(3) 1.3314(3) 0.2306(2) 0.0664(12) Uani 1 1 d . . . H66 H 1.5051 1.3548 0.2048 0.080 Uiso 1 1 calc R . . C67 C 1.5126(3) 1.3675(2) 0.2977(2) 0.0548(11) Uani 1 1 d . . . H67 H 1.5640 1.4159 0.3189 0.066 Uiso 1 1 calc R . . C68 C 1.4727(3) 1.33348(19) 0.33395(19) 0.0450(9) Uani 1 1 d . . . O109 O 0.1210(2) 0.67264(14) 0.17227(13) 0.0590(7) Uani 1 1 d . . . O110 O 0.0669(3) 0.56417(16) 0.09118(16) 0.0934(11) Uani 1 1 d . . . N9 N 0.0610(2) 0.78747(16) 0.16525(16) 0.0500(8) Uani 1 1 d D . . H9N H 0.101(3) 0.771(2) 0.1911(17) 0.060 Uiso 1 1 d D . . N10 N 0.0687(3) 0.63113(17) 0.11549(16) 0.0520(8) Uani 1 1 d . . . C69 C 0.1678(3) 0.91557(19) 0.19747(19) 0.0473(9) Uani 1 1 d . . . H69A H 0.1793 0.9009 0.1520 0.057 Uiso 1 1 calc R . . H69B H 0.1618 0.9683 0.2166 0.057 Uiso 1 1 calc R . . C70 C 0.0601(3) 0.86591(18) 0.1967(2) 0.0559(11) Uani 1 1 d . . . H70A H 0.0512 0.8801 0.2426 0.067 Uiso 1 1 calc R . . H70B H -0.0075 0.8736 0.1731 0.067 Uiso 1 1 calc R . . C71 C 0.0092(3) 0.73672(19) 0.10230(18) 0.0452(9) Uani 1 1 d . . . C72 C -0.0518(3) 0.7573(2) 0.0579(2) 0.0590(11) Uani 1 1 d . . . H72 H -0.0544 0.8082 0.0724 0.071 Uiso 1 1 calc R . . C73 C -0.1064(4) 0.7068(3) -0.0044(2) 0.0704(12) Uani 1 1 d . . . H73 H -0.1482 0.7227 -0.0320 0.084 Uiso 1 1 calc R . . C74 C -0.1023(4) 0.6321(3) -0.0287(2) 0.0754(13) Uani 1 1 d . . . H74 H -0.1397 0.5973 -0.0728 0.090 Uiso 1 1 calc R . . C75 C -0.0439(4) 0.6097(2) 0.01159(19) 0.0629(11) Uani 1 1 d . . . H75 H -0.0410 0.5587 -0.0047 0.076 Uiso 1 1 calc R . . C76 C 0.0117(3) 0.66003(19) 0.07629(17) 0.0438(8) Uani 1 1 d . . . O111 O 0.4700(2) 1.07129(16) -0.02044(13) 0.0680(8) Uani 1 1 d . . . O112 O 0.5265(2) 1.10516(15) -0.09157(13) 0.0588(7) Uani 1 1 d . . . N11 N 0.5865(2) 1.13680(17) 0.10257(14) 0.0459(8) Uani 1 1 d D . . H11N H 0.530(2) 1.0964(15) 0.0706(14) 0.055 Uiso 1 1 d D . . N12 N 0.5401(2) 1.11055(17) -0.03490(15) 0.0488(8) Uani 1 1 d . . . C77 C 0.5256(3) 1.09120(18) 0.17920(15) 0.0357(8) Uani 1 1 d . . . H77A H 0.4450 1.0932 0.1661 0.043 Uiso 1 1 calc R . . H77B H 0.5341 1.0399 0.1530 0.043 Uiso 1 1 calc R . . C78 C 0.6103(3) 1.14795(19) 0.17027(16) 0.0388(8) Uani 1 1 d . . . H78A H 0.6053 1.1990 0.2001 0.047 Uiso 1 1 calc R . . H78B H 0.6899 1.1435 0.1820 0.047 Uiso 1 1 calc R . . C79 C 0.6559(3) 1.17606(19) 0.08013(16) 0.0397(8) Uani 1 1 d . . . C80 C 0.7547(3) 1.23302(19) 0.12316(18) 0.0454(9) Uani 1 1 d . . . H80 H 0.7695 1.2446 0.1686 0.055 Uiso 1 1 calc R . . C81 C 0.8292(3) 1.2717(2) 0.10118(19) 0.0503(9) Uani 1 1 d . . . H81 H 0.8949 1.3091 0.1316 0.060 Uiso 1 1 calc R . . C82 C 0.8116(3) 1.2579(2) 0.03578(19) 0.0512(10) Uani 1 1 d . . . H82 H 0.8644 1.2853 0.0213 0.061 Uiso 1 1 calc R . . C83 C 0.7168(3) 1.2042(2) -0.00772(19) 0.0484(9) Uani 1 1 d . . . H83 H 0.7041 1.1939 -0.0529 0.058 Uiso 1 1 calc R . . C84 C 0.6383(3) 1.16429(19) 0.01342(16) 0.0403(8) Uani 1 1 d . . . O113 O 0.1595(2) 0.34610(16) 0.17559(14) 0.0705(8) Uani 1 1 d . . . O114 O 0.0767(2) 0.29681(15) 0.23190(14) 0.0681(8) Uani 1 1 d . . . N13 N 0.3248(3) 0.47055(17) 0.23456(17) 0.0552(8) Uani 1 1 d D . . H13N H 0.281(3) 0.4330(18) 0.1937(13) 0.066 Uiso 1 1 d D . . N14 N 0.1499(2) 0.34616(17) 0.22946(16) 0.0519(8) Uani 1 1 d . . . C85 C 0.3549(3) 0.6004(2) 0.2586(3) 0.0713(13) Uani 1 1 d . . . H85A H 0.3012 0.5985 0.2212 0.086 Uiso 1 1 calc R . . H85B H 0.3108 0.6003 0.2925 0.086 Uiso 1 1 calc R . . C86 C 0.4075(3) 0.5324(2) 0.2351(2) 0.0632(12) Uani 1 1 d . . . H86A H 0.4217 0.5196 0.1903 0.076 Uiso 1 1 calc R . . H86B H 0.4821 0.5434 0.2653 0.076 Uiso 1 1 calc R . . C87 C 0.3059(3) 0.4639(2) 0.2893(2) 0.0519(10) Uani 1 1 d . . . C88 C 0.3721(3) 0.5178(2) 0.3514(2) 0.0689(13) Uani 1 1 d . . . H88 H 0.4287 0.5588 0.3546 0.083 Uiso 1 1 calc R . . C89 C 0.3555(4) 0.5117(3) 0.4081(2) 0.0844(16) Uani 1 1 d . . . H89 H 0.4014 0.5489 0.4495 0.101 Uiso 1 1 calc R . . C90 C 0.2745(4) 0.4531(3) 0.4065(2) 0.0813(14) Uani 1 1 d . . . H90 H 0.2649 0.4502 0.4461 0.098 Uiso 1 1 calc R . . C91 C 0.2085(4) 0.3998(2) 0.3471(2) 0.0622(11) Uani 1 1 d . . . H91 H 0.1524 0.3594 0.3452 0.075 Uiso 1 1 calc R . . C92 C 0.2231(3) 0.4043(2) 0.28887(18) 0.0484(9) Uani 1 1 d . . . O115 O -0.2800(2) 0.59428(16) 0.28013(15) 0.0706(8) Uani 1 1 d . . . O116 O -0.3278(3) 0.52438(18) 0.3257(2) 0.1020(13) Uani 1 1 d . . . N15 N -0.1120(2) 0.71469(16) 0.33950(16) 0.0446(7) Uani 1 1 d D . . H15N H -0.166(3) 0.6825(18) 0.3003(12) 0.054 Uiso 1 1 d D . . N16 N -0.2684(2) 0.58124(17) 0.3285(2) 0.0579(9) Uani 1 1 d . . . C93 C 0.0803(3) 0.75232(19) 0.32528(18) 0.0430(9) Uani 1 1 d . . . H93A H 0.1132 0.7382 0.3590 0.052 Uiso 1 1 calc R . . H93B H 0.0645 0.7084 0.2815 0.052 Uiso 1 1 calc R . . C94 C -0.0287(3) 0.7753(2) 0.3391(2) 0.0492(9) Uani 1 1 d . . . H94A H -0.0120 0.8199 0.3825 0.059 Uiso 1 1 calc R . . H94B H -0.0615 0.7889 0.3050 0.059 Uiso 1 1 calc R . . C95 C -0.1098(3) 0.69713(19) 0.39128(19) 0.0436(9) Uani 1 1 d . . . C96 C -0.0324(3) 0.7428(2) 0.4520(2) 0.0556(10) Uani 1 1 d . . . H96 H 0.0227 0.7853 0.4566 0.067 Uiso 1 1 calc R . . C97 C -0.0345(4) 0.7275(3) 0.5042(2) 0.0681(12) Uani 1 1 d . . . H97 H 0.0199 0.7595 0.5444 0.082 Uiso 1 1 calc R . . C98 C -0.1121(4) 0.6676(3) 0.5014(3) 0.0805(14) Uani 1 1 d . . . H98 H -0.1125 0.6590 0.5392 0.097 Uiso 1 1 calc R . . C99 C -0.1895(4) 0.6200(3) 0.4429(3) 0.0685(12) Uani 1 1 d . . . H99 H -0.2436 0.5781 0.4400 0.082 Uiso 1 1 calc R . . C100 C -0.1882(3) 0.6334(2) 0.38839(19) 0.0459(9) 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 O4 0.0312(11) 0.0463(13) 0.0436(14) 0.0265(11) 0.0069(10) 0.0028(10) O6 0.0298(11) 0.0361(12) 0.0382(13) 0.0148(10) -0.0011(9) -0.0010(9) O11 0.0233(10) 0.0299(11) 0.0544(14) 0.0229(10) 0.0079(9) 0.0018(9) O13 0.0257(10) 0.0313(12) 0.0702(16) 0.0206(11) 0.0204(10) 0.0055(9) O18 0.0305(10) 0.0300(11) 0.0368(12) 0.0168(10) -0.0057(9) -0.0029(9) O20 0.0347(11) 0.0443(13) 0.0322(13) 0.0212(10) 0.0020(9) -0.0055(10) O25 0.0362(12) 0.0272(12) 0.0795(18) 0.0184(12) 0.0063(12) 0.0059(10) O27 0.0268(10) 0.0350(12) 0.0585(15) 0.0248(11) 0.0120(10) 0.0027(9) C1 0.0250(14) 0.0284(16) 0.0365(19) 0.0138(14) 0.0032(13) 0.0046(13) C2 0.0262(14) 0.0310(16) 0.0368(18) 0.0149(14) 0.0044(13) 0.0083(13) C3 0.0229(14) 0.0293(16) 0.0408(19) 0.0158(14) 0.0063(13) 0.0087(12) C4 0.0280(15) 0.0347(17) 0.0391(19) 0.0187(15) 0.0090(14) 0.0054(13) C5 0.0322(16) 0.0381(18) 0.0336(18) 0.0138(15) 0.0036(14) 0.0020(14) C6 0.0233(14) 0.0301(16) 0.042(2) 0.0139(14) 0.0061(14) 0.0011(13) C7 0.0216(14) 0.0307(16) 0.047(2) 0.0174(15) 0.0062(14) 0.0052(13) C8 0.0259(15) 0.0313(16) 0.0370(18) 0.0153(14) 0.0042(13) 0.0056(13) C9 0.0236(14) 0.0282(16) 0.0396(19) 0.0177(14) 0.0051(13) 0.0009(12) C10 0.0218(14) 0.0277(15) 0.0283(16) 0.0097(13) 0.0029(12) -0.0010(12) C11 0.0236(14) 0.0260(15) 0.0342(18) 0.0116(13) 0.0039(13) 0.0041(12) C12 0.0240(14) 0.0334(17) 0.048(2) 0.0214(15) 0.0079(14) 0.0005(13) C13 0.0255(15) 0.0342(17) 0.044(2) 0.0156(15) 0.0100(14) 0.0041(13) C14 0.0252(14) 0.0271(15) 0.0345(18) 0.0152(13) 0.0064(13) 0.0035(12) C15 0.0212(13) 0.0286(15) 0.0299(17) 0.0144(13) 0.0030(12) 0.0051(12) C16 0.0253(14) 0.0295(15) 0.0271(16) 0.0119(13) 0.0052(12) 0.0068(12) C17 0.0210(13) 0.0261(15) 0.0342(18) 0.0158(13) 0.0026(13) 0.0023(12) C18 0.0192(13) 0.0272(15) 0.0347(18) 0.0128(13) 0.0025(13) 0.0027(12) C19 0.0282(15) 0.0331(16) 0.0290(17) 0.0143(14) 0.0037(13) 0.0030(13) C20 0.0250(14) 0.0277(15) 0.0379(19) 0.0183(14) 0.0090(13) 0.0062(12) C21 0.0183(13) 0.0287(15) 0.0390(18) 0.0186(14) 0.0037(12) 0.0037(12) C22 0.0278(15) 0.0303(16) 0.0305(17) 0.0188(13) 0.0052(13) 0.0060(13) C23 0.0257(15) 0.0287(16) 0.0322(17) 0.0141(13) 0.0026(13) 0.0014(12) C24 0.0279(15) 0.0344(17) 0.0346(18) 0.0174(14) 0.0094(13) 0.0059(13) C25 0.0351(17) 0.0282(16) 0.0409(19) 0.0169(14) 0.0095(14) 0.0068(13) C26 0.0336(16) 0.0291(16) 0.048(2) 0.0197(15) 0.0111(15) 0.0008(13) C27 0.0211(14) 0.0361(17) 0.0382(18) 0.0193(14) 0.0086(13) 0.0060(13) C28 0.0287(15) 0.0296(16) 0.0351(18) 0.0129(14) 0.0083(13) 0.0060(13) C29 0.0313(16) 0.0361(18) 0.054(2) 0.0218(16) -0.0042(15) 0.0037(14) C30 0.0402(18) 0.0366(19) 0.066(3) 0.0198(18) -0.0120(18) 0.0010(15) C31 0.0301(15) 0.0344(17) 0.0351(18) 0.0141(14) 0.0074(14) -0.0001(13) C32 0.046(2) 0.058(2) 0.046(2) 0.0078(19) 0.0127(17) -0.0020(18) C33 0.0304(15) 0.0349(17) 0.0349(18) 0.0161(14) 0.0038(14) 0.0047(13) C34 0.0491(19) 0.048(2) 0.040(2) 0.0244(17) 0.0152(16) 0.0070(16) C35 0.0313(16) 0.0404(18) 0.0398(19) 0.0212(15) 0.0067(14) 0.0090(14) C36 0.0363(18) 0.065(2) 0.055(2) 0.035(2) 0.0073(16) 0.0106(17) O101 0.0538(14) 0.0526(15) 0.0467(16) 0.0222(14) -0.0084(12) -0.0038(12) O102 0.0397(15) 0.083(2) 0.080(2) 0.0270(17) 0.0027(14) 0.0055(14) N1 0.0393(16) 0.0565(19) 0.049(2) 0.0287(16) 0.0016(14) -0.0038(14) N2 0.0437(18) 0.0464(18) 0.051(2) 0.0263(17) -0.0027(15) -0.0006(14) C37 0.0384(18) 0.066(2) 0.048(2) 0.036(2) 0.0056(16) 0.0079(17) C38 0.050(2) 0.061(2) 0.063(3) 0.040(2) 0.0163(19) 0.0131(18) C39 0.0419(19) 0.0424(19) 0.046(2) 0.0304(18) 0.0005(16) -0.0008(16) C40 0.049(2) 0.053(2) 0.050(2) 0.032(2) -0.0051(18) -0.0070(18) C41 0.068(3) 0.051(2) 0.053(3) 0.028(2) -0.020(2) -0.010(2) C42 0.070(3) 0.047(2) 0.046(2) 0.0188(19) -0.001(2) 0.010(2) C43 0.054(2) 0.047(2) 0.055(3) 0.026(2) 0.0028(19) 0.0095(18) C44 0.0420(19) 0.0401(19) 0.043(2) 0.0228(17) -0.0032(16) 0.0011(15) O103 0.071(2) 0.147(3) 0.062(2) 0.036(2) 0.0241(18) 0.005(2) O104 0.106(3) 0.286(7) 0.071(3) 0.080(4) 0.048(2) 0.057(3) N3 0.0406(15) 0.062(2) 0.0367(18) 0.0154(15) 0.0054(14) 0.0050(14) N4 0.077(3) 0.170(5) 0.054(3) 0.053(3) 0.026(2) 0.043(3) C45 0.0311(16) 0.047(2) 0.040(2) 0.0191(16) 0.0020(15) 0.0043(15) C46 0.0303(16) 0.048(2) 0.039(2) 0.0177(16) 0.0016(15) 0.0018(15) C47 0.056(2) 0.058(2) 0.038(2) 0.0146(19) 0.0040(18) 0.0205(19) C48 0.069(3) 0.048(2) 0.050(2) 0.0121(19) -0.003(2) 0.012(2) C49 0.095(3) 0.056(3) 0.061(3) 0.009(2) -0.017(3) 0.013(2) C50 0.122(5) 0.079(3) 0.041(3) 0.011(2) -0.003(3) 0.032(3) C51 0.108(4) 0.108(4) 0.054(3) 0.034(3) 0.023(3) 0.056(4) C52 0.066(3) 0.089(3) 0.044(3) 0.025(2) 0.012(2) 0.034(2) O105 0.079(2) 0.0593(19) 0.071(2) 0.0170(16) 0.0113(16) -0.0167(16) O106 0.078(2) 0.0456(17) 0.108(3) 0.0056(17) 0.0275(18) -0.0218(16) N5 0.0463(17) 0.0316(16) 0.075(2) 0.0227(16) 0.0121(16) 0.0008(13) N6 0.0547(19) 0.0334(17) 0.088(3) 0.0136(18) 0.024(2) -0.0019(15) C53 0.0277(15) 0.0311(17) 0.057(2) 0.0214(16) 0.0033(15) -0.0035(14) C54 0.0347(17) 0.0311(18) 0.069(3) 0.0204(17) 0.0093(17) 0.0020(15) C55 0.0422(19) 0.0298(18) 0.079(3) 0.0232(19) 0.011(2) 0.0078(16) C56 0.046(2) 0.045(2) 0.086(3) 0.035(2) 0.003(2) 0.0061(18) C57 0.063(2) 0.070(3) 0.085(3) 0.048(3) 0.008(2) 0.017(2) C58 0.065(3) 0.059(3) 0.100(4) 0.053(3) 0.027(3) 0.013(2) C59 0.053(2) 0.039(2) 0.107(4) 0.041(2) 0.030(2) 0.0122(18) C60 0.0437(19) 0.0290(18) 0.080(3) 0.0186(19) 0.016(2) 0.0063(16) O107 0.100(2) 0.077(2) 0.060(2) 0.0287(17) -0.0032(17) -0.0186(18) O108 0.0624(17) 0.0500(17) 0.085(2) 0.0140(16) -0.0067(15) -0.0105(14) N7 0.0377(15) 0.0456(18) 0.080(2) 0.0293(17) 0.0120(16) 0.0018(14) N8 0.0451(17) 0.052(2) 0.069(2) 0.0216(19) -0.0058(17) -0.0083(16) C61 0.0301(16) 0.0343(18) 0.085(3) 0.0277(19) 0.0199(18) 0.0048(14) C62 0.0321(17) 0.042(2) 0.092(3) 0.033(2) 0.0179(18) 0.0043(15) C63 0.0202(14) 0.0385(18) 0.062(2) 0.0223(18) 0.0065(15) 0.0056(14) C64 0.0303(17) 0.047(2) 0.066(3) 0.013(2) 0.0055(18) 0.0051(16) C65 0.043(2) 0.080(3) 0.054(3) 0.027(2) 0.0105(19) 0.003(2) C66 0.046(2) 0.080(3) 0.072(3) 0.039(3) 0.005(2) 0.003(2) C67 0.0336(18) 0.048(2) 0.084(3) 0.036(2) 0.0035(19) 0.0011(16) C68 0.0270(16) 0.0389(19) 0.064(3) 0.0220(18) 0.0010(16) 0.0031(15) O109 0.0684(16) 0.0472(15) 0.0466(16) 0.0127(13) -0.0059(13) 0.0126(13) O110 0.141(3) 0.0365(16) 0.077(2) 0.0087(15) -0.015(2) 0.0310(18) N9 0.0373(15) 0.0289(15) 0.065(2) 0.0099(15) -0.0048(15) 0.0011(12) N10 0.0610(18) 0.0377(17) 0.049(2) 0.0129(15) 0.0042(16) 0.0127(15) C69 0.0345(17) 0.0377(19) 0.061(2) 0.0227(17) -0.0097(17) -0.0014(15) C70 0.0365(18) 0.0304(18) 0.081(3) 0.0104(18) 0.0019(18) 0.0064(15) C71 0.0371(17) 0.0336(18) 0.057(2) 0.0171(17) 0.0048(17) 0.0009(15) C72 0.051(2) 0.049(2) 0.076(3) 0.032(2) 0.003(2) 0.0063(19) C73 0.070(3) 0.072(3) 0.074(3) 0.043(3) -0.001(2) 0.012(2) C74 0.091(3) 0.070(3) 0.048(3) 0.021(2) -0.011(2) 0.009(3) C75 0.079(3) 0.043(2) 0.047(2) 0.0101(19) -0.005(2) 0.006(2) C76 0.0456(19) 0.0342(18) 0.047(2) 0.0160(16) 0.0045(17) 0.0074(15) O111 0.0641(16) 0.0774(19) 0.0497(16) 0.0360(15) -0.0048(13) -0.0234(15) O112 0.0714(17) 0.0648(17) 0.0393(16) 0.0272(13) 0.0036(13) 0.0099(14) N11 0.0467(16) 0.0533(18) 0.0322(16) 0.0239(14) 0.0014(13) -0.0092(14) N12 0.0499(17) 0.0555(19) 0.0367(18) 0.0217(15) 0.0027(14) 0.0038(15) C77 0.0363(16) 0.0361(17) 0.0302(18) 0.0139(14) 0.0059(14) 0.0009(14) C78 0.0371(17) 0.0446(19) 0.0352(19) 0.0211(16) 0.0059(14) 0.0042(15) C79 0.0359(17) 0.0444(19) 0.041(2) 0.0246(16) 0.0055(15) 0.0033(15) C80 0.0447(19) 0.043(2) 0.043(2) 0.0193(17) 0.0058(16) -0.0004(16) C81 0.0451(19) 0.047(2) 0.055(2) 0.0250(18) 0.0054(18) 0.0002(17) C82 0.046(2) 0.055(2) 0.062(3) 0.035(2) 0.0196(19) 0.0074(18) C83 0.054(2) 0.056(2) 0.050(2) 0.0352(19) 0.0161(18) 0.0166(19) C84 0.0419(18) 0.0415(19) 0.039(2) 0.0217(16) 0.0072(15) 0.0046(15) O113 0.0754(18) 0.0662(19) 0.0477(17) 0.0209(14) 0.0006(14) -0.0171(15) O114 0.0610(16) 0.0551(17) 0.072(2) 0.0259(15) 0.0051(14) -0.0128(14) N13 0.0500(18) 0.0407(18) 0.061(2) 0.0137(16) 0.0115(16) 0.0021(14) N14 0.0472(17) 0.0468(18) 0.049(2) 0.0148(15) 0.0014(15) 0.0029(15) C85 0.049(2) 0.035(2) 0.111(4) 0.021(2) 0.002(2) 0.0038(18) C86 0.0421(19) 0.036(2) 0.104(3) 0.027(2) 0.012(2) 0.0056(17) C87 0.0379(18) 0.050(2) 0.052(2) 0.0087(19) 0.0001(18) 0.0149(17) C88 0.056(2) 0.056(3) 0.067(3) 0.011(2) -0.012(2) 0.006(2) C89 0.083(3) 0.077(3) 0.054(3) 0.001(3) -0.021(3) 0.023(3) C90 0.091(3) 0.082(3) 0.058(3) 0.021(3) 0.001(3) 0.026(3) C91 0.068(3) 0.064(3) 0.055(3) 0.027(2) 0.005(2) 0.023(2) C92 0.0412(19) 0.046(2) 0.046(2) 0.0139(17) -0.0020(17) 0.0080(17) O115 0.0642(17) 0.0583(18) 0.065(2) 0.0145(16) 0.0107(15) -0.0096(14) O116 0.0693(19) 0.067(2) 0.160(4) 0.068(2) -0.006(2) -0.0308(17) N15 0.0335(14) 0.0413(17) 0.056(2) 0.0220(15) 0.0132(14) 0.0000(12) N16 0.0350(16) 0.0438(19) 0.088(3) 0.0257(19) 0.0165(17) 0.0007(14) C93 0.0321(16) 0.0388(19) 0.057(2) 0.0224(17) 0.0139(16) -0.0007(14) C94 0.0360(18) 0.044(2) 0.070(3) 0.0281(19) 0.0150(17) 0.0072(16) C95 0.0293(16) 0.0366(19) 0.064(3) 0.0182(18) 0.0169(17) 0.0116(15) C96 0.042(2) 0.054(2) 0.060(3) 0.015(2) 0.0134(19) 0.0132(18) C97 0.061(3) 0.078(3) 0.060(3) 0.025(2) 0.009(2) 0.023(2) C98 0.081(3) 0.119(4) 0.081(4) 0.070(3) 0.032(3) 0.045(3) C99 0.068(3) 0.072(3) 0.094(4) 0.056(3) 0.032(3) 0.027(2) C100 0.0304(16) 0.043(2) 0.066(3) 0.0248(19) 0.0146(17) 0.0083(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O4 C4 1.374(4) . ? O4 C37 1.424(4) . ? O6 C6 1.394(3) . ? O6 C45 1.440(4) . ? O11 C11 1.386(4) . ? O11 C53 1.419(3) . ? O13 C13 1.390(4) . ? O13 C61 1.431(4) . ? O18 C18 1.392(3) . ? O18 C69 1.404(4) . ? O20 C20 1.370(3) . ? O20 C77 1.420(4) . ? O25 C85 1.386(4) . ? O25 C25 1.391(4) . ? O27 C27 1.391(3) . ? O27 C93 1.427(4) . ? C1 C6 1.380(4) . ? C1 C2 1.404(4) . ? C1 C28 1.515(4) . ? C2 C3 1.389(4) . ? C3 C4 1.390(4) . ? C3 C7 1.524(4) . ? C4 C5 1.386(4) . ? C5 C6 1.383(4) . ? C7 C29 1.516(5) . ? C7 C8 1.529(4) . ? C8 C13 1.386(4) . ? C8 C9 1.391(4) . ? C9 C10 1.394(4) . ? C10 C11 1.391(4) . ? C10 C14 1.518(4) . ? C11 C12 1.385(4) . ? C12 C13 1.391(4) . ? C14 C31 1.527(4) . ? C14 C15 1.529(4) . ? C15 C16 1.380(4) . ? C15 C20 1.393(4) . ? C16 C17 1.406(4) . ? C17 C18 1.379(4) . ? C17 C21 1.521(4) . ? C18 C19 1.394(4) . ? C19 C20 1.392(4) . ? C21 C22 1.530(4) . ? C21 C33 1.533(4) . ? C22 C27 1.381(4) . ? C22 C23 1.391(4) . ? C23 C24 1.394(4) . ? C24 C25 1.385(4) . ? C24 C28 1.528(4) . ? C25 C26 1.388(4) . ? C26 C27 1.390(4) . ? C28 C35 1.534(4) . ? C29 C30 1.527(4) . ? C31 C32 1.495(5) . ? C33 C34 1.518(4) . ? C35 C36 1.516(4) . ? O101 N2 1.243(4) . ? O102 N2 1.230(4) . ? N1 C39 1.351(5) . ? N1 C38 1.449(5) . ? N2 C44 1.435(4) . ? C37 C38 1.502(5) . ? C39 C44 1.415(5) . ? C39 C40 1.424(5) . ? C40 C41 1.352(6) . ? C41 C42 1.394(6) . ? C42 C43 1.364(5) . ? C43 C44 1.396(5) . ? O103 N4 1.241(6) . ? O104 N4 1.242(5) . ? N3 C47 1.364(5) . ? N3 C46 1.450(4) . ? N4 C52 1.440(6) . ? C45 C46 1.506(4) . ? C47 C52 1.398(6) . ? C47 C48 1.404(5) . ? C48 C49 1.375(6) . ? C49 C50 1.378(7) . ? C50 C51 1.348(7) . ? C51 C52 1.417(7) . ? O105 N6 1.233(4) . ? O106 N6 1.235(4) . ? N5 C55 1.359(5) . ? N5 C54 1.451(4) . ? N6 C60 1.451(5) . ? C53 C54 1.502(5) . ? C55 C56 1.410(6) . ? C55 C60 1.421(5) . ? C56 C57 1.361(6) . ? C57 C58 1.386(6) . ? C58 C59 1.353(6) . ? C59 C60 1.401(6) . ? O107 N8 1.242(4) . ? O108 N8 1.217(4) . ? N7 C63 1.346(5) . ? N7 C62 1.466(4) . ? N8 C68 1.458(5) . ? C61 C62 1.527(5) . ? C63 C68 1.417(4) . ? C63 C64 1.421(5) . ? C64 C65 1.361(6) . ? C65 C66 1.387(6) . ? C66 C67 1.366(6) . ? C67 C68 1.361(5) . ? O109 N10 1.223(4) . ? O110 N10 1.228(4) . ? N9 C71 1.358(5) . ? N9 C70 1.448(4) . ? N10 C76 1.428(5) . ? C69 C70 1.491(5) . ? C71 C76 1.420(5) . ? C71 C72 1.421(5) . ? C72 C73 1.354(6) . ? C73 C74 1.389(6) . ? C74 C75 1.359(6) . ? C75 C76 1.393(5) . ? O111 N12 1.229(4) . ? O112 N12 1.241(4) . ? N11 C79 1.345(4) . ? N11 C78 1.451(4) . ? N12 C84 1.427(4) . ? C77 C78 1.499(4) . ? C79 C80 1.417(4) . ? C79 C84 1.424(5) . ? C80 C81 1.366(5) . ? C81 C82 1.383(5) . ? C82 C83 1.366(5) . ? C83 C84 1.398(5) . ? O113 N14 1.250(4) . ? O114 N14 1.239(4) . ? N13 C87 1.353(5) . ? N13 C86 1.455(5) . ? N14 C92 1.423(4) . ? C85 C86 1.531(6) . ? C87 C88 1.406(5) . ? C87 C92 1.424(5) . ? C88 C89 1.386(7) . ? C89 C90 1.385(7) . ? C90 C91 1.363(6) . ? C91 C92 1.401(6) . ? O115 N16 1.237(4) . ? O116 N16 1.219(4) . ? N15 C95 1.370(5) . ? N15 C94 1.449(4) . ? N16 C100 1.430(5) . ? C93 C94 1.487(5) . ? C95 C96 1.403(5) . ? C95 C100 1.435(5) . ? C96 C97 1.356(6) . ? C97 C98 1.371(7) . ? C98 C99 1.378(7) . ? C99 C100 1.382(6) . ? 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 C4 O4 C37 117.0(2) . . ? C6 O6 C45 115.8(2) . . ? C11 O11 C53 116.1(2) . . ? C13 O13 C61 114.9(2) . . ? C18 O18 C69 117.7(2) . . ? C20 O20 C77 120.3(2) . . ? C85 O25 C25 117.8(3) . . ? C27 O27 C93 115.8(2) . . ? C6 C1 C2 116.3(3) . . ? C6 C1 C28 120.4(2) . . ? C2 C1 C28 123.2(3) . . ? C3 C2 C1 123.3(3) . . ? C2 C3 C4 117.5(3) . . ? C2 C3 C7 123.0(3) . . ? C4 C3 C7 119.2(3) . . ? O4 C4 C5 123.1(3) . . ? O4 C4 C3 116.0(2) . . ? C5 C4 C3 120.9(3) . . ? C6 C5 C4 119.5(3) . . ? C1 C6 C5 122.3(3) . . ? C1 C6 O6 119.3(3) . . ? C5 C6 O6 118.2(3) . . ? C29 C7 C3 114.4(3) . . ? C29 C7 C8 112.1(3) . . ? C3 C7 C8 108.8(2) . . ? C13 C8 C9 117.2(3) . . ? C13 C8 C7 122.8(3) . . ? C9 C8 C7 120.0(3) . . ? C8 C9 C10 123.7(3) . . ? C11 C10 C9 116.9(3) . . ? C11 C10 C14 122.5(3) . . ? C9 C10 C14 120.4(3) . . ? C12 C11 O11 121.2(3) . . ? C12 C11 C10 121.3(3) . . ? O11 C11 C10 117.5(3) . . ? C11 C12 C13 119.8(3) . . ? C8 C13 O13 118.0(3) . . ? C8 C13 C12 121.1(3) . . ? O13 C13 C12 120.9(3) . . ? C10 C14 C31 108.7(2) . . ? C10 C14 C15 111.2(2) . . ? C31 C14 C15 114.8(2) . . ? C16 C15 C20 117.1(2) . . ? C16 C15 C14 124.6(3) . . ? C20 C15 C14 118.3(2) . . ? C15 C16 C17 123.4(3) . . ? C18 C17 C16 116.8(3) . . ? C18 C17 C21 120.2(2) . . ? C16 C17 C21 123.0(3) . . ? C17 C18 O18 117.3(2) . . ? C17 C18 C19 122.4(2) . . ? O18 C18 C19 120.2(3) . . ? C20 C19 C18 118.2(3) . . ? O20 C20 C19 123.5(3) . . ? O20 C20 C15 114.5(2) . . ? C19 C20 C15 122.0(3) . . ? C17 C21 C22 110.8(2) . . ? C17 C21 C33 114.0(2) . . ? C22 C21 C33 111.3(2) . . ? C27 C22 C23 116.6(3) . . ? C27 C22 C21 122.9(2) . . ? C23 C22 C21 120.5(2) . . ? C22 C23 C24 123.8(3) . . ? C25 C24 C23 117.1(3) . . ? C25 C24 C28 122.2(3) . . ? C23 C24 C28 120.6(3) . . ? C24 C25 C26 121.2(3) . . ? C24 C25 O25 117.3(3) . . ? C26 C25 O25 121.6(3) . . ? C25 C26 C27 119.4(3) . . ? C22 C27 C26 121.9(3) . . ? C22 C27 O27 117.3(3) . . ? C26 C27 O27 120.8(2) . . ? C1 C28 C24 110.5(3) . . ? C1 C28 C35 114.5(2) . . ? C24 C28 C35 110.0(2) . . ? C7 C29 C30 113.5(3) . . ? C32 C31 C14 115.3(3) . . ? C34 C33 C21 113.5(2) . . ? C36 C35 C28 113.1(3) . . ? C39 N1 C38 124.9(3) . . ? O102 N2 O101 121.4(3) . . ? O102 N2 C44 118.9(3) . . ? O101 N2 C44 119.6(3) . . ? O4 C37 C38 107.0(3) . . ? N1 C38 C37 114.1(3) . . ? N1 C39 C44 124.3(3) . . ? N1 C39 C40 120.8(3) . . ? C44 C39 C40 114.9(3) . . ? C41 C40 C39 121.6(4) . . ? C40 C41 C42 122.7(3) . . ? C43 C42 C41 117.6(4) . . ? C42 C43 C44 121.1(4) . . ? C43 C44 C39 122.1(3) . . ? C43 C44 N2 116.0(3) . . ? C39 C44 N2 121.9(3) . . ? C47 N3 C46 123.8(3) . . ? O103 N4 O104 120.3(5) . . ? O103 N4 C52 120.7(4) . . ? O104 N4 C52 118.9(5) . . ? O6 C45 C46 107.0(3) . . ? N3 C46 C45 108.8(3) . . ? N3 C47 C52 123.2(4) . . ? N3 C47 C48 120.1(4) . . ? C52 C47 C48 116.6(4) . . ? C49 C48 C47 121.2(4) . . ? C48 C49 C50 121.2(5) . . ? C51 C50 C49 119.6(5) . . ? C50 C51 C52 120.4(5) . . ? C47 C52 C51 120.9(4) . . ? C47 C52 N4 122.0(4) . . ? C51 C52 N4 117.1(4) . . ? C55 N5 C54 125.3(3) . . ? O105 N6 O106 121.2(4) . . ? O105 N6 C60 120.0(3) . . ? O106 N6 C60 118.8(4) . . ? O11 C53 C54 107.8(2) . . ? N5 C54 C53 110.6(3) . . ? N5 C55 C56 121.8(3) . . ? N5 C55 C60 123.1(4) . . ? C56 C55 C60 115.0(4) . . ? C57 C56 C55 121.9(4) . . ? C56 C57 C58 121.8(5) . . ? C59 C58 C57 118.9(4) . . ? C58 C59 C60 120.4(4) . . ? C59 C60 C55 121.9(4) . . ? C59 C60 N6 116.8(3) . . ? C55 C60 N6 121.2(4) . . ? C63 N7 C62 124.2(3) . . ? O108 N8 O107 121.3(4) . . ? O108 N8 C68 119.6(4) . . ? O107 N8 C68 119.1(3) . . ? O13 C61 C62 108.1(3) . . ? N7 C62 C61 108.6(3) . . ? N7 C63 C68 124.7(3) . . ? N7 C63 C64 121.4(3) . . ? C68 C63 C64 113.8(3) . . ? C65 C64 C63 122.2(3) . . ? C64 C65 C66 120.6(4) . . ? C67 C66 C65 119.7(4) . . ? C68 C67 C66 119.5(4) . . ? C67 C68 C63 124.0(4) . . ? C67 C68 N8 115.4(3) . . ? C63 C68 N8 120.6(3) . . ? C71 N9 C70 126.9(3) . . ? O109 N10 O110 120.0(3) . . ? O109 N10 C76 120.7(3) . . ? O110 N10 C76 119.3(3) . . ? O18 C69 C70 108.3(3) . . ? N9 C70 C69 112.4(3) . . ? N9 C71 C76 122.9(3) . . ? N9 C71 C72 121.7(3) . . ? C76 C71 C72 115.4(3) . . ? C73 C72 C71 122.2(4) . . ? C72 C73 C74 121.2(4) . . ? C75 C74 C73 118.9(4) . . ? C74 C75 C76 121.4(4) . . ? C75 C76 C71 120.9(3) . . ? C75 C76 N10 117.5(3) . . ? C71 C76 N10 121.6(3) . . ? C79 N11 C78 122.6(3) . . ? O111 N12 O112 120.9(3) . . ? O111 N12 C84 120.7(3) . . ? O112 N12 C84 118.4(3) . . ? O20 C77 C78 103.7(2) . . ? N11 C78 C77 110.7(2) . . ? N11 C79 C80 120.7(3) . . ? N11 C79 C84 124.1(3) . . ? C80 C79 C84 115.2(3) . . ? C81 C80 C79 121.9(3) . . ? C80 C81 C82 121.7(3) . . ? C83 C82 C81 118.8(3) . . ? C82 C83 C84 120.8(3) . . ? C83 C84 C79 121.5(3) . . ? C83 C84 N12 117.1(3) . . ? C79 C84 N12 121.3(3) . . ? C87 N13 C86 124.4(3) . . ? O114 N14 O113 120.9(3) . . ? O114 N14 C92 119.6(3) . . ? O113 N14 C92 119.5(3) . . ? O25 C85 C86 108.6(3) . . ? N13 C86 C85 107.2(3) . . ? N13 C87 C88 119.5(4) . . ? N13 C87 C92 124.4(3) . . ? C88 C87 C92 116.1(4) . . ? C89 C88 C87 120.6(4) . . ? C90 C89 C88 122.3(4) . . ? C91 C90 C89 118.8(5) . . ? C90 C91 C92 120.4(4) . . ? C91 C92 N14 116.2(3) . . ? C91 C92 C87 121.8(3) . . ? N14 C92 C87 122.0(4) . . ? C95 N15 C94 124.2(3) . . ? O116 N16 O115 119.8(4) . . ? O116 N16 C100 119.6(4) . . ? O115 N16 C100 120.5(3) . . ? O27 C93 C94 108.4(3) . . ? N15 C94 C93 110.2(3) . . ? N15 C95 C96 121.4(3) . . ? N15 C95 C100 123.0(3) . . ? C96 C95 C100 115.6(4) . . ? C97 C96 C95 121.2(4) . . ? C96 C97 C98 122.6(4) . . ? C97 C98 C99 118.9(4) . . ? C98 C99 C100 119.9(4) . . ? C99 C100 N16 117.6(4) . . ? C99 C100 C95 121.7(4) . . ? N16 C100 C95 120.7(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 C6 C1 C2 C3 -2.3(5) . . . . ? C28 C1 C2 C3 179.1(3) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C1 C2 C3 C7 175.1(3) . . . . ? C37 O4 C4 C5 20.4(5) . . . . ? C37 O4 C4 C3 -160.0(3) . . . . ? C2 C3 C4 O4 -179.0(3) . . . . ? C7 C3 C4 O4 6.2(4) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C7 C3 C4 C5 -174.3(3) . . . . ? O4 C4 C5 C6 179.8(3) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? C2 C1 C6 C5 3.2(5) . . . . ? C28 C1 C6 C5 -178.2(3) . . . . ? C2 C1 C6 O6 178.5(3) . . . . ? C28 C1 C6 O6 -2.9(4) . . . . ? C4 C5 C6 C1 -2.3(5) . . . . ? C4 C5 C6 O6 -177.6(3) . . . . ? C45 O6 C6 C1 117.3(3) . . . . ? C45 O6 C6 C5 -67.2(4) . . . . ? C2 C3 C7 C29 11.1(4) . . . . ? C4 C3 C7 C29 -174.3(3) . . . . ? C2 C3 C7 C8 -115.1(3) . . . . ? C4 C3 C7 C8 59.5(4) . . . . ? C29 C7 C8 C13 99.7(3) . . . . ? C3 C7 C8 C13 -132.8(3) . . . . ? C29 C7 C8 C9 -81.2(3) . . . . ? C3 C7 C8 C9 46.3(4) . . . . ? C13 C8 C9 C10 -0.8(5) . . . . ? C7 C8 C9 C10 -180.0(3) . . . . ? C8 C9 C10 C11 1.9(4) . . . . ? C8 C9 C10 C14 -173.8(3) . . . . ? C53 O11 C11 C12 -28.3(4) . . . . ? C53 O11 C11 C10 151.6(3) . . . . ? C9 C10 C11 C12 -0.7(4) . . . . ? C14 C10 C11 C12 174.8(3) . . . . ? C9 C10 C11 O11 179.4(3) . . . . ? C14 C10 C11 O11 -5.1(4) . . . . ? O11 C11 C12 C13 178.4(3) . . . . ? C10 C11 C12 C13 -1.4(5) . . . . ? C9 C8 C13 O13 179.7(3) . . . . ? C7 C8 C13 O13 -1.2(4) . . . . ? C9 C8 C13 C12 -1.4(5) . . . . ? C7 C8 C13 C12 177.7(3) . . . . ? C61 O13 C13 C8 -148.1(3) . . . . ? C61 O13 C13 C12 33.0(4) . . . . ? C11 C12 C13 C8 2.5(5) . . . . ? C11 C12 C13 O13 -178.6(3) . . . . ? C11 C10 C14 C31 -103.0(3) . . . . ? C9 C10 C14 C31 72.3(3) . . . . ? C11 C10 C14 C15 129.6(3) . . . . ? C9 C10 C14 C15 -55.1(4) . . . . ? C10 C14 C15 C16 115.3(3) . . . . ? C31 C14 C15 C16 -8.6(4) . . . . ? C10 C14 C15 C20 -65.3(3) . . . . ? C31 C14 C15 C20 170.7(3) . . . . ? C20 C15 C16 C17 -0.5(4) . . . . ? C14 C15 C16 C17 178.8(3) . . . . ? C15 C16 C17 C18 1.0(4) . . . . ? C15 C16 C17 C21 -177.5(3) . . . . ? C16 C17 C18 O18 178.4(2) . . . . ? C21 C17 C18 O18 -3.1(4) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? C21 C17 C18 C19 178.7(3) . . . . ? C69 O18 C18 C17 130.2(3) . . . . ? C69 O18 C18 C19 -51.5(4) . . . . ? C17 C18 C19 C20 -1.7(5) . . . . ? O18 C18 C19 C20 -179.9(3) . . . . ? C77 O20 C20 C19 -5.4(4) . . . . ? C77 O20 C20 C15 174.5(3) . . . . ? C18 C19 C20 O20 -177.9(3) . . . . ? C18 C19 C20 C15 2.2(5) . . . . ? C16 C15 C20 O20 178.9(3) . . . . ? C14 C15 C20 O20 -0.5(4) . . . . ? C16 C15 C20 C19 -1.1(4) . . . . ? C14 C15 C20 C19 179.5(3) . . . . ? C18 C17 C21 C22 73.9(3) . . . . ? C16 C17 C21 C22 -107.6(3) . . . . ? C18 C17 C21 C33 -159.7(3) . . . . ? C16 C17 C21 C33 18.8(4) . . . . ? C17 C21 C22 C27 -131.9(3) . . . . ? C33 C21 C22 C27 100.2(3) . . . . ? C17 C21 C22 C23 47.6(4) . . . . ? C33 C21 C22 C23 -80.3(3) . . . . ? C27 C22 C23 C24 1.2(5) . . . . ? C21 C22 C23 C24 -178.3(3) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C22 C23 C24 C28 178.6(3) . . . . ? C23 C24 C25 C26 -1.8(5) . . . . ? C28 C24 C25 C26 179.9(3) . . . . ? C23 C24 C25 O25 177.9(3) . . . . ? C28 C24 C25 O25 -0.5(5) . . . . ? C85 O25 C25 C24 -175.3(4) . . . . ? C85 O25 C25 C26 4.3(5) . . . . ? C24 C25 C26 C27 1.9(5) . . . . ? O25 C25 C26 C27 -177.7(3) . . . . ? C23 C22 C27 C26 -1.1(5) . . . . ? C21 C22 C27 C26 178.5(3) . . . . ? C23 C22 C27 O27 -179.4(3) . . . . ? C21 C22 C27 O27 0.1(4) . . . . ? C25 C26 C27 C22 -0.5(5) . . . . ? C25 C26 C27 O27 177.9(3) . . . . ? C93 O27 C27 C22 -161.1(3) . . . . ? C93 O27 C27 C26 20.5(4) . . . . ? C6 C1 C28 C24 -55.2(4) . . . . ? C2 C1 C28 C24 123.3(3) . . . . ? C6 C1 C28 C35 179.9(3) . . . . ? C2 C1 C28 C35 -1.6(4) . . . . ? C25 C24 C28 C1 128.5(3) . . . . ? C23 C24 C28 C1 -49.8(4) . . . . ? C25 C24 C28 C35 -104.1(3) . . . . ? C23 C24 C28 C35 77.6(4) . . . . ? C3 C7 C29 C30 171.8(3) . . . . ? C8 C7 C29 C30 -63.7(4) . . . . ? C10 C14 C31 C32 164.7(3) . . . . ? C15 C14 C31 C32 -70.0(4) . . . . ? C17 C21 C33 C34 172.2(3) . . . . ? C22 C21 C33 C34 -61.6(3) . . . . ? C1 C28 C35 C36 -173.6(3) . . . . ? C24 C28 C35 C36 61.2(4) . . . . ? C4 O4 C37 C38 165.2(3) . . . . ? C39 N1 C38 C37 78.6(4) . . . . ? O4 C37 C38 N1 61.5(4) . . . . ? C38 N1 C39 C44 175.3(3) . . . . ? C38 N1 C39 C40 -3.8(5) . . . . ? N1 C39 C40 C41 179.9(3) . . . . ? C44 C39 C40 C41 0.7(5) . . . . ? C39 C40 C41 C42 0.1(6) . . . . ? C40 C41 C42 C43 -0.4(6) . . . . ? C41 C42 C43 C44 -0.2(6) . . . . ? C42 C43 C44 C39 1.1(6) . . . . ? C42 C43 C44 N2 -176.8(3) . . . . ? N1 C39 C44 C43 179.5(3) . . . . ? C40 C39 C44 C43 -1.3(5) . . . . ? N1 C39 C44 N2 -2.8(5) . . . . ? C40 C39 C44 N2 176.4(3) . . . . ? O102 N2 C44 C43 1.3(5) . . . . ? O101 N2 C44 C43 -179.4(3) . . . . ? O102 N2 C44 C39 -176.5(3) . . . . ? O101 N2 C44 C39 2.8(5) . . . . ? C6 O6 C45 C46 151.2(3) . . . . ? C47 N3 C46 C45 -177.2(3) . . . . ? O6 C45 C46 N3 -66.2(3) . . . . ? C46 N3 C47 C52 177.7(4) . . . . ? C46 N3 C47 C48 -4.9(6) . . . . ? N3 C47 C48 C49 179.3(4) . . . . ? C52 C47 C48 C49 -3.1(6) . . . . ? C47 C48 C49 C50 1.8(7) . . . . ? C48 C49 C50 C51 0.5(8) . . . . ? C49 C50 C51 C52 -1.4(8) . . . . ? N3 C47 C52 C51 179.7(4) . . . . ? C48 C47 C52 C51 2.2(6) . . . . ? N3 C47 C52 N4 -1.3(7) . . . . ? C48 C47 C52 N4 -178.9(4) . . . . ? C50 C51 C52 C47 0.0(8) . . . . ? C50 C51 C52 N4 -179.0(5) . . . . ? O103 N4 C52 C47 -6.5(7) . . . . ? O104 N4 C52 C47 171.5(5) . . . . ? O103 N4 C52 C51 172.5(5) . . . . ? O104 N4 C52 C51 -9.5(7) . . . . ? C11 O11 C53 C54 -163.1(3) . . . . ? C55 N5 C54 C53 78.3(5) . . . . ? O11 C53 C54 N5 168.3(3) . . . . ? C54 N5 C55 C56 12.4(6) . . . . ? C54 N5 C55 C60 -171.1(3) . . . . ? N5 C55 C56 C57 176.0(4) . . . . ? C60 C55 C56 C57 -0.7(6) . . . . ? C55 C56 C57 C58 0.0(7) . . . . ? C56 C57 C58 C59 1.2(7) . . . . ? C57 C58 C59 C60 -1.6(6) . . . . ? C58 C59 C60 C55 0.8(6) . . . . ? C58 C59 C60 N6 178.0(4) . . . . ? N5 C55 C60 C59 -176.3(4) . . . . ? C56 C55 C60 C59 0.4(5) . . . . ? N5 C55 C60 N6 6.6(6) . . . . ? C56 C55 C60 N6 -176.7(3) . . . . ? O105 N6 C60 C59 -177.4(4) . . . . ? O106 N6 C60 C59 2.1(5) . . . . ? O105 N6 C60 C55 -0.2(6) . . . . ? O106 N6 C60 C55 179.4(4) . . . . ? C13 O13 C61 C62 156.1(3) . . . . ? C63 N7 C62 C61 -78.2(5) . . . . ? O13 C61 C62 N7 -170.4(3) . . . . ? C62 N7 C63 C68 171.3(3) . . . . ? C62 N7 C63 C64 -11.1(5) . . . . ? N7 C63 C64 C65 -173.9(4) . . . . ? C68 C63 C64 C65 4.0(5) . . . . ? C63 C64 C65 C66 -4.3(6) . . . . ? C64 C65 C66 C67 2.4(7) . . . . ? C65 C66 C67 C68 -0.4(6) . . . . ? C66 C67 C68 C63 0.4(6) . . . . ? C66 C67 C68 N8 -179.3(3) . . . . ? N7 C63 C68 C67 175.8(3) . . . . ? C64 C63 C68 C67 -2.0(5) . . . . ? N7 C63 C68 N8 -4.6(5) . . . . ? C64 C63 C68 N8 177.6(3) . . . . ? O108 N8 C68 C67 -3.1(5) . . . . ? O107 N8 C68 C67 175.2(4) . . . . ? O108 N8 C68 C63 177.2(3) . . . . ? O107 N8 C68 C63 -4.4(5) . . . . ? C18 O18 C69 C70 -148.8(3) . . . . ? C71 N9 C70 C69 -98.8(4) . . . . ? O18 C69 C70 N9 -63.5(4) . . . . ? C70 N9 C71 C76 -177.9(3) . . . . ? C70 N9 C71 C72 2.0(6) . . . . ? N9 C71 C72 C73 -178.2(4) . . . . ? C76 C71 C72 C73 1.7(6) . . . . ? C71 C72 C73 C74 -2.0(7) . . . . ? C72 C73 C74 C75 1.2(7) . . . . ? C73 C74 C75 C76 -0.2(7) . . . . ? C74 C75 C76 C71 0.0(6) . . . . ? C74 C75 C76 N10 178.6(4) . . . . ? N9 C71 C76 C75 179.2(4) . . . . ? C72 C71 C76 C75 -0.7(5) . . . . ? N9 C71 C76 N10 0.6(5) . . . . ? C72 C71 C76 N10 -179.2(3) . . . . ? O109 N10 C76 C75 178.6(3) . . . . ? O110 N10 C76 C75 0.2(5) . . . . ? O109 N10 C76 C71 -2.8(5) . . . . ? O110 N10 C76 C71 178.8(4) . . . . ? C20 O20 C77 C78 -175.9(3) . . . . ? C79 N11 C78 C77 -174.1(3) . . . . ? O20 C77 C78 N11 -176.2(3) . . . . ? C78 N11 C79 C80 -2.5(5) . . . . ? C78 N11 C79 C84 177.0(3) . . . . ? N11 C79 C80 C81 177.3(4) . . . . ? C84 C79 C80 C81 -2.2(5) . . . . ? C79 C80 C81 C82 0.7(6) . . . . ? C80 C81 C82 C83 0.1(6) . . . . ? C81 C82 C83 C84 0.6(6) . . . . ? C82 C83 C84 C79 -2.2(6) . . . . ? C82 C83 C84 N12 178.4(3) . . . . ? N11 C79 C84 C83 -176.6(4) . . . . ? C80 C79 C84 C83 2.9(5) . . . . ? N11 C79 C84 N12 2.7(6) . . . . ? C80 C79 C84 N12 -177.8(3) . . . . ? O111 N12 C84 C83 177.1(3) . . . . ? O112 N12 C84 C83 -3.9(5) . . . . ? O111 N12 C84 C79 -2.3(5) . . . . ? O112 N12 C84 C79 176.8(3) . . . . ? C25 O25 C85 C86 177.7(3) . . . . ? C87 N13 C86 C85 -74.6(5) . . . . ? O25 C85 C86 N13 156.2(4) . . . . ? C86 N13 C87 C88 -2.6(6) . . . . ? C86 N13 C87 C92 178.4(3) . . . . ? N13 C87 C88 C89 -179.1(4) . . . . ? C92 C87 C88 C89 0.0(6) . . . . ? C87 C88 C89 C90 0.1(7) . . . . ? C88 C89 C90 C91 -0.1(8) . . . . ? C89 C90 C91 C92 0.2(7) . . . . ? C90 C91 C92 N14 -179.7(4) . . . . ? C90 C91 C92 C87 -0.1(6) . . . . ? O114 N14 C92 C91 1.8(5) . . . . ? O113 N14 C92 C91 -178.9(4) . . . . ? O114 N14 C92 C87 -177.8(3) . . . . ? O113 N14 C92 C87 1.5(5) . . . . ? N13 C87 C92 C91 179.1(4) . . . . ? C88 C87 C92 C91 0.0(6) . . . . ? N13 C87 C92 N14 -1.3(6) . . . . ? C88 C87 C92 N14 179.6(3) . . . . ? C27 O27 C93 C94 167.5(3) . . . . ? C95 N15 C94 C93 79.1(4) . . . . ? O27 C93 C94 N15 -179.1(3) . . . . ? C94 N15 C95 C96 7.3(5) . . . . ? C94 N15 C95 C100 -175.1(3) . . . . ? N15 C95 C96 C97 176.4(4) . . . . ? C100 C95 C96 C97 -1.3(5) . . . . ? C95 C96 C97 C98 -0.6(7) . . . . ? C96 C97 C98 C99 1.4(7) . . . . ? C97 C98 C99 C100 -0.2(7) . . . . ? C98 C99 C100 N16 178.5(4) . . . . ? C98 C99 C100 C95 -1.7(6) . . . . ? O116 N16 C100 C99 -6.0(5) . . . . ? O115 N16 C100 C99 172.3(4) . . . . ? O116 N16 C100 C95 174.2(4) . . . . ? O115 N16 C100 C95 -7.5(5) . . . . ? N15 C95 C100 C99 -175.3(3) . . . . ? C96 C95 C100 C99 2.4(5) . . . . ? N15 C95 C100 N16 4.5(5) . . . . ? C96 C95 C100 N16 -177.8(3) . . . . ? 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 N1 H1N O101 0.913(19) 1.91(3) 2.629(4) 134(3) . N3 H3N O103 0.931(19) 1.92(3) 2.627(4) 131(3) . N5 H5N O105 0.926(19) 1.93(3) 2.612(4) 129(3) . N5 H5N O105 0.926(19) 2.27(3) 3.038(5) 140(3) 2_786 N7 H7N O107 0.950(19) 1.80(3) 2.612(4) 142(3) . N7 H7N N8 0.950(19) 2.43(4) 2.931(4) 113(3) . N9 H9N O109 0.920(19) 1.92(3) 2.609(4) 131(3) . N11 H11N O111 0.923(19) 1.93(3) 2.630(4) 131(3) . N13 H13N O113 0.938(19) 1.94(3) 2.631(4) 129(3) . N15 H15N O115 0.936(19) 1.90(3) 2.599(4) 130(3) . _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 66.98 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.615 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.055 #===end data_2D _database_code_depnum_ccdc_archive 'CCDC 781924' #TrackingRef '- Octapodands.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H107 N17 O24' _chemical_formula_weight 1955.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 12.0137(3) _cell_length_b 20.2750(4) _cell_length_c 22.8339(4) _cell_angle_alpha 115.0720(10) _cell_angle_beta 96.5780(10) _cell_angle_gamma 99.681(2) _cell_volume 4857.30(18) _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 block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 0.802 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8561 _exptl_absorpt_correction_T_max 0.9241 _exptl_absorpt_process_details 'Denzo (Otwinowski, Majewski, Borek & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 23282 _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 67.12 _reflns_number_total 16813 _reflns_number_gt 11874 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0966P)^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 16813 _refine_ls_number_parameters 1310 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1913 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_restrained_S_all 1.230 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.304 0.515 0.084 18 3 ' ' 2 0.695 0.485 0.915 18 3 ' ' _platon_squeeze_details ; ; 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 O4 O 0.83518(15) 0.95153(11) 0.19644(9) 0.0359(4) Uani 1 1 d . . . O6 O 0.53822(14) 0.75968(10) 0.19620(9) 0.0333(4) Uani 1 1 d . . . O11 O 0.78018(14) 1.25457(10) 0.33114(9) 0.0319(4) Uani 1 1 d . . . O13 O 1.06667(14) 1.10836(11) 0.29181(10) 0.0377(5) Uani 1 1 d . . . O18 O 0.26515(14) 0.90931(10) 0.23683(9) 0.0324(4) Uani 1 1 d . . . O20 O 0.55666(15) 1.11340(11) 0.24827(9) 0.0356(4) Uani 1 1 d . . . O25 O 0.44647(15) 0.66558(10) 0.28335(10) 0.0381(5) Uani 1 1 d . . . O27 O 0.16460(14) 0.81560(10) 0.32891(10) 0.0335(4) Uani 1 1 d . . . C1 C 0.6857(2) 0.83683(14) 0.29390(12) 0.0251(5) Uani 1 1 d . . . C2 C 0.7854(2) 0.89555(14) 0.32353(13) 0.0263(5) Uani 1 1 d . . . H2 H 0.8210 0.9094 0.3678 0.032 Uiso 1 1 calc R . . C3 C 0.8354(2) 0.93472(14) 0.29215(13) 0.0278(6) Uani 1 1 d . . . C4 C 0.7824(2) 0.91290(15) 0.22662(13) 0.0300(6) Uani 1 1 d . . . C5 C 0.6832(2) 0.85584(16) 0.19563(13) 0.0329(6) Uani 1 1 d . . . H5 H 0.6478 0.8419 0.1513 0.039 Uiso 1 1 calc R . . C6 C 0.6354(2) 0.81892(15) 0.22918(13) 0.0300(6) Uani 1 1 d . . . C7 C 0.9378(2) 1.00223(15) 0.32582(13) 0.0297(6) Uani 1 1 d . . . H7 H 0.9968 0.9927 0.2976 0.036 Uiso 1 1 calc R . . C8 C 0.8997(2) 1.07139(14) 0.32791(13) 0.0284(6) Uani 1 1 d . . . C9 C 0.7965(2) 1.08554(14) 0.34663(12) 0.0265(5) Uani 1 1 d . . . H9 H 0.7516 1.0516 0.3584 0.032 Uiso 1 1 calc R . . C10 C 0.7556(2) 1.14651(14) 0.34909(12) 0.0251(5) Uani 1 1 d . . . C11 C 0.8209(2) 1.19456(14) 0.32974(12) 0.0271(5) Uani 1 1 d . . . C12 C 0.9234(2) 1.18131(15) 0.30960(13) 0.0303(6) Uani 1 1 d . . . H12 H 0.9663 1.2136 0.2954 0.036 Uiso 1 1 calc R . . C13 C 0.9632(2) 1.12116(15) 0.31015(13) 0.0292(6) Uani 1 1 d . . . C14 C 0.6480(2) 1.16253(14) 0.37668(12) 0.0259(5) Uani 1 1 d . . . H14 H 0.6275 1.2038 0.3679 0.031 Uiso 1 1 calc R . . C15 C 0.54563(19) 1.09463(14) 0.34105(12) 0.0235(5) Uani 1 1 d . . . C16 C 0.4921(2) 1.05472(14) 0.37095(12) 0.0248(5) Uani 1 1 d . . . H16 H 0.5218 1.0696 0.4162 0.030 Uiso 1 1 calc R . . C17 C 0.39634(19) 0.99344(14) 0.33738(12) 0.0247(5) Uani 1 1 d . . . C18 C 0.3575(2) 0.97139(14) 0.27052(12) 0.0262(5) Uani 1 1 d . . . C19 C 0.4094(2) 1.00897(15) 0.23814(13) 0.0285(6) Uani 1 1 d . . . H19 H 0.3820 0.9927 0.1924 0.034 Uiso 1 1 calc R . . C20 C 0.5021(2) 1.07066(15) 0.27409(12) 0.0267(5) Uani 1 1 d . . . C21 C 0.3351(2) 0.95058(14) 0.37017(12) 0.0249(5) Uani 1 1 d . . . H21 H 0.2503 0.9411 0.3538 0.030 Uiso 1 1 calc R . . C22 C 0.3626(2) 0.87442(14) 0.34917(12) 0.0248(5) Uani 1 1 d . . . C23 C 0.4758(2) 0.86646(14) 0.34885(12) 0.0260(5) Uani 1 1 d . . . H23 H 0.5359 0.9104 0.3635 0.031 Uiso 1 1 calc R . . C24 C 0.5057(2) 0.79813(15) 0.32843(12) 0.0267(5) Uani 1 1 d . . . C25 C 0.4164(2) 0.73367(15) 0.30680(13) 0.0293(6) Uani 1 1 d . . . C26 C 0.3032(2) 0.73951(15) 0.30747(13) 0.0311(6) Uani 1 1 d . . . H26 H 0.2433 0.6956 0.2933 0.037 Uiso 1 1 calc R . . C27 C 0.2767(2) 0.80846(15) 0.32852(13) 0.0269(5) Uani 1 1 d . . . C28 C 0.6313(2) 0.79402(14) 0.32825(12) 0.0263(5) Uani 1 1 d . . . H28 H 0.6317 0.7401 0.3021 0.032 Uiso 1 1 calc R . . C29 C 0.9957(2) 1.01574(16) 0.39503(14) 0.0370(7) Uani 1 1 d . . . H29A H 0.9414 1.0301 0.4252 0.044 Uiso 1 1 calc R . . H29B H 1.0123 0.9684 0.3923 0.044 Uiso 1 1 calc R . . C30 C 1.1073(3) 1.07682(18) 0.42378(17) 0.0475(8) Uani 1 1 d . . . H30A H 1.1636 1.0612 0.3959 0.071 Uiso 1 1 calc R . . H30B H 1.1385 1.0851 0.4686 0.071 Uiso 1 1 calc R . . H30C H 1.0919 1.1234 0.4253 0.071 Uiso 1 1 calc R . . C31 C 0.6790(2) 1.19273(16) 0.45211(13) 0.0334(6) Uani 1 1 d . . . H31A H 0.6871 1.1505 0.4621 0.040 Uiso 1 1 calc R . . H31B H 0.7551 1.2292 0.4691 0.040 Uiso 1 1 calc R . . C32 C 0.5932(3) 1.2302(2) 0.48860(16) 0.0522(8) Uani 1 1 d . . . H32A H 0.5920 1.2760 0.4840 0.078 Uiso 1 1 calc R . . H32B H 0.6154 1.2430 0.5355 0.078 Uiso 1 1 calc R . . H32C H 0.5163 1.1960 0.4701 0.078 Uiso 1 1 calc R . . C33 C 0.3588(2) 0.99566(15) 0.44594(12) 0.0278(6) Uani 1 1 d . . . H33A H 0.4412 1.0028 0.4641 0.033 Uiso 1 1 calc R . . H33B H 0.3440 1.0459 0.4576 0.033 Uiso 1 1 calc R . . C34 C 0.2847(3) 0.95753(17) 0.47785(14) 0.0393(7) Uani 1 1 d . . . H34A H 0.2029 0.9511 0.4607 0.059 Uiso 1 1 calc R . . H34B H 0.3030 0.9886 0.5259 0.059 Uiso 1 1 calc R . . H34C H 0.3004 0.9083 0.4675 0.059 Uiso 1 1 calc R . . C35 C 0.6970(2) 0.82034(16) 0.39952(13) 0.0303(6) Uani 1 1 d . . . H35A H 0.7791 0.8195 0.3992 0.036 Uiso 1 1 calc R . . H35B H 0.6938 0.8727 0.4272 0.036 Uiso 1 1 calc R . . C36 C 0.6473(2) 0.77158(19) 0.42985(15) 0.0426(7) Uani 1 1 d . . . H36A H 0.5684 0.7760 0.4342 0.064 Uiso 1 1 calc R . . H36B H 0.6950 0.7880 0.4736 0.064 Uiso 1 1 calc R . . H36C H 0.6464 0.7192 0.4014 0.064 Uiso 1 1 calc R . . O101 O 1.17009(18) 1.04475(13) 0.14279(11) 0.0529(6) Uani 1 1 d . . . O102 O 1.2699(2) 0.99494(16) 0.07066(14) 0.0720(8) Uani 1 1 d . . . N1 N 0.9432(2) 1.00171(17) 0.11283(13) 0.0463(6) Uani 1 1 d D . . H1N H 1.007(2) 1.0301(17) 0.1435(14) 0.056 Uiso 1 1 d D . . N2 N 1.1762(2) 0.99892(15) 0.08708(14) 0.0451(6) Uani 1 1 d . . . C37 C 0.7662(2) 0.9499(2) 0.14024(16) 0.0454(8) Uani 1 1 d . . . H37A H 0.6902 0.9590 0.1494 0.055 Uiso 1 1 calc R . . H37B H 0.7536 0.9004 0.1014 0.055 Uiso 1 1 calc R . . C38 C 0.8309(3) 1.0106(2) 0.12723(17) 0.0477(8) Uani 1 1 d . . . H38A H 0.7837 1.0119 0.0894 0.057 Uiso 1 1 calc R . . H38B H 0.8409 1.0594 0.1664 0.057 Uiso 1 1 calc R . . C39 C 0.9620(3) 0.95433(17) 0.05405(15) 0.0414(7) Uani 1 1 d . . . C40 C 0.8676(3) 0.90536(19) 0.00140(16) 0.0496(8) Uani 1 1 d . . . H40 H 0.7911 0.9064 0.0078 0.060 Uiso 1 1 calc R . . C41 C 0.8849(3) 0.8565(2) -0.05845(17) 0.0562(9) Uani 1 1 d . . . H41 H 0.8197 0.8247 -0.0926 0.067 Uiso 1 1 calc R . . C42 C 0.9937(3) 0.8522(2) -0.07056(17) 0.0546(9) Uani 1 1 d . . . H42 H 1.0037 0.8173 -0.1122 0.065 Uiso 1 1 calc R . . C43 C 1.0874(3) 0.89930(19) -0.02139(16) 0.0498(8) Uani 1 1 d . . . H43 H 1.1631 0.8975 -0.0292 0.060 Uiso 1 1 calc R . . C44 C 1.0729(2) 0.94969(17) 0.03982(15) 0.0404(7) Uani 1 1 d . . . O103 O 0.5847(2) 0.7423(2) 0.00965(15) 0.0849(9) Uani 1 1 d . . . O104 O 0.6021(3) 0.6657(3) -0.08669(15) 0.1224(15) Uani 1 1 d . . . N3 N 0.4212(2) 0.70102(16) 0.06332(12) 0.0449(6) Uani 1 1 d D . . H3N H 0.486(2) 0.7324(17) 0.0671(17) 0.054 Uiso 1 1 d D . . N4 N 0.5468(3) 0.6833(3) -0.04221(17) 0.0771(11) Uani 1 1 d . . . C45 C 0.4340(2) 0.77990(17) 0.17855(14) 0.0359(6) Uani 1 1 d . . . H45A H 0.4532 0.8239 0.1698 0.043 Uiso 1 1 calc R . . H45B H 0.3914 0.7927 0.2150 0.043 Uiso 1 1 calc R . . C46 C 0.3624(2) 0.71346(18) 0.11780(13) 0.0393(7) Uani 1 1 d . . . H46A H 0.3503 0.6685 0.1256 0.047 Uiso 1 1 calc R . . H46B H 0.2860 0.7224 0.1069 0.047 Uiso 1 1 calc R . . C47 C 0.3808(3) 0.6442(2) 0.00105(15) 0.0487(8) Uani 1 1 d . . . C48 C 0.2759(3) 0.5915(2) -0.01367(17) 0.0606(10) Uani 1 1 d . . . H48 H 0.2349 0.5957 0.0205 0.073 Uiso 1 1 calc R . . C49 C 0.2317(4) 0.5341(2) -0.0763(2) 0.0782(13) Uani 1 1 d . . . H49 H 0.1601 0.5000 -0.0849 0.094 Uiso 1 1 calc R . . C50 C 0.2900(5) 0.5252(3) -0.1271(2) 0.0943(16) Uani 1 1 d . . . H50 H 0.2591 0.4850 -0.1701 0.113 Uiso 1 1 calc R . . C51 C 0.3932(5) 0.5752(3) -0.1146(2) 0.0811(14) Uani 1 1 d . . . H51 H 0.4332 0.5697 -0.1493 0.097 Uiso 1 1 calc R . . C52 C 0.4391(3) 0.6336(2) -0.05149(16) 0.0588(10) Uani 1 1 d . . . O105 O 1.0682(2) 1.55348(15) 0.48198(14) 0.0747(8) Uani 1 1 d . . . O106 O 1.1878(2) 1.63172(15) 0.46459(16) 0.0883(9) Uani 1 1 d . . . N5 N 0.8981(2) 1.45393(15) 0.38756(15) 0.0492(7) Uani 1 1 d D . . H5N H 0.933(3) 1.4716(19) 0.4303(10) 0.059 Uiso 1 1 d D . . N6 N 1.1032(2) 1.57854(16) 0.44470(17) 0.0621(8) Uani 1 1 d . . . C53 C 0.8653(2) 1.31915(15) 0.34198(15) 0.0359(6) Uani 1 1 d . . . H53A H 0.8933 1.3110 0.3009 0.043 Uiso 1 1 calc R . . H53B H 0.9320 1.3290 0.3769 0.043 Uiso 1 1 calc R . . C54 C 0.8103(2) 1.38461(16) 0.36294(17) 0.0443(7) Uani 1 1 d . . . H54A H 0.7543 1.3791 0.3248 0.053 Uiso 1 1 calc R . . H54B H 0.7679 1.3858 0.3980 0.053 Uiso 1 1 calc R . . C55 C 0.9480(3) 1.48117(18) 0.34952(19) 0.0493(8) Uani 1 1 d . . . C56 C 0.9053(3) 1.4505(2) 0.28093(19) 0.0563(9) Uani 1 1 d . . . H56 H 0.8421 1.4076 0.2602 0.068 Uiso 1 1 calc R . . C57 C 0.9522(3) 1.4807(2) 0.2435(2) 0.0669(10) Uani 1 1 d . . . H57 H 0.9199 1.4590 0.1976 0.080 Uiso 1 1 calc R . . C58 C 1.0466(3) 1.5427(2) 0.2712(2) 0.0676(11) Uani 1 1 d . . . H58 H 1.0784 1.5632 0.2446 0.081 Uiso 1 1 calc R . . C59 C 1.0922(3) 1.5731(2) 0.3367(2) 0.0595(10) Uani 1 1 d . . . H59 H 1.1562 1.6154 0.3561 0.071 Uiso 1 1 calc R . . C60 C 1.0468(3) 1.54337(18) 0.37600(19) 0.0512(8) Uani 1 1 d . . . O107 O 1.4773(3) 1.35240(17) 0.44092(13) 0.0811(9) Uani 1 1 d . . . O108 O 1.5825(2) 1.43843(14) 0.42546(14) 0.0723(8) Uani 1 1 d . . . N7 N 1.3616(2) 1.22610(16) 0.34008(14) 0.0483(7) Uani 1 1 d D . . H7N H 1.381(3) 1.2685(15) 0.3801(12) 0.058 Uiso 1 1 d D . . N8 N 1.5140(2) 1.37676(17) 0.40379(15) 0.0570(7) Uani 1 1 d . . . C61 C 1.1536(2) 1.17476(17) 0.30851(18) 0.0444(7) Uani 1 1 d . . . H61A H 1.1493 1.2152 0.3515 0.053 Uiso 1 1 calc R . . H61B H 1.1414 1.1922 0.2743 0.053 Uiso 1 1 calc R . . C62 C 1.2708(2) 1.15657(17) 0.31276(18) 0.0455(8) Uani 1 1 d . . . H62A H 1.2775 1.1314 0.3414 0.055 Uiso 1 1 calc R . . H62B H 1.2793 1.1221 0.2682 0.055 Uiso 1 1 calc R . . C63 C 1.3971(2) 1.26216(17) 0.30508(16) 0.0404(7) Uani 1 1 d . . . C64 C 1.3613(3) 1.2280(2) 0.23532(17) 0.0496(8) Uani 1 1 d . . . H64 H 1.3066 1.1809 0.2136 0.060 Uiso 1 1 calc R . . C65 C 1.4032(3) 1.2607(2) 0.19870(18) 0.0590(9) Uani 1 1 d . . . H65 H 1.3797 1.2351 0.1519 0.071 Uiso 1 1 calc R . . C66 C 1.4798(3) 1.3311(2) 0.22842(19) 0.0600(10) Uani 1 1 d . . . H66 H 1.5082 1.3537 0.2024 0.072 Uiso 1 1 calc R . . C67 C 1.5132(3) 1.36681(19) 0.29538(18) 0.0500(8) Uani 1 1 d . . . H67 H 1.5639 1.4154 0.3165 0.060 Uiso 1 1 calc R . . C68 C 1.4745(2) 1.33347(18) 0.33267(17) 0.0446(8) Uani 1 1 d . . . O109 O 0.12270(19) 0.67216(13) 0.17266(11) 0.0517(6) Uani 1 1 d . . . O110 O 0.0601(3) 0.56301(15) 0.09197(14) 0.0904(10) Uani 1 1 d . . . N9 N 0.0643(2) 0.78824(14) 0.16727(13) 0.0428(6) Uani 1 1 d D . . H9N H 0.101(3) 0.7661(18) 0.1873(15) 0.051 Uiso 1 1 d D . . N10 N 0.0675(2) 0.63027(15) 0.11574(13) 0.0468(6) Uani 1 1 d . . . C69 C 0.1701(2) 0.91691(17) 0.19894(15) 0.0404(7) Uani 1 1 d . . . H69A H 0.1812 0.9025 0.1532 0.048 Uiso 1 1 calc R . . H69B H 0.1635 0.9696 0.2188 0.048 Uiso 1 1 calc R . . C70 C 0.0635(2) 0.86656(17) 0.19852(18) 0.0489(8) Uani 1 1 d . . . H70A H 0.0548 0.8811 0.2447 0.059 Uiso 1 1 calc R . . H70B H -0.0043 0.8739 0.1751 0.059 Uiso 1 1 calc R . . C71 C 0.0129(2) 0.73770(16) 0.10407(15) 0.0386(7) Uani 1 1 d . . . C72 C -0.0469(3) 0.7596(2) 0.06045(18) 0.0554(9) Uani 1 1 d . . . H72 H -0.0488 0.8108 0.0755 0.066 Uiso 1 1 calc R . . C73 C -0.1018(3) 0.7087(2) -0.0027(2) 0.0649(10) Uani 1 1 d . . . H73 H -0.1416 0.7252 -0.0303 0.078 Uiso 1 1 calc R . . C74 C -0.1007(3) 0.6338(2) -0.02720(18) 0.0681(11) Uani 1 1 d . . . H74 H -0.1388 0.5993 -0.0713 0.082 Uiso 1 1 calc R . . C75 C -0.0442(3) 0.6099(2) 0.01258(16) 0.0538(9) Uani 1 1 d . . . H75 H -0.0430 0.5585 -0.0038 0.065 Uiso 1 1 calc R . . C76 C 0.0118(3) 0.66086(17) 0.07739(14) 0.0406(7) Uani 1 1 d . . . O111 O 0.4711(2) 1.07085(15) -0.02062(11) 0.0663(7) Uani 1 1 d . . . O112 O 0.5251(2) 1.10578(14) -0.09126(10) 0.0556(6) Uani 1 1 d . . . N11 N 0.5868(2) 1.13756(15) 0.10302(12) 0.0429(6) Uani 1 1 d D . . H11N H 0.532(2) 1.0978(14) 0.0746(14) 0.052 Uiso 1 1 d D . . N12 N 0.5395(2) 1.11115(15) -0.03523(12) 0.0454(6) Uani 1 1 d . . . C77 C 0.5268(2) 1.09210(16) 0.17997(13) 0.0327(6) Uani 1 1 d . . . H77A H 0.4461 1.0939 0.1673 0.039 Uiso 1 1 calc R . . H77B H 0.5359 1.0409 0.1532 0.039 Uiso 1 1 calc R . . C78 C 0.6109(2) 1.14965(17) 0.17107(13) 0.0370(7) Uani 1 1 d . . . H78A H 0.6047 1.2006 0.2009 0.044 Uiso 1 1 calc R . . H78B H 0.6907 1.1458 0.1828 0.044 Uiso 1 1 calc R . . C79 C 0.6551(2) 1.17752(17) 0.08020(14) 0.0375(7) Uani 1 1 d . . . C80 C 0.7526(3) 1.23474(18) 0.12326(15) 0.0443(7) Uani 1 1 d . . . H80 H 0.7672 1.2464 0.1688 0.053 Uiso 1 1 calc R . . C81 C 0.8266(3) 1.2737(2) 0.10133(17) 0.0514(8) Uani 1 1 d . . . H81 H 0.8913 1.3117 0.1319 0.062 Uiso 1 1 calc R . . C82 C 0.8092(3) 1.2593(2) 0.03579(17) 0.0507(8) Uani 1 1 d . . . H82 H 0.8619 1.2865 0.0212 0.061 Uiso 1 1 calc R . . C83 C 0.7151(3) 1.20530(19) -0.00774(16) 0.0449(8) Uani 1 1 d . . . H83 H 0.7022 1.1950 -0.0529 0.054 Uiso 1 1 calc R . . C84 C 0.6378(2) 1.16514(17) 0.01375(14) 0.0383(7) Uani 1 1 d . . . O113 O 0.1601(2) 0.34584(14) 0.17578(12) 0.0647(7) Uani 1 1 d . . . O114 O 0.0746(2) 0.29679(14) 0.23145(13) 0.0660(7) Uani 1 1 d . . . N13 N 0.3256(2) 0.46914(15) 0.23572(14) 0.0462(6) Uani 1 1 d D . . H13N H 0.284(3) 0.4293(15) 0.1993(12) 0.055 Uiso 1 1 d D . . N14 N 0.1488(2) 0.34529(15) 0.22898(14) 0.0476(6) Uani 1 1 d . . . C85 C 0.3553(3) 0.60040(17) 0.26043(18) 0.0468(8) Uani 1 1 d . . . H85A H 0.2986 0.5968 0.2235 0.056 Uiso 1 1 calc R . . H85B H 0.3150 0.6028 0.2965 0.056 Uiso 1 1 calc R . . C86 C 0.4069(3) 0.53256(17) 0.2373(2) 0.0524(8) Uani 1 1 d . . . H86A H 0.4225 0.5199 0.1926 0.063 Uiso 1 1 calc R . . H86B H 0.4808 0.5439 0.2677 0.063 Uiso 1 1 calc R . . C87 C 0.3059(2) 0.46261(17) 0.29005(15) 0.0410(7) Uani 1 1 d . . . C88 C 0.3702(3) 0.5161(2) 0.35351(18) 0.0545(9) Uani 1 1 d . . . H88 H 0.4257 0.5579 0.3575 0.065 Uiso 1 1 calc R . . C89 C 0.3549(4) 0.5093(2) 0.40878(19) 0.0671(11) Uani 1 1 d . . . H89 H 0.4020 0.5455 0.4502 0.081 Uiso 1 1 calc R . . C90 C 0.2725(4) 0.4511(2) 0.40655(19) 0.0678(11) Uani 1 1 d . . . H90 H 0.2621 0.4479 0.4460 0.081 Uiso 1 1 calc R . . C91 C 0.2063(3) 0.3983(2) 0.34671(17) 0.0532(8) Uani 1 1 d . . . H91 H 0.1494 0.3582 0.3445 0.064 Uiso 1 1 calc R . . C92 C 0.2218(2) 0.40286(16) 0.28937(14) 0.0391(7) Uani 1 1 d . . . O115 O -0.27936(19) 0.59852(13) 0.28103(12) 0.0555(6) Uani 1 1 d . . . O116 O -0.3301(2) 0.52750(16) 0.32558(16) 0.0840(9) Uani 1 1 d . . . N15 N -0.10836(18) 0.71738(14) 0.34254(12) 0.0361(5) Uani 1 1 d D . . H15N H -0.155(2) 0.6840(15) 0.3038(11) 0.043 Uiso 1 1 d D . . N16 N -0.2698(2) 0.58452(15) 0.32858(15) 0.0476(7) Uani 1 1 d . . . C93 C 0.0853(2) 0.75447(15) 0.32873(14) 0.0328(6) Uani 1 1 d . . . H93A H 0.1186 0.7408 0.3625 0.039 Uiso 1 1 calc R . . H93B H 0.0687 0.7101 0.2850 0.039 Uiso 1 1 calc R . . C94 C -0.0240(2) 0.77925(16) 0.34388(16) 0.0375(7) Uani 1 1 d . . . H94A H -0.0071 0.8231 0.3880 0.045 Uiso 1 1 calc R . . H94B H -0.0556 0.7943 0.3107 0.045 Uiso 1 1 calc R . . C95 C -0.1089(2) 0.69872(16) 0.39251(14) 0.0352(6) Uani 1 1 d . . . C96 C -0.0315(3) 0.74290(19) 0.45431(15) 0.0448(7) Uani 1 1 d . . . H96 H 0.0242 0.7854 0.4598 0.054 Uiso 1 1 calc R . . C97 C -0.0344(3) 0.7265(2) 0.50556(18) 0.0576(9) Uani 1 1 d . . . H97 H 0.0196 0.7577 0.5460 0.069 Uiso 1 1 calc R . . C98 C -0.1144(3) 0.6651(2) 0.50094(19) 0.0633(10) Uani 1 1 d . . . H98 H -0.1161 0.6551 0.5379 0.076 Uiso 1 1 calc R . . C99 C -0.1902(3) 0.6195(2) 0.44213(19) 0.0549(9) Uani 1 1 d . . . H99 H -0.2448 0.5771 0.4379 0.066 Uiso 1 1 calc R . . C100 C -0.1874(2) 0.63517(17) 0.38878(15) 0.0391(7) Uani 1 1 d . . . N50A N 0.1672(4) 0.3261(3) -0.1928(2) 0.0786(13) Uiso 0.827(5) 1 d P A 1 C50A C 0.2269(3) 0.3353(2) -0.15322(19) 0.0448(10) Uiso 0.827(5) 1 d P A 1 C55A C 0.3125(6) 0.3529(4) -0.0949(3) 0.124(2) Uiso 0.827(5) 1 d P A 1 H55A H 0.3901 0.3616 -0.1039 0.187 Uiso 0.827(5) 1 calc PR A 1 H55B H 0.3007 0.3109 -0.0838 0.187 Uiso 0.827(5) 1 calc PR A 1 H55C H 0.3045 0.3982 -0.0577 0.187 Uiso 0.827(5) 1 calc PR A 1 N50B N 0.4712(11) 0.4782(8) -0.0188(6) 0.040(4) Uiso 0.173(5) 1 d P . 2 C50B C 0.383(2) 0.4275(11) -0.0485(11) 0.078(7) Uiso 0.173(5) 1 d PD A 2 C55B C 0.3125(6) 0.3529(4) -0.0949(3) 0.124(2) Uiso 0.173(5) 1 d PD A 2 H55D H 0.2612 0.3566 -0.1294 0.187 Uiso 0.173(5) 1 calc PR A 2 H55E H 0.2662 0.3322 -0.0712 0.187 Uiso 0.173(5) 1 calc PR A 2 H55F H 0.3627 0.3200 -0.1152 0.187 Uiso 0.173(5) 1 calc PR A 2 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 O4 0.0295(10) 0.0419(12) 0.0385(11) 0.0243(9) 0.0032(8) 0.0004(8) O6 0.0262(9) 0.0300(10) 0.0373(10) 0.0141(9) -0.0005(8) -0.0014(8) O11 0.0232(9) 0.0265(10) 0.0508(11) 0.0232(9) 0.0070(8) 0.0032(7) O13 0.0229(9) 0.0294(11) 0.0632(13) 0.0213(10) 0.0168(8) 0.0063(8) O18 0.0281(9) 0.0273(10) 0.0364(10) 0.0164(8) -0.0081(7) -0.0026(8) O20 0.0341(10) 0.0401(11) 0.0309(10) 0.0215(9) -0.0003(8) -0.0054(8) O25 0.0285(10) 0.0228(10) 0.0617(13) 0.0182(9) 0.0087(9) 0.0055(8) O27 0.0203(9) 0.0274(10) 0.0571(12) 0.0236(9) 0.0090(8) 0.0036(7) C1 0.0203(12) 0.0253(13) 0.0310(13) 0.0126(11) 0.0060(10) 0.0082(10) C2 0.0220(12) 0.0240(13) 0.0319(13) 0.0124(11) 0.0008(10) 0.0067(10) C3 0.0222(12) 0.0248(14) 0.0361(14) 0.0135(12) 0.0032(10) 0.0074(10) C4 0.0249(13) 0.0309(15) 0.0364(14) 0.0168(12) 0.0068(11) 0.0075(11) C5 0.0261(13) 0.0375(16) 0.0288(14) 0.0130(12) -0.0003(11) 0.0018(12) C6 0.0219(12) 0.0281(14) 0.0352(14) 0.0119(12) 0.0023(10) 0.0034(10) C7 0.0207(12) 0.0263(14) 0.0416(15) 0.0155(12) 0.0041(11) 0.0062(10) C8 0.0232(13) 0.0233(14) 0.0345(14) 0.0120(12) 0.0006(10) 0.0012(10) C9 0.0225(12) 0.0238(13) 0.0324(14) 0.0144(11) 0.0015(10) 0.0019(10) C10 0.0204(12) 0.0267(14) 0.0262(13) 0.0121(11) 0.0015(9) 0.0024(10) C11 0.0268(13) 0.0219(13) 0.0309(13) 0.0129(11) -0.0010(10) 0.0034(10) C12 0.0251(13) 0.0264(14) 0.0406(15) 0.0180(12) 0.0061(11) 0.0017(11) C13 0.0222(12) 0.0272(14) 0.0344(14) 0.0126(12) 0.0043(10) 0.0014(10) C14 0.0226(12) 0.0240(13) 0.0309(13) 0.0129(11) 0.0040(10) 0.0047(10) C15 0.0204(12) 0.0235(13) 0.0279(13) 0.0124(11) 0.0035(10) 0.0071(10) C16 0.0227(12) 0.0276(14) 0.0259(13) 0.0136(11) 0.0026(10) 0.0081(10) C17 0.0207(12) 0.0244(13) 0.0325(13) 0.0160(11) 0.0038(10) 0.0067(10) C18 0.0220(12) 0.0229(13) 0.0317(13) 0.0130(11) -0.0001(10) 0.0023(10) C19 0.0264(13) 0.0288(14) 0.0292(13) 0.0144(12) 0.0003(10) 0.0044(11) C20 0.0256(13) 0.0279(14) 0.0321(14) 0.0186(12) 0.0067(10) 0.0062(11) C21 0.0188(12) 0.0271(14) 0.0318(13) 0.0171(11) 0.0022(10) 0.0045(10) C22 0.0229(12) 0.0278(14) 0.0266(13) 0.0166(11) 0.0024(10) 0.0038(10) C23 0.0221(12) 0.0251(14) 0.0314(13) 0.0156(11) 0.0017(10) 0.0024(10) C24 0.0245(12) 0.0270(14) 0.0310(13) 0.0162(12) 0.0033(10) 0.0057(10) C25 0.0268(13) 0.0236(14) 0.0392(15) 0.0159(12) 0.0059(11) 0.0064(11) C26 0.0275(13) 0.0265(14) 0.0397(15) 0.0178(12) 0.0041(11) 0.0017(11) C27 0.0201(12) 0.0284(14) 0.0354(14) 0.0182(12) 0.0041(10) 0.0046(10) C28 0.0231(12) 0.0220(13) 0.0332(14) 0.0121(11) 0.0049(10) 0.0056(10) C29 0.0284(14) 0.0339(16) 0.0444(16) 0.0180(14) -0.0040(12) 0.0040(12) C30 0.0360(16) 0.0369(18) 0.060(2) 0.0215(16) -0.0118(14) -0.0004(13) C31 0.0299(14) 0.0307(15) 0.0299(14) 0.0098(12) 0.0026(11) -0.0039(11) C32 0.0430(18) 0.052(2) 0.0447(18) 0.0086(16) 0.0131(14) 0.0022(15) C33 0.0275(13) 0.0281(14) 0.0306(14) 0.0165(12) 0.0045(10) 0.0056(11) C34 0.0493(17) 0.0378(17) 0.0325(15) 0.0187(13) 0.0102(12) 0.0057(13) C35 0.0262(13) 0.0335(15) 0.0357(14) 0.0198(13) 0.0036(11) 0.0093(11) C36 0.0359(15) 0.056(2) 0.0449(17) 0.0320(16) 0.0051(13) 0.0105(14) O101 0.0502(13) 0.0509(14) 0.0460(13) 0.0219(12) -0.0080(10) -0.0046(11) O102 0.0336(13) 0.083(2) 0.0800(18) 0.0254(15) -0.0017(12) 0.0046(12) N1 0.0381(14) 0.0558(18) 0.0455(15) 0.0300(14) 0.0004(11) -0.0017(12) N2 0.0411(15) 0.0422(16) 0.0492(17) 0.0254(14) -0.0071(12) 0.0013(12) C37 0.0367(16) 0.060(2) 0.0477(18) 0.0345(17) 0.0039(13) 0.0064(14) C38 0.0471(18) 0.055(2) 0.0539(19) 0.0372(17) 0.0080(14) 0.0124(15) C39 0.0423(17) 0.0421(18) 0.0424(17) 0.0301(15) -0.0063(13) -0.0032(13) C40 0.0428(17) 0.055(2) 0.052(2) 0.0364(18) -0.0078(14) -0.0083(15) C41 0.061(2) 0.051(2) 0.048(2) 0.0280(18) -0.0166(17) -0.0054(17) C42 0.068(2) 0.044(2) 0.0471(19) 0.0222(16) -0.0045(17) 0.0089(17) C43 0.056(2) 0.0445(19) 0.054(2) 0.0301(17) -0.0004(15) 0.0113(16) C44 0.0384(16) 0.0384(17) 0.0430(17) 0.0242(15) -0.0061(13) 0.0001(13) O103 0.0614(17) 0.122(3) 0.0607(18) 0.0361(19) 0.0183(14) 0.0045(17) O104 0.092(2) 0.222(5) 0.0603(19) 0.060(2) 0.0388(17) 0.049(3) N3 0.0369(14) 0.0518(17) 0.0322(13) 0.0113(12) 0.0009(11) 0.0013(12) N4 0.065(2) 0.131(4) 0.0446(19) 0.043(2) 0.0164(16) 0.034(2) C45 0.0279(14) 0.0407(17) 0.0363(15) 0.0183(13) -0.0004(11) 0.0037(12) C46 0.0306(14) 0.0470(18) 0.0338(15) 0.0169(14) 0.0008(11) 0.0010(13) C47 0.0528(19) 0.052(2) 0.0352(17) 0.0143(15) 0.0005(14) 0.0187(16) C48 0.066(2) 0.050(2) 0.0434(19) 0.0078(17) -0.0079(17) 0.0069(18) C49 0.102(3) 0.050(2) 0.053(2) 0.008(2) -0.014(2) 0.003(2) C50 0.147(5) 0.066(3) 0.041(2) 0.004(2) -0.006(3) 0.026(3) C51 0.114(4) 0.088(4) 0.045(2) 0.023(2) 0.020(2) 0.049(3) C52 0.069(2) 0.073(3) 0.0352(18) 0.0200(18) 0.0090(16) 0.031(2) O105 0.0729(17) 0.0559(17) 0.0739(18) 0.0212(15) 0.0079(14) -0.0112(13) O106 0.0678(17) 0.0443(16) 0.111(2) 0.0077(15) 0.0185(16) -0.0174(13) N5 0.0450(15) 0.0301(14) 0.0691(18) 0.0236(14) 0.0081(13) 0.0004(11) N6 0.0533(17) 0.0314(16) 0.083(2) 0.0117(16) 0.0182(16) -0.0017(13) C53 0.0273(14) 0.0277(15) 0.0535(17) 0.0212(14) 0.0060(12) 0.0025(11) C54 0.0330(15) 0.0294(16) 0.068(2) 0.0207(15) 0.0080(14) 0.0054(12) C55 0.0431(17) 0.0294(17) 0.078(2) 0.0254(17) 0.0112(16) 0.0119(14) C56 0.052(2) 0.045(2) 0.078(3) 0.037(2) 0.0046(18) 0.0079(16) C57 0.067(2) 0.062(3) 0.082(3) 0.043(2) 0.010(2) 0.017(2) C58 0.062(2) 0.057(2) 0.105(3) 0.052(3) 0.029(2) 0.0194(19) C59 0.053(2) 0.040(2) 0.096(3) 0.037(2) 0.027(2) 0.0150(16) C60 0.0453(18) 0.0307(17) 0.077(2) 0.0217(17) 0.0173(17) 0.0115(14) O107 0.096(2) 0.0697(19) 0.0578(16) 0.0290(15) -0.0067(15) -0.0163(16) O108 0.0623(16) 0.0448(15) 0.0787(18) 0.0134(14) -0.0062(13) -0.0112(12) N7 0.0336(13) 0.0439(16) 0.0620(18) 0.0227(14) 0.0061(12) 0.0018(12) N8 0.0454(16) 0.0506(18) 0.0602(18) 0.0216(16) -0.0067(13) -0.0041(14) C61 0.0299(15) 0.0291(16) 0.075(2) 0.0228(16) 0.0196(14) 0.0061(12) C62 0.0270(14) 0.0350(17) 0.078(2) 0.0297(17) 0.0123(14) 0.0044(12) C63 0.0207(13) 0.0388(17) 0.063(2) 0.0257(16) 0.0051(13) 0.0062(12) C64 0.0328(16) 0.048(2) 0.057(2) 0.0181(17) 0.0026(14) 0.0036(14) C65 0.0450(19) 0.072(3) 0.055(2) 0.029(2) 0.0061(16) 0.0022(17) C66 0.0423(19) 0.074(3) 0.069(2) 0.041(2) 0.0087(17) 0.0056(18) C67 0.0312(16) 0.046(2) 0.079(3) 0.0374(19) 0.0022(15) 0.0062(14) C68 0.0298(15) 0.0362(17) 0.065(2) 0.0222(16) 0.0032(14) 0.0060(13) O109 0.0573(13) 0.0462(14) 0.0440(13) 0.0171(11) -0.0034(10) 0.0117(11) O110 0.147(3) 0.0334(15) 0.0688(18) 0.0097(13) -0.0162(18) 0.0299(16) N9 0.0332(13) 0.0266(13) 0.0558(16) 0.0108(12) -0.0027(11) 0.0042(10) N10 0.0555(16) 0.0358(15) 0.0444(16) 0.0146(13) 0.0036(12) 0.0137(12) C69 0.0325(15) 0.0323(16) 0.0496(18) 0.0176(14) -0.0063(13) 0.0031(12) C70 0.0314(15) 0.0316(17) 0.068(2) 0.0107(16) 0.0039(14) 0.0051(13) C71 0.0290(14) 0.0331(16) 0.0496(17) 0.0186(14) 0.0035(12) 0.0011(12) C72 0.0514(19) 0.043(2) 0.070(2) 0.0307(18) -0.0033(17) 0.0023(16) C73 0.064(2) 0.067(3) 0.069(2) 0.044(2) -0.0068(19) 0.0070(19) C74 0.077(3) 0.064(3) 0.046(2) 0.0206(19) -0.0085(18) -0.002(2) C75 0.065(2) 0.0423(19) 0.0426(18) 0.0150(16) -0.0026(16) 0.0053(16) C76 0.0467(17) 0.0303(16) 0.0387(16) 0.0127(13) 0.0018(13) 0.0062(13) O111 0.0662(15) 0.0752(18) 0.0450(13) 0.0349(13) -0.0071(11) -0.0230(13) O112 0.0696(15) 0.0637(16) 0.0334(12) 0.0266(11) 0.0003(10) 0.0105(12) N11 0.0435(14) 0.0484(16) 0.0318(13) 0.0225(12) -0.0003(10) -0.0085(12) N12 0.0542(16) 0.0474(16) 0.0327(14) 0.0217(12) -0.0001(11) 0.0037(13) C77 0.0350(14) 0.0347(16) 0.0270(13) 0.0160(12) 0.0019(11) 0.0021(12) C78 0.0392(15) 0.0434(18) 0.0302(14) 0.0218(13) 0.0022(11) 0.0038(13) C79 0.0378(15) 0.0374(17) 0.0376(16) 0.0200(14) 0.0057(12) 0.0030(13) C80 0.0442(17) 0.0464(19) 0.0374(16) 0.0202(15) 0.0040(13) -0.0017(14) C81 0.0458(18) 0.050(2) 0.056(2) 0.0282(17) 0.0043(15) -0.0005(15) C82 0.0494(19) 0.055(2) 0.065(2) 0.0418(19) 0.0207(16) 0.0102(16) C83 0.0505(18) 0.053(2) 0.0478(18) 0.0351(17) 0.0158(14) 0.0159(16) C84 0.0406(16) 0.0423(18) 0.0365(15) 0.0237(14) 0.0051(12) 0.0076(13) O113 0.0763(17) 0.0554(16) 0.0426(13) 0.0183(12) -0.0004(11) -0.0149(13) O114 0.0612(15) 0.0525(15) 0.0669(16) 0.0246(13) 0.0029(12) -0.0161(12) N13 0.0454(15) 0.0301(14) 0.0554(17) 0.0159(13) 0.0078(12) 0.0010(11) N14 0.0460(15) 0.0370(15) 0.0511(17) 0.0180(13) 0.0012(12) -0.0003(12) C85 0.0388(16) 0.0286(16) 0.067(2) 0.0180(15) 0.0102(14) 0.0050(13) C86 0.0430(17) 0.0290(17) 0.083(2) 0.0237(17) 0.0158(16) 0.0067(13) C87 0.0358(15) 0.0300(16) 0.0506(18) 0.0133(14) -0.0007(13) 0.0112(13) C88 0.0445(18) 0.043(2) 0.058(2) 0.0135(17) -0.0078(15) 0.0036(15) C89 0.071(3) 0.058(2) 0.048(2) 0.0074(18) -0.0104(18) 0.015(2) C90 0.079(3) 0.072(3) 0.048(2) 0.025(2) 0.0031(19) 0.018(2) C91 0.056(2) 0.051(2) 0.052(2) 0.0241(17) 0.0040(16) 0.0123(16) C92 0.0375(15) 0.0307(16) 0.0413(16) 0.0123(13) -0.0023(12) 0.0066(12) O115 0.0480(13) 0.0496(14) 0.0551(14) 0.0192(12) 0.0061(10) -0.0081(10) O116 0.0639(16) 0.0583(17) 0.122(2) 0.0559(18) -0.0101(16) -0.0264(13) N15 0.0241(11) 0.0345(14) 0.0462(14) 0.0171(12) 0.0071(10) 0.0017(10) N16 0.0332(13) 0.0380(15) 0.0706(19) 0.0269(14) 0.0080(12) 0.0017(11) C93 0.0247(13) 0.0269(14) 0.0492(17) 0.0201(13) 0.0082(11) 0.0038(11) C94 0.0258(14) 0.0322(16) 0.0549(18) 0.0214(14) 0.0085(12) 0.0029(11) C95 0.0255(13) 0.0336(16) 0.0471(17) 0.0164(14) 0.0116(12) 0.0107(12) C96 0.0366(16) 0.0432(19) 0.0476(18) 0.0150(15) 0.0063(13) 0.0087(14) C97 0.049(2) 0.067(3) 0.053(2) 0.0232(19) 0.0075(16) 0.0170(18) C98 0.067(2) 0.083(3) 0.059(2) 0.045(2) 0.0186(19) 0.025(2) C99 0.0469(19) 0.060(2) 0.078(3) 0.046(2) 0.0209(18) 0.0170(17) C100 0.0297(14) 0.0351(16) 0.0545(18) 0.0213(15) 0.0120(13) 0.0081(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O4 C4 1.371(3) . ? O4 C37 1.430(3) . ? O6 C6 1.390(3) . ? O6 C45 1.448(3) . ? O11 C11 1.375(3) . ? O11 C53 1.428(3) . ? O13 C13 1.386(3) . ? O13 C61 1.431(3) . ? O18 C18 1.386(3) . ? O18 C69 1.422(3) . ? O20 C20 1.364(3) . ? O20 C77 1.413(3) . ? O25 C25 1.381(3) . ? O25 C85 1.420(3) . ? O27 C27 1.379(3) . ? O27 C93 1.429(3) . ? C1 C6 1.396(4) . ? C1 C2 1.401(3) . ? C1 C28 1.517(3) . ? C2 C3 1.388(4) . ? C3 C4 1.402(4) . ? C3 C7 1.517(3) . ? C4 C5 1.382(4) . ? C5 C6 1.386(4) . ? C7 C8 1.531(4) . ? C7 C29 1.541(4) . ? C8 C13 1.387(4) . ? C8 C9 1.393(4) . ? C9 C10 1.387(4) . ? C10 C11 1.396(3) . ? C10 C14 1.526(3) . ? C11 C12 1.392(4) . ? C12 C13 1.387(4) . ? C14 C15 1.523(3) . ? C14 C31 1.537(4) . ? C15 C16 1.388(3) . ? C15 C20 1.396(3) . ? C16 C17 1.402(3) . ? C17 C18 1.392(3) . ? C17 C21 1.523(3) . ? C18 C19 1.393(4) . ? C19 C20 1.389(4) . ? C21 C22 1.518(3) . ? C21 C33 1.539(3) . ? C22 C23 1.398(3) . ? C22 C27 1.402(3) . ? C23 C24 1.387(4) . ? C24 C25 1.401(4) . ? C24 C28 1.525(3) . ? C25 C26 1.385(4) . ? C26 C27 1.379(4) . ? C28 C35 1.544(3) . ? C29 C30 1.521(4) . ? C31 C32 1.502(4) . ? C33 C34 1.522(4) . ? C35 C36 1.513(4) . ? O101 N2 1.237(3) . ? O102 N2 1.231(4) . ? N1 C39 1.351(4) . ? N1 C38 1.447(4) . ? N2 C44 1.437(4) . ? C37 C38 1.498(4) . ? C39 C44 1.416(4) . ? C39 C40 1.419(4) . ? C40 C41 1.370(5) . ? C41 C42 1.376(5) . ? C42 C43 1.371(5) . ? C43 C44 1.391(5) . ? O103 N4 1.238(5) . ? O104 N4 1.236(4) . ? N3 C47 1.360(4) . ? N3 C46 1.451(4) . ? N4 C52 1.433(5) . ? C45 C46 1.494(4) . ? C47 C48 1.410(5) . ? C47 C52 1.415(5) . ? C48 C49 1.374(5) . ? C49 C50 1.385(7) . ? C50 C51 1.377(7) . ? C51 C52 1.391(6) . ? O105 N6 1.239(4) . ? O106 N6 1.230(4) . ? N5 C55 1.354(4) . ? N5 C54 1.449(4) . ? N6 C60 1.440(5) . ? C53 C54 1.503(4) . ? C55 C56 1.409(5) . ? C55 C60 1.432(4) . ? C56 C57 1.363(5) . ? C57 C58 1.397(6) . ? C58 C59 1.355(6) . ? C59 C60 1.386(5) . ? O107 N8 1.235(4) . ? O108 N8 1.234(4) . ? N7 C63 1.350(4) . ? N7 C62 1.466(4) . ? N8 C68 1.452(4) . ? C61 C62 1.517(4) . ? C63 C68 1.412(4) . ? C63 C64 1.418(5) . ? C64 C65 1.359(5) . ? C65 C66 1.392(5) . ? C66 C67 1.359(5) . ? C67 C68 1.368(4) . ? O109 N10 1.236(3) . ? O110 N10 1.218(3) . ? N9 C71 1.358(4) . ? N9 C70 1.441(4) . ? N10 C76 1.437(4) . ? C69 C70 1.494(4) . ? C71 C76 1.409(4) . ? C71 C72 1.423(4) . ? C72 C73 1.368(5) . ? C73 C74 1.380(5) . ? C74 C75 1.366(5) . ? C75 C76 1.397(4) . ? O111 N12 1.234(3) . ? O112 N12 1.226(3) . ? N11 C79 1.354(4) . ? N11 C78 1.452(3) . ? N12 C84 1.438(4) . ? C77 C78 1.509(4) . ? C79 C84 1.413(4) . ? C79 C80 1.413(4) . ? C80 C81 1.366(4) . ? C81 C82 1.380(5) . ? C82 C83 1.367(5) . ? C83 C84 1.398(4) . ? O113 N14 1.242(3) . ? O114 N14 1.236(3) . ? N13 C87 1.345(4) . ? N13 C86 1.462(4) . ? N14 C92 1.431(4) . ? C85 C86 1.517(4) . ? C87 C88 1.415(4) . ? C87 C92 1.434(4) . ? C88 C89 1.355(5) . ? C89 C90 1.386(6) . ? C90 C91 1.367(5) . ? C91 C92 1.382(4) . ? O115 N16 1.231(3) . ? O116 N16 1.227(3) . ? N15 C95 1.346(4) . ? N15 C94 1.461(3) . ? N16 C100 1.440(4) . ? C93 C94 1.508(4) . ? C95 C96 1.417(4) . ? C95 C100 1.427(4) . ? C96 C97 1.347(5) . ? C97 C98 1.396(5) . ? C98 C99 1.369(5) . ? C99 C100 1.386(4) . ? N50A C50A 1.014(5) . ? C50A C55A 1.456(7) . ? N50B N50B 1.01(3) 2_665 ? N50B C50B 1.23(2) . ? 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 C4 O4 C37 117.0(2) . . ? C6 O6 C45 115.4(2) . . ? C11 O11 C53 116.09(19) . . ? C13 O13 C61 114.7(2) . . ? C18 O18 C69 117.3(2) . . ? C20 O20 C77 120.1(2) . . ? C25 O25 C85 116.8(2) . . ? C27 O27 C93 115.59(19) . . ? C6 C1 C2 116.2(2) . . ? C6 C1 C28 119.9(2) . . ? C2 C1 C28 123.9(2) . . ? C3 C2 C1 124.0(2) . . ? C2 C3 C4 117.1(2) . . ? C2 C3 C7 124.0(2) . . ? C4 C3 C7 118.7(2) . . ? O4 C4 C5 123.3(2) . . ? O4 C4 C3 115.8(2) . . ? C5 C4 C3 120.9(2) . . ? C4 C5 C6 120.0(2) . . ? C5 C6 O6 119.0(2) . . ? C5 C6 C1 121.8(2) . . ? O6 C6 C1 119.1(2) . . ? C3 C7 C8 109.03(19) . . ? C3 C7 C29 113.7(2) . . ? C8 C7 C29 111.6(2) . . ? C13 C8 C9 117.3(2) . . ? C13 C8 C7 122.4(2) . . ? C9 C8 C7 120.3(2) . . ? C10 C9 C8 123.6(2) . . ? C9 C10 C11 117.4(2) . . ? C9 C10 C14 120.5(2) . . ? C11 C10 C14 122.0(2) . . ? O11 C11 C12 121.8(2) . . ? O11 C11 C10 117.8(2) . . ? C12 C11 C10 120.5(2) . . ? C13 C12 C11 120.3(2) . . ? O13 C13 C12 120.9(2) . . ? O13 C13 C8 118.2(2) . . ? C12 C13 C8 120.9(2) . . ? C15 C14 C10 111.3(2) . . ? C15 C14 C31 115.2(2) . . ? C10 C14 C31 108.43(19) . . ? C16 C15 C20 117.4(2) . . ? C16 C15 C14 124.2(2) . . ? C20 C15 C14 118.4(2) . . ? C15 C16 C17 123.0(2) . . ? C18 C17 C16 117.1(2) . . ? C18 C17 C21 119.5(2) . . ? C16 C17 C21 123.5(2) . . ? O18 C18 C17 117.1(2) . . ? O18 C18 C19 121.0(2) . . ? C17 C18 C19 122.0(2) . . ? C20 C19 C18 118.7(2) . . ? O20 C20 C19 123.8(2) . . ? O20 C20 C15 114.4(2) . . ? C19 C20 C15 121.8(2) . . ? C22 C21 C17 111.4(2) . . ? C22 C21 C33 111.48(19) . . ? C17 C21 C33 113.0(2) . . ? C23 C22 C27 116.4(2) . . ? C23 C22 C21 121.3(2) . . ? C27 C22 C21 122.3(2) . . ? C24 C23 C22 123.8(2) . . ? C23 C24 C25 117.6(2) . . ? C23 C24 C28 120.6(2) . . ? C25 C24 C28 121.8(2) . . ? O25 C25 C26 122.7(2) . . ? O25 C25 C24 117.1(2) . . ? C26 C25 C24 120.2(2) . . ? C27 C26 C25 120.7(2) . . ? O27 C27 C26 121.7(2) . . ? O27 C27 C22 116.9(2) . . ? C26 C27 C22 121.3(2) . . ? C1 C28 C24 110.67(19) . . ? C1 C28 C35 113.7(2) . . ? C24 C28 C35 109.7(2) . . ? C30 C29 C7 112.6(2) . . ? C32 C31 C14 114.8(2) . . ? C34 C33 C21 112.9(2) . . ? C36 C35 C28 112.3(2) . . ? C39 N1 C38 125.1(3) . . ? O102 N2 O101 121.2(3) . . ? O102 N2 C44 118.7(3) . . ? O101 N2 C44 120.1(3) . . ? O4 C37 C38 106.9(2) . . ? N1 C38 C37 114.3(3) . . ? N1 C39 C44 124.2(3) . . ? N1 C39 C40 120.3(3) . . ? C44 C39 C40 115.5(3) . . ? C41 C40 C39 121.3(3) . . ? C40 C41 C42 122.0(3) . . ? C43 C42 C41 118.7(4) . . ? C42 C43 C44 120.7(3) . . ? C43 C44 C39 121.8(3) . . ? C43 C44 N2 116.5(3) . . ? C39 C44 N2 121.6(3) . . ? C47 N3 C46 124.5(3) . . ? O104 N4 O103 120.5(4) . . ? O104 N4 C52 118.7(4) . . ? O103 N4 C52 120.8(3) . . ? O6 C45 C46 107.0(2) . . ? N3 C46 C45 109.2(2) . . ? N3 C47 C48 120.0(3) . . ? N3 C47 C52 123.5(3) . . ? C48 C47 C52 116.5(3) . . ? C49 C48 C47 121.5(4) . . ? C48 C49 C50 121.0(5) . . ? C51 C50 C49 119.3(4) . . ? C50 C51 C52 120.4(4) . . ? C51 C52 C47 121.3(4) . . ? C51 C52 N4 117.3(4) . . ? C47 C52 N4 121.4(3) . . ? C55 N5 C54 125.3(3) . . ? O106 N6 O105 121.4(4) . . ? O106 N6 C60 118.8(3) . . ? O105 N6 C60 119.8(3) . . ? O11 C53 C54 107.8(2) . . ? N5 C54 C53 109.9(2) . . ? N5 C55 C56 122.1(3) . . ? N5 C55 C60 122.6(3) . . ? C56 C55 C60 115.3(3) . . ? C57 C56 C55 121.7(3) . . ? C56 C57 C58 121.5(4) . . ? C59 C58 C57 118.8(4) . . ? C58 C59 C60 121.1(4) . . ? C59 C60 C55 121.5(4) . . ? C59 C60 N6 116.8(3) . . ? C55 C60 N6 121.7(3) . . ? C63 N7 C62 124.3(3) . . ? O108 N8 O107 121.7(3) . . ? O108 N8 C68 118.2(3) . . ? O107 N8 C68 120.1(3) . . ? O13 C61 C62 108.5(2) . . ? N7 C62 C61 109.4(2) . . ? N7 C63 C68 124.5(3) . . ? N7 C63 C64 120.9(3) . . ? C68 C63 C64 114.5(3) . . ? C65 C64 C63 121.8(3) . . ? C64 C65 C66 121.3(3) . . ? C67 C66 C65 118.7(3) . . ? C66 C67 C68 120.6(3) . . ? C67 C68 C63 123.0(3) . . ? C67 C68 N8 116.3(3) . . ? C63 C68 N8 120.6(3) . . ? C71 N9 C70 126.3(3) . . ? O110 N10 O109 120.2(3) . . ? O110 N10 C76 119.8(3) . . ? O109 N10 C76 120.0(3) . . ? O18 C69 C70 107.8(2) . . ? N9 C70 C69 113.4(3) . . ? N9 C71 C76 123.5(3) . . ? N9 C71 C72 121.1(3) . . ? C76 C71 C72 115.3(3) . . ? C73 C72 C71 121.4(3) . . ? C72 C73 C74 121.6(3) . . ? C75 C74 C73 119.3(3) . . ? C74 C75 C76 120.1(3) . . ? C75 C76 C71 122.2(3) . . ? C75 C76 N10 116.1(3) . . ? C71 C76 N10 121.7(3) . . ? C79 N11 C78 122.4(2) . . ? O112 N12 O111 120.9(3) . . ? O112 N12 C84 119.2(3) . . ? O111 N12 C84 119.9(2) . . ? O20 C77 C78 103.6(2) . . ? N11 C78 C77 110.2(2) . . ? N11 C79 C84 124.2(3) . . ? N11 C79 C80 120.3(3) . . ? C84 C79 C80 115.5(3) . . ? C81 C80 C79 121.9(3) . . ? C80 C81 C82 121.5(3) . . ? C83 C82 C81 119.0(3) . . ? C82 C83 C84 120.5(3) . . ? C83 C84 C79 121.6(3) . . ? C83 C84 N12 116.5(3) . . ? C79 C84 N12 121.9(3) . . ? C87 N13 C86 123.9(3) . . ? O114 N14 O113 121.7(3) . . ? O114 N14 C92 118.7(3) . . ? O113 N14 C92 119.6(3) . . ? O25 C85 C86 108.1(2) . . ? N13 C86 C85 109.1(3) . . ? N13 C87 C88 120.7(3) . . ? N13 C87 C92 124.4(3) . . ? C88 C87 C92 114.9(3) . . ? C89 C88 C87 121.8(4) . . ? C88 C89 C90 121.8(3) . . ? C91 C90 C89 119.0(4) . . ? C90 C91 C92 120.5(4) . . ? C91 C92 N14 116.7(3) . . ? C91 C92 C87 121.9(3) . . ? N14 C92 C87 121.3(3) . . ? C95 N15 C94 124.5(2) . . ? O116 N16 O115 120.8(3) . . ? O116 N16 C100 118.9(3) . . ? O115 N16 C100 120.3(2) . . ? O27 C93 C94 107.6(2) . . ? N15 C94 C93 109.2(2) . . ? N15 C95 C96 121.5(3) . . ? N15 C95 C100 123.8(3) . . ? C96 C95 C100 114.7(3) . . ? C97 C96 C95 122.1(3) . . ? C96 C97 C98 121.9(3) . . ? C99 C98 C97 118.8(3) . . ? C98 C99 C100 120.0(3) . . ? C99 C100 C95 122.6(3) . . ? C99 C100 N16 116.7(3) . . ? C95 C100 N16 120.7(3) . . ? N50A C50A C55A 176.7(5) . . ? N50B N50B C50B 160(3) 2_665 . ? 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 -0.8(4) . . . . ? C28 C1 C2 C3 179.9(2) . . . . ? C1 C2 C3 C4 -0.7(4) . . . . ? C1 C2 C3 C7 175.0(2) . . . . ? C37 O4 C4 C5 20.8(4) . . . . ? C37 O4 C4 C3 -159.2(2) . . . . ? C2 C3 C4 O4 -178.7(2) . . . . ? C7 C3 C4 O4 5.5(3) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C7 C3 C4 C5 -174.5(2) . . . . ? O4 C4 C5 C6 179.4(2) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C4 C5 C6 O6 -177.4(2) . . . . ? C4 C5 C6 C1 -1.0(4) . . . . ? C45 O6 C6 C5 -67.4(3) . . . . ? C45 O6 C6 C1 116.1(3) . . . . ? C2 C1 C6 C5 1.6(4) . . . . ? C28 C1 C6 C5 -179.0(2) . . . . ? C2 C1 C6 O6 178.1(2) . . . . ? C28 C1 C6 O6 -2.6(4) . . . . ? C2 C3 C7 C8 -115.1(3) . . . . ? C4 C3 C7 C8 60.5(3) . . . . ? C2 C3 C7 C29 10.1(4) . . . . ? C4 C3 C7 C29 -174.3(2) . . . . ? C3 C7 C8 C13 -133.3(3) . . . . ? C29 C7 C8 C13 100.3(3) . . . . ? C3 C7 C8 C9 45.1(3) . . . . ? C29 C7 C8 C9 -81.2(3) . . . . ? C13 C8 C9 C10 -0.8(4) . . . . ? C7 C8 C9 C10 -179.3(2) . . . . ? C8 C9 C10 C11 1.9(4) . . . . ? C8 C9 C10 C14 -173.8(2) . . . . ? C53 O11 C11 C12 -28.6(3) . . . . ? C53 O11 C11 C10 151.6(2) . . . . ? C9 C10 C11 O11 179.1(2) . . . . ? C14 C10 C11 O11 -5.2(3) . . . . ? C9 C10 C11 C12 -0.7(4) . . . . ? C14 C10 C11 C12 175.0(2) . . . . ? O11 C11 C12 C13 178.6(2) . . . . ? C10 C11 C12 C13 -1.6(4) . . . . ? C61 O13 C13 C12 33.5(4) . . . . ? C61 O13 C13 C8 -147.6(3) . . . . ? C11 C12 C13 O13 -178.4(2) . . . . ? C11 C12 C13 C8 2.8(4) . . . . ? C9 C8 C13 O13 179.5(2) . . . . ? C7 C8 C13 O13 -2.0(4) . . . . ? C9 C8 C13 C12 -1.6(4) . . . . ? C7 C8 C13 C12 176.9(2) . . . . ? C9 C10 C14 C15 -55.1(3) . . . . ? C11 C10 C14 C15 129.3(2) . . . . ? C9 C10 C14 C31 72.6(3) . . . . ? C11 C10 C14 C31 -102.9(3) . . . . ? C10 C14 C15 C16 115.2(3) . . . . ? C31 C14 C15 C16 -8.8(3) . . . . ? C10 C14 C15 C20 -65.0(3) . . . . ? C31 C14 C15 C20 171.1(2) . . . . ? C20 C15 C16 C17 -1.4(4) . . . . ? C14 C15 C16 C17 178.5(2) . . . . ? C15 C16 C17 C18 2.2(4) . . . . ? C15 C16 C17 C21 -178.3(2) . . . . ? C69 O18 C18 C17 129.1(3) . . . . ? C69 O18 C18 C19 -51.7(3) . . . . ? C16 C17 C18 O18 178.0(2) . . . . ? C21 C17 C18 O18 -1.5(3) . . . . ? C16 C17 C18 C19 -1.2(4) . . . . ? C21 C17 C18 C19 179.3(2) . . . . ? O18 C18 C19 C20 -179.7(2) . . . . ? C17 C18 C19 C20 -0.6(4) . . . . ? C77 O20 C20 C19 -5.8(4) . . . . ? C77 O20 C20 C15 175.3(2) . . . . ? C18 C19 C20 O20 -177.4(2) . . . . ? C18 C19 C20 C15 1.4(4) . . . . ? C16 C15 C20 O20 178.4(2) . . . . ? C14 C15 C20 O20 -1.4(3) . . . . ? C16 C15 C20 C19 -0.5(4) . . . . ? C14 C15 C20 C19 179.6(2) . . . . ? C18 C17 C21 C22 73.3(3) . . . . ? C16 C17 C21 C22 -106.2(3) . . . . ? C18 C17 C21 C33 -160.4(2) . . . . ? C16 C17 C21 C33 20.2(3) . . . . ? C17 C21 C22 C23 46.8(3) . . . . ? C33 C21 C22 C23 -80.4(3) . . . . ? C17 C21 C22 C27 -132.5(2) . . . . ? C33 C21 C22 C27 100.3(3) . . . . ? C27 C22 C23 C24 1.3(4) . . . . ? C21 C22 C23 C24 -178.1(2) . . . . ? C22 C23 C24 C25 0.2(4) . . . . ? C22 C23 C24 C28 178.7(2) . . . . ? C85 O25 C25 C26 -1.0(4) . . . . ? C85 O25 C25 C24 -178.9(3) . . . . ? C23 C24 C25 O25 176.7(2) . . . . ? C28 C24 C25 O25 -1.8(4) . . . . ? C23 C24 C25 C26 -1.2(4) . . . . ? C28 C24 C25 C26 -179.8(2) . . . . ? O25 C25 C26 C27 -177.0(2) . . . . ? C24 C25 C26 C27 0.9(4) . . . . ? C93 O27 C27 C26 20.7(3) . . . . ? C93 O27 C27 C22 -160.6(2) . . . . ? C25 C26 C27 O27 179.2(2) . . . . ? C25 C26 C27 C22 0.6(4) . . . . ? C23 C22 C27 O27 179.7(2) . . . . ? C21 C22 C27 O27 -0.9(3) . . . . ? C23 C22 C27 C26 -1.6(4) . . . . ? C21 C22 C27 C26 177.7(2) . . . . ? C6 C1 C28 C24 -56.0(3) . . . . ? C2 C1 C28 C24 123.2(3) . . . . ? C6 C1 C28 C35 180.0(2) . . . . ? C2 C1 C28 C35 -0.8(3) . . . . ? C23 C24 C28 C1 -49.4(3) . . . . ? C25 C24 C28 C1 129.1(3) . . . . ? C23 C24 C28 C35 76.9(3) . . . . ? C25 C24 C28 C35 -104.6(3) . . . . ? C3 C7 C29 C30 172.1(2) . . . . ? C8 C7 C29 C30 -64.1(3) . . . . ? C15 C14 C31 C32 -70.0(3) . . . . ? C10 C14 C31 C32 164.5(2) . . . . ? C22 C21 C33 C34 -61.8(3) . . . . ? C17 C21 C33 C34 171.9(2) . . . . ? C1 C28 C35 C36 -174.3(2) . . . . ? C24 C28 C35 C36 61.1(3) . . . . ? C4 O4 C37 C38 165.5(2) . . . . ? C39 N1 C38 C37 78.5(4) . . . . ? O4 C37 C38 N1 60.4(4) . . . . ? C38 N1 C39 C44 176.1(3) . . . . ? C38 N1 C39 C40 -3.3(4) . . . . ? N1 C39 C40 C41 -179.6(3) . . . . ? C44 C39 C40 C41 0.9(4) . . . . ? C39 C40 C41 C42 0.2(5) . . . . ? C40 C41 C42 C43 -1.1(5) . . . . ? C41 C42 C43 C44 0.9(5) . . . . ? C42 C43 C44 C39 0.3(5) . . . . ? C42 C43 C44 N2 -177.3(3) . . . . ? N1 C39 C44 C43 179.3(3) . . . . ? C40 C39 C44 C43 -1.2(4) . . . . ? N1 C39 C44 N2 -3.2(4) . . . . ? C40 C39 C44 N2 176.3(3) . . . . ? O102 N2 C44 C43 1.5(4) . . . . ? O101 N2 C44 C43 -179.3(3) . . . . ? O102 N2 C44 C39 -176.2(3) . . . . ? O101 N2 C44 C39 3.0(4) . . . . ? C6 O6 C45 C46 151.2(2) . . . . ? C47 N3 C46 C45 178.8(3) . . . . ? O6 C45 C46 N3 -66.3(3) . . . . ? C46 N3 C47 C48 -1.4(5) . . . . ? C46 N3 C47 C52 179.4(3) . . . . ? N3 C47 C48 C49 179.0(3) . . . . ? C52 C47 C48 C49 -1.7(5) . . . . ? C47 C48 C49 C50 1.2(6) . . . . ? C48 C49 C50 C51 -0.7(7) . . . . ? C49 C50 C51 C52 0.6(7) . . . . ? C50 C51 C52 C47 -1.2(6) . . . . ? C50 C51 C52 N4 179.9(4) . . . . ? N3 C47 C52 C51 -179.1(3) . . . . ? C48 C47 C52 C51 1.7(5) . . . . ? N3 C47 C52 N4 -0.2(5) . . . . ? C48 C47 C52 N4 -179.5(3) . . . . ? O104 N4 C52 C51 -11.2(6) . . . . ? O103 N4 C52 C51 169.6(4) . . . . ? O104 N4 C52 C47 169.8(4) . . . . ? O103 N4 C52 C47 -9.3(6) . . . . ? C11 O11 C53 C54 -162.5(2) . . . . ? C55 N5 C54 C53 79.9(4) . . . . ? O11 C53 C54 N5 168.3(3) . . . . ? C54 N5 C55 C56 10.9(5) . . . . ? C54 N5 C55 C60 -169.7(3) . . . . ? N5 C55 C56 C57 176.5(3) . . . . ? C60 C55 C56 C57 -3.0(5) . . . . ? C55 C56 C57 C58 1.3(6) . . . . ? C56 C57 C58 C59 0.1(6) . . . . ? C57 C58 C59 C60 0.3(5) . . . . ? C58 C59 C60 C55 -2.1(5) . . . . ? C58 C59 C60 N6 178.5(3) . . . . ? N5 C55 C60 C59 -176.1(3) . . . . ? C56 C55 C60 C59 3.3(5) . . . . ? N5 C55 C60 N6 3.3(5) . . . . ? C56 C55 C60 N6 -177.3(3) . . . . ? O106 N6 C60 C59 -0.7(5) . . . . ? O105 N6 C60 C59 -178.4(3) . . . . ? O106 N6 C60 C55 179.9(3) . . . . ? O105 N6 C60 C55 2.2(5) . . . . ? C13 O13 C61 C62 156.6(3) . . . . ? C63 N7 C62 C61 -78.9(4) . . . . ? O13 C61 C62 N7 -171.0(3) . . . . ? C62 N7 C63 C68 172.1(3) . . . . ? C62 N7 C63 C64 -10.7(4) . . . . ? N7 C63 C64 C65 -174.7(3) . . . . ? C68 C63 C64 C65 2.8(4) . . . . ? C63 C64 C65 C66 -2.7(5) . . . . ? C64 C65 C66 C67 0.4(5) . . . . ? C65 C66 C67 C68 1.6(5) . . . . ? C66 C67 C68 C63 -1.4(5) . . . . ? C66 C67 C68 N8 -179.2(3) . . . . ? N7 C63 C68 C67 176.6(3) . . . . ? C64 C63 C68 C67 -0.8(4) . . . . ? N7 C63 C68 N8 -5.7(4) . . . . ? C64 C63 C68 N8 177.0(3) . . . . ? O108 N8 C68 C67 -2.9(4) . . . . ? O107 N8 C68 C67 175.6(3) . . . . ? O108 N8 C68 C63 179.2(3) . . . . ? O107 N8 C68 C63 -2.3(5) . . . . ? C18 O18 C69 C70 -149.5(2) . . . . ? C71 N9 C70 C69 -97.9(3) . . . . ? O18 C69 C70 N9 -62.8(4) . . . . ? C70 N9 C71 C76 -176.6(3) . . . . ? C70 N9 C71 C72 1.7(5) . . . . ? N9 C71 C72 C73 -178.0(3) . . . . ? C76 C71 C72 C73 0.4(5) . . . . ? C71 C72 C73 C74 -0.7(6) . . . . ? C72 C73 C74 C75 0.5(6) . . . . ? C73 C74 C75 C76 -0.1(6) . . . . ? C74 C75 C76 C71 -0.2(5) . . . . ? C74 C75 C76 N10 179.2(3) . . . . ? N9 C71 C76 C75 178.4(3) . . . . ? C72 C71 C76 C75 0.0(5) . . . . ? N9 C71 C76 N10 -0.9(5) . . . . ? C72 C71 C76 N10 -179.3(3) . . . . ? O110 N10 C76 C75 -2.8(5) . . . . ? O109 N10 C76 C75 177.2(3) . . . . ? O110 N10 C76 C71 176.5(3) . . . . ? O109 N10 C76 C71 -3.4(5) . . . . ? C20 O20 C77 C78 -176.1(2) . . . . ? C79 N11 C78 C77 -174.5(3) . . . . ? O20 C77 C78 N11 -176.9(2) . . . . ? C78 N11 C79 C84 176.9(3) . . . . ? C78 N11 C79 C80 -1.6(5) . . . . ? N11 C79 C80 C81 176.8(3) . . . . ? C84 C79 C80 C81 -1.8(5) . . . . ? C79 C80 C81 C82 0.3(5) . . . . ? C80 C81 C82 C83 0.8(5) . . . . ? C81 C82 C83 C84 -0.2(5) . . . . ? C82 C83 C84 C79 -1.4(5) . . . . ? C82 C83 C84 N12 178.1(3) . . . . ? N11 C79 C84 C83 -176.2(3) . . . . ? C80 C79 C84 C83 2.3(4) . . . . ? N11 C79 C84 N12 4.3(5) . . . . ? C80 C79 C84 N12 -177.2(3) . . . . ? O112 N12 C84 C83 -3.8(4) . . . . ? O111 N12 C84 C83 176.1(3) . . . . ? O112 N12 C84 C79 175.8(3) . . . . ? O111 N12 C84 C79 -4.4(5) . . . . ? C25 O25 C85 C86 -179.9(3) . . . . ? C87 N13 C86 C85 -73.9(4) . . . . ? O25 C85 C86 N13 160.1(3) . . . . ? C86 N13 C87 C88 -4.3(4) . . . . ? C86 N13 C87 C92 176.3(3) . . . . ? N13 C87 C88 C89 -177.5(3) . . . . ? C92 C87 C88 C89 1.9(5) . . . . ? C87 C88 C89 C90 -2.4(6) . . . . ? C88 C89 C90 C91 1.2(6) . . . . ? C89 C90 C91 C92 0.2(6) . . . . ? C90 C91 C92 N14 180.0(3) . . . . ? C90 C91 C92 C87 -0.5(5) . . . . ? O114 N14 C92 C91 2.3(4) . . . . ? O113 N14 C92 C91 -178.8(3) . . . . ? O114 N14 C92 C87 -177.1(3) . . . . ? O113 N14 C92 C87 1.7(4) . . . . ? N13 C87 C92 C91 178.9(3) . . . . ? C88 C87 C92 C91 -0.5(4) . . . . ? N13 C87 C92 N14 -1.6(4) . . . . ? C88 C87 C92 N14 179.0(3) . . . . ? C27 O27 C93 C94 168.1(2) . . . . ? C95 N15 C94 C93 80.4(3) . . . . ? O27 C93 C94 N15 178.6(2) . . . . ? C94 N15 C95 C96 5.7(4) . . . . ? C94 N15 C95 C100 -175.8(3) . . . . ? N15 C95 C96 C97 177.3(3) . . . . ? C100 C95 C96 C97 -1.4(4) . . . . ? C95 C96 C97 C98 -0.3(5) . . . . ? C96 C97 C98 C99 1.4(6) . . . . ? C97 C98 C99 C100 -0.7(5) . . . . ? C98 C99 C100 C95 -1.2(5) . . . . ? C98 C99 C100 N16 179.9(3) . . . . ? N15 C95 C100 C99 -176.5(3) . . . . ? C96 C95 C100 C99 2.2(4) . . . . ? N15 C95 C100 N16 2.4(4) . . . . ? C96 C95 C100 N16 -179.0(2) . . . . ? O116 N16 C100 C99 -6.4(4) . . . . ? O115 N16 C100 C99 173.5(3) . . . . ? O116 N16 C100 C95 174.6(3) . . . . ? O115 N16 C100 C95 -5.4(4) . . . . ? 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 N1 H1N O101 0.894(18) 1.93(3) 2.632(3) 134(3) . N3 H3N O103 0.892(18) 1.91(3) 2.632(4) 137(3) . N5 H5N O105 0.903(18) 1.94(3) 2.610(4) 129(3) . N5 H5N O105 0.903(18) 2.27(3) 3.031(4) 142(3) 2_786 N7 H7N O107 0.920(18) 1.77(2) 2.620(4) 152(3) . N7 H7N N8 0.920(18) 2.30(3) 2.923(4) 125(3) . N9 H9N O109 0.898(18) 1.86(3) 2.613(3) 141(3) . N9 H9N N10 0.898(18) 2.46(3) 2.916(4) 112(3) . N11 H11N O111 0.883(18) 2.01(3) 2.639(3) 127(3) . N13 H13N O113 0.891(18) 1.89(3) 2.623(3) 138(3) . N13 H13N N14 0.891(18) 2.51(3) 2.940(4) 110(3) . N15 H15N O115 0.897(18) 1.92(3) 2.609(3) 132(3) . N15 H15N N50A 0.897(18) 2.44(3) 3.107(5) 131(3) 2_565 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 67.12 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.880 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.059 #===end data_5A _database_code_depnum_ccdc_archive 'CCDC 781925' #TrackingRef '- Octapodands.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H163 N16 O25.50' _chemical_formula_weight 2381.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 12.6739(5) _cell_length_b 20.5874(7) _cell_length_c 25.8506(9) _cell_angle_alpha 77.841(3) _cell_angle_beta 77.976(2) _cell_angle_gamma 74.025(2) _cell_volume 6257.4(4) _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 rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2542 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8696 _exptl_absorpt_correction_T_max 0.9316 _exptl_absorpt_process_details 'Denzo (Otwinowski, Majewski, Borek & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\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 20941 _diffrn_reflns_av_R_equivalents 0.1675 _diffrn_reflns_av_sigmaI/netI 0.1515 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 64.85 _reflns_number_total 14939 _reflns_number_gt 7014 _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14939 _refine_ls_number_parameters 1489 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.2509 _refine_ls_R_factor_gt 0.1458 _refine_ls_wR_factor_ref 0.4282 _refine_ls_wR_factor_gt 0.3528 _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_restrained_S_all 1.287 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.003 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 C29 C 1.3749(8) 0.0326(6) 0.1720(4) 0.085(3) Uani 1 1 d . . . H29A H 1.2974 0.0402 0.1661 0.102 Uiso 1 1 calc R . . H29B H 1.3995 0.0751 0.1557 0.102 Uiso 1 1 calc R . . C30 C 1.4472(9) -0.0248(7) 0.1429(4) 0.107(4) Uani 1 1 d . . . H30A H 1.5249 -0.0207 0.1374 0.128 Uiso 1 1 calc R . . H30B H 1.4437 -0.0686 0.1672 0.128 Uiso 1 1 calc R . . C31 C 1.4244(14) -0.0300(12) 0.0931(7) 0.216(11) Uani 1 1 d . A . H31A H 1.4327 0.0126 0.0681 0.259 Uiso 1 1 calc R . . H31B H 1.3453 -0.0312 0.0980 0.259 Uiso 1 1 calc R . . C32 C 1.4944(12) -0.0912(9) 0.0654(6) 0.161(8) Uani 1 1 d D . . H32A H 1.4949 -0.1330 0.0925 0.193 Uiso 0.48(3) 1 calc PR A 1 H32B H 1.5718 -0.0860 0.0561 0.193 Uiso 0.48(3) 1 calc PR A 1 H32C H 1.5580 -0.1119 0.0850 0.193 Uiso 0.52(3) 1 calc PR A 2 H32D H 1.5258 -0.0707 0.0292 0.193 Uiso 0.52(3) 1 calc PR A 2 C33A C 1.4639(19) -0.1052(14) 0.0143(9) 0.105(12) Uiso 0.48(3) 1 d PD A 1 H33A H 1.3943 -0.1212 0.0246 0.126 Uiso 0.48(3) 1 calc PR A 1 H33B H 1.4488 -0.0616 -0.0109 0.126 Uiso 0.48(3) 1 calc PR A 1 C34A C 1.5536(19) -0.1585(14) -0.0150(11) 0.084(9) Uiso 0.48(3) 1 d PD A 1 H34A H 1.6148 -0.1375 -0.0350 0.101 Uiso 0.48(3) 1 calc PR A 1 H34B H 1.5847 -0.1975 0.0116 0.101 Uiso 0.48(3) 1 calc PR A 1 C33B C 1.454(3) -0.153(2) 0.0566(18) 0.24(2) Uiso 0.52(3) 1 d PD A 2 H33C H 1.3737 -0.1372 0.0540 0.288 Uiso 0.52(3) 1 calc PR A 2 H33D H 1.4623 -0.1891 0.0885 0.288 Uiso 0.52(3) 1 calc PR A 2 C34B C 1.518(3) -0.185(2) 0.0053(12) 0.152(14) Uiso 0.52(3) 1 d PD A 2 H34C H 1.5903 -0.1734 0.0007 0.183 Uiso 0.52(3) 1 calc PR A 2 H34D H 1.5324 -0.2344 0.0197 0.183 Uiso 0.52(3) 1 calc PR A 2 C35 C 1.507(2) -0.1840(15) -0.0531(10) 0.304(15) Uiso 1 1 d D . . H35A H 1.4602 -0.1441 -0.0735 0.365 Uiso 0.48(3) 1 calc PR A 1 H35B H 1.4572 -0.2131 -0.0319 0.365 Uiso 0.48(3) 1 calc PR A 1 H35C H 1.4358 -0.1966 -0.0512 0.365 Uiso 0.52(3) 1 calc PR A 2 H35D H 1.4955 -0.1354 -0.0705 0.365 Uiso 0.52(3) 1 calc PR A 2 C36 C 1.5915(17) -0.2251(11) -0.0934(9) 0.206(8) Uiso 1 1 d D A . H36A H 1.6517 -0.2015 -0.1097 0.247 Uiso 1 1 calc R . . H36B H 1.6249 -0.2712 -0.0750 0.247 Uiso 1 1 calc R . . C37 C 1.532(2) -0.2311(13) -0.1362(10) 0.228(10) Uiso 1 1 d D . . H37 H 1.4752 -0.2552 -0.1243 0.274 Uiso 1 1 calc R A . C38 C 1.549(3) -0.207(2) -0.1879(12) 0.40(2) Uiso 1 1 d D A . H38A H 1.6044 -0.1829 -0.2024 0.481 Uiso 1 1 calc R . . H38B H 1.5048 -0.2150 -0.2107 0.481 Uiso 1 1 calc R . . O13A O 0.548(2) 0.7036(14) 0.2035(13) 0.182(13) Uiso 0.48(2) 1 d PD B 1 O14A O 0.661(3) 0.6509(16) 0.2615(14) 0.160(16) Uiso 0.48(2) 1 d PD B 1 N13A N 0.817(5) 0.534(2) 0.2243(19) 0.29(4) Uiso 0.48(2) 1 d PD B 1 H13A H 0.8012 0.5620 0.2477 0.352 Uiso 0.48(2) 1 calc PR B 1 N14A N 0.613(2) 0.6627(16) 0.2082(19) 0.153(13) Uiso 0.48(2) 1 d PD B 1 C19A C 0.766(2) 0.5625(12) 0.1931(14) 0.084(9) Uiso 0.48(2) 1 d PD B 1 C20A C 0.807(2) 0.5256(15) 0.1525(12) 0.114(11) Uiso 0.48(2) 1 d PD B 1 H20A H 0.8659 0.4858 0.1582 0.137 Uiso 0.48(2) 1 calc PR B 1 C21A C 0.769(3) 0.5423(19) 0.1011(12) 0.143(13) Uiso 0.48(2) 1 d PD B 1 H21A H 0.7960 0.5066 0.0801 0.172 Uiso 0.48(2) 1 calc PR B 1 C22A C 0.702(5) 0.600(3) 0.077(2) 0.34(5) Uiso 0.48(2) 1 d PD B 1 H22A H 0.6952 0.6162 0.0404 0.412 Uiso 0.48(2) 1 calc PR B 1 C23A C 0.633(3) 0.6349(18) 0.1324(15) 0.152(14) Uiso 0.48(2) 1 d PD B 1 H23A H 0.5606 0.6650 0.1351 0.183 Uiso 0.48(2) 1 calc PR B 1 C24A C 0.693(3) 0.6141(17) 0.1705(17) 0.132(13) Uiso 0.48(2) 1 d PD B 1 O13B O 0.573(3) 0.6931(19) 0.2487(18) 0.28(2) Uiso 0.52(2) 1 d PD B 2 O14B O 0.709(3) 0.6351(18) 0.2916(16) 0.246(16) Uiso 0.52(2) 1 d PD B 2 N13B N 0.8262(19) 0.5401(11) 0.2463(11) 0.112(8) Uiso 0.52(2) 1 d PD B 2 H13B H 0.8160 0.5628 0.2729 0.135 Uiso 0.52(2) 1 calc PR B 2 N14B N 0.635(3) 0.6509(18) 0.2464(19) 0.143(15) Uiso 0.52(2) 1 d PD B 2 C19B C 0.784(2) 0.5626(12) 0.2136(13) 0.079(8) Uiso 0.52(2) 1 d PD B 2 C20B C 0.830(5) 0.539(3) 0.1669(16) 0.28(4) Uiso 0.52(2) 1 d PD B 2 H20B H 0.8863 0.4973 0.1688 0.336 Uiso 0.52(2) 1 calc PR B 2 C21B C 0.800(3) 0.571(2) 0.1133(14) 0.170(15) Uiso 0.52(2) 1 d PD B 2 H21B H 0.8517 0.5558 0.0834 0.204 Uiso 0.52(2) 1 calc PR B 2 C22B C 0.706(3) 0.620(2) 0.1019(19) 0.188(18) Uiso 0.52(2) 1 d PD B 2 H22B H 0.6798 0.6349 0.0685 0.225 Uiso 0.52(2) 1 calc PR B 2 C23B C 0.648(2) 0.6481(14) 0.1612(13) 0.102(9) Uiso 0.52(2) 1 d PD B 2 H23B H 0.5807 0.6827 0.1661 0.122 Uiso 0.52(2) 1 calc PR B 2 C24B C 0.705(3) 0.6167(17) 0.1984(16) 0.162(15) Uiso 0.52(2) 1 d PD B 2 O4 O 1.4107(5) 0.0305(3) 0.3297(2) 0.077(2) Uani 1 1 d . . . O6 O 1.1071(5) 0.2346(4) 0.3431(2) 0.0748(19) Uani 1 1 d . . . O11 O 1.2373(6) -0.2291(4) 0.3025(3) 0.091(2) Uani 1 1 d . . . O13 O 1.5269(5) -0.1066(4) 0.2605(3) 0.087(2) Uani 1 1 d . . . O18 O 0.7628(5) 0.0803(3) 0.3998(2) 0.0627(17) Uani 1 1 d . . . O20 O 1.0577(5) -0.1278(3) 0.3873(2) 0.0687(18) Uani 1 1 d . . . O25 O 0.9109(6) 0.3541(4) 0.2763(3) 0.080(2) Uani 1 1 d . . . O27 O 0.6227(5) 0.2298(3) 0.3186(3) 0.0715(18) Uani 1 1 d . . . O101 O 1.4380(6) -0.1789(4) 0.4007(3) 0.081(2) Uani 1 1 d . . . O102 O 1.5211(6) -0.2817(5) 0.3854(3) 0.103(3) Uani 1 1 d . . . O103 O 0.6033(6) 0.3713(4) 0.4210(3) 0.101(3) Uani 1 1 d . . . O104 O 0.7571(6) 0.2944(4) 0.4259(3) 0.077(2) Uani 1 1 d . . . O105 O 1.5885(11) -0.5712(7) 0.2527(10) 0.306(13) Uani 1 1 d . . . O106 O 1.487(2) -0.5220(13) 0.3122(10) 0.248(14) Uani 1 1 d . . . O107 O 1.9645(8) -0.3158(6) 0.2449(5) 0.141(4) Uani 1 1 d . . . O108 O 2.0452(10) -0.3837(7) 0.1859(5) 0.196(6) Uani 1 1 d . . . O109 O 0.2341(6) 0.1164(4) 0.4945(3) 0.090(2) Uani 1 1 d . . . O110 O 0.4057(6) 0.0609(4) 0.4951(3) 0.0723(19) Uani 1 1 d . . . O111 O 0.9696(7) -0.3262(5) 0.4610(4) 0.109(3) Uani 1 1 d . . . O112 O 1.0059(8) -0.4343(6) 0.4718(6) 0.170(5) Uani 1 1 d . . . O115 O 0.2240(9) 0.4329(6) 0.3943(5) 0.148(4) Uani 1 1 d . . . O116 O 0.1279(9) 0.5257(6) 0.3521(5) 0.154(4) Uani 1 1 d . . . N1 N 1.5506(7) -0.0856(4) 0.3857(3) 0.068(2) Uani 1 1 d . . . H1N H 1.4838 -0.0933 0.3954 0.082 Uiso 1 1 calc R . . N2 N 1.5230(9) -0.2220(6) 0.3889(3) 0.078(2) Uani 1 1 d . . . N3 N 0.9497(6) 0.3297(4) 0.4093(3) 0.067(2) Uani 1 1 d . . . H3N H 0.9209 0.2938 0.4179 0.081 Uiso 1 1 calc R . . N4 N 0.7072(8) 0.3541(5) 0.4198(3) 0.078(2) Uani 1 1 d . . . N5 N 1.3307(10) -0.4069(6) 0.2894(6) 0.131(4) Uani 1 1 d . . . H5N H 1.3558 -0.4391 0.3153 0.157 Uiso 1 1 calc R . . N6 N 1.5124(15) -0.5231(10) 0.2659(13) 0.202(13) Uani 1 1 d . . . N7 N 1.8092(7) -0.2063(5) 0.2194(4) 0.089(3) Uani 1 1 d . . . H7N H 1.8501 -0.2293 0.2440 0.106 Uiso 1 1 calc R . . N8 N 1.9752(10) -0.3290(7) 0.2003(7) 0.133(5) Uani 1 1 d . . . N9 N 0.5604(6) 0.1283(4) 0.4769(3) 0.066(2) Uani 1 1 d . . . H9N H 0.5476 0.0893 0.4744 0.079 Uiso 1 1 calc R . . N10 N 0.3344(7) 0.1163(5) 0.4932(3) 0.070(2) Uani 1 1 d . . . N11 N 1.1238(6) -0.2626(4) 0.4508(3) 0.063(2) Uani 1 1 d . . . H11N H 1.0532 -0.2580 0.4498 0.076 Uiso 1 1 calc R . . N12 N 1.0342(9) -0.3794(7) 0.4636(4) 0.092(3) Uani 1 1 d . . . N15 N 0.3374(7) 0.3342(6) 0.3420(5) 0.112(3) Uani 1 1 d . . . H15N H 0.3059 0.3462 0.3734 0.135 Uiso 1 1 calc R . . N16 N 0.1923(10) 0.4690(6) 0.3509(7) 0.119(4) Uani 1 1 d . . . C1 C 1.1580(8) 0.1834(5) 0.2662(4) 0.066(3) Uani 1 1 d . . . C2 C 1.2235(7) 0.1289(5) 0.2398(4) 0.068(3) Uani 1 1 d . . . H2 H 1.2112 0.1278 0.2050 0.081 Uiso 1 1 calc R . . C3 C 1.3040(8) 0.0773(5) 0.2618(4) 0.067(3) Uani 1 1 d . . . C4 C 1.3223(8) 0.0815(5) 0.3123(4) 0.070(3) Uani 1 1 d . . . C5 C 1.2587(8) 0.1307(6) 0.3407(4) 0.078(3) Uani 1 1 d . . . H5 H 1.2708 0.1306 0.3758 0.093 Uiso 1 1 calc R . . C6 C 1.1752(8) 0.1817(6) 0.3182(4) 0.073(3) Uani 1 1 d . . . C7 C 1.3758(8) 0.0203(6) 0.2329(4) 0.076(3) Uani 1 1 d . . . H7 H 1.4541 0.0135 0.2384 0.092 Uiso 1 1 calc R . . C8 C 1.3408(7) -0.0459(6) 0.2564(4) 0.065(3) Uani 1 1 d . . . C9 C 1.2296(7) -0.0496(6) 0.2630(3) 0.065(3) Uani 1 1 d . . . H9 H 1.1749 -0.0078 0.2574 0.077 Uiso 1 1 calc R . . C10 C 1.1942(7) -0.1097(6) 0.2771(4) 0.062(3) Uani 1 1 d . . . C11 C 1.2741(8) -0.1707(6) 0.2879(4) 0.072(3) Uani 1 1 d . . . C12 C 1.3850(9) -0.1704(6) 0.2827(4) 0.074(3) Uani 1 1 d . . . H12 H 1.4387 -0.2122 0.2900 0.089 Uiso 1 1 calc R . . C13 C 1.4175(7) -0.1101(7) 0.2671(4) 0.075(3) Uani 1 1 d . . . C14 C 1.0741(7) -0.1105(5) 0.2787(3) 0.059(2) Uani 1 1 d . . . H14 H 1.0650 -0.1568 0.2975 0.071 Uiso 1 1 calc R . . C15 C 0.9946(7) -0.0590(5) 0.3107(3) 0.056(2) Uani 1 1 d . . . C16 C 0.9231(7) 0.0002(5) 0.2876(4) 0.057(2) Uani 1 1 d . . . H16 H 0.9277 0.0090 0.2497 0.069 Uiso 1 1 calc R . . C17 C 0.8471(7) 0.0459(5) 0.3167(4) 0.059(2) Uani 1 1 d . . . C18 C 0.8413(7) 0.0339(5) 0.3723(4) 0.054(2) Uani 1 1 d . . . C19 C 0.9113(7) -0.0226(5) 0.3967(3) 0.061(3) Uani 1 1 d . . . H19 H 0.9077 -0.0308 0.4345 0.074 Uiso 1 1 calc R . . C20 C 0.9859(7) -0.0668(5) 0.3661(4) 0.059(2) Uani 1 1 d . . . C21 C 0.7703(7) 0.1115(5) 0.2906(3) 0.057(2) Uani 1 1 d . . . H21 H 0.6955 0.1164 0.3136 0.068 Uiso 1 1 calc R . . C22 C 0.8079(7) 0.1751(5) 0.2898(3) 0.057(2) Uani 1 1 d . . . C23 C 0.9187(7) 0.1795(5) 0.2722(3) 0.060(3) Uani 1 1 d . . . H23 H 0.9730 0.1393 0.2641 0.072 Uiso 1 1 calc R . . C24 C 0.9519(7) 0.2380(6) 0.2662(3) 0.060(2) Uani 1 1 d . . . C25 C 0.8752(8) 0.2952(5) 0.2801(4) 0.064(3) Uani 1 1 d . . . C26 C 0.7652(9) 0.2944(6) 0.2985(4) 0.070(3) Uani 1 1 d . . . H26 H 0.7132 0.3347 0.3081 0.083 Uiso 1 1 calc R . . C27 C 0.7307(7) 0.2357(5) 0.3031(4) 0.061(3) Uani 1 1 d . . . C28 C 1.0715(7) 0.2422(5) 0.2421(3) 0.061(3) Uani 1 1 d . . . H28 H 1.0816 0.2851 0.2507 0.074 Uiso 1 1 calc R . . C39 C 1.0517(7) -0.1028(5) 0.2209(3) 0.067(3) Uani 1 1 d . . . H39A H 0.9719 -0.0997 0.2221 0.080 Uiso 1 1 calc R . . H39B H 1.0679 -0.0594 0.2002 0.080 Uiso 1 1 calc R . . C40 C 1.1199(8) -0.1610(5) 0.1922(4) 0.074(3) Uani 1 1 d . . . H40A H 1.1002 -0.2039 0.2118 0.088 Uiso 1 1 calc R . . H40B H 1.1995 -0.1660 0.1931 0.088 Uiso 1 1 calc R . . C41 C 1.1040(8) -0.1519(6) 0.1347(4) 0.076(3) Uani 1 1 d . . . H41A H 1.0240 -0.1456 0.1339 0.092 Uiso 1 1 calc R . . H41B H 1.1250 -0.1093 0.1152 0.092 Uiso 1 1 calc R . . C42 C 1.1684(9) -0.2091(6) 0.1051(4) 0.086(3) Uani 1 1 d . . . H42A H 1.1453 -0.2514 0.1237 0.103 Uiso 1 1 calc R . . H42B H 1.2482 -0.2167 0.1069 0.103 Uiso 1 1 calc R . . C43 C 1.1547(10) -0.1979(7) 0.0468(4) 0.107(4) Uani 1 1 d . . . H43A H 1.0748 -0.1898 0.0449 0.128 Uiso 1 1 calc R . . H43B H 1.1790 -0.1560 0.0280 0.128 Uiso 1 1 calc R . . C44 C 1.2182(12) -0.2559(8) 0.0183(5) 0.127(5) Uani 1 1 d . . . H44A H 1.1890 -0.2966 0.0352 0.152 Uiso 1 1 calc R . . H44B H 1.2969 -0.2668 0.0234 0.152 Uiso 1 1 calc R . . C45 C 1.2145(12) -0.2432(8) -0.0418(5) 0.134(5) Uani 1 1 d D . . H45A H 1.1359 -0.2303 -0.0473 0.161 Uiso 1 1 calc R . . H45B H 1.2478 -0.2043 -0.0593 0.161 Uiso 1 1 calc R . . C46 C 1.2750(18) -0.3044(9) -0.0682(5) 0.194(9) Uani 1 1 d D . . H46A H 1.2489 -0.3452 -0.0483 0.233 Uiso 1 1 calc R . . H46B H 1.3557 -0.3136 -0.0679 0.233 Uiso 1 1 calc R . . C47 C 1.253(2) -0.2904(12) -0.1268(7) 0.204(10) Uani 1 1 d D . . H47 H 1.1852 -0.2617 -0.1365 0.245 Uiso 1 1 calc R . . C48 C 1.328(2) -0.3184(13) -0.1608(11) 0.249(13) Uani 1 1 d D . . H48A H 1.3957 -0.3469 -0.1503 0.299 Uiso 1 1 calc R . . H48B H 1.3177 -0.3109 -0.1971 0.299 Uiso 1 1 calc R . . C49 C 0.7541(7) 0.1079(5) 0.2347(4) 0.065(3) Uani 1 1 d . . . H49A H 0.7137 0.1538 0.2190 0.078 Uiso 1 1 calc R . . H49B H 0.8283 0.0974 0.2123 0.078 Uiso 1 1 calc R . . C50 C 0.6930(8) 0.0571(6) 0.2302(4) 0.082(3) Uani 1 1 d . . . H50A H 0.6187 0.0670 0.2525 0.099 Uiso 1 1 calc R . . H50B H 0.7338 0.0107 0.2449 0.099 Uiso 1 1 calc R . . C51 C 0.6779(10) 0.0569(6) 0.1716(4) 0.094(4) Uani 1 1 d . . . H51A H 0.6171 0.0346 0.1733 0.112 Uiso 1 1 calc R . . H51B H 0.6548 0.1049 0.1537 0.112 Uiso 1 1 calc R . . C52 C 0.7809(9) 0.0208(7) 0.1377(4) 0.091(4) Uani 1 1 d . . . H52A H 0.8398 0.0457 0.1332 0.110 Uiso 1 1 calc R . . H52B H 0.8080 -0.0259 0.1570 0.110 Uiso 1 1 calc R . . C53 C 0.7626(9) 0.0158(7) 0.0838(4) 0.094(4) Uani 1 1 d . . . H53A H 0.6947 -0.0011 0.0887 0.113 Uiso 1 1 calc R . . H53B H 0.7469 0.0628 0.0631 0.113 Uiso 1 1 calc R . . C54 C 0.8502(12) -0.0268(8) 0.0514(5) 0.118(5) Uani 1 1 d . . . H54A H 0.8660 -0.0739 0.0718 0.141 Uiso 1 1 calc R . . H54B H 0.9183 -0.0099 0.0461 0.141 Uiso 1 1 calc R . . C55 C 0.8280(11) -0.0302(7) -0.0024(4) 0.106(4) Uani 1 1 d D . . H55A H 0.8193 0.0161 -0.0242 0.127 Uiso 1 1 calc R . . H55B H 0.7566 -0.0433 0.0024 0.127 Uiso 1 1 calc R . . C56 C 0.9177(14) -0.0802(9) -0.0335(6) 0.153(6) Uani 1 1 d D . . H56A H 0.9853 -0.0623 -0.0450 0.184 Uiso 1 1 calc R . . H56B H 0.9371 -0.1246 -0.0096 0.184 Uiso 1 1 calc R . . C57 C 0.8817(18) -0.0917(12) -0.0821(7) 0.214(12) Uani 1 1 d D . . H57 H 0.8135 -0.1048 -0.0770 0.256 Uiso 1 1 calc R . . C58 C 0.9346(13) -0.0855(11) -0.1289(9) 0.182(8) Uani 1 1 d D . . H58A H 1.0033 -0.0726 -0.1358 0.219 Uiso 1 1 calc R . . H58B H 0.9061 -0.0937 -0.1575 0.219 Uiso 1 1 calc R . . C59 C 1.0881(8) 0.2500(5) 0.1802(4) 0.074(3) Uani 1 1 d . . . H59A H 1.1683 0.2449 0.1659 0.089 Uiso 1 1 calc R . . H59B H 1.0647 0.2127 0.1705 0.089 Uiso 1 1 calc R . . C60 C 1.0241(10) 0.3178(6) 0.1539(4) 0.094(4) Uani 1 1 d . . . H60A H 0.9446 0.3246 0.1701 0.112 Uiso 1 1 calc R . . H60B H 1.0516 0.3550 0.1612 0.112 Uiso 1 1 calc R . . C61 C 1.0343(11) 0.3224(6) 0.0947(4) 0.110(4) Uani 1 1 d . . . H61A H 1.1132 0.3178 0.0781 0.132 Uiso 1 1 calc R . . H61B H 1.0095 0.2842 0.0872 0.132 Uiso 1 1 calc R . . C62 C 0.9663(16) 0.3887(8) 0.0704(5) 0.164(7) Uani 1 1 d . . . H62A H 0.9997 0.4258 0.0732 0.197 Uiso 1 1 calc R . . H62B H 0.8910 0.3967 0.0920 0.197 Uiso 1 1 calc R . . C63 C 0.9545(18) 0.3946(9) 0.0129(8) 0.193(8) Uani 1 1 d . . . H63A H 0.9302 0.3547 0.0082 0.232 Uiso 1 1 calc R . . H63B H 1.0272 0.3949 -0.0104 0.232 Uiso 1 1 calc R . . C64 C 0.863(2) 0.4655(15) -0.0043(12) 0.274(13) Uiso 1 1 d . . . H64A H 0.8021 0.4693 0.0268 0.328 Uiso 1 1 calc R . . H64B H 0.8991 0.5030 -0.0063 0.328 Uiso 1 1 calc R . . C65 C 0.813(3) 0.482(2) -0.0473(17) 0.36(2) Uiso 1 1 d D . . H65A H 0.7525 0.4578 -0.0417 0.436 Uiso 1 1 calc R . . H65B H 0.8669 0.4682 -0.0792 0.436 Uiso 1 1 calc R . . C66 C 0.766(3) 0.560(2) -0.0548(18) 0.41(2) Uiso 1 1 d D . . H66A H 0.7721 0.5826 -0.0257 0.488 Uiso 1 1 calc R . . H66B H 0.7882 0.5851 -0.0908 0.488 Uiso 1 1 calc R . . C67 C 0.656(3) 0.538(2) -0.0477(15) 0.339(18) Uiso 1 1 d D . . H67 H 0.6475 0.5024 -0.0640 0.407 Uiso 1 1 calc R . . C68 C 0.575(4) 0.574(2) -0.0157(17) 0.42(3) Uiso 1 1 d D . . H68A H 0.5899 0.6085 -0.0008 0.509 Uiso 1 1 calc R . . H68B H 0.5032 0.5655 -0.0078 0.509 Uiso 1 1 calc R . . C69 C 1.4501(7) 0.0354(5) 0.3765(4) 0.074(3) Uani 1 1 d . . . H69A H 1.3970 0.0247 0.4092 0.089 Uiso 1 1 calc R . . H69B H 1.4591 0.0821 0.3746 0.089 Uiso 1 1 calc R . . C70 C 1.5612(8) -0.0165(6) 0.3774(4) 0.070(3) Uani 1 1 d . . . H70A H 1.6106 -0.0074 0.3430 0.084 Uiso 1 1 calc R . . H70B H 1.5965 -0.0109 0.4064 0.084 Uiso 1 1 calc R . . C71 C 1.6379(8) -0.1389(6) 0.3792(4) 0.069(3) Uani 1 1 d . . . C72 C 1.7480(7) -0.1303(5) 0.3711(4) 0.066(3) Uani 1 1 d . . . H72 H 1.7598 -0.0868 0.3716 0.079 Uiso 1 1 calc R . . C73 C 1.8369(9) -0.1844(6) 0.3626(4) 0.076(3) Uani 1 1 d . . . H73 H 1.9094 -0.1770 0.3573 0.091 Uiso 1 1 calc R . . C74 C 1.8274(9) -0.2482(7) 0.3613(4) 0.085(3) Uani 1 1 d . . . H74 H 1.8919 -0.2840 0.3549 0.102 Uiso 1 1 calc R . . C75 C 1.7227(10) -0.2602(6) 0.3695(4) 0.079(3) Uani 1 1 d . . . H75 H 1.7138 -0.3043 0.3687 0.095 Uiso 1 1 calc R . . C76 C 1.6294(8) -0.2057(6) 0.3792(4) 0.068(3) Uani 1 1 d . . . C77 C 1.1279(8) 0.2468(6) 0.3925(4) 0.076(3) Uani 1 1 d . . . H77A H 1.2088 0.2397 0.3916 0.091 Uiso 1 1 calc R . . H77B H 1.0994 0.2151 0.4232 0.091 Uiso 1 1 calc R . . C78 C 1.0692(8) 0.3192(6) 0.3977(4) 0.078(3) Uani 1 1 d . . . H78A H 1.0948 0.3325 0.4268 0.094 Uiso 1 1 calc R . . H78B H 1.0894 0.3494 0.3639 0.094 Uiso 1 1 calc R . . C79 C 0.8809(8) 0.3929(6) 0.4073(4) 0.073(3) Uani 1 1 d . . . C80 C 0.9245(10) 0.4520(7) 0.4027(5) 0.093(4) Uani 1 1 d . . . H80 H 1.0019 0.4456 0.4020 0.112 Uiso 1 1 calc R . . C81 C 0.8585(11) 0.5164(7) 0.3993(6) 0.120(5) Uani 1 1 d . . . H81 H 0.8898 0.5538 0.3982 0.144 Uiso 1 1 calc R . . C82 C 0.7457(11) 0.5288(7) 0.3974(6) 0.123(5) Uani 1 1 d . . . H82 H 0.7024 0.5744 0.3905 0.148 Uiso 1 1 calc R . . C83 C 0.6982(10) 0.4757(6) 0.4053(5) 0.098(4) Uani 1 1 d . . . H83 H 0.6199 0.4844 0.4075 0.117 Uiso 1 1 calc R . . C84 C 0.7617(8) 0.4081(6) 0.4103(4) 0.074(3) Uani 1 1 d . . . C85 C 1.3125(10) -0.2904(7) 0.2996(6) 0.109(4) Uani 1 1 d . . . H85A H 1.3601 -0.3001 0.3276 0.131 Uiso 1 1 calc R . . H85B H 1.3608 -0.2887 0.2642 0.131 Uiso 1 1 calc R . . C86 C 1.2513(12) -0.3467(7) 0.3078(7) 0.126(5) Uani 1 1 d . . . H86A H 1.2206 -0.3578 0.3461 0.151 Uiso 1 1 calc R . . H86B H 1.1890 -0.3315 0.2870 0.151 Uiso 1 1 calc R . . C87 C 1.3727(9) -0.4216(6) 0.2390(5) 0.111(4) Uani 1 1 d G . . C88 C 1.4582(9) -0.4779(5) 0.2272(7) 0.149(7) Uani 1 1 d G . . C89 C 1.4919(10) -0.4899(6) 0.1746(8) 0.177(8) Uani 1 1 d G . . H89 H 1.5503 -0.5284 0.1666 0.212 Uiso 1 1 calc R . . C90 C 1.4401(15) -0.4455(10) 0.1338(6) 0.268(16) Uani 1 1 d G . . H90 H 1.4632 -0.4536 0.0979 0.321 Uiso 1 1 calc R . . C91 C 1.3546(14) -0.3891(8) 0.1456(5) 0.198(9) Uani 1 1 d G . . H91 H 1.3192 -0.3587 0.1177 0.237 Uiso 1 1 calc R . . C92 C 1.3209(8) -0.3772(5) 0.1982(6) 0.137(5) Uani 1 1 d G . . H92 H 1.2625 -0.3386 0.2062 0.164 Uiso 1 1 calc R . . C93 C 1.6076(7) -0.1647(6) 0.2454(4) 0.074(3) Uani 1 1 d . . . H93A H 1.5909 -0.1771 0.2135 0.088 Uiso 1 1 calc R . . H93B H 1.6077 -0.2041 0.2749 0.088 Uiso 1 1 calc R . . C94 C 1.7189(7) -0.1473(6) 0.2328(4) 0.087(3) Uani 1 1 d . . . H94A H 1.7186 -0.1091 0.2022 0.105 Uiso 1 1 calc R . . H94B H 1.7321 -0.1319 0.2641 0.105 Uiso 1 1 calc R . . C95 C 1.8328(8) -0.2273(6) 0.1716(5) 0.081(3) Uani 1 1 d . . . C96 C 1.7757(9) -0.1918(7) 0.1293(5) 0.097(4) Uani 1 1 d . . . H96 H 1.7182 -0.1518 0.1348 0.117 Uiso 1 1 calc R . . C97 C 1.7995(12) -0.2123(9) 0.0809(6) 0.130(5) Uani 1 1 d . . . H97 H 1.7597 -0.1853 0.0532 0.156 Uiso 1 1 calc R . . C98 C 1.8811(13) -0.2723(9) 0.0698(6) 0.137(6) Uani 1 1 d . . . H98 H 1.8963 -0.2858 0.0355 0.164 Uiso 1 1 calc R . . C99 C 1.9355(11) -0.3088(8) 0.1090(7) 0.113(5) Uani 1 1 d . . . H99 H 1.9903 -0.3497 0.1032 0.136 Uiso 1 1 calc R . . C100 C 1.9134(10) -0.2883(7) 0.1568(7) 0.108(4) Uani 1 1 d . . . C101 C 0.7589(7) 0.0710(5) 0.4570(3) 0.062(3) Uani 1 1 d . . . H10A H 0.8329 0.0678 0.4656 0.075 Uiso 1 1 calc R . . H10B H 0.7351 0.0286 0.4748 0.075 Uiso 1 1 calc R . . C102 C 0.6760(7) 0.1327(5) 0.4751(4) 0.066(3) Uani 1 1 d . . . H10C H 0.6861 0.1366 0.5111 0.080 Uiso 1 1 calc R . . H10D H 0.6894 0.1743 0.4501 0.080 Uiso 1 1 calc R . . C103 C 0.4735(7) 0.1845(5) 0.4825(3) 0.059(3) Uani 1 1 d . . . C104 C 0.4884(8) 0.2496(6) 0.4797(4) 0.069(3) Uani 1 1 d . . . H104 H 0.5618 0.2555 0.4746 0.083 Uiso 1 1 calc R . . C105 C 0.4002(9) 0.3056(5) 0.4840(4) 0.075(3) Uani 1 1 d . . . H105 H 0.4139 0.3494 0.4810 0.090 Uiso 1 1 calc R . . C106 C 0.2908(8) 0.2992(6) 0.4928(4) 0.070(3) Uani 1 1 d . . . H106 H 0.2303 0.3382 0.4961 0.084 Uiso 1 1 calc R . . C116 C 1.1533(9) -0.3840(6) 0.4576(4) 0.074(3) Uani 1 1 d . . . C107 C 0.2728(8) 0.2379(6) 0.4963(4) 0.071(3) Uani 1 1 d . . . H107 H 0.1986 0.2331 0.5030 0.085 Uiso 1 1 calc R . . C108 C 0.3622(7) 0.1791(5) 0.4904(3) 0.055(2) Uani 1 1 d . . . C109 C 1.0670(8) -0.1389(5) 0.4427(3) 0.067(3) Uani 1 1 d . . . H10E H 0.9967 -0.1464 0.4654 0.080 Uiso 1 1 calc R . . H10F H 1.0839 -0.0989 0.4519 0.080 Uiso 1 1 calc R . . C110 C 1.1587(8) -0.2004(5) 0.4512(4) 0.066(3) Uani 1 1 d . . . H11A H 1.2230 -0.1966 0.4225 0.080 Uiso 1 1 calc R . . H11B H 1.1823 -0.2035 0.4859 0.080 Uiso 1 1 calc R . . C111 C 1.1909(8) -0.3259(5) 0.4519(4) 0.062(3) Uani 1 1 d . . . C112 C 1.3065(8) -0.3356(6) 0.4490(4) 0.078(3) Uani 1 1 d . . . H112 H 1.3359 -0.2974 0.4475 0.094 Uiso 1 1 calc R . . C113 C 1.3772(10) -0.3994(7) 0.4482(5) 0.099(4) Uani 1 1 d . . . H113 H 1.4549 -0.4038 0.4445 0.119 Uiso 1 1 calc R . . C114 C 1.3390(11) -0.4578(7) 0.4525(6) 0.108(4) Uani 1 1 d . . . H114 H 1.3887 -0.5017 0.4519 0.130 Uiso 1 1 calc R . . C115 C 1.2279(11) -0.4493(6) 0.4575(5) 0.098(4) Uani 1 1 d . . . H115 H 1.1990 -0.4883 0.4611 0.117 Uiso 1 1 calc R . . C117 C 0.8363(10) 0.4175(6) 0.2646(5) 0.091(3) Uani 1 1 d . B . H11C H 0.7794 0.4270 0.2965 0.109 Uiso 1 1 calc R . . H11D H 0.7981 0.4170 0.2350 0.109 Uiso 1 1 calc R . . C118 C 0.9018(12) 0.4722(7) 0.2485(6) 0.124(5) Uani 1 1 d D . . H11E H 0.9687 0.4587 0.2217 0.149 Uiso 0.48(2) 1 calc PR B 1 H11F H 0.9246 0.4817 0.2800 0.149 Uiso 0.48(2) 1 calc PR B 1 H11G H 0.9518 0.4661 0.2748 0.149 Uiso 0.52(2) 1 calc PR B 2 H11H H 0.9482 0.4675 0.2129 0.149 Uiso 0.52(2) 1 calc PR B 2 C125 C 0.5424(7) 0.2900(6) 0.3279(5) 0.089(3) Uani 1 1 d . . . H12A H 0.5449 0.3259 0.2958 0.106 Uiso 1 1 calc R . . H12B H 0.5553 0.3073 0.3584 0.106 Uiso 1 1 calc R . . C126 C 0.4279(8) 0.2709(5) 0.3409(5) 0.091(4) Uani 1 1 d . . . H12C H 0.4218 0.2459 0.3133 0.109 Uiso 1 1 calc R . . H12D H 0.4216 0.2407 0.3761 0.109 Uiso 1 1 calc R . . C127 C 0.3008(4) 0.3739(3) 0.2986(3) 0.083(3) Uani 1 1 d G . . C128 C 0.3253(5) 0.3502(4) 0.2499(3) 0.147(6) Uani 1 1 d G . . H128 H 0.3735 0.3064 0.2466 0.176 Uiso 1 1 calc R . . C129 C 0.2792(5) 0.3907(5) 0.2060(3) 0.168(8) Uani 1 1 d G . . H129 H 0.2959 0.3745 0.1727 0.202 Uiso 1 1 calc R . . C130 C 0.2085(5) 0.4548(4) 0.2109(3) 0.162(7) Uani 1 1 d G . . H130 H 0.1770 0.4825 0.1809 0.194 Uiso 1 1 calc R . . C131 C 0.1841(4) 0.4785(3) 0.2596(4) 0.120(5) Uani 1 1 d G . . H131 H 0.1358 0.5223 0.2629 0.144 Uiso 1 1 calc R . . C132 C 0.2302(4) 0.4380(4) 0.3034(3) 0.109(4) Uani 1 1 d G . . O300 O 0.9345(5) 0.1632(3) 0.4041(3) 0.062(3) Uani 0.50 1 d PG . . O301 O 1.0774(5) 0.0435(4) 0.4555(3) 0.094(5) Uani 0.50 1 d PG . . O302 O 1.2458(6) -0.0489(4) 0.3968(4) 0.097(5) Uani 0.50 1 d PG . . 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 C29 0.064(6) 0.128(10) 0.072(7) -0.038(7) -0.010(5) -0.021(6) C30 0.082(8) 0.161(13) 0.076(8) -0.056(8) -0.015(6) 0.001(8) C31 0.146(14) 0.32(3) 0.197(18) -0.183(19) -0.081(13) 0.071(16) C32 0.143(13) 0.183(16) 0.146(13) -0.110(13) -0.062(10) 0.068(12) O4 0.074(4) 0.092(5) 0.068(4) -0.027(4) -0.034(4) -0.001(4) O6 0.064(4) 0.091(5) 0.074(4) -0.028(4) -0.028(3) -0.003(4) O11 0.074(5) 0.075(6) 0.123(6) -0.016(5) -0.035(4) -0.001(5) O13 0.043(4) 0.114(6) 0.105(5) -0.050(5) -0.018(4) 0.006(4) O18 0.056(4) 0.069(4) 0.061(4) -0.015(3) -0.018(3) -0.002(3) O20 0.068(4) 0.066(4) 0.069(4) -0.006(3) -0.027(3) -0.004(3) O25 0.081(5) 0.067(5) 0.094(5) -0.017(4) -0.021(4) -0.014(4) O27 0.048(4) 0.059(4) 0.104(5) -0.022(4) -0.018(3) 0.002(3) O101 0.058(4) 0.107(6) 0.084(5) -0.018(4) -0.016(4) -0.025(4) O102 0.090(5) 0.098(7) 0.132(7) -0.005(5) -0.039(5) -0.036(5) O103 0.071(5) 0.103(6) 0.139(7) -0.023(5) -0.023(5) -0.031(4) O104 0.087(5) 0.063(5) 0.092(5) -0.015(4) -0.021(4) -0.027(4) O105 0.110(9) 0.106(10) 0.61(4) 0.063(15) -0.019(14) 0.010(8) O106 0.26(2) 0.151(16) 0.34(3) 0.029(19) -0.17(2) -0.004(15) O107 0.092(7) 0.168(11) 0.123(8) 0.000(8) -0.034(7) 0.025(6) O108 0.151(10) 0.167(11) 0.207(12) -0.010(10) -0.039(9) 0.058(9) O109 0.074(5) 0.090(6) 0.118(6) -0.012(4) -0.037(4) -0.027(4) O110 0.079(5) 0.070(5) 0.077(5) -0.019(4) -0.026(4) -0.018(4) O111 0.075(6) 0.100(7) 0.161(8) -0.014(6) -0.041(5) -0.024(5) O112 0.126(8) 0.102(8) 0.306(16) -0.008(9) -0.088(9) -0.047(7) O115 0.150(9) 0.124(9) 0.171(10) -0.038(8) -0.048(8) -0.009(7) O116 0.133(8) 0.095(8) 0.219(12) -0.054(8) 0.012(8) -0.009(6) N1 0.058(5) 0.071(6) 0.083(6) -0.011(5) -0.020(4) -0.021(5) N2 0.090(8) 0.080(8) 0.073(6) -0.007(5) -0.021(5) -0.034(6) N3 0.060(5) 0.058(6) 0.087(6) -0.014(5) -0.020(4) -0.011(4) N4 0.084(7) 0.070(7) 0.093(7) -0.005(6) -0.023(5) -0.037(6) N5 0.135(10) 0.101(10) 0.154(11) -0.006(9) -0.049(9) -0.015(8) N6 0.085(10) 0.064(10) 0.41(4) 0.063(19) -0.075(18) 0.001(8) N7 0.063(6) 0.108(8) 0.088(7) -0.012(6) -0.020(5) -0.005(5) N8 0.078(8) 0.108(11) 0.179(14) 0.010(11) -0.016(10) 0.002(7) N9 0.060(5) 0.088(6) 0.062(5) -0.016(4) -0.018(4) -0.029(5) N10 0.065(6) 0.099(8) 0.060(5) -0.013(5) -0.021(4) -0.033(6) N11 0.055(5) 0.067(6) 0.070(5) -0.004(4) -0.022(4) -0.015(4) N12 0.109(9) 0.083(8) 0.101(7) -0.008(7) -0.029(6) -0.048(7) N15 0.067(6) 0.134(10) 0.125(9) -0.012(7) 0.002(6) -0.026(6) N16 0.107(9) 0.067(8) 0.186(14) -0.047(9) -0.019(9) -0.006(7) C1 0.064(6) 0.075(8) 0.069(7) -0.003(6) -0.023(5) -0.028(6) C2 0.055(6) 0.076(7) 0.074(7) -0.019(6) -0.020(5) -0.008(5) C3 0.058(6) 0.086(8) 0.065(7) -0.024(6) -0.012(5) -0.019(6) C4 0.071(7) 0.075(8) 0.072(7) -0.004(6) -0.039(6) -0.017(6) C5 0.078(7) 0.086(8) 0.075(7) -0.032(7) -0.028(6) -0.005(6) C6 0.057(6) 0.085(8) 0.080(7) -0.023(6) -0.022(6) -0.008(6) C7 0.052(6) 0.118(10) 0.068(7) -0.032(7) -0.014(5) -0.019(6) C8 0.045(6) 0.100(9) 0.055(6) -0.034(6) -0.018(5) -0.002(6) C9 0.056(6) 0.084(8) 0.050(6) -0.019(5) -0.016(5) 0.001(5) C10 0.052(6) 0.067(7) 0.070(7) -0.012(5) -0.023(5) -0.007(5) C11 0.068(7) 0.083(9) 0.075(7) -0.024(6) -0.029(6) -0.010(6) C12 0.072(7) 0.075(8) 0.080(7) -0.028(6) -0.030(6) -0.001(6) C13 0.036(6) 0.102(10) 0.085(7) -0.040(7) -0.022(5) 0.010(6) C14 0.058(6) 0.071(7) 0.046(5) -0.009(5) -0.010(4) -0.011(5) C15 0.048(5) 0.066(7) 0.052(6) -0.014(5) -0.014(4) -0.006(5) C16 0.052(5) 0.071(7) 0.050(5) -0.008(5) -0.018(5) -0.011(5) C17 0.054(6) 0.066(7) 0.057(6) -0.003(5) -0.015(5) -0.013(5) C18 0.059(6) 0.047(6) 0.057(6) -0.005(5) -0.016(5) -0.012(5) C19 0.068(6) 0.073(7) 0.038(5) -0.014(5) -0.008(5) -0.004(6) C20 0.057(6) 0.069(7) 0.057(6) -0.009(5) -0.019(5) -0.017(5) C21 0.052(5) 0.065(7) 0.054(6) -0.011(5) -0.018(4) -0.006(5) C22 0.058(6) 0.063(7) 0.052(6) -0.010(5) -0.021(5) -0.008(5) C23 0.054(6) 0.066(7) 0.060(6) -0.008(5) -0.024(5) -0.006(5) C24 0.055(6) 0.069(7) 0.055(6) -0.010(5) -0.020(5) -0.006(6) C25 0.067(7) 0.057(7) 0.074(7) -0.010(5) -0.026(5) -0.016(6) C26 0.074(7) 0.068(8) 0.070(7) -0.015(6) -0.016(5) -0.017(6) C27 0.051(6) 0.071(8) 0.060(6) -0.006(5) -0.021(5) -0.009(5) C28 0.066(6) 0.062(7) 0.057(6) -0.010(5) -0.017(5) -0.012(5) C39 0.058(6) 0.078(7) 0.066(6) -0.029(6) -0.018(5) -0.002(5) C40 0.083(7) 0.076(7) 0.066(7) -0.015(6) -0.023(5) -0.016(6) C41 0.080(7) 0.085(8) 0.064(7) -0.017(6) -0.016(5) -0.013(6) C42 0.092(8) 0.098(9) 0.063(7) -0.031(6) -0.012(6) -0.002(7) C43 0.112(9) 0.131(12) 0.076(8) -0.041(8) -0.020(7) -0.006(8) C44 0.145(12) 0.171(15) 0.073(9) -0.051(9) -0.020(8) -0.027(11) C45 0.132(11) 0.193(16) 0.085(9) -0.063(10) -0.014(8) -0.024(11) C46 0.30(2) 0.182(18) 0.072(10) -0.063(11) -0.022(12) 0.009(17) C47 0.25(3) 0.21(2) 0.16(2) -0.089(17) 0.000(17) -0.05(2) C48 0.31(3) 0.20(3) 0.23(3) -0.10(2) -0.06(2) 0.01(2) C49 0.063(6) 0.065(7) 0.067(6) -0.004(5) -0.025(5) -0.010(5) C50 0.072(7) 0.099(9) 0.081(8) -0.022(6) -0.023(6) -0.016(6) C51 0.094(9) 0.113(10) 0.088(8) -0.018(7) -0.038(7) -0.029(7) C52 0.092(8) 0.141(11) 0.059(7) -0.022(7) -0.015(6) -0.052(8) C53 0.085(8) 0.128(11) 0.067(7) -0.012(7) -0.016(6) -0.020(7) C54 0.141(12) 0.158(14) 0.073(8) -0.020(9) -0.025(8) -0.060(11) C55 0.120(10) 0.132(12) 0.068(8) -0.009(8) -0.029(7) -0.028(9) C56 0.199(17) 0.186(17) 0.087(10) -0.023(11) -0.059(11) -0.038(14) C57 0.19(2) 0.27(3) 0.122(15) -0.058(17) -0.040(15) 0.067(18) C58 0.097(12) 0.27(2) 0.20(2) -0.096(19) -0.019(13) -0.028(13) C59 0.075(7) 0.082(8) 0.061(7) -0.001(6) -0.015(5) -0.016(6) C60 0.097(8) 0.092(9) 0.079(8) -0.009(7) -0.019(6) -0.002(7) C61 0.142(11) 0.098(10) 0.054(7) 0.000(7) -0.017(7) 0.022(8) C62 0.28(2) 0.115(13) 0.075(9) -0.011(9) -0.061(12) 0.016(13) C63 0.24(2) 0.124(16) 0.20(2) -0.006(14) -0.053(17) -0.018(15) C69 0.062(6) 0.097(8) 0.069(6) -0.021(6) -0.040(5) -0.001(6) C70 0.065(6) 0.086(9) 0.060(6) -0.005(6) -0.016(5) -0.018(6) C71 0.058(7) 0.089(9) 0.068(7) -0.015(6) -0.021(5) -0.018(6) C72 0.049(6) 0.075(7) 0.075(7) -0.017(6) -0.021(5) -0.009(5) C73 0.068(7) 0.096(9) 0.067(7) -0.004(6) -0.012(5) -0.030(7) C74 0.060(7) 0.096(10) 0.101(9) -0.017(7) -0.028(6) -0.012(6) C75 0.101(9) 0.068(8) 0.075(7) -0.006(6) -0.032(7) -0.022(7) C76 0.059(7) 0.088(9) 0.074(7) -0.005(6) -0.021(5) -0.043(6) C77 0.069(7) 0.088(9) 0.079(7) -0.029(6) -0.023(6) -0.015(6) C78 0.060(7) 0.103(9) 0.083(7) -0.016(7) -0.030(6) -0.024(6) C79 0.071(7) 0.081(8) 0.074(7) -0.019(6) -0.010(5) -0.026(7) C80 0.078(8) 0.088(9) 0.131(10) -0.048(8) -0.010(7) -0.029(7) C81 0.089(10) 0.092(11) 0.201(15) -0.060(10) -0.010(9) -0.041(8) C82 0.086(10) 0.063(9) 0.220(16) -0.038(9) -0.001(9) -0.023(7) C83 0.079(8) 0.064(9) 0.143(11) -0.016(8) -0.006(7) -0.017(7) C84 0.061(7) 0.081(9) 0.089(8) -0.016(6) -0.015(5) -0.031(6) C85 0.092(9) 0.086(10) 0.145(12) -0.020(9) -0.035(8) -0.001(9) C86 0.108(10) 0.074(10) 0.175(14) 0.006(9) -0.043(10) 0.005(9) C87 0.102(10) 0.068(9) 0.150(13) 0.015(10) -0.042(10) -0.008(8) C88 0.090(11) 0.065(11) 0.27(2) -0.005(13) -0.012(14) -0.011(9) C89 0.164(17) 0.144(19) 0.19(2) -0.065(17) 0.010(16) 0.005(14) C90 0.40(5) 0.14(2) 0.22(3) -0.06(2) 0.00(3) -0.01(2) C91 0.26(3) 0.16(2) 0.141(18) -0.012(14) -0.057(17) 0.010(17) C92 0.138(13) 0.103(12) 0.146(14) -0.012(12) -0.008(12) -0.008(10) C93 0.050(6) 0.107(9) 0.061(6) -0.012(6) -0.012(5) -0.012(6) C94 0.050(6) 0.119(10) 0.093(8) -0.036(7) -0.019(6) 0.000(6) C95 0.042(6) 0.080(8) 0.102(9) -0.011(7) -0.011(6) 0.013(5) C96 0.081(8) 0.118(11) 0.079(9) -0.019(8) -0.001(7) -0.008(7) C97 0.106(11) 0.188(17) 0.090(11) -0.030(11) -0.017(8) -0.017(11) C98 0.120(12) 0.159(16) 0.099(11) -0.037(11) 0.010(10) 0.011(11) C99 0.103(10) 0.121(12) 0.090(10) -0.027(10) 0.001(9) 0.010(8) C100 0.068(8) 0.104(11) 0.128(12) 0.022(10) -0.027(8) -0.006(7) C101 0.066(6) 0.072(7) 0.058(6) -0.013(5) -0.025(5) -0.018(5) C102 0.067(6) 0.076(7) 0.065(6) -0.020(5) -0.022(5) -0.015(5) C103 0.048(6) 0.069(7) 0.056(6) -0.009(5) -0.015(4) -0.002(5) C104 0.072(7) 0.068(8) 0.078(7) -0.001(6) -0.030(5) -0.031(6) C105 0.078(7) 0.055(7) 0.091(8) -0.006(6) -0.028(6) -0.006(6) C106 0.052(6) 0.066(8) 0.097(8) -0.010(6) -0.028(5) -0.012(5) C116 0.074(7) 0.082(9) 0.080(7) -0.010(6) -0.026(6) -0.032(6) C107 0.065(7) 0.090(9) 0.067(7) -0.003(6) -0.024(5) -0.031(7) C108 0.055(6) 0.057(7) 0.058(6) -0.011(5) -0.010(5) -0.021(5) C109 0.086(7) 0.074(7) 0.045(6) -0.013(5) -0.026(5) -0.013(6) C110 0.065(6) 0.053(7) 0.081(7) 0.006(5) -0.038(5) -0.007(5) C111 0.071(7) 0.056(7) 0.065(6) -0.011(5) -0.026(5) -0.015(6) C112 0.052(6) 0.075(8) 0.110(8) -0.020(6) -0.022(6) -0.007(6) C113 0.075(8) 0.081(9) 0.137(11) -0.034(8) -0.020(7) 0.004(7) C114 0.081(9) 0.077(10) 0.169(13) -0.043(9) -0.009(8) -0.014(7) C115 0.105(10) 0.060(8) 0.131(11) -0.028(7) -0.018(8) -0.015(7) C117 0.096(8) 0.072(9) 0.099(9) -0.009(7) -0.004(7) -0.023(8) C118 0.120(11) 0.094(11) 0.164(13) -0.023(9) -0.015(9) -0.040(9) C125 0.049(6) 0.089(9) 0.119(9) -0.027(7) 0.014(6) -0.013(6) C126 0.065(7) 0.054(7) 0.131(10) -0.023(7) 0.022(6) 0.001(6) C127 0.062(7) 0.070(8) 0.097(9) 0.022(7) -0.023(6) -0.005(6) C128 0.155(14) 0.213(19) 0.074(9) -0.006(11) -0.017(10) -0.061(13) C129 0.118(12) 0.25(2) 0.090(10) -0.011(12) -0.031(9) 0.027(13) C130 0.108(12) 0.177(18) 0.163(16) -0.011(14) -0.027(11) 0.018(11) C131 0.076(8) 0.117(12) 0.144(13) 0.037(10) -0.019(9) -0.026(8) C132 0.080(9) 0.089(11) 0.149(13) 0.000(10) -0.022(9) -0.019(8) O300 0.064(7) 0.070(9) 0.063(8) -0.003(6) -0.020(6) -0.033(6) O301 0.111(11) 0.087(11) 0.104(11) -0.013(8) -0.069(9) -0.018(8) O302 0.097(11) 0.094(12) 0.108(11) -0.026(9) -0.009(9) -0.036(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 C29 C30 1.513(14) . ? C29 C7 1.544(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.408(16) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.545(18) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33A 1.551(16) . ? C32 C33B 1.567(19) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 H32C 0.9900 . ? C32 H32D 0.9900 . ? C33A C34A 1.542(18) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A C35 1.494(18) . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C33B C34B 1.572(19) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B C35 1.542(19) . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? C35 C36 1.537(17) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 H35C 0.9900 . ? C35 H35D 0.9900 . ? C36 C37 1.501(17) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.316(19) . ? C37 H37 0.9500 . ? C38 H38A 0.9500 . ? C38 H38B 0.9500 . ? O13A N14A 1.01(3) . ? O14A N14A 1.56(5) . ? N13A C19A 1.11(4) . ? N13A C118 1.53(2) . ? N13A H13A 0.8800 . ? N14A C24A 1.55(4) . ? C19A C24A 1.32(3) . ? C19A C20A 1.36(3) . ? C20A C21A 1.45(3) . ? C20A H20A 0.9500 . ? C21A C22A 1.37(4) . ? C21A H21A 0.9500 . ? C22A C23A 1.70(5) . ? C22A H22A 0.9500 . ? C23A C24A 1.30(4) . ? C23A H23A 0.9500 . ? O13B N14B 1.00(3) . ? O14B N14B 1.57(5) . ? N13B C19B 1.05(4) . ? N13B C118 1.46(2) . ? N13B H13B 0.8800 . ? N14B C24B 1.55(4) . ? C19B C24B 1.32(3) . ? C19B C20B 1.36(4) . ? C20B C21B 1.48(3) . ? C20B H20B 0.9500 . ? C21B C22B 1.37(3) . ? C21B H21B 0.9500 . ? C22B C23B 1.70(5) . ? C22B H22B 0.9500 . ? C23B C24B 1.28(4) . ? C23B H23B 0.9500 . ? O4 C4 1.386(10) . ? O4 C69 1.433(9) . ? O6 C6 1.374(11) . ? O6 C77 1.441(10) . ? O11 C11 1.360(12) . ? O11 C85 1.362(13) . ? O13 C13 1.381(11) . ? O13 C93 1.410(11) . ? O18 C18 1.370(10) . ? O18 C101 1.443(10) . ? O20 C20 1.413(10) . ? O20 C109 1.427(10) . ? O25 C25 1.383(11) . ? O25 C117 1.401(12) . ? O27 C27 1.376(10) . ? O27 C125 1.400(11) . ? O101 N2 1.222(10) . ? O102 N2 1.258(10) . ? O103 N4 1.261(10) . ? O104 N4 1.211(10) . ? O105 N6 1.23(3) . ? O106 N6 1.18(4) . ? O107 N8 1.210(16) . ? O108 N8 1.298(16) . ? O109 N10 1.264(9) . ? O110 N10 1.245(10) . ? O111 N12 1.171(11) . ? O112 N12 1.241(12) . ? O115 N16 1.283(15) . ? O116 N16 1.227(13) . ? N1 C71 1.337(12) . ? N1 C70 1.433(12) . ? N1 H1N 0.8800 . ? N2 C76 1.437(12) . ? N3 C79 1.349(12) . ? N3 C78 1.446(11) . ? N3 H3N 0.8800 . ? N4 C84 1.418(13) . ? N5 C87 1.365(15) . ? N5 C86 1.461(16) . ? N5 H5N 0.8800 . ? N6 C88 1.37(2) . ? N7 C95 1.342(13) . ? N7 C94 1.467(12) . ? N7 H7N 0.8800 . ? N8 C100 1.481(18) . ? N9 C103 1.369(11) . ? N9 C102 1.482(11) . ? N9 H9N 0.8800 . ? N10 C108 1.415(12) . ? N11 C111 1.344(11) . ? N11 C110 1.466(11) . ? N11 H11N 0.8800 . ? N12 C116 1.464(14) . ? N15 C127 1.329(12) . ? N15 C126 1.481(13) . ? N15 H15N 0.8800 . ? N16 C132 1.436(15) . ? C1 C6 1.399(13) . ? C1 C2 1.410(13) . ? C1 C28 1.514(12) . ? C2 C3 1.373(12) . ? C2 H2 0.9500 . ? C3 C4 1.397(12) . ? C3 C7 1.504(13) . ? C4 C5 1.355(13) . ? C5 C6 1.396(13) . ? C5 H5 0.9500 . ? C7 C8 1.514(14) . ? C7 H7 1.0000 . ? C8 C9 1.404(12) . ? C8 C13 1.420(14) . ? C9 C10 1.384(13) . ? C9 H9 0.9500 . ? C10 C11 1.397(13) . ? C10 C14 1.520(12) . ? C11 C12 1.386(14) . ? C12 C13 1.369(14) . ? C12 H12 0.9500 . ? C14 C15 1.504(12) . ? C14 C39 1.545(11) . ? C14 H14 1.0000 . ? C15 C20 1.389(12) . ? C15 C16 1.405(11) . ? C16 C17 1.371(12) . ? C16 H16 0.9500 . ? C17 C18 1.395(12) . ? C17 C21 1.547(12) . ? C18 C19 1.375(11) . ? C19 C20 1.366(12) . ? C19 H19 0.9500 . ? C21 C22 1.507(12) . ? C21 C49 1.523(11) . ? C21 H21 1.0000 . ? C22 C23 1.405(12) . ? C22 C27 1.413(12) . ? C23 C24 1.351(12) . ? C23 H23 0.9500 . ? C24 C25 1.367(13) . ? C24 C28 1.532(12) . ? C25 C26 1.380(13) . ? C26 C27 1.369(13) . ? C26 H26 0.9500 . ? C28 C59 1.549(12) . ? C28 H28 1.0000 . ? C39 C40 1.506(12) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.509(12) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.493(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.514(14) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.488(16) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.529(16) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.500(14) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.548(16) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.256(16) . ? C47 H47 0.9500 . ? C48 H48A 0.9500 . ? C48 H48B 0.9500 . ? C49 C50 1.496(13) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.566(13) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.513(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.488(13) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.447(16) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.495(15) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.524(14) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.506(15) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.254(15) . ? C57 H57 0.9500 . ? C58 H58A 0.9500 . ? C58 H58B 0.9500 . ? C59 C60 1.507(13) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.495(14) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.489(16) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.50(2) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.64(3) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.33(4) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.548(19) . ? C65 C67 2.01(5) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.544(19) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.336(19) . ? C67 H67 0.9500 . ? C68 H68A 0.9500 . ? C68 H68B 0.9500 . ? C69 C70 1.517(12) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C76 1.410(14) . ? C71 C72 1.421(13) . ? C72 C73 1.366(13) . ? C72 H72 0.9500 . ? C73 C74 1.359(14) . ? C73 H73 0.9500 . ? C74 C75 1.381(14) . ? C74 H74 0.9500 . ? C75 C76 1.408(14) . ? C75 H75 0.9500 . ? C77 C78 1.492(13) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 C84 1.444(13) . ? C79 C80 1.444(15) . ? C80 C81 1.355(16) . ? C80 H80 0.9500 . ? C81 C82 1.391(16) . ? C81 H81 0.9500 . ? C82 C83 1.348(15) . ? C82 H82 0.9500 . ? C83 C84 1.398(14) . ? C83 H83 0.9500 . ? C85 C86 1.522(17) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.3900 . ? C87 C92 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C89 H89 0.9500 . ? C90 C91 1.3900 . ? C90 H90 0.9500 . ? C91 C92 1.3900 . ? C91 H91 0.9500 . ? C92 H92 0.9500 . ? C93 C94 1.504(13) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.399(15) . ? C95 C100 1.448(17) . ? C96 C97 1.354(16) . ? C96 H96 0.9500 . ? C97 C98 1.414(19) . ? C97 H97 0.9500 . ? C98 C99 1.324(17) . ? C98 H98 0.9500 . ? C99 C100 1.340(17) . ? C99 H99 0.9500 . ? C101 C102 1.498(12) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.389(13) . ? C103 C108 1.414(12) . ? C104 C105 1.373(13) . ? C104 H104 0.9500 . ? C105 C106 1.396(13) . ? C105 H105 0.9500 . ? C106 C107 1.324(13) . ? C106 H106 0.9500 . ? C116 C111 1.375(13) . ? C116 C115 1.414(14) . ? C107 C108 1.423(13) . ? C107 H107 0.9500 . ? C109 C110 1.477(12) . ? C109 H10E 0.9900 . ? C109 H10F 0.9900 . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? C111 C112 1.411(13) . ? C112 C113 1.373(14) . ? C112 H112 0.9500 . ? C113 C114 1.390(16) . ? C113 H113 0.9500 . ? C114 C115 1.352(15) . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C117 C118 1.518(16) . ? C117 H11C 0.9900 . ? C117 H11D 0.9900 . ? C118 H11E 0.9900 . ? C118 H11F 0.9900 . ? C118 H11G 0.9900 . ? C118 H11H 0.9900 . ? C125 C126 1.559(14) . ? C125 H12A 0.9900 . ? C125 H12B 0.9900 . ? C126 H12C 0.9900 . ? C126 H12D 0.9900 . ? C127 C128 1.3900 . ? C127 C132 1.3900 . ? C128 C129 1.3900 . ? C128 H128 0.9500 . ? C129 C130 1.3900 . ? C129 H129 0.9500 . ? C130 C131 1.3900 . ? C130 H130 0.9500 . ? C131 C132 1.3900 . ? C131 H131 0.9500 . ? 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 C30 C29 C7 115.2(9) . . ? C30 C29 H29A 108.5 . . ? C7 C29 H29A 108.5 . . ? C30 C29 H29B 108.5 . . ? C7 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? C31 C30 C29 119.0(11) . . ? C31 C30 H30A 107.6 . . ? C29 C30 H30A 107.6 . . ? C31 C30 H30B 107.6 . . ? C29 C30 H30B 107.6 . . ? H30A C30 H30B 107.0 . . ? C30 C31 C32 118.5(13) . . ? C30 C31 H31A 107.7 . . ? C32 C31 H31A 107.7 . . ? C30 C31 H31B 107.7 . . ? C32 C31 H31B 107.7 . . ? H31A C31 H31B 107.1 . . ? C31 C32 C33A 121.1(13) . . ? C31 C32 C33B 127(2) . . ? C33A C32 C33B 49.9(18) . . ? C31 C32 H32A 107.0 . . ? C33A C32 H32A 107.0 . . ? C33B C32 H32A 57.7 . . ? C31 C32 H32B 107.1 . . ? C33A C32 H32B 107.1 . . ? C33B C32 H32B 125.7 . . ? H32A C32 H32B 106.8 . . ? C31 C32 H32C 105.5 . . ? C33A C32 H32C 133.1 . . ? C33B C32 H32C 105.5 . . ? H32A C32 H32C 59.2 . . ? H32B C32 H32C 50.0 . . ? C31 C32 H32D 105.5 . . ? C33A C32 H32D 59.2 . . ? C33B C32 H32D 105.5 . . ? H32A C32 H32D 146.9 . . ? H32B C32 H32D 57.2 . . ? H32C C32 H32D 106.1 . . ? C34A C33A C32 114.9(15) . . ? C34A C33A H33A 108.5 . . ? C32 C33A H33A 108.6 . . ? C34A C33A H33B 108.6 . . ? C32 C33A H33B 108.5 . . ? H33A C33A H33B 107.5 . . ? C35 C34A C33A 111.3(17) . . ? C35 C34A H34A 109.4 . . ? C33A C34A H34A 109.4 . . ? C35 C34A H34B 109.4 . . ? C33A C34A H34B 109.4 . . ? H34A C34A H34B 108.0 . . ? C32 C33B C34B 114(2) . . ? C32 C33B H33C 108.7 . . ? C34B C33B H33C 108.7 . . ? C32 C33B H33D 108.7 . . ? C34B C33B H33D 108.6 . . ? H33C C33B H33D 107.6 . . ? C35 C34B C33B 142(3) . . ? C35 C34B H34C 101.6 . . ? C33B C34B H34C 101.6 . . ? C35 C34B H34D 101.6 . . ? C33B C34B H34D 101.6 . . ? H34C C34B H34D 104.6 . . ? C34A C35 C36 116(2) . . ? C36 C35 C34B 126(2) . . ? C34A C35 H35A 108.2 . . ? C36 C35 H35A 108.2 . . ? C34B C35 H35A 121.3 . . ? C34A C35 H35B 108.2 . . ? C36 C35 H35B 108.3 . . ? C34B C35 H35B 76.5 . . ? H35A C35 H35B 107.4 . . ? C34A C35 H35C 133.5 . . ? C36 C35 H35C 105.7 . . ? C34B C35 H35C 105.7 . . ? H35A C35 H35C 74.7 . . ? C34A C35 H35D 81.7 . . ? C36 C35 H35D 105.7 . . ? C34B C35 H35D 105.7 . . ? H35B C35 H35D 134.8 . . ? H35C C35 H35D 106.2 . . ? C37 C36 C35 108.4(18) . . ? C37 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? C37 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? C38 C37 C36 129(3) . . ? C38 C37 H37 115.7 . . ? C36 C37 H37 115.7 . . ? C37 C38 H38A 120.0 . . ? C37 C38 H38B 120.0 . . ? H38A C38 H38B 120.0 . . ? C19A N13A C118 153(5) . . ? C19A N13A H13A 103.3 . . ? C118 N13A H13A 103.3 . . ? O13A N14A C24A 135(5) . . ? O13A N14A O14A 115(4) . . ? C24A N14A O14A 109(3) . . ? N13A C19A C24A 156(4) . . ? N13A C19A C20A 103(3) . . ? C24A C19A C20A 101(3) . . ? C19A C20A C21A 125(3) . . ? C19A C20A H20A 117.6 . . ? C21A C20A H20A 117.6 . . ? C22A C21A C20A 132(4) . . ? C22A C21A H21A 114.0 . . ? C20A C21A H21A 114.1 . . ? C21A C22A C23A 99(3) . . ? C21A C22A H22A 130.3 . . ? C23A C22A H22A 130.3 . . ? C24A C23A C22A 110(3) . . ? C24A C23A H23A 125.0 . . ? C22A C23A H23A 125.0 . . ? C23A C24A C19A 145(4) . . ? C23A C24A N14A 94(3) . . ? C19A C24A N14A 116(4) . . ? C19B N13B C118 122(2) . . ? C19B N13B H13B 119.2 . . ? C118 N13B H13B 119.2 . . ? O13B N14B C24B 132(6) . . ? O13B N14B O14B 113(5) . . ? C24B N14B O14B 108(3) . . ? N13B C19B C24B 141(3) . . ? N13B C19B C20B 116(3) . . ? C24B C19B C20B 102(3) . . ? C19B C20B C21B 126(3) . . ? C19B C20B H20B 117.0 . . ? C21B C20B H20B 117.0 . . ? C22B C21B C20B 127(4) . . ? C22B C21B H21B 116.3 . . ? C20B C21B H21B 116.3 . . ? C21B C22B C23B 104(3) . . ? C21B C22B H22B 127.8 . . ? C23B C22B H22B 127.8 . . ? C24B C23B C22B 111(3) . . ? C24B C23B H23B 124.3 . . ? C22B C23B H23B 124.3 . . ? C23B C24B C19B 146(4) . . ? C23B C24B N14B 101(3) . . ? C19B C24B N14B 112(4) . . ? C4 O4 C69 118.7(7) . . ? C6 O6 C77 121.0(7) . . ? C11 O11 C85 118.8(10) . . ? C13 O13 C93 115.8(8) . . ? C18 O18 C101 117.5(6) . . ? C20 O20 C109 118.5(7) . . ? C25 O25 C117 118.3(8) . . ? C27 O27 C125 116.3(8) . . ? C71 N1 C70 122.8(9) . . ? C71 N1 H1N 118.6 . . ? C70 N1 H1N 118.6 . . ? O101 N2 O102 121.8(9) . . ? O101 N2 C76 120.3(10) . . ? O102 N2 C76 117.9(10) . . ? C79 N3 C78 122.0(9) . . ? C79 N3 H3N 119.0 . . ? C78 N3 H3N 119.0 . . ? O104 N4 O103 121.2(9) . . ? O104 N4 C84 122.3(10) . . ? O103 N4 C84 116.6(10) . . ? C87 N5 C86 131.0(12) . . ? C87 N5 H5N 114.5 . . ? C86 N5 H5N 114.5 . . ? O106 N6 O105 116(3) . . ? O106 N6 C88 125(3) . . ? O105 N6 C88 119(3) . . ? C95 N7 C94 123.7(8) . . ? C95 N7 H7N 118.2 . . ? C94 N7 H7N 118.2 . . ? O107 N8 O108 121.5(15) . . ? O107 N8 C100 126.6(15) . . ? O108 N8 C100 111.9(16) . . ? C103 N9 C102 120.6(8) . . ? C103 N9 H9N 119.7 . . ? C102 N9 H9N 119.7 . . ? O110 N10 O109 119.0(9) . . ? O110 N10 C108 121.9(8) . . ? O109 N10 C108 119.1(9) . . ? C111 N11 C110 125.4(8) . . ? C111 N11 H11N 117.3 . . ? C110 N11 H11N 117.3 . . ? O111 N12 O112 122.4(12) . . ? O111 N12 C116 121.0(11) . . ? O112 N12 C116 116.7(12) . . ? C127 N15 C126 124.1(10) . . ? C127 N15 H15N 118.0 . . ? C126 N15 H15N 118.0 . . ? O116 N16 O115 119.8(15) . . ? O116 N16 C132 123.4(14) . . ? O115 N16 C132 116.6(10) . . ? C6 C1 C2 116.7(9) . . ? C6 C1 C28 118.8(9) . . ? C2 C1 C28 124.5(8) . . ? C3 C2 C1 123.4(9) . . ? C3 C2 H2 118.3 . . ? C1 C2 H2 118.3 . . ? C2 C3 C4 116.9(9) . . ? C2 C3 C7 123.2(8) . . ? C4 C3 C7 119.8(9) . . ? C5 C4 O4 124.5(8) . . ? C5 C4 C3 122.4(9) . . ? O4 C4 C3 113.2(9) . . ? C4 C5 C6 119.7(9) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? O6 C6 C5 124.5(9) . . ? O6 C6 C1 114.7(9) . . ? C5 C6 C1 120.7(10) . . ? C3 C7 C8 110.3(8) . . ? C3 C7 C29 115.2(9) . . ? C8 C7 C29 107.3(8) . . ? C3 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C29 C7 H7 107.9 . . ? C9 C8 C13 114.6(11) . . ? C9 C8 C7 121.6(9) . . ? C13 C8 C7 123.3(9) . . ? C10 C9 C8 124.6(9) . . ? C10 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? C9 C10 C11 117.6(9) . . ? C9 C10 C14 121.8(9) . . ? C11 C10 C14 120.6(10) . . ? O11 C11 C12 122.9(10) . . ? O11 C11 C10 116.7(9) . . ? C12 C11 C10 120.4(12) . . ? C13 C12 C11 120.4(10) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 O13 123.0(10) . . ? C12 C13 C8 122.4(9) . . ? O13 C13 C8 114.6(11) . . ? C15 C14 C10 111.7(7) . . ? C15 C14 C39 114.2(7) . . ? C10 C14 C39 109.4(7) . . ? C15 C14 H14 107.1 . . ? C10 C14 H14 107.1 . . ? C39 C14 H14 107.1 . . ? C20 C15 C16 114.8(8) . . ? C20 C15 C14 122.1(8) . . ? C16 C15 C14 123.1(8) . . ? C17 C16 C15 123.5(8) . . ? C17 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? C16 C17 C18 118.5(8) . . ? C16 C17 C21 122.9(8) . . ? C18 C17 C21 118.6(8) . . ? O18 C18 C19 123.5(8) . . ? O18 C18 C17 116.4(8) . . ? C19 C18 C17 120.1(9) . . ? C20 C19 C18 119.5(8) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C15 123.6(8) . . ? C19 C20 O20 123.9(8) . . ? C15 C20 O20 112.4(8) . . ? C22 C21 C49 110.1(7) . . ? C22 C21 C17 112.4(7) . . ? C49 C21 C17 113.6(7) . . ? C22 C21 H21 106.8 . . ? C49 C21 H21 106.8 . . ? C17 C21 H21 106.8 . . ? C23 C22 C27 116.3(9) . . ? C23 C22 C21 122.5(9) . . ? C27 C22 C21 121.1(8) . . ? C24 C23 C22 123.4(9) . . ? C24 C23 H23 118.3 . . ? C22 C23 H23 118.3 . . ? C23 C24 C25 118.6(9) . . ? C23 C24 C28 121.8(9) . . ? C25 C24 C28 119.6(10) . . ? C24 C25 C26 121.1(10) . . ? C24 C25 O25 118.3(9) . . ? C26 C25 O25 120.6(9) . . ? C27 C26 C25 120.3(10) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 O27 125.2(9) . . ? C26 C27 C22 120.3(9) . . ? O27 C27 C22 114.5(9) . . ? C1 C28 C24 113.2(8) . . ? C1 C28 C59 112.3(8) . . ? C24 C28 C59 110.1(7) . . ? C1 C28 H28 106.9 . . ? C24 C28 H28 106.9 . . ? C59 C28 H28 106.9 . . ? C40 C39 C14 113.6(7) . . ? C40 C39 H39A 108.8 . . ? C14 C39 H39A 108.8 . . ? C40 C39 H39B 108.8 . . ? C14 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C39 C40 C41 114.1(8) . . ? C39 C40 H40A 108.7 . . ? C41 C40 H40A 108.7 . . ? C39 C40 H40B 108.7 . . ? C41 C40 H40B 108.7 . . ? H40A C40 H40B 107.6 . . ? C42 C41 C40 115.7(8) . . ? C42 C41 H41A 108.3 . . ? C40 C41 H41A 108.3 . . ? C42 C41 H41B 108.3 . . ? C40 C41 H41B 108.3 . . ? H41A C41 H41B 107.4 . . ? C41 C42 C43 114.9(9) . . ? C41 C42 H42A 108.5 . . ? C43 C42 H42A 108.5 . . ? C41 C42 H42B 108.5 . . ? C43 C42 H42B 108.5 . . ? H42A C42 H42B 107.5 . . ? C44 C43 C42 114.1(10) . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C43 C44 C45 115.2(12) . . ? C43 C44 H44A 108.5 . . ? C45 C44 H44A 108.5 . . ? C43 C44 H44B 108.5 . . ? C45 C44 H44B 108.5 . . ? H44A C44 H44B 107.5 . . ? C46 C45 C44 113.2(12) . . ? C46 C45 H45A 108.9 . . ? C44 C45 H45A 108.9 . . ? C46 C45 H45B 108.9 . . ? C44 C45 H45B 108.9 . . ? H45A C45 H45B 107.8 . . ? C45 C46 C47 109.5(14) . . ? C45 C46 H46A 109.8 . . ? C47 C46 H46A 109.8 . . ? C45 C46 H46B 109.8 . . ? C47 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? C48 C47 C46 118(2) . . ? C48 C47 H47 121.1 . . ? C46 C47 H47 121.1 . . ? C47 C48 H48A 120.0 . . ? C47 C48 H48B 120.0 . . ? H48A C48 H48B 120.0 . . ? C50 C49 C21 117.1(8) . . ? C50 C49 H49A 108.0 . . ? C21 C49 H49A 108.0 . . ? C50 C49 H49B 108.0 . . ? C21 C49 H49B 108.0 . . ? H49A C49 H49B 107.3 . . ? C49 C50 C51 114.3(9) . . ? C49 C50 H50A 108.7 . . ? C51 C50 H50A 108.7 . . ? C49 C50 H50B 108.7 . . ? C51 C50 H50B 108.7 . . ? H50A C50 H50B 107.6 . . ? C52 C51 C50 114.3(8) . . ? C52 C51 H51A 108.7 . . ? C50 C51 H51A 108.7 . . ? C52 C51 H51B 108.7 . . ? C50 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C53 C52 C51 113.7(9) . . ? C53 C52 H52A 108.8 . . ? C51 C52 H52A 108.8 . . ? C53 C52 H52B 108.8 . . ? C51 C52 H52B 108.8 . . ? H52A C52 H52B 107.7 . . ? C54 C53 C52 118.2(10) . . ? C54 C53 H53A 107.7 . . ? C52 C53 H53A 107.7 . . ? C54 C53 H53B 107.7 . . ? C52 C53 H53B 107.7 . . ? H53A C53 H53B 107.1 . . ? C53 C54 C55 116.3(11) . . ? C53 C54 H54A 108.2 . . ? C55 C54 H54A 108.2 . . ? C53 C54 H54B 108.2 . . ? C55 C54 H54B 108.2 . . ? H54A C54 H54B 107.4 . . ? C54 C55 C56 114.9(11) . . ? C54 C55 H55A 108.5 . . ? C56 C55 H55A 108.5 . . ? C54 C55 H55B 108.5 . . ? C56 C55 H55B 108.5 . . ? H55A C55 H55B 107.5 . . ? C57 C56 C55 112.6(13) . . ? C57 C56 H56A 109.1 . . ? C55 C56 H56A 109.1 . . ? C57 C56 H56B 109.1 . . ? C55 C56 H56B 109.1 . . ? H56A C56 H56B 107.8 . . ? C58 C57 C56 125(2) . . ? C58 C57 H57 117.4 . . ? C56 C57 H57 117.4 . . ? C57 C58 H58A 120.0 . . ? C57 C58 H58B 120.0 . . ? H58A C58 H58B 120.0 . . ? C60 C59 C28 113.6(8) . . ? C60 C59 H59A 108.9 . . ? C28 C59 H59A 108.9 . . ? C60 C59 H59B 108.9 . . ? C28 C59 H59B 108.8 . . ? H59A C59 H59B 107.7 . . ? C61 C60 C59 112.9(9) . . ? C61 C60 H60A 109.0 . . ? C59 C60 H60A 109.0 . . ? C61 C60 H60B 109.0 . . ? C59 C60 H60B 109.0 . . ? H60A C60 H60B 107.8 . . ? C62 C61 C60 111.4(10) . . ? C62 C61 H61A 109.4 . . ? C60 C61 H61A 109.4 . . ? C62 C61 H61B 109.4 . . ? C60 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? C61 C62 C63 116.1(13) . . ? C61 C62 H62A 108.3 . . ? C63 C62 H62A 108.3 . . ? C61 C62 H62B 108.3 . . ? C63 C62 H62B 108.3 . . ? H62A C62 H62B 107.4 . . ? C62 C63 C64 109.4(18) . . ? C62 C63 H63A 109.8 . . ? C64 C63 H63A 109.8 . . ? C62 C63 H63B 109.8 . . ? C64 C63 H63B 109.8 . . ? H63A C63 H63B 108.2 . . ? C65 C64 C63 127(3) . . ? C65 C64 H64A 105.6 . . ? C63 C64 H64A 105.6 . . ? C65 C64 H64B 105.6 . . ? C63 C64 H64B 105.6 . . ? H64A C64 H64B 106.1 . . ? C64 C65 C66 106(4) . . ? C64 C65 C67 123(3) . . ? C66 C65 C67 49.5(14) . . ? C64 C65 H65A 110.5 . . ? C66 C65 H65A 110.5 . . ? C67 C65 H65A 61.1 . . ? C64 C65 H65B 110.5 . . ? C66 C65 H65B 110.5 . . ? C67 C65 H65B 125.6 . . ? H65A C65 H65B 108.7 . . ? C67 C66 C65 81(3) . . ? C67 C66 H66A 115.1 . . ? C65 C66 H66A 115.1 . . ? C67 C66 H66B 115.1 . . ? C65 C66 H66B 115.1 . . ? H66A C66 H66B 112.2 . . ? C68 C67 C66 111(4) . . ? C68 C67 C65 139(4) . . ? C66 C67 C65 49.6(14) . . ? C68 C67 H67 124.5 . . ? C66 C67 H67 124.5 . . ? C65 C67 H67 84.7 . . ? C67 C68 H68A 120.0 . . ? C67 C68 H68B 120.0 . . ? H68A C68 H68B 120.0 . . ? O4 C69 C70 106.1(7) . . ? O4 C69 H69A 110.5 . . ? C70 C69 H69A 110.5 . . ? O4 C69 H69B 110.5 . . ? C70 C69 H69B 110.5 . . ? H69A C69 H69B 108.7 . . ? N1 C70 C69 112.4(8) . . ? N1 C70 H70A 109.1 . . ? C69 C70 H70A 109.1 . . ? N1 C70 H70B 109.1 . . ? C69 C70 H70B 109.1 . . ? H70A C70 H70B 107.8 . . ? N1 C71 C76 124.0(9) . . ? N1 C71 C72 120.5(10) . . ? C76 C71 C72 115.5(10) . . ? C73 C72 C71 120.2(10) . . ? C73 C72 H72 119.9 . . ? C71 C72 H72 119.9 . . ? C74 C73 C72 123.7(10) . . ? C74 C73 H73 118.2 . . ? C72 C73 H73 118.2 . . ? C73 C74 C75 119.1(11) . . ? C73 C74 H74 120.5 . . ? C75 C74 H74 120.5 . . ? C74 C75 C76 118.6(10) . . ? C74 C75 H75 120.7 . . ? C76 C75 H75 120.7 . . ? C75 C76 C71 122.9(9) . . ? C75 C76 N2 115.9(10) . . ? C71 C76 N2 121.2(10) . . ? O6 C77 C78 106.9(8) . . ? O6 C77 H77A 110.3 . . ? C78 C77 H77A 110.3 . . ? O6 C77 H77B 110.3 . . ? C78 C77 H77B 110.3 . . ? H77A C77 H77B 108.6 . . ? N3 C78 C77 112.8(9) . . ? N3 C78 H78A 109.0 . . ? C77 C78 H78A 109.0 . . ? N3 C78 H78B 109.0 . . ? C77 C78 H78B 109.0 . . ? H78A C78 H78B 107.8 . . ? N3 C79 C84 125.2(10) . . ? N3 C79 C80 120.3(10) . . ? C84 C79 C80 114.4(10) . . ? C81 C80 C79 122.1(11) . . ? C81 C80 H80 119.0 . . ? C79 C80 H80 119.0 . . ? C80 C81 C82 121.1(12) . . ? C80 C81 H81 119.5 . . ? C82 C81 H81 119.5 . . ? C83 C82 C81 119.7(13) . . ? C83 C82 H82 120.2 . . ? C81 C82 H82 120.2 . . ? C82 C83 C84 121.3(11) . . ? C82 C83 H83 119.3 . . ? C84 C83 H83 119.3 . . ? C83 C84 N4 119.0(10) . . ? C83 C84 C79 120.9(10) . . ? N4 C84 C79 120.1(10) . . ? O11 C85 C86 109.4(11) . . ? O11 C85 H85A 109.8 . . ? C86 C85 H85A 109.8 . . ? O11 C85 H85B 109.8 . . ? C86 C85 H85B 109.8 . . ? H85A C85 H85B 108.2 . . ? N5 C86 C85 107.8(12) . . ? N5 C86 H86A 110.1 . . ? C85 C86 H86A 110.2 . . ? N5 C86 H86B 110.2 . . ? C85 C86 H86B 110.1 . . ? H86A C86 H86B 108.5 . . ? N5 C87 C88 124.5(11) . . ? N5 C87 C92 115.5(11) . . ? C88 C87 C92 120.0 . . ? N6 C88 C87 122.3(17) . . ? N6 C88 C89 117.7(17) . . ? C87 C88 C89 120.0 . . ? C90 C89 C88 120.0 . . ? C90 C89 H89 120.0 . . ? C88 C89 H89 120.0 . . ? C89 C90 C91 120.0 . . ? C89 C90 H90 120.0 . . ? C91 C90 H90 120.0 . . ? C92 C91 C90 120.0 . . ? C92 C91 H91 120.0 . . ? C90 C91 H91 120.0 . . ? C91 C92 C87 120.0 . . ? C91 C92 H92 120.0 . . ? C87 C92 H92 120.0 . . ? O13 C93 C94 107.7(9) . . ? O13 C93 H93A 110.2 . . ? C94 C93 H93A 110.2 . . ? O13 C93 H93B 110.2 . . ? C94 C93 H93B 110.2 . . ? H93A C93 H93B 108.5 . . ? N7 C94 C93 111.6(10) . . ? N7 C94 H94A 109.3 . . ? C93 C94 H94A 109.3 . . ? N7 C94 H94B 109.3 . . ? C93 C94 H94B 109.3 . . ? H94A C94 H94B 108.0 . . ? N7 C95 C96 121.8(10) . . ? N7 C95 C100 127.1(11) . . ? C96 C95 C100 111.1(12) . . ? C97 C96 C95 122.2(12) . . ? C97 C96 H96 118.9 . . ? C95 C96 H96 118.9 . . ? C96 C97 C98 122.7(13) . . ? C96 C97 H97 118.6 . . ? C98 C97 H97 118.6 . . ? C99 C98 C97 117.4(14) . . ? C99 C98 H98 121.3 . . ? C97 C98 H98 121.3 . . ? C98 C99 C100 120.2(14) . . ? C98 C99 H99 119.9 . . ? C100 C99 H99 119.9 . . ? C99 C100 C95 126.3(12) . . ? C99 C100 N8 120.0(14) . . ? C95 C100 N8 113.7(14) . . ? O18 C101 C102 105.7(7) . . ? O18 C101 H10A 110.6 . . ? C102 C101 H10A 110.6 . . ? O18 C101 H10B 110.6 . . ? C102 C101 H10B 110.6 . . ? H10A C101 H10B 108.7 . . ? N9 C102 C101 111.5(8) . . ? N9 C102 H10C 109.3 . . ? C101 C102 H10C 109.3 . . ? N9 C102 H10D 109.3 . . ? C101 C102 H10D 109.3 . . ? H10C C102 H10D 108.0 . . ? N9 C103 C104 122.8(9) . . ? N9 C103 C108 121.0(9) . . ? C104 C103 C108 116.2(9) . . ? C105 C104 C103 121.9(9) . . ? C105 C104 H104 119.0 . . ? C103 C104 H104 119.1 . . ? C104 C105 C106 121.2(10) . . ? C104 C105 H105 119.4 . . ? C106 C105 H105 119.4 . . ? C107 C106 C105 118.8(10) . . ? C107 C106 H106 120.6 . . ? C105 C106 H106 120.6 . . ? C111 C116 C115 121.3(10) . . ? C111 C116 N12 120.3(11) . . ? C115 C116 N12 118.4(11) . . ? C106 C107 C108 121.5(9) . . ? C106 C107 H107 119.2 . . ? C108 C107 H107 119.2 . . ? C103 C108 N10 122.5(9) . . ? C103 C108 C107 120.3(9) . . ? N10 C108 C107 117.2(9) . . ? O20 C109 C110 106.1(7) . . ? O20 C109 H10E 110.5 . . ? C110 C109 H10E 110.5 . . ? O20 C109 H10F 110.5 . . ? C110 C109 H10F 110.5 . . ? H10E C109 H10F 108.7 . . ? N11 C110 C109 110.9(7) . . ? N11 C110 H11A 109.5 . . ? C109 C110 H11A 109.5 . . ? N11 C110 H11B 109.5 . . ? C109 C110 H11B 109.5 . . ? H11A C110 H11B 108.1 . . ? N11 C111 C116 123.7(9) . . ? N11 C111 C112 119.9(9) . . ? C116 C111 C112 116.3(10) . . ? C113 C112 C111 121.0(11) . . ? C113 C112 H112 119.5 . . ? C111 C112 H112 119.5 . . ? C112 C113 C114 122.3(11) . . ? C112 C113 H113 118.8 . . ? C114 C113 H113 118.8 . . ? C115 C114 C113 117.0(12) . . ? C115 C114 H114 121.5 . . ? C113 C114 H114 121.5 . . ? C114 C115 C116 121.9(12) . . ? C114 C115 H115 119.1 . . ? C116 C115 H115 119.1 . . ? O25 C117 C118 108.0(10) . . ? O25 C117 H11C 110.1 . . ? C118 C117 H11C 110.1 . . ? O25 C117 H11D 110.1 . . ? C118 C117 H11D 110.1 . . ? H11C C117 H11D 108.4 . . ? N13B C118 C117 110.1(14) . . ? C117 C118 N13A 102(3) . . ? N13B C118 H11E 125.2 . . ? C117 C118 H11E 111.3 . . ? N13A C118 H11E 111.3 . . ? N13B C118 H11F 86.8 . . ? C117 C118 H11F 111.3 . . ? N13A C118 H11F 111.4 . . ? H11E C118 H11F 109.2 . . ? N13B C118 H11G 109.7 . . ? C117 C118 H11G 109.6 . . ? N13A C118 H11G 133.3 . . ? H11E C118 H11G 88.2 . . ? N13B C118 H11H 109.6 . . ? C117 C118 H11H 109.6 . . ? N13A C118 H11H 91.7 . . ? H11F C118 H11H 126.5 . . ? H11G C118 H11H 108.2 . . ? O27 C125 C126 106.2(9) . . ? O27 C125 H12A 110.5 . . ? C126 C125 H12A 110.5 . . ? O27 C125 H12B 110.5 . . ? C126 C125 H12B 110.5 . . ? H12A C125 H12B 108.7 . . ? N15 C126 C125 109.4(9) . . ? N15 C126 H12C 109.8 . . ? C125 C126 H12C 109.8 . . ? N15 C126 H12D 109.8 . . ? C125 C126 H12D 109.8 . . ? H12C C126 H12D 108.3 . . ? N15 C127 C128 121.0(6) . . ? N15 C127 C132 118.8(6) . . ? C128 C127 C132 120.0 . . ? C129 C128 C127 120.0 . . ? C129 C128 H128 120.0 . . ? C127 C128 H128 120.0 . . ? C128 C129 C130 120.0 . . ? C128 C129 H129 120.0 . . ? C130 C129 H129 120.0 . . ? C129 C130 C131 120.0 . . ? C129 C130 H130 120.0 . . ? C131 C130 H130 120.0 . . ? C132 C131 C130 120.0 . . ? C132 C131 H131 120.0 . . ? C130 C131 H131 120.0 . . ? C131 C132 C127 120.0 . . ? C131 C132 N16 112.5(6) . . ? C127 C132 N16 127.4(7) . . ? 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 C7 C29 C30 C31 158.5(15) . . . . ? C29 C30 C31 C32 -176.4(16) . . . . ? C30 C31 C32 C33A 172(2) . . . . ? C30 C31 C32 C33B 111(3) . . . . ? C31 C32 C33A C34A 168(2) . . . . ? C33B C32 C33A C34A -77(3) . . . . ? C32 C33A C34A C35 163(3) . . . . ? C31 C32 C33B C34B 150(2) . . . . ? C33A C32 C33B C34B 48(3) . . . . ? C32 C33B C34B C35 -100(7) . . . . ? C33A C34A C35 C36 167(2) . . . . ? C33A C34A C35 C34B -75(3) . . . . ? C33B C34B C35 C34A 99(6) . . . . ? C33B C34B C35 C36 -179(4) . . . . ? C34A C35 C36 C37 -166(2) . . . . ? C34B C35 C36 C37 158(3) . . . . ? C35 C36 C37 C38 117(4) . . . . ? C118 N13A C19A C24A 179(7) . . . . ? C118 N13A C19A C20A -12(15) . . . . ? N13A C19A C20A C21A -179(5) . . . . ? C24A C19A C20A C21A -3(4) . . . . ? C19A C20A C21A C22A 12(8) . . . . ? C20A C21A C22A C23A -22(8) . . . . ? C21A C22A C23A C24A 25(6) . . . . ? C22A C23A C24A C19A -35(7) . . . . ? C22A C23A C24A N14A 172(4) . . . . ? N13A C19A C24A C23A -170(11) . . . . ? C20A C19A C24A C23A 21(7) . . . . ? N13A C19A C24A N14A -20(13) . . . . ? C20A C19A C24A N14A 171(3) . . . . ? O13A N14A C24A C23A -13(6) . . . . ? O14A N14A C24A C23A 179(3) . . . . ? O13A N14A C24A C19A -176(5) . . . . ? O14A N14A C24A C19A 16(4) . . . . ? C118 N13B C19B C24B 172(4) . . . . ? C118 N13B C19B C20B -23(5) . . . . ? N13B C19B C20B C21B -166(5) . . . . ? C24B C19B C20B C21B 4(7) . . . . ? C19B C20B C21B C22B -17(10) . . . . ? C20B C21B C22B C23B 12(7) . . . . ? C21B C22B C23B C24B 0(4) . . . . ? C22B C23B C24B C19B -17(7) . . . . ? C22B C23B C24B N14B -180(3) . . . . ? N13B C19B C24B C23B -179(5) . . . . ? C20B C19B C24B C23B 15(7) . . . . ? N13B C19B C24B N14B -17(6) . . . . ? C20B C19B C24B N14B 177(4) . . . . ? O13B N14B C24B C23B -14(7) . . . . ? O14B N14B C24B C23B -164(3) . . . . ? O13B N14B C24B C19B 176(6) . . . . ? O14B N14B C24B C19B 27(4) . . . . ? C6 C1 C2 C3 -2.5(15) . . . . ? C28 C1 C2 C3 177.8(9) . . . . ? C1 C2 C3 C4 -2.0(15) . . . . ? C1 C2 C3 C7 -178.3(10) . . . . ? C69 O4 C4 C5 -10.4(15) . . . . ? C69 O4 C4 C3 169.8(9) . . . . ? C2 C3 C4 C5 5.1(15) . . . . ? C7 C3 C4 C5 -178.4(10) . . . . ? C2 C3 C4 O4 -175.1(8) . . . . ? C7 C3 C4 O4 1.3(13) . . . . ? O4 C4 C5 C6 176.7(9) . . . . ? C3 C4 C5 C6 -3.6(17) . . . . ? C77 O6 C6 C5 9.0(15) . . . . ? C77 O6 C6 C1 -168.7(8) . . . . ? C4 C5 C6 O6 -178.9(10) . . . . ? C4 C5 C6 C1 -1.3(16) . . . . ? C2 C1 C6 O6 -178.0(9) . . . . ? C28 C1 C6 O6 1.7(13) . . . . ? C2 C1 C6 C5 4.2(15) . . . . ? C28 C1 C6 C5 -176.1(9) . . . . ? C2 C3 C7 C8 -106.7(11) . . . . ? C4 C3 C7 C8 77.1(11) . . . . ? C2 C3 C7 C29 14.9(15) . . . . ? C4 C3 C7 C29 -161.3(9) . . . . ? C30 C29 C7 C3 180.0(9) . . . . ? C30 C29 C7 C8 -56.7(11) . . . . ? C3 C7 C8 C9 51.5(10) . . . . ? C29 C7 C8 C9 -74.7(10) . . . . ? C3 C7 C8 C13 -136.7(8) . . . . ? C29 C7 C8 C13 97.1(10) . . . . ? C13 C8 C9 C10 -1.8(12) . . . . ? C7 C8 C9 C10 170.6(8) . . . . ? C8 C9 C10 C11 3.1(13) . . . . ? C8 C9 C10 C14 -174.4(8) . . . . ? C85 O11 C11 C12 -16.1(14) . . . . ? C85 O11 C11 C10 162.7(10) . . . . ? C9 C10 C11 O11 179.0(8) . . . . ? C14 C10 C11 O11 -3.5(13) . . . . ? C9 C10 C11 C12 -2.2(14) . . . . ? C14 C10 C11 C12 175.3(8) . . . . ? O11 C11 C12 C13 179.1(9) . . . . ? C10 C11 C12 C13 0.3(15) . . . . ? C11 C12 C13 O13 -179.2(8) . . . . ? C11 C12 C13 C8 1.0(15) . . . . ? C93 O13 C13 C12 29.4(13) . . . . ? C93 O13 C13 C8 -150.8(8) . . . . ? C9 C8 C13 C12 -0.2(13) . . . . ? C7 C8 C13 C12 -172.6(9) . . . . ? C9 C8 C13 O13 179.9(7) . . . . ? C7 C8 C13 O13 7.6(12) . . . . ? C9 C10 C14 C15 -50.7(11) . . . . ? C11 C10 C14 C15 131.9(9) . . . . ? C9 C10 C14 C39 76.8(11) . . . . ? C11 C10 C14 C39 -100.6(10) . . . . ? C10 C14 C15 C20 -69.7(11) . . . . ? C39 C14 C15 C20 165.5(8) . . . . ? C10 C14 C15 C16 110.9(9) . . . . ? C39 C14 C15 C16 -13.9(13) . . . . ? C20 C15 C16 C17 -2.4(13) . . . . ? C14 C15 C16 C17 177.1(8) . . . . ? C15 C16 C17 C18 1.1(14) . . . . ? C15 C16 C17 C21 179.0(8) . . . . ? C101 O18 C18 C19 3.9(12) . . . . ? C101 O18 C18 C17 -176.9(7) . . . . ? C16 C17 C18 O18 -178.9(8) . . . . ? C21 C17 C18 O18 3.1(12) . . . . ? C16 C17 C18 C19 0.3(13) . . . . ? C21 C17 C18 C19 -177.7(8) . . . . ? O18 C18 C19 C20 178.9(8) . . . . ? C17 C18 C19 C20 -0.3(13) . . . . ? C18 C19 C20 C15 -1.2(14) . . . . ? C18 C19 C20 O20 -177.0(8) . . . . ? C16 C15 C20 C19 2.4(13) . . . . ? C14 C15 C20 C19 -177.1(9) . . . . ? C16 C15 C20 O20 178.7(7) . . . . ? C14 C15 C20 O20 -0.8(12) . . . . ? C109 O20 C20 C19 -10.8(12) . . . . ? C109 O20 C20 C15 173.0(7) . . . . ? C16 C17 C21 C22 -104.0(10) . . . . ? C18 C17 C21 C22 73.9(10) . . . . ? C16 C17 C21 C49 21.8(12) . . . . ? C18 C17 C21 C49 -160.2(8) . . . . ? C49 C21 C22 C23 -79.8(9) . . . . ? C17 C21 C22 C23 48.0(11) . . . . ? C49 C21 C22 C27 95.4(9) . . . . ? C17 C21 C22 C27 -136.8(8) . . . . ? C27 C22 C23 C24 -2.1(12) . . . . ? C21 C22 C23 C24 173.3(8) . . . . ? C22 C23 C24 C25 3.0(13) . . . . ? C22 C23 C24 C28 -174.4(7) . . . . ? C23 C24 C25 C26 -1.9(13) . . . . ? C28 C24 C25 C26 175.6(8) . . . . ? C23 C24 C25 O25 177.0(7) . . . . ? C28 C24 C25 O25 -5.4(12) . . . . ? C117 O25 C25 C24 149.4(9) . . . . ? C117 O25 C25 C26 -31.7(13) . . . . ? C24 C25 C26 C27 0.0(14) . . . . ? O25 C25 C26 C27 -179.0(8) . . . . ? C25 C26 C27 O27 -176.9(8) . . . . ? C25 C26 C27 C22 1.0(13) . . . . ? C125 O27 C27 C26 3.1(13) . . . . ? C125 O27 C27 C22 -175.0(8) . . . . ? C23 C22 C27 C26 0.0(12) . . . . ? C21 C22 C27 C26 -175.4(8) . . . . ? C23 C22 C27 O27 178.1(7) . . . . ? C21 C22 C27 O27 2.7(11) . . . . ? C6 C1 C28 C24 -73.2(11) . . . . ? C2 C1 C28 C24 106.5(11) . . . . ? C6 C1 C28 C59 161.3(9) . . . . ? C2 C1 C28 C59 -19.0(13) . . . . ? C23 C24 C28 C1 -47.6(11) . . . . ? C25 C24 C28 C1 134.9(9) . . . . ? C23 C24 C28 C59 79.0(10) . . . . ? C25 C24 C28 C59 -98.4(10) . . . . ? C15 C14 C39 C40 -171.0(8) . . . . ? C10 C14 C39 C40 63.0(11) . . . . ? C14 C39 C40 C41 -176.4(8) . . . . ? C39 C40 C41 C42 -178.8(9) . . . . ? C40 C41 C42 C43 -177.8(10) . . . . ? C41 C42 C43 C44 -179.2(11) . . . . ? C42 C43 C44 C45 -174.6(11) . . . . ? C43 C44 C45 C46 -177.1(15) . . . . ? C44 C45 C46 C47 172.2(15) . . . . ? C45 C46 C47 C48 149(2) . . . . ? C22 C21 C49 C50 -166.6(8) . . . . ? C17 C21 C49 C50 66.3(11) . . . . ? C21 C49 C50 C51 179.1(8) . . . . ? C49 C50 C51 C52 77.3(13) . . . . ? C50 C51 C52 C53 175.0(10) . . . . ? C51 C52 C53 C54 -170.5(11) . . . . ? C52 C53 C54 C55 -180.0(11) . . . . ? C53 C54 C55 C56 -175.0(13) . . . . ? C54 C55 C56 C57 169.0(15) . . . . ? C55 C56 C57 C58 127(2) . . . . ? C1 C28 C59 C60 -164.9(9) . . . . ? C24 C28 C59 C60 68.0(11) . . . . ? C28 C59 C60 C61 -175.7(10) . . . . ? C59 C60 C61 C62 177.6(12) . . . . ? C60 C61 C62 C63 -170.1(16) . . . . ? C61 C62 C63 C64 171.5(18) . . . . ? C62 C63 C64 C65 -165(4) . . . . ? C63 C64 C65 C66 -162(3) . . . . ? C63 C64 C65 C67 146(3) . . . . ? C64 C65 C66 C67 -120(4) . . . . ? C65 C66 C67 C68 137(4) . . . . ? C64 C65 C67 C68 8(8) . . . . ? C66 C65 C67 C68 -75(6) . . . . ? C64 C65 C67 C66 83(4) . . . . ? C4 O4 C69 C70 -166.7(8) . . . . ? C71 N1 C70 C69 168.6(8) . . . . ? O4 C69 C70 N1 -66.2(10) . . . . ? C70 N1 C71 C76 -170.2(9) . . . . ? C70 N1 C71 C72 9.1(13) . . . . ? N1 C71 C72 C73 -177.7(9) . . . . ? C76 C71 C72 C73 1.7(13) . . . . ? C71 C72 C73 C74 -0.1(15) . . . . ? C72 C73 C74 C75 -0.7(16) . . . . ? C73 C74 C75 C76 -0.3(15) . . . . ? C74 C75 C76 C71 2.0(14) . . . . ? C74 C75 C76 N2 -178.3(9) . . . . ? N1 C71 C76 C75 176.7(9) . . . . ? C72 C71 C76 C75 -2.6(13) . . . . ? N1 C71 C76 N2 -3.1(14) . . . . ? C72 C71 C76 N2 177.6(8) . . . . ? O101 N2 C76 C75 175.8(9) . . . . ? O102 N2 C76 C75 -3.6(12) . . . . ? O101 N2 C76 C71 -4.4(13) . . . . ? O102 N2 C76 C71 176.1(9) . . . . ? C6 O6 C77 C78 159.6(9) . . . . ? C79 N3 C78 C77 -169.5(8) . . . . ? O6 C77 C78 N3 70.9(10) . . . . ? C78 N3 C79 C84 170.2(9) . . . . ? C78 N3 C79 C80 -10.9(14) . . . . ? N3 C79 C80 C81 178.4(12) . . . . ? C84 C79 C80 C81 -2.6(17) . . . . ? C79 C80 C81 C82 -3(2) . . . . ? C80 C81 C82 C83 8(2) . . . . ? C81 C82 C83 C84 -6(2) . . . . ? C82 C83 C84 N4 178.7(12) . . . . ? C82 C83 C84 C79 0.1(19) . . . . ? O104 N4 C84 C83 -178.1(10) . . . . ? O103 N4 C84 C83 2.6(14) . . . . ? O104 N4 C84 C79 0.5(15) . . . . ? O103 N4 C84 C79 -178.9(9) . . . . ? N3 C79 C84 C83 -176.9(10) . . . . ? C80 C79 C84 C83 4.2(15) . . . . ? N3 C79 C84 N4 4.6(15) . . . . ? C80 C79 C84 N4 -174.4(9) . . . . ? C11 O11 C85 C86 -169.6(10) . . . . ? C87 N5 C86 C85 -77.7(17) . . . . ? O11 C85 C86 N5 163.9(11) . . . . ? C86 N5 C87 C88 172.1(12) . . . . ? C86 N5 C87 C92 -10.4(18) . . . . ? O106 N6 C88 C87 6(4) . . . . ? O105 N6 C88 C87 -178.8(13) . . . . ? O106 N6 C88 C89 -174(3) . . . . ? O105 N6 C88 C89 1(2) . . . . ? N5 C87 C88 N6 -3.0(15) . . . . ? C92 C87 C88 N6 179.6(13) . . . . ? N5 C87 C88 C89 177.4(12) . . . . ? C92 C87 C88 C89 0.0 . . . . ? N6 C88 C89 C90 -179.7(13) . . . . ? C87 C88 C89 C90 0.0 . . . . ? C88 C89 C90 C91 0.0 . . . . ? C89 C90 C91 C92 0.0 . . . . ? C90 C91 C92 C87 0.0 . . . . ? N5 C87 C92 C91 -177.6(11) . . . . ? C88 C87 C92 C91 0.0 . . . . ? C13 O13 C93 C94 172.1(8) . . . . ? C95 N7 C94 C93 77.9(13) . . . . ? O13 C93 C94 N7 176.9(8) . . . . ? C94 N7 C95 C96 3.3(17) . . . . ? C94 N7 C95 C100 -174.0(11) . . . . ? N7 C95 C96 C97 179.5(12) . . . . ? C100 C95 C96 C97 -2.7(17) . . . . ? C95 C96 C97 C98 2(2) . . . . ? C96 C97 C98 C99 0(2) . . . . ? C97 C98 C99 C100 -1(2) . . . . ? C98 C99 C100 C95 0(2) . . . . ? C98 C99 C100 N8 -179.4(14) . . . . ? N7 C95 C100 C99 179.5(13) . . . . ? C96 C95 C100 C99 1.9(19) . . . . ? N7 C95 C100 N8 -1.3(18) . . . . ? C96 C95 C100 N8 -178.9(10) . . . . ? O107 N8 C100 C99 178.9(16) . . . . ? O108 N8 C100 C99 -1.8(19) . . . . ? O107 N8 C100 C95 0(2) . . . . ? O108 N8 C100 C95 178.9(12) . . . . ? C18 O18 C101 C102 173.5(7) . . . . ? C103 N9 C102 C101 -167.7(8) . . . . ? O18 C101 C102 N9 76.3(9) . . . . ? C102 N9 C103 C104 8.7(12) . . . . ? C102 N9 C103 C108 -172.8(8) . . . . ? N9 C103 C104 C105 178.3(9) . . . . ? C108 C103 C104 C105 -0.3(13) . . . . ? C103 C104 C105 C106 1.5(15) . . . . ? C104 C105 C106 C107 -0.7(15) . . . . ? O111 N12 C116 C111 3.9(16) . . . . ? O112 N12 C116 C111 -175.7(11) . . . . ? O111 N12 C116 C115 -175.8(11) . . . . ? O112 N12 C116 C115 4.7(16) . . . . ? C105 C106 C107 C108 -1.2(14) . . . . ? N9 C103 C108 N10 0.4(13) . . . . ? C104 C103 C108 N10 179.0(8) . . . . ? N9 C103 C108 C107 179.7(8) . . . . ? C104 C103 C108 C107 -1.6(12) . . . . ? O110 N10 C108 C103 8.3(13) . . . . ? O109 N10 C108 C103 -172.3(8) . . . . ? O110 N10 C108 C107 -171.1(8) . . . . ? O109 N10 C108 C107 8.3(12) . . . . ? C106 C107 C108 C103 2.5(14) . . . . ? C106 C107 C108 N10 -178.1(8) . . . . ? C20 O20 C109 C110 -171.8(7) . . . . ? C111 N11 C110 C109 172.8(8) . . . . ? O20 C109 C110 N11 -74.3(10) . . . . ? C110 N11 C111 C116 172.5(9) . . . . ? C110 N11 C111 C112 -5.4(14) . . . . ? C115 C116 C111 N11 178.8(9) . . . . ? N12 C116 C111 N11 -0.8(15) . . . . ? C115 C116 C111 C112 -3.3(15) . . . . ? N12 C116 C111 C112 177.1(9) . . . . ? N11 C111 C112 C113 -177.7(10) . . . . ? C116 C111 C112 C113 4.3(15) . . . . ? C111 C112 C113 C114 -2.8(18) . . . . ? C112 C113 C114 C115 0(2) . . . . ? C113 C114 C115 C116 1(2) . . . . ? C111 C116 C115 C114 0.7(18) . . . . ? N12 C116 C115 C114 -179.6(11) . . . . ? C25 O25 C117 C118 -165.7(9) . . . . ? C19B N13B C118 C117 -78(3) . . . . ? C19B N13B C118 N13A -3(7) . . . . ? O25 C117 C118 N13B -168.7(14) . . . . ? O25 C117 C118 N13A 167(2) . . . . ? C19A N13A C118 N13B 179(21) . . . . ? C19A N13A C118 C117 -69(14) . . . . ? C27 O27 C125 C126 176.2(8) . . . . ? C127 N15 C126 C125 81.8(12) . . . . ? O27 C125 C126 N15 -170.3(9) . . . . ? C126 N15 C127 C128 16.5(12) . . . . ? C126 N15 C127 C132 -168.4(8) . . . . ? N15 C127 C128 C129 175.0(5) . . . . ? C132 C127 C128 C129 0.0 . . . . ? C127 C128 C129 C130 0.0 . . . . ? C128 C129 C130 C131 0.0 . . . . ? C129 C130 C131 C132 0.0 . . . . ? C130 C131 C132 C127 0.0 . . . . ? C130 C131 C132 N16 -177.4(7) . . . . ? N15 C127 C132 C131 -175.1(5) . . . . ? C128 C127 C132 C131 0.0 . . . . ? N15 C127 C132 N16 1.8(8) . . . . ? C128 C127 C132 N16 177.0(8) . . . . ? O116 N16 C132 C131 -1.4(14) . . . . ? O115 N16 C132 C131 174.8(9) . . . . ? O116 N16 C132 C127 -178.6(9) . . . . ? O115 N16 C132 C127 -2.4(14) . . . . ? 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 N13A H13A O14A 0.88 2.21 2.87(5) 131.5 . N13B H13B O14B 0.88 1.79 2.46(4) 130.9 . N1 H1N O101 0.88 1.97 2.616(11) 128.9 . N3 H3N O104 0.88 2.04 2.660(10) 126.6 . N5 H5N O106 0.88 2.03 2.68(3) 130.2 . N7 H7N O107 0.88 1.96 2.619(13) 130.3 . N9 H9N O110 0.88 1.98 2.615(9) 128.2 . N11 H11N O111 0.88 1.92 2.581(11) 130.3 . N15 H15N O115 0.88 1.92 2.600(15) 132.3 . _diffrn_measured_fraction_theta_max 0.704 _diffrn_reflns_theta_full 64.85 _diffrn_measured_fraction_theta_full 0.704 _refine_diff_density_max 0.714 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.114