# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'J.Rebek Junior' _publ_contact_author_address ; The Skaggs Institute for Chem. Biol The Scripps Research Institute 10550 North Torrey Pines Rd. MB26 La Jolla CA 92037 UNITED STATES OF AMERICA ; _publ_contact_author_email JREBEK@SCRIPPS.EDU _publ_section_title ; Metal Directed Assembly of Ditopic Containers and their Complexes with Alkylammonium Salts ; loop_ _publ_author_name 'J.Rebek Junior' 'Edoardo Menozzi' data_edor _database_code_depnum_ccdc_archive 'CCDC 278172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H94.50 Cl2.50 N6 O20.50' _chemical_formula_weight 1496.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.133(3) _cell_length_b 15.339(3) _cell_length_c 18.436(4) _cell_angle_alpha 112.60(3) _cell_angle_beta 103.94(3) _cell_angle_gamma 92.58(3) _cell_volume 3789.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 5872 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 24.4 _exptl_crystal_description Block-shaped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1586 _exptl_absorpt_coefficient_mu 0.179 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9382 _exptl_absorpt_correction_T_max 0.9582 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 28181 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.1004 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13290 _reflns_number_gt 8097 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1540P)^2^+5.7819P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13290 _refine_ls_number_parameters 970 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1435 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2907 _refine_ls_wR_factor_gt 0.2523 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.00480(18) 0.36153(19) 0.15030(16) 0.0205(6) Uani 1 1 d . . . O2 O 0.90750(19) 0.2194(2) 0.16663(17) 0.0223(7) Uani 1 1 d . . . O3 O 0.62889(19) 0.1636(2) 0.23121(17) 0.0229(7) Uani 1 1 d . . . O4 O 0.49509(19) 0.2550(2) 0.29556(17) 0.0231(7) Uani 1 1 d . . . O5 O 0.4293(2) 0.5580(2) 0.3070(2) 0.0323(8) Uani 1 1 d . . . H5A H 0.4551 0.6005 0.2976 0.039 Uiso 1 1 calc R . . O6 O 0.51754(19) 0.6937(2) 0.27740(18) 0.0291(7) Uani 1 1 d . . . H6A H 0.4970 0.6500 0.2885 0.035 Uiso 1 1 calc R . . O7 O 0.7910(2) 0.7617(2) 0.21164(17) 0.0234(7) Uani 1 1 d . . . O8 O 0.93943(18) 0.67278(19) 0.17732(16) 0.0211(6) Uani 1 1 d . . . O9 O 0.8737(2) 0.3831(2) -0.11006(18) 0.0301(7) Uani 1 1 d . . . O10 O 0.8159(3) 0.0337(3) -0.2137(2) 0.0583(12) Uani 1 1 d . . . O11 O 0.5798(2) 0.1053(2) -0.05618(19) 0.0364(8) Uani 1 1 d . . . O12 O 0.2559(2) 0.0211(2) -0.0660(2) 0.0352(8) Uani 1 1 d . . . O13A O 0.5164(4) 0.6595(6) -0.0004(4) 0.0405(19) Uani 0.50 1 d P A 1 O13B O 0.5222(5) 0.5807(7) 0.0008(4) 0.058(2) Uani 0.50 1 d P A 2 O14 O 0.7463(2) 0.6599(2) -0.14791(19) 0.0373(8) Uani 1 1 d . . . N1 N 0.8579(3) 0.2246(3) -0.1408(2) 0.0272(9) Uani 1 1 d . . . H1A H 0.8498 0.1679 -0.1812 0.033 Uiso 1 1 calc R . . N2 N 0.7397(2) 0.0908(2) -0.1179(2) 0.0249(9) Uani 1 1 d . . . H2A H 0.6854 0.0878 -0.1088 0.030 Uiso 1 1 calc R . . N3 N 0.4352(2) 0.0992(3) -0.0417(2) 0.0268(9) Uani 1 1 d . . . H3A H 0.3769 0.0815 -0.0702 0.032 Uiso 1 1 calc R . . N4 N 0.2920(2) 0.1711(3) 0.0311(2) 0.0254(9) Uani 1 1 d . . . H4A H 0.2744 0.2278 0.0458 0.030 Uiso 1 1 calc R . . N5 N 0.6162(3) 0.5954(3) -0.0726(2) 0.0331(10) Uani 1 1 d . A . H5B H 0.6205 0.5778 -0.1228 0.040 Uiso 1 1 calc R . . N6 N 0.7826(3) 0.5398(3) -0.1103(2) 0.0285(9) Uani 1 1 d . . . H6B H 0.7922 0.4800 -0.1266 0.034 Uiso 1 1 calc R . . C1 C 0.9289(3) 0.6226(3) 0.2838(2) 0.0198(9) Uani 1 1 d . . . C2 C 0.9426(3) 0.6018(3) 0.2074(2) 0.0191(9) Uani 1 1 d . . . C3 C 0.9649(3) 0.5146(3) 0.1624(2) 0.0206(9) Uani 1 1 d . . . H3B H 0.9740 0.5022 0.1104 0.025 Uiso 1 1 calc R . . C4 C 0.9737(3) 0.4460(3) 0.1937(2) 0.0203(9) Uani 1 1 d . . . C5 C 0.9602(3) 0.4625(3) 0.2698(2) 0.0192(9) Uani 1 1 d . . . C6 C 0.9376(3) 0.5505(3) 0.3121(2) 0.0203(9) Uani 1 1 d . . . H6C H 0.9273 0.5626 0.3637 0.024 Uiso 1 1 calc R . . C7 C 0.9729(3) 0.3896(3) 0.3069(2) 0.0210(9) Uani 1 1 d . . . H7A H 1.0119 0.3449 0.2786 0.025 Uiso 1 1 calc R . . C8 C 1.0252(3) 0.4360(3) 0.3976(3) 0.0256(10) Uani 1 1 d . . . H8A H 1.0792 0.4810 0.4055 0.031 Uiso 1 1 calc R . . H8B H 0.9847 0.4735 0.4285 0.031 Uiso 1 1 calc R . . C9 C 1.0580(4) 0.3644(4) 0.4326(3) 0.0410(13) Uani 1 1 d . . . H9A H 1.0896 0.3983 0.4911 0.049 Uiso 1 1 calc R . . H9B H 1.1007 0.3291 0.4042 0.049 Uiso 1 1 calc R . . H9C H 1.0050 0.3196 0.4251 0.049 Uiso 1 1 calc R . . C10 C 0.8805(3) 0.3305(3) 0.2883(2) 0.0205(9) Uani 1 1 d . . . C11 C 0.8476(3) 0.2505(3) 0.2157(2) 0.0201(9) Uani 1 1 d . . . C12 C 0.7637(3) 0.1966(3) 0.1951(3) 0.0218(10) Uani 1 1 d . . . H12A H 0.7427 0.1415 0.1450 0.026 Uiso 1 1 calc R . . C13 C 0.7104(3) 0.2237(3) 0.2486(2) 0.0205(9) Uani 1 1 d . . . C14 C 0.7407(3) 0.3006(3) 0.3239(2) 0.0200(9) Uani 1 1 d . . . C15 C 0.8255(3) 0.3536(3) 0.3412(2) 0.0188(9) Uani 1 1 d . . . H15A H 0.8469 0.4081 0.3917 0.023 Uiso 1 1 calc R . . C16 C 0.6835(3) 0.3231(3) 0.3848(2) 0.0216(9) Uani 1 1 d . . . H16A H 0.6453 0.2614 0.3722 0.026 Uiso 1 1 calc R . . C17 C 0.7402(3) 0.3594(3) 0.4734(3) 0.0268(10) Uani 1 1 d . . . H17A H 0.7720 0.4251 0.4911 0.032 Uiso 1 1 calc R . . H17B H 0.7877 0.3182 0.4785 0.032 Uiso 1 1 calc R . . C18 C 0.6793(4) 0.3599(4) 0.5291(3) 0.0423(13) Uani 1 1 d . . . H18A H 0.7175 0.3847 0.5860 0.051 Uiso 1 1 calc R . . H18B H 0.6495 0.2946 0.5128 0.051 Uiso 1 1 calc R . . H18C H 0.6322 0.4006 0.5241 0.051 Uiso 1 1 calc R . . C19 C 0.6164(3) 0.3893(3) 0.3695(2) 0.0204(9) Uani 1 1 d . . . C20 C 0.5248(3) 0.3531(3) 0.3243(2) 0.0208(9) Uani 1 1 d . . . C21 C 0.4644(3) 0.4113(3) 0.3058(3) 0.0254(10) Uani 1 1 d . . . H21A H 0.4021 0.3850 0.2754 0.031 Uiso 1 1 calc R . . C22 C 0.4937(3) 0.5071(3) 0.3310(3) 0.0233(10) Uani 1 1 d . . . C23 C 0.5831(3) 0.5479(3) 0.3785(2) 0.0212(9) Uani 1 1 d . . . C24 C 0.6420(3) 0.4870(3) 0.3952(2) 0.0216(10) Uani 1 1 d . . . H24A H 0.7040 0.5138 0.4263 0.026 Uiso 1 1 calc R . . C25 C 0.6142(3) 0.6558(3) 0.4122(2) 0.0227(10) Uani 1 1 d . . . H25A H 0.5569 0.6858 0.4098 0.027 Uiso 1 1 calc R . . C26 C 0.6701(3) 0.6976(3) 0.5021(3) 0.0281(11) Uani 1 1 d . . . H26A H 0.7254 0.6660 0.5079 0.034 Uiso 1 1 calc R . . H26B H 0.6911 0.7665 0.5200 0.034 Uiso 1 1 calc R . . C27 C 0.6157(3) 0.6852(4) 0.5571(3) 0.0375(12) Uani 1 1 d . . . H27A H 0.6542 0.7135 0.6139 0.045 Uiso 1 1 calc R . . H27B H 0.5962 0.6169 0.5407 0.045 Uiso 1 1 calc R . . H27C H 0.5612 0.7171 0.5523 0.045 Uiso 1 1 calc R . . C28 C 0.6622(3) 0.6808(3) 0.3576(2) 0.0220(10) Uani 1 1 d . . . C29 C 0.6109(3) 0.6998(3) 0.2927(3) 0.0250(10) Uani 1 1 d . . . C30 C 0.6541(3) 0.7261(3) 0.2445(2) 0.0218(9) Uani 1 1 d . . . H30A H 0.6188 0.7409 0.2018 0.026 Uiso 1 1 calc R . . C31 C 0.7478(3) 0.7308(3) 0.2583(2) 0.0220(10) Uani 1 1 d . . . C32 C 0.8021(3) 0.7125(3) 0.3213(2) 0.0213(9) Uani 1 1 d . . . C33 C 0.7571(3) 0.6875(3) 0.3696(2) 0.0224(10) Uani 1 1 d . . . H33A H 0.7930 0.6744 0.4131 0.027 Uiso 1 1 calc R . . C34 C 0.9055(3) 0.7186(3) 0.3342(2) 0.0210(9) Uani 1 1 d . . . H34A H 0.9233 0.7643 0.3116 0.025 Uiso 1 1 calc R . . C35 C 0.9612(3) 0.7595(3) 0.4247(3) 0.0256(10) Uani 1 1 d . . . H35A H 0.9415 0.8209 0.4542 0.031 Uiso 1 1 calc R . . H35B H 0.9475 0.7148 0.4489 0.031 Uiso 1 1 calc R . . C36 C 1.0637(3) 0.7760(4) 0.4366(3) 0.0351(12) Uani 1 1 d . . . H36A H 1.0958 0.8023 0.4952 0.042 Uiso 1 1 calc R . . H36B H 1.0779 0.8212 0.4137 0.042 Uiso 1 1 calc R . . H36C H 1.0839 0.7152 0.4087 0.042 Uiso 1 1 calc R . . C37 C 0.9396(3) 0.2945(3) 0.0830(2) 0.0213(9) Uani 1 1 d . . . C38 C 0.9309(3) 0.2934(3) 0.0063(3) 0.0238(10) Uani 1 1 d . . . H38A H 0.9693 0.3396 0.0005 0.029 Uiso 1 1 calc R . . C39 C 0.8673(3) 0.2263(3) -0.0620(2) 0.0213(9) Uani 1 1 d . . . C40 C 0.8123(3) 0.1587(3) -0.0530(3) 0.0236(10) Uani 1 1 d . . . C41 C 0.8242(3) 0.1570(3) 0.0238(3) 0.0233(10) Uani 1 1 d . . . H41A H 0.7885 0.1088 0.0295 0.028 Uiso 1 1 calc R . . C42 C 0.8870(3) 0.2245(3) 0.0906(2) 0.0206(9) Uani 1 1 d . . . C43 C 0.8599(3) 0.2999(3) -0.1610(3) 0.0269(10) Uani 1 1 d . . . C44 C 0.8393(4) 0.2739(4) -0.2516(3) 0.0351(12) Uani 1 1 d . . . H44A H 0.8697 0.2186 -0.2765 0.042 Uiso 1 1 calc R . . H44B H 0.8649 0.3284 -0.2604 0.042 Uiso 1 1 calc R . . C45 C 0.7370(4) 0.2492(5) -0.2933(4) 0.067(2) Uani 1 1 d . . . H45A H 0.7262 0.2321 -0.3520 0.080 Uiso 1 1 calc R . . H45B H 0.7069 0.3045 -0.2698 0.080 Uiso 1 1 calc R . . H45C H 0.7115 0.1950 -0.2850 0.080 Uiso 1 1 calc R . . C46 C 0.7457(4) 0.0306(3) -0.1919(3) 0.0364(12) Uani 1 1 d . . . C47 C 0.6613(4) -0.0399(4) -0.2461(3) 0.0449(14) Uani 1 1 d . . . H47A H 0.6777 -0.1051 -0.2616 0.054 Uiso 1 1 calc R . . H47B H 0.6156 -0.0349 -0.2149 0.054 Uiso 1 1 calc R . . C48 C 0.6183(7) -0.0271(7) -0.3213(4) 0.116(4) Uani 1 1 d . . . H48A H 0.5641 -0.0762 -0.3539 0.140 Uiso 1 1 calc R . . H48B H 0.6627 -0.0329 -0.3532 0.140 Uiso 1 1 calc R . . H48C H 0.5995 0.0363 -0.3067 0.140 Uiso 1 1 calc R . . C49 C 0.5497(3) 0.1702(3) 0.1788(3) 0.0225(10) Uani 1 1 d . . . C50 C 0.5353(3) 0.1314(3) 0.0946(3) 0.0238(10) Uani 1 1 d . . . H50A H 0.5828 0.1042 0.0720 0.029 Uiso 1 1 calc R . . C51 C 0.4517(3) 0.1321(3) 0.0431(3) 0.0228(10) Uani 1 1 d . . . C52 C 0.3798(3) 0.1656(3) 0.0770(3) 0.0224(10) Uani 1 1 d . . . C53 C 0.3953(3) 0.2035(3) 0.1605(3) 0.0225(10) Uani 1 1 d . . . H53A H 0.3464 0.2257 0.1832 0.027 Uiso 1 1 calc R . . C54 C 0.4799(3) 0.2099(3) 0.2117(2) 0.0209(9) Uani 1 1 d . . . C55 C 0.4964(3) 0.0906(3) -0.0864(3) 0.0291(11) Uani 1 1 d . . . C56 C 0.4542(3) 0.0625(4) -0.1768(3) 0.0359(12) Uani 1 1 d . . . H56A H 0.4835 0.1095 -0.1920 0.043 Uiso 1 1 calc R . . H56B H 0.4716 -0.0001 -0.2065 0.043 Uiso 1 1 calc R . . C57 C 0.3520(3) 0.0548(3) -0.2083(3) 0.0350(12) Uani 1 1 d . . . H57A H 0.3349 0.0352 -0.2678 0.042 Uiso 1 1 calc R . . H57B H 0.3331 0.1170 -0.1823 0.042 Uiso 1 1 calc R . . H57C H 0.3211 0.0072 -0.1956 0.042 Uiso 1 1 calc R . . C58 C 0.2333(3) 0.0993(3) -0.0320(3) 0.0276(11) Uani 1 1 d . . . C59 C 0.1382(3) 0.1214(4) -0.0596(3) 0.0356(12) Uani 1 1 d . . . H59A H 0.1339 0.1867 -0.0223 0.043 Uiso 1 1 calc R . . H59B H 0.1283 0.1200 -0.1152 0.043 Uiso 1 1 calc R . . C60 C 0.0666(5) 0.0545(7) -0.0611(8) 0.161(4) Uani 1 1 d . . . H60A H 0.0062 0.0707 -0.0810 0.193 Uiso 1 1 calc R . . H60B H 0.0742 0.0580 -0.0057 0.193 Uiso 1 1 calc R . . H60C H 0.0709 -0.0104 -0.0975 0.193 Uiso 1 1 calc R . . C61 C 0.7835(3) 0.6984(3) 0.1321(3) 0.0234(10) Uani 1 1 d . . . C62 C 0.7045(3) 0.6806(3) 0.0699(3) 0.0234(10) Uani 1 1 d . . . H62A H 0.6522 0.7086 0.0822 0.028 Uiso 1 1 calc R . . C63 C 0.6997(3) 0.6226(3) -0.0104(3) 0.0266(10) Uani 1 1 d . . . C64 C 0.7802(3) 0.5902(3) -0.0281(3) 0.0249(10) Uani 1 1 d . . . C65 C 0.8582(3) 0.6066(3) 0.0338(3) 0.0247(10) Uani 1 1 d . . . H65A H 0.9118 0.5825 0.0210 0.030 Uiso 1 1 calc R . . C66 C 0.8609(3) 0.6576(3) 0.1149(2) 0.0224(10) Uani 1 1 d . . . C67 C 0.5312(4) 0.5934(6) -0.0641(3) 0.066(2) Uani 1 1 d . . . C68 C 0.4532(4) 0.5408(5) -0.1395(3) 0.0527(16) Uani 1 1 d . A . H68A H 0.4782 0.5066 -0.1859 0.063 Uiso 1 1 calc R . . H68B H 0.4161 0.4926 -0.1309 0.063 Uiso 1 1 calc R . . C69 C 0.3950(6) 0.6048(6) -0.1593(5) 0.090(3) Uani 1 1 d . . . H69A H 0.3461 0.5687 -0.2100 0.108 Uiso 1 1 calc R A . H69B H 0.4318 0.6533 -0.1667 0.108 Uiso 1 1 calc R . . H69C H 0.3674 0.6361 -0.1147 0.108 Uiso 1 1 calc R . . C70 C 0.7706(3) 0.5815(3) -0.1644(3) 0.0245(10) Uani 1 1 d . . . C71 C 0.7876(3) 0.5250(3) -0.2449(2) 0.0271(11) Uani 1 1 d . . . H71A H 0.7382 0.4692 -0.2765 0.033 Uiso 1 1 calc R . . H71B H 0.8468 0.5007 -0.2351 0.033 Uiso 1 1 calc R . . C72 C 0.7905(3) 0.5831(4) -0.2946(3) 0.0368(12) Uani 1 1 d . . . H72A H 0.8020 0.5432 -0.3465 0.044 Uiso 1 1 calc R . . H72B H 0.8399 0.6379 -0.2640 0.044 Uiso 1 1 calc R . . H72C H 0.7314 0.6060 -0.3057 0.044 Uiso 1 1 calc R . . Cl1 Cl 1.00206(19) 0.9295(2) 0.27834(16) 0.0494(7) Uani 0.50 1 d P . . Cl2 Cl 0.8952(3) 1.0859(2) 0.3022(2) 0.0643(9) Uani 0.50 1 d P . . Cl3 Cl 0.9169(3) 0.9809(2) 0.4035(2) 0.0786(11) Uani 0.50 1 d P . . C73 C 0.9152(9) 0.9772(9) 0.3076(7) 0.059(3) Uani 0.50 1 d P . . H73 H 0.8592 0.9307 0.2690 0.071 Uiso 0.50 1 calc PR . . Cl4 Cl 0.1589(4) 0.1794(3) 0.3138(3) 0.1022(15) Uani 0.50 1 d P . . Cl5 Cl 0.1375(3) 0.1377(4) 0.1432(3) 0.1095(15) Uani 0.50 1 d P . . C74 C 0.0874(9) 0.1238(12) 0.2165(10) 0.081(4) Uani 0.50 1 d P . . H74A H 0.0290 0.1506 0.2136 0.098 Uiso 0.50 1 calc PR . . H74B H 0.0727 0.0549 0.2030 0.098 Uiso 0.50 1 calc PR . . O15 O 0.4482(4) 0.6936(4) 0.1306(4) 0.0391(15) Uiso 0.60 1 d P B 1 H15A' H 0.4680 0.7193 0.1818 0.047 Uiso 0.60 1 calc PR B 1 O15' O 0.4357(6) 0.6500(7) 0.1220(5) 0.036(2) Uiso 0.40 1 d P C 2 H15B H 0.4603 0.6160 0.0868 0.043 Uiso 0.40 1 calc PR C 2 C75 C 0.3006(5) 0.6252(5) 0.0154(4) 0.0619(17) Uiso 1 1 d . . . H75A H 0.2336 0.6132 0.0047 0.074 Uiso 1 1 calc R D 1 H75B H 0.3230 0.5648 -0.0094 0.074 Uiso 1 1 calc R D 1 H75C H 0.3162 0.6691 -0.0083 0.074 Uiso 1 1 calc R D 1 C76 C 0.3449(7) 0.6688(7) 0.1056(6) 0.051(2) Uiso 0.60 1 d P B 1 H76A H 0.3285 0.6237 0.1286 0.061 Uiso 0.60 1 calc PR B 1 H76B H 0.3188 0.7277 0.1302 0.061 Uiso 0.60 1 calc PR B 1 C76' C 0.3694(9) 0.6988(9) 0.0858(8) 0.038(3) Uiso 0.40 1 d P C 2 H76A' H 0.4012 0.7412 0.0677 0.045 Uiso 0.40 1 calc PR C 2 H76B' H 0.3392 0.7382 0.1265 0.045 Uiso 0.40 1 calc PR C 2 O1W O 0.7832(3) 0.9695(4) 0.5414(3) 0.0778(14) Uiso 1 1 d . E 1 O2W O 0.6887(4) 1.0777(4) 0.4451(4) 0.0781(18) Uiso 0.80 1 d P F 1 O3W O 0.5843(4) 0.9192(4) 0.4462(4) 0.0797(18) Uiso 0.80 1 d P G 1 O4W O 0.8830(6) 0.9300(6) 0.5982(5) 0.064(2) Uiso 0.50 1 d P H 1 O1W' O 0.7332(15) 0.9420(16) 0.4445(13) 0.064(6) Uiso 0.20 1 d P I 2 O2W' O 0.5927(9) 1.0962(9) 0.4099(8) 0.051(3) Uiso 0.30 1 d P J 2 O3W' O 0.4872(8) 0.8825(8) 0.4548(7) 0.039(3) Uiso 0.30 1 d P K 2 O4W' O 0.9556(6) 1.1060(6) 0.3152(5) 0.054(2) Uiso 0.50 1 d P L 2 O1W" O 0.8289(6) 0.9746(7) 0.4108(6) 0.048(2) Uiso 0.40 1 d P M 3 O2W" O 0.6633(15) 0.9905(16) 0.4450(13) 0.065(6) Uiso 0.20 1 d P N 3 O3W" O 0.5106(11) 0.9261(11) 0.4212(10) 0.072(4) Uiso 0.30 1 d P O 3 O4W" O 1.0273(15) 1.0082(17) 0.3017(14) 0.067(6) Uiso 0.20 1 d P P 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0190(14) 0.0246(15) 0.0188(14) 0.0085(12) 0.0073(11) 0.0050(12) O2 0.0237(14) 0.0264(15) 0.0227(14) 0.0130(12) 0.0114(12) 0.0066(12) O3 0.0200(14) 0.0244(15) 0.0260(15) 0.0118(12) 0.0068(12) 0.0016(12) O4 0.0272(15) 0.0228(15) 0.0243(15) 0.0123(12) 0.0120(12) 0.0025(12) O5 0.0205(15) 0.0358(17) 0.0482(19) 0.0257(15) 0.0080(13) 0.0075(13) O6 0.0237(15) 0.0368(17) 0.0386(17) 0.0240(14) 0.0148(13) 0.0072(13) O7 0.0328(16) 0.0220(15) 0.0202(14) 0.0088(12) 0.0155(12) 0.0061(12) O8 0.0210(14) 0.0258(15) 0.0209(14) 0.0131(12) 0.0075(11) 0.0040(12) O9 0.0375(17) 0.0271(16) 0.0280(16) 0.0109(13) 0.0134(13) 0.0086(14) O10 0.079(2) 0.034(2) 0.053(2) -0.0076(17) 0.049(2) -0.0138(19) O11 0.0309(17) 0.049(2) 0.0297(17) 0.0147(15) 0.0123(14) 0.0039(15) O12 0.0343(18) 0.0231(17) 0.0405(19) 0.0062(14) 0.0092(15) -0.0010(14) O13A 0.024(3) 0.062(5) 0.027(4) 0.007(3) 0.010(3) 0.006(3) O13B 0.029(4) 0.102(7) 0.031(4) 0.013(4) 0.013(3) 0.001(4) O14 0.053(2) 0.0458(19) 0.0309(17) 0.0245(14) 0.0244(15) 0.0314(16) N1 0.038(2) 0.0250(19) 0.0189(18) 0.0057(15) 0.0140(16) 0.0016(16) N2 0.0269(19) 0.0263(19) 0.0199(18) 0.0067(15) 0.0091(15) -0.0001(16) N3 0.0247(19) 0.026(2) 0.0244(19) 0.0071(16) 0.0040(15) 0.0022(16) N4 0.0231(18) 0.0199(18) 0.032(2) 0.0107(16) 0.0042(15) 0.0048(15) N5 0.030(2) 0.050(2) 0.0221(19) 0.0166(17) 0.0097(16) 0.0122(18) N6 0.042(2) 0.029(2) 0.0219(18) 0.0124(15) 0.0161(16) 0.0143(17) C1 0.0164(19) 0.022(2) 0.021(2) 0.0092(17) 0.0067(16) 0.0014(17) C2 0.0160(19) 0.024(2) 0.021(2) 0.0131(17) 0.0054(16) 0.0016(17) C3 0.020(2) 0.026(2) 0.019(2) 0.0105(17) 0.0086(16) 0.0044(17) C4 0.0148(19) 0.024(2) 0.021(2) 0.0064(17) 0.0071(16) 0.0025(17) C5 0.0134(19) 0.026(2) 0.019(2) 0.0109(17) 0.0037(16) 0.0038(16) C6 0.021(2) 0.025(2) 0.015(2) 0.0075(17) 0.0068(16) 0.0003(17) C7 0.020(2) 0.025(2) 0.020(2) 0.0103(17) 0.0070(16) 0.0060(17) C8 0.022(2) 0.034(2) 0.021(2) 0.0127(19) 0.0039(17) 0.0043(19) C9 0.043(3) 0.051(3) 0.033(3) 0.027(2) 0.001(2) 0.013(2) C10 0.018(2) 0.027(2) 0.024(2) 0.0180(17) 0.0057(16) 0.0071(17) C11 0.020(2) 0.026(2) 0.020(2) 0.0114(17) 0.0097(16) 0.0072(17) C12 0.027(2) 0.019(2) 0.021(2) 0.0103(17) 0.0057(17) 0.0085(17) C13 0.020(2) 0.025(2) 0.023(2) 0.0171(17) 0.0052(16) 0.0051(17) C14 0.024(2) 0.027(2) 0.0149(19) 0.0133(17) 0.0074(16) 0.0056(17) C15 0.020(2) 0.021(2) 0.018(2) 0.0096(17) 0.0061(16) 0.0059(17) C16 0.022(2) 0.028(2) 0.022(2) 0.0135(17) 0.0109(17) 0.0078(17) C17 0.030(2) 0.033(2) 0.023(2) 0.0159(19) 0.0094(18) 0.0078(19) C18 0.051(3) 0.059(3) 0.022(2) 0.021(2) 0.014(2) 0.003(3) C19 0.024(2) 0.029(2) 0.0140(19) 0.0122(17) 0.0093(16) 0.0088(18) C20 0.023(2) 0.023(2) 0.024(2) 0.0129(17) 0.0139(17) 0.0066(17) C21 0.017(2) 0.035(2) 0.023(2) 0.0099(19) 0.0078(17) 0.0006(18) C22 0.019(2) 0.031(2) 0.025(2) 0.0141(18) 0.0103(17) 0.0091(18) C23 0.026(2) 0.026(2) 0.0186(19) 0.0123(17) 0.0140(17) 0.0051(18) C24 0.020(2) 0.028(2) 0.016(2) 0.0074(17) 0.0063(16) 0.0020(18) C25 0.024(2) 0.029(2) 0.018(2) 0.0095(18) 0.0107(17) 0.0050(18) C26 0.037(2) 0.029(2) 0.022(2) 0.0097(19) 0.0149(19) 0.006(2) C27 0.045(3) 0.047(3) 0.023(2) 0.011(2) 0.020(2) 0.009(2) C28 0.030(2) 0.021(2) 0.019(2) 0.0086(17) 0.0126(17) 0.0075(18) C29 0.027(2) 0.023(2) 0.026(2) 0.0082(18) 0.0132(18) 0.0064(18) C30 0.028(2) 0.025(2) 0.018(2) 0.0128(17) 0.0079(17) 0.0089(18) C31 0.031(2) 0.018(2) 0.021(2) 0.0078(17) 0.0146(17) 0.0054(18) C32 0.029(2) 0.019(2) 0.018(2) 0.0061(17) 0.0129(17) 0.0061(17) C33 0.029(2) 0.023(2) 0.015(2) 0.0073(17) 0.0060(17) 0.0072(18) C34 0.024(2) 0.022(2) 0.019(2) 0.0092(17) 0.0072(17) 0.0016(17) C35 0.032(2) 0.024(2) 0.019(2) 0.0070(18) 0.0057(18) 0.0024(19) C36 0.031(3) 0.042(3) 0.023(2) 0.007(2) 0.003(2) 0.000(2) C37 0.019(2) 0.025(2) 0.022(2) 0.0081(17) 0.0098(16) 0.0089(17) C38 0.025(2) 0.022(2) 0.030(2) 0.0132(18) 0.0143(18) 0.0066(18) C39 0.027(2) 0.022(2) 0.015(2) 0.0063(17) 0.0103(17) 0.0051(18) C40 0.026(2) 0.025(2) 0.023(2) 0.0072(18) 0.0149(17) 0.0064(18) C41 0.025(2) 0.020(2) 0.027(2) 0.0094(18) 0.0117(18) 0.0030(18) C42 0.023(2) 0.025(2) 0.018(2) 0.0095(17) 0.0102(16) 0.0091(17) C43 0.027(2) 0.031(2) 0.029(2) 0.014(2) 0.0143(18) 0.0066(19) C44 0.050(3) 0.035(3) 0.021(2) 0.014(2) 0.010(2) 0.006(2) C45 0.064(4) 0.091(5) 0.039(3) 0.038(3) -0.009(3) -0.024(4) C46 0.057(3) 0.024(2) 0.033(3) 0.010(2) 0.027(2) 0.001(2) C47 0.060(3) 0.039(3) 0.028(3) 0.004(2) 0.016(2) -0.008(3) C48 0.145(8) 0.132(7) 0.051(4) 0.047(5) -0.013(5) -0.063(6) C49 0.022(2) 0.016(2) 0.031(2) 0.0130(17) 0.0065(18) 0.0005(17) C50 0.026(2) 0.020(2) 0.026(2) 0.0058(18) 0.0131(18) 0.0049(18) C51 0.030(2) 0.016(2) 0.021(2) 0.0050(17) 0.0086(18) 0.0023(18) C52 0.022(2) 0.018(2) 0.027(2) 0.0101(17) 0.0062(17) -0.0008(17) C53 0.020(2) 0.024(2) 0.028(2) 0.0135(18) 0.0106(17) 0.0047(17) C54 0.023(2) 0.023(2) 0.021(2) 0.0115(17) 0.0098(17) 0.0028(17) C55 0.034(3) 0.029(2) 0.027(2) 0.0119(19) 0.013(2) 0.005(2) C56 0.049(3) 0.030(3) 0.027(2) 0.009(2) 0.012(2) 0.001(2) C57 0.045(3) 0.034(3) 0.029(2) 0.015(2) 0.011(2) 0.011(2) C58 0.029(2) 0.026(2) 0.025(2) 0.0070(19) 0.0088(19) 0.0006(19) C59 0.029(2) 0.035(3) 0.035(3) 0.011(2) 0.000(2) 0.004(2) C60 0.030(4) 0.169(7) 0.375(14) 0.210(8) 0.050(6) 0.030(4) C61 0.028(2) 0.025(2) 0.022(2) 0.0118(18) 0.0135(18) 0.0047(18) C62 0.029(2) 0.026(2) 0.025(2) 0.0153(18) 0.0137(18) 0.0111(18) C63 0.032(2) 0.036(2) 0.020(2) 0.0183(19) 0.0078(18) 0.012(2) C64 0.028(2) 0.030(2) 0.023(2) 0.0140(18) 0.0133(18) 0.0101(19) C65 0.027(2) 0.029(2) 0.027(2) 0.0151(18) 0.0157(18) 0.0104(18) C66 0.026(2) 0.026(2) 0.022(2) 0.0160(18) 0.0101(17) 0.0048(18) C67 0.033(3) 0.126(6) 0.022(3) 0.012(3) 0.012(2) 0.004(3) C68 0.036(3) 0.080(4) 0.031(3) 0.011(3) 0.008(2) 0.014(3) C69 0.141(7) 0.076(5) 0.067(5) 0.031(4) 0.047(5) 0.038(5) C70 0.021(2) 0.034(3) 0.021(2) 0.0126(19) 0.0075(17) 0.0092(19) C71 0.020(2) 0.044(3) 0.016(2) 0.0098(19) 0.0053(17) 0.0057(19) C72 0.026(2) 0.061(3) 0.029(2) 0.022(2) 0.0101(19) 0.006(2) Cl1 0.0606(15) 0.0707(17) 0.0365(13) 0.0326(12) 0.0232(11) 0.0471(14) Cl2 0.071(2) 0.0525(17) 0.078(2) 0.0436(15) 0.0058(17) 0.0164(16) Cl3 0.150(3) 0.0500(17) 0.0549(18) 0.0286(14) 0.047(2) 0.033(2) C73 0.067(8) 0.060(7) 0.052(7) 0.026(6) 0.015(6) -0.010(6) Cl4 0.123(3) 0.088(3) 0.080(3) 0.014(2) 0.030(3) 0.039(3) Cl5 0.099(3) 0.135(4) 0.118(3) 0.078(3) 0.029(3) -0.008(3) C74 0.049(7) 0.106(10) 0.121(12) 0.076(9) 0.026(7) 0.029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C37 1.382(5) . ? O1 C4 1.407(5) . ? O2 C42 1.395(5) . ? O2 C11 1.403(5) . ? O3 C49 1.381(5) . ? O3 C13 1.398(5) . ? O4 C54 1.384(5) . ? O4 C20 1.400(5) . ? O5 C22 1.372(5) . ? O6 C29 1.364(5) . ? O7 C61 1.387(5) . ? O7 C31 1.397(5) . ? O8 C66 1.379(5) . ? O8 C2 1.398(5) . ? O9 C43 1.231(5) . ? O10 C46 1.228(6) . ? O11 C55 1.223(5) . ? O12 C58 1.229(5) . ? O13A C67 1.300(9) . ? O13B C67 1.320(10) . ? O14 C70 1.219(5) . ? N1 C43 1.343(6) . ? N1 C39 1.416(5) . ? N2 C46 1.348(6) . ? N2 C40 1.425(5) . ? N3 C55 1.359(6) . ? N3 C51 1.399(5) . ? N4 C58 1.337(5) . ? N4 C52 1.418(5) . ? N5 C67 1.334(7) . ? N5 C63 1.404(6) . ? N6 C70 1.361(6) . ? N6 C64 1.423(5) . ? C1 C2 1.388(6) . ? C1 C6 1.392(6) . ? C1 C34 1.521(6) . ? C2 C3 1.382(6) . ? C3 C4 1.378(6) . ? C4 C5 1.394(6) . ? C5 C6 1.382(6) . ? C5 C7 1.517(6) . ? C7 C10 1.521(6) . ? C7 C8 1.526(6) . ? C8 C9 1.519(7) . ? C10 C11 1.381(6) . ? C10 C15 1.388(6) . ? C11 C12 1.369(6) . ? C12 C13 1.376(6) . ? C13 C14 1.383(6) . ? C14 C15 1.384(6) . ? C14 C16 1.526(6) . ? C16 C17 1.516(6) . ? C16 C19 1.521(6) . ? C17 C18 1.534(6) . ? C19 C24 1.391(6) . ? C19 C20 1.394(6) . ? C20 C21 1.381(6) . ? C21 C22 1.375(6) . ? C22 C23 1.385(6) . ? C23 C24 1.388(6) . ? C23 C25 1.532(6) . ? C25 C28 1.520(6) . ? C25 C26 1.527(6) . ? C26 C27 1.509(6) . ? C28 C33 1.392(6) . ? C28 C29 1.400(6) . ? C29 C30 1.383(6) . ? C30 C31 1.373(6) . ? C31 C32 1.384(6) . ? C32 C33 1.390(6) . ? C32 C34 1.518(6) . ? C34 C35 1.535(6) . ? C35 C36 1.508(6) . ? C37 C42 1.378(6) . ? C37 C38 1.382(6) . ? C38 C39 1.379(6) . ? C39 C40 1.383(6) . ? C40 C41 1.394(6) . ? C41 C42 1.363(6) . ? C43 C44 1.508(6) . ? C44 C45 1.511(8) . ? C46 C47 1.493(7) . ? C47 C48 1.473(9) . ? C49 C50 1.389(6) . ? C49 C54 1.391(6) . ? C50 C51 1.390(6) . ? C51 C52 1.403(6) . ? C52 C53 1.375(6) . ? C53 C54 1.368(6) . ? C55 C56 1.509(6) . ? C56 C57 1.498(7) . ? C58 C59 1.506(7) . ? C59 C60 1.447(9) . ? C61 C62 1.374(6) . ? C61 C66 1.399(6) . ? C62 C63 1.385(6) . ? C63 C64 1.400(6) . ? C64 C65 1.365(6) . ? C65 C66 1.384(6) . ? C67 C68 1.496(7) . ? C68 C69 1.441(10) . ? C70 C71 1.494(6) . ? C71 C72 1.511(7) . ? Cl1 C73 1.637(14) . ? Cl2 C73 1.743(13) . ? Cl3 C73 1.741(13) . ? Cl4 C74 1.710(16) . ? Cl5 C74 1.773(16) . ? O15 C76 1.506(11) . ? O15' C76' 1.463(16) . ? C75 C76' 1.470(13) . ? C75 C76 1.493(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 C37 O1 C4 115.6(3) . . ? C42 O2 C11 118.9(3) . . ? C49 O3 C13 119.1(3) . . ? C54 O4 C20 111.2(3) . . ? C61 O7 C31 118.1(3) . . ? C66 O8 C2 113.2(3) . . ? C43 N1 C39 127.3(4) . . ? C46 N2 C40 126.7(4) . . ? C55 N3 C51 129.3(4) . . ? C58 N4 C52 126.8(4) . . ? C67 N5 C63 127.4(4) . . ? C70 N6 C64 121.9(4) . . ? C2 C1 C6 116.3(4) . . ? C2 C1 C34 122.3(4) . . ? C6 C1 C34 121.3(4) . . ? C3 C2 C1 121.9(4) . . ? C3 C2 O8 118.9(4) . . ? C1 C2 O8 119.1(4) . . ? C4 C3 C2 119.5(4) . . ? C3 C4 C5 121.3(4) . . ? C3 C4 O1 118.3(4) . . ? C5 C4 O1 120.2(4) . . ? C6 C5 C4 117.0(4) . . ? C6 C5 C7 120.7(4) . . ? C4 C5 C7 122.3(4) . . ? C5 C6 C1 124.0(4) . . ? C5 C7 C10 109.9(3) . . ? C5 C7 C8 111.8(3) . . ? C10 C7 C8 114.0(4) . . ? C9 C8 C7 113.4(4) . . ? C11 C10 C15 117.1(4) . . ? C11 C10 C7 120.0(4) . . ? C15 C10 C7 122.8(4) . . ? C12 C11 C10 122.2(4) . . ? C12 C11 O2 120.0(4) . . ? C10 C11 O2 117.5(3) . . ? C11 C12 C13 118.6(4) . . ? C12 C13 C14 122.2(4) . . ? C12 C13 O3 118.4(4) . . ? C14 C13 O3 118.7(4) . . ? C13 C14 C15 116.8(4) . . ? C13 C14 C16 120.7(4) . . ? C15 C14 C16 122.4(4) . . ? C14 C15 C10 122.9(4) . . ? C17 C16 C19 112.9(3) . . ? C17 C16 C14 114.1(3) . . ? C19 C16 C14 109.7(3) . . ? C16 C17 C18 111.2(4) . . ? C24 C19 C20 115.8(4) . . ? C24 C19 C16 123.4(4) . . ? C20 C19 C16 120.7(4) . . ? C21 C20 C19 121.5(4) . . ? C21 C20 O4 119.9(4) . . ? C19 C20 O4 118.5(4) . . ? C22 C21 C20 120.4(4) . . ? O5 C22 C21 115.9(4) . . ? O5 C22 C23 123.3(4) . . ? C21 C22 C23 120.7(4) . . ? C22 C23 C24 117.1(4) . . ? C22 C23 C25 121.0(4) . . ? C24 C23 C25 121.9(4) . . ? C23 C24 C19 124.4(4) . . ? C28 C25 C26 113.5(3) . . ? C28 C25 C23 111.2(3) . . ? C26 C25 C23 112.4(4) . . ? C27 C26 C25 112.6(4) . . ? C33 C28 C29 117.1(4) . . ? C33 C28 C25 122.9(4) . . ? C29 C28 C25 120.0(4) . . ? O6 C29 C30 119.4(4) . . ? O6 C29 C28 120.0(4) . . ? C30 C29 C28 120.6(4) . . ? C31 C30 C29 120.0(4) . . ? C30 C31 C32 121.9(4) . . ? C30 C31 O7 119.5(4) . . ? C32 C31 O7 118.5(4) . . ? C31 C32 C33 116.8(4) . . ? C31 C32 C34 120.0(4) . . ? C33 C32 C34 123.2(4) . . ? C32 C33 C28 123.5(4) . . ? C32 C34 C1 110.1(3) . . ? C32 C34 C35 113.6(3) . . ? C1 C34 C35 113.1(4) . . ? C36 C35 C34 112.8(4) . . ? C42 C37 O1 120.7(4) . . ? C42 C37 C38 119.3(4) . . ? O1 C37 C38 119.9(4) . . ? C39 C38 C37 121.0(4) . . ? C38 C39 C40 119.1(4) . . ? C38 C39 N1 121.4(4) . . ? C40 C39 N1 119.5(4) . . ? C39 C40 C41 119.9(4) . . ? C39 C40 N2 123.9(4) . . ? C41 C40 N2 116.2(4) . . ? C42 C41 C40 120.1(4) . . ? C41 C42 C37 120.6(4) . . ? C41 C42 O2 121.6(4) . . ? C37 C42 O2 117.5(3) . . ? O9 C43 N1 122.9(4) . . ? O9 C43 C44 122.6(4) . . ? N1 C43 C44 114.4(4) . . ? C43 C44 C45 111.7(4) . . ? O10 C46 N2 122.3(4) . . ? O10 C46 C47 121.8(4) . . ? N2 C46 C47 115.9(4) . . ? C48 C47 C46 114.2(5) . . ? O3 C49 C50 121.8(4) . . ? O3 C49 C54 118.4(4) . . ? C50 C49 C54 119.7(4) . . ? C49 C50 C51 120.3(4) . . ? C50 C51 N3 122.8(4) . . ? C50 C51 C52 119.0(4) . . ? N3 C51 C52 118.2(4) . . ? C53 C52 C51 119.6(4) . . ? C53 C52 N4 115.9(4) . . ? C51 C52 N4 124.3(4) . . ? C54 C53 C52 121.3(4) . . ? C53 C54 O4 119.8(4) . . ? C53 C54 C49 119.7(4) . . ? O4 C54 C49 120.5(4) . . ? O11 C55 N3 122.9(4) . . ? O11 C55 C56 121.8(4) . . ? N3 C55 C56 115.3(4) . . ? C57 C56 C55 118.9(4) . . ? O12 C58 N4 122.2(4) . . ? O12 C58 C59 122.4(4) . . ? N4 C58 C59 115.4(4) . . ? C60 C59 C58 112.6(5) . . ? C62 C61 O7 121.4(4) . . ? C62 C61 C66 120.1(4) . . ? O7 C61 C66 118.3(4) . . ? C61 C62 C63 121.1(4) . . ? C62 C63 C64 118.3(4) . . ? C62 C63 N5 121.2(4) . . ? C64 C63 N5 120.5(4) . . ? C65 C64 C63 120.2(4) . . ? C65 C64 N6 118.8(4) . . ? C63 C64 N6 121.0(4) . . ? C64 C65 C66 121.4(4) . . ? O8 C66 C65 121.2(4) . . ? O8 C66 C61 120.3(4) . . ? C65 C66 C61 118.3(4) . . ? O13A C67 O13B 55.7(5) . . ? O13A C67 N5 118.4(6) . . ? O13B C67 N5 115.5(6) . . ? O13A C67 C68 120.1(6) . . ? O13B C67 C68 113.9(6) . . ? N5 C67 C68 117.5(5) . . ? C69 C68 C67 111.4(6) . . ? O14 C70 N6 121.4(4) . . ? O14 C70 C71 122.5(4) . . ? N6 C70 C71 116.1(4) . . ? C70 C71 C72 112.6(4) . . ? Cl1 C73 Cl3 110.8(8) . . ? Cl1 C73 Cl2 118.6(7) . . ? Cl3 C73 Cl2 111.1(7) . . ? Cl4 C74 Cl5 112.1(8) . . ? C76' C75 C76 31.9(6) . . ? C75 C76 O15 114.9(8) . . ? O15' C76' C75 107.6(10) . . ? 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(6) . . . . ? C34 C1 C2 C3 179.2(4) . . . . ? C6 C1 C2 O8 -176.8(3) . . . . ? C34 C1 C2 O8 3.3(6) . . . . ? C66 O8 C2 C3 76.8(4) . . . . ? C66 O8 C2 C1 -107.2(4) . . . . ? C1 C2 C3 C4 0.2(6) . . . . ? O8 C2 C3 C4 176.1(3) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C2 C3 C4 O1 -174.1(3) . . . . ? C37 O1 C4 C3 -78.8(4) . . . . ? C37 O1 C4 C5 106.7(4) . . . . ? C3 C4 C5 C6 0.1(6) . . . . ? O1 C4 C5 C6 174.4(3) . . . . ? C3 C4 C5 C7 -177.7(4) . . . . ? O1 C4 C5 C7 -3.5(6) . . . . ? C4 C5 C6 C1 -0.9(6) . . . . ? C7 C5 C6 C1 177.0(4) . . . . ? C2 C1 C6 C5 1.2(6) . . . . ? C34 C1 C6 C5 -178.8(4) . . . . ? C6 C5 C7 C10 86.3(4) . . . . ? C4 C5 C7 C10 -95.9(4) . . . . ? C6 C5 C7 C8 -41.3(5) . . . . ? C4 C5 C7 C8 136.5(4) . . . . ? C5 C7 C8 C9 -167.1(4) . . . . ? C10 C7 C8 C9 67.5(5) . . . . ? C5 C7 C10 C11 86.0(5) . . . . ? C8 C7 C10 C11 -147.6(4) . . . . ? C5 C7 C10 C15 -93.4(5) . . . . ? C8 C7 C10 C15 33.0(6) . . . . ? C15 C10 C11 C12 1.3(6) . . . . ? C7 C10 C11 C12 -178.1(4) . . . . ? C15 C10 C11 O2 -171.9(4) . . . . ? C7 C10 C11 O2 8.7(6) . . . . ? C42 O2 C11 C12 73.1(5) . . . . ? C42 O2 C11 C10 -113.6(4) . . . . ? C10 C11 C12 C13 0.5(6) . . . . ? O2 C11 C12 C13 173.5(4) . . . . ? C11 C12 C13 C14 -3.4(6) . . . . ? C11 C12 C13 O3 -173.9(4) . . . . ? C49 O3 C13 C12 -84.4(5) . . . . ? C49 O3 C13 C14 104.7(4) . . . . ? C12 C13 C14 C15 4.2(6) . . . . ? O3 C13 C14 C15 174.7(4) . . . . ? C12 C13 C14 C16 -174.3(4) . . . . ? O3 C13 C14 C16 -3.8(6) . . . . ? C13 C14 C15 C10 -2.3(6) . . . . ? C16 C14 C15 C10 176.2(4) . . . . ? C11 C10 C15 C14 -0.3(6) . . . . ? C7 C10 C15 C14 179.0(4) . . . . ? C13 C14 C16 C17 143.3(4) . . . . ? C15 C14 C16 C17 -35.1(6) . . . . ? C13 C14 C16 C19 -88.9(5) . . . . ? C15 C14 C16 C19 92.7(5) . . . . ? C19 C16 C17 C18 66.1(5) . . . . ? C14 C16 C17 C18 -167.7(4) . . . . ? C17 C16 C19 C24 50.4(5) . . . . ? C14 C16 C19 C24 -78.1(5) . . . . ? C17 C16 C19 C20 -132.9(4) . . . . ? C14 C16 C19 C20 98.6(4) . . . . ? C24 C19 C20 C21 0.8(6) . . . . ? C16 C19 C20 C21 -176.1(4) . . . . ? C24 C19 C20 O4 179.0(3) . . . . ? C16 C19 C20 O4 2.2(6) . . . . ? C54 O4 C20 C21 70.0(5) . . . . ? C54 O4 C20 C19 -108.3(4) . . . . ? C19 C20 C21 C22 0.7(6) . . . . ? O4 C20 C21 C22 -177.6(4) . . . . ? C20 C21 C22 O5 177.8(4) . . . . ? C20 C21 C22 C23 -2.8(6) . . . . ? O5 C22 C23 C24 -177.3(4) . . . . ? C21 C22 C23 C24 3.3(6) . . . . ? O5 C22 C23 C25 3.9(6) . . . . ? C21 C22 C23 C25 -175.4(4) . . . . ? C22 C23 C24 C19 -1.9(6) . . . . ? C25 C23 C24 C19 176.9(4) . . . . ? C20 C19 C24 C23 -0.1(6) . . . . ? C16 C19 C24 C23 176.6(4) . . . . ? C22 C23 C25 C28 -96.6(5) . . . . ? C24 C23 C25 C28 84.8(5) . . . . ? C22 C23 C25 C26 134.9(4) . . . . ? C24 C23 C25 C26 -43.7(5) . . . . ? C28 C25 C26 C27 171.0(4) . . . . ? C23 C25 C26 C27 -61.7(5) . . . . ? C26 C25 C28 C33 36.1(6) . . . . ? C23 C25 C28 C33 -91.8(5) . . . . ? C26 C25 C28 C29 -142.8(4) . . . . ? C23 C25 C28 C29 89.3(5) . . . . ? C33 C28 C29 O6 179.6(4) . . . . ? C25 C28 C29 O6 -1.4(6) . . . . ? C33 C28 C29 C30 -1.4(6) . . . . ? C25 C28 C29 C30 177.6(4) . . . . ? O6 C29 C30 C31 -178.8(4) . . . . ? C28 C29 C30 C31 2.1(6) . . . . ? C29 C30 C31 C32 -1.9(6) . . . . ? C29 C30 C31 O7 -177.0(4) . . . . ? C61 O7 C31 C30 -76.6(5) . . . . ? C61 O7 C31 C32 108.1(4) . . . . ? C30 C31 C32 C33 1.0(6) . . . . ? O7 C31 C32 C33 176.1(3) . . . . ? C30 C31 C32 C34 -180.0(4) . . . . ? O7 C31 C32 C34 -4.8(6) . . . . ? C31 C32 C33 C28 -0.3(6) . . . . ? C34 C32 C33 C28 -179.3(4) . . . . ? C29 C28 C33 C32 0.5(6) . . . . ? C25 C28 C33 C32 -178.5(4) . . . . ? C31 C32 C34 C1 -88.7(5) . . . . ? C33 C32 C34 C1 90.3(5) . . . . ? C31 C32 C34 C35 143.2(4) . . . . ? C33 C32 C34 C35 -37.7(6) . . . . ? C2 C1 C34 C32 96.6(4) . . . . ? C6 C1 C34 C32 -83.3(5) . . . . ? C2 C1 C34 C35 -135.1(4) . . . . ? C6 C1 C34 C35 45.0(5) . . . . ? C32 C34 C35 C36 -173.2(4) . . . . ? C1 C34 C35 C36 60.3(5) . . . . ? C4 O1 C37 C42 -90.9(5) . . . . ? C4 O1 C37 C38 93.4(4) . . . . ? C42 C37 C38 C39 3.2(6) . . . . ? O1 C37 C38 C39 179.0(4) . . . . ? C37 C38 C39 C40 -0.6(6) . . . . ? C37 C38 C39 N1 180.0(4) . . . . ? C43 N1 C39 C38 -40.9(7) . . . . ? C43 N1 C39 C40 139.7(5) . . . . ? C38 C39 C40 C41 -2.5(6) . . . . ? N1 C39 C40 C41 176.9(4) . . . . ? C38 C39 C40 N2 174.9(4) . . . . ? N1 C39 C40 N2 -5.6(6) . . . . ? C46 N2 C40 C39 52.5(7) . . . . ? C46 N2 C40 C41 -130.0(5) . . . . ? C39 C40 C41 C42 3.0(6) . . . . ? N2 C40 C41 C42 -174.6(4) . . . . ? C40 C41 C42 C37 -0.4(6) . . . . ? C40 C41 C42 O2 -173.3(4) . . . . ? O1 C37 C42 C41 -178.4(4) . . . . ? C38 C37 C42 C41 -2.7(6) . . . . ? O1 C37 C42 O2 -5.3(6) . . . . ? C38 C37 C42 O2 170.5(4) . . . . ? C11 O2 C42 C41 -80.3(5) . . . . ? C11 O2 C42 C37 106.6(4) . . . . ? C39 N1 C43 O9 2.3(7) . . . . ? C39 N1 C43 C44 -174.8(4) . . . . ? O9 C43 C44 C45 -96.4(6) . . . . ? N1 C43 C44 C45 80.8(6) . . . . ? C40 N2 C46 O10 -5.9(8) . . . . ? C40 N2 C46 C47 174.5(5) . . . . ? O10 C46 C47 C48 -64.4(9) . . . . ? N2 C46 C47 C48 115.2(7) . . . . ? C13 O3 C49 C50 76.9(5) . . . . ? C13 O3 C49 C54 -108.5(4) . . . . ? O3 C49 C50 C51 174.5(4) . . . . ? C54 C49 C50 C51 0.0(6) . . . . ? C49 C50 C51 N3 176.1(4) . . . . ? C49 C50 C51 C52 -4.9(6) . . . . ? C55 N3 C51 C50 -22.9(7) . . . . ? C55 N3 C51 C52 158.1(4) . . . . ? C50 C51 C52 C53 4.7(6) . . . . ? N3 C51 C52 C53 -176.2(4) . . . . ? C50 C51 C52 N4 179.0(4) . . . . ? N3 C51 C52 N4 -1.9(6) . . . . ? C58 N4 C52 C53 -128.2(5) . . . . ? C58 N4 C52 C51 57.3(6) . . . . ? C51 C52 C53 C54 0.5(6) . . . . ? N4 C52 C53 C54 -174.3(4) . . . . ? C52 C53 C54 O4 175.1(4) . . . . ? C52 C53 C54 C49 -5.5(6) . . . . ? C20 O4 C54 C53 -88.5(4) . . . . ? C20 O4 C54 C49 92.2(4) . . . . ? O3 C49 C54 C53 -169.5(4) . . . . ? C50 C49 C54 C53 5.2(6) . . . . ? O3 C49 C54 O4 9.9(6) . . . . ? C50 C49 C54 O4 -175.4(4) . . . . ? C51 N3 C55 O11 5.8(8) . . . . ? C51 N3 C55 C56 -173.6(4) . . . . ? O11 C55 C56 C57 -174.2(5) . . . . ? N3 C55 C56 C57 5.2(6) . . . . ? C52 N4 C58 O12 -11.7(7) . . . . ? C52 N4 C58 C59 169.3(4) . . . . ? O12 C58 C59 C60 55.8(8) . . . . ? N4 C58 C59 C60 -125.2(7) . . . . ? C31 O7 C61 C62 77.5(5) . . . . ? C31 O7 C61 C66 -107.0(4) . . . . ? O7 C61 C62 C63 175.3(4) . . . . ? C66 C61 C62 C63 -0.1(7) . . . . ? C61 C62 C63 C64 -6.3(7) . . . . ? C61 C62 C63 N5 172.6(4) . . . . ? C67 N5 C63 C62 -22.0(8) . . . . ? C67 N5 C63 C64 156.9(6) . . . . ? C62 C63 C64 C65 7.3(7) . . . . ? N5 C63 C64 C65 -171.6(4) . . . . ? C62 C63 C64 N6 -172.6(4) . . . . ? N5 C63 C64 N6 8.5(7) . . . . ? C70 N6 C64 C65 -115.8(5) . . . . ? C70 N6 C64 C63 64.0(6) . . . . ? C63 C64 C65 C66 -1.8(7) . . . . ? N6 C64 C65 C66 178.0(4) . . . . ? C2 O8 C66 C65 -90.7(5) . . . . ? C2 O8 C66 C61 92.9(4) . . . . ? C64 C65 C66 O8 179.0(4) . . . . ? C64 C65 C66 C61 -4.6(6) . . . . ? C62 C61 C66 O8 -178.0(4) . . . . ? O7 C61 C66 O8 6.5(6) . . . . ? C62 C61 C66 C65 5.6(6) . . . . ? O7 C61 C66 C65 -170.0(4) . . . . ? C63 N5 C67 O13A 36.2(11) . . . . ? C63 N5 C67 O13B -26.9(10) . . . . ? C63 N5 C67 C68 -166.0(5) . . . . ? O13A C67 C68 C69 43.9(10) . . . . ? O13B C67 C68 C69 106.8(9) . . . . ? N5 C67 C68 C69 -113.5(8) . . . . ? C64 N6 C70 O14 -8.9(6) . . . . ? C64 N6 C70 C71 171.9(4) . . . . ? O14 C70 C71 C72 11.7(6) . . . . ? N6 C70 C71 C72 -169.1(4) . . . . ? C76' C75 C76 O15 -43.2(12) . . . . ? C76 C75 C76' O15' 62.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.111 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.103 data_ed50lt _database_code_depnum_ccdc_archive 'CCDC 278173' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H94 N8 O18' _chemical_formula_weight 1611.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.284(2) _cell_length_b 26.028(5) _cell_length_c 28.804(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.98(3) _cell_angle_gamma 90.00 _cell_volume 8448(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 6025 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.91 _exptl_crystal_description Plate-like _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9722 _exptl_absorpt_correction_T_max 0.9965 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1 _diffrn_reflns_number 49055 _diffrn_reflns_av_R_equivalents 0.1450 _diffrn_reflns_av_sigmaI/netI 0.1309 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 22.50 _reflns_number_total 11037 _reflns_number_gt 6393 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1600P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0074(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11037 _refine_ls_number_parameters 1050 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1956 _refine_ls_R_factor_gt 0.1293 _refine_ls_wR_factor_ref 0.3467 _refine_ls_wR_factor_gt 0.3080 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 1.063 _refine_ls_shift/su_mean 0.086 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2608(4) 0.08824(18) 1.05426(15) 0.0295(12) Uani 1 1 d . . . O2 O 0.0602(4) 0.10460(18) 0.99910(15) 0.0311(12) Uani 1 1 d . . . O3 O 0.0052(4) 0.20390(18) 0.85916(16) 0.0322(13) Uani 1 1 d . . . O4 O 0.1390(4) 0.2440(2) 0.79060(18) 0.0413(14) Uani 1 1 d . . . O5 O 0.5495(4) 0.2570(2) 0.75958(17) 0.0404(14) Uani 1 1 d . . . O6 O 0.7230(4) 0.2397(2) 0.80690(17) 0.0430(14) Uani 1 1 d . . . O7 O 0.7826(4) 0.19540(18) 0.96717(16) 0.0307(12) Uani 1 1 d . . . O8 O 0.6536(4) 0.15504(18) 1.03716(15) 0.0308(12) Uani 1 1 d . . . O9 O 0.3610(5) 0.2551(3) 1.1254(2) 0.077(2) Uani 1 1 d . . . O10 O -0.0690(5) 0.2384(2) 1.16018(18) 0.0505(16) Uani 1 1 d . . . O11 O -0.0086(5) 0.3063(2) 0.9986(2) 0.0559(17) Uani 1 1 d . . . O12 O 0.0377(8) 0.4549(3) 0.8925(3) 0.103(3) Uani 1 1 d . . . O13 O 0.6518(10) 0.3615(3) 0.9189(3) 0.116(3) Uani 1 1 d . . . O14 O 0.6134(7) 0.3975(3) 1.0840(2) 0.074(2) Uani 1 1 d . . . N1 N 0.1749(5) 0.2378(3) 1.1451(2) 0.0433(18) Uani 1 1 d . . . H1A H 0.1202 0.2440 1.1651 0.052 Uiso 1 1 calc R . . N2 N -0.0328(6) 0.2555(2) 1.0859(2) 0.0428(18) Uani 1 1 d . . . H2A H -0.0487 0.2761 1.0621 0.051 Uiso 1 1 calc R . . N3 N 0.0361(6) 0.3652(3) 0.9438(3) 0.056(2) Uani 1 1 d . . . H3A H 0.0405 0.3986 0.9390 0.067 Uiso 1 1 calc R . . N4 N 0.1863(8) 0.4026(3) 0.8723(3) 0.083(3) Uani 1 1 d . . . H4A H 0.2616 0.4024 0.8657 0.100 Uiso 1 1 calc R . . N5 N 1.0935(7) 0.4977(3) 0.6745(3) 0.065(2) Uani 1 1 d . . . N6 N 0.6390(6) 0.3661(3) 0.9972(3) 0.060(2) Uani 1 1 d . . . H6A H 0.6272 0.3875 1.0201 0.072 Uiso 1 1 calc R . . N7 N 0.5083(6) 0.3236(3) 1.0730(2) 0.051(2) Uani 1 1 d . . . H7A H 0.4406 0.3092 1.0795 0.061 Uiso 1 1 calc R . . C1 C 0.5656(6) 0.0989(3) 0.9776(2) 0.0281(18) Uani 1 1 d . . . C2 C 0.5557(6) 0.1269(3) 1.0188(2) 0.0256(17) Uani 1 1 d . . . C3 C 0.4542(6) 0.1229(3) 1.0441(2) 0.0265(18) Uani 1 1 d . . . H3B H 0.4512 0.1394 1.0735 0.032 Uiso 1 1 calc R . . C4 C 0.3594(5) 0.0954(2) 1.0268(2) 0.0222(17) Uani 1 1 d . . . C5 C 0.3599(6) 0.0700(3) 0.9838(2) 0.0259(17) Uani 1 1 d . . . C6 C 0.4648(6) 0.0726(3) 0.9609(2) 0.0301(18) Uani 1 1 d . . . H6B H 0.4680 0.0555 0.9319 0.036 Uiso 1 1 calc R . . C7 C 0.2469(6) 0.0453(3) 0.9633(2) 0.0276(18) Uani 1 1 d . . . H7B H 0.1972 0.0362 0.9899 0.033 Uiso 1 1 calc R . . C8 C 0.2693(6) -0.0048(3) 0.9367(2) 0.0319(19) Uani 1 1 d . . . H8A H 0.3263 -0.0263 0.9554 0.038 Uiso 1 1 calc R . . H8B H 0.3054 0.0036 0.9071 0.038 Uiso 1 1 calc R . . C9 C 0.1544(7) -0.0353(3) 0.9265(3) 0.049(2) Uani 1 1 d . . . H9A H 0.1737 -0.0689 0.9134 0.059 Uiso 1 1 calc R . . H9B H 0.1025 -0.0163 0.9043 0.059 Uiso 1 1 calc R . . H9C H 0.1138 -0.0404 0.9554 0.059 Uiso 1 1 calc R . . C10 C 0.1785(6) 0.0852(2) 0.9344(2) 0.0260(18) Uani 1 1 d . . . C11 C 0.0945(6) 0.1164(3) 0.9542(2) 0.0264(18) Uani 1 1 d . . . C12 C 0.0405(6) 0.1565(3) 0.9302(3) 0.0314(19) Uani 1 1 d . . . H12A H -0.0127 0.1785 0.9451 0.038 Uiso 1 1 calc R . . C13 C 0.0639(6) 0.1643(3) 0.8847(2) 0.0291(18) Uani 1 1 d . . . C14 C 0.1392(6) 0.1318(3) 0.8611(2) 0.0296(18) Uani 1 1 d . . . C15 C 0.1965(6) 0.0937(3) 0.8875(2) 0.0261(17) Uani 1 1 d . . . H15A H 0.2511 0.0722 0.8727 0.031 Uiso 1 1 calc R . . C16 C 0.1515(6) 0.1366(3) 0.8094(2) 0.037(2) Uani 1 1 d . . . H16A H 0.0801 0.1559 0.7969 0.044 Uiso 1 1 calc R . . C17 C 0.1493(7) 0.0849(3) 0.7850(3) 0.048(2) Uani 1 1 d . . . H17A H 0.2138 0.0631 0.7988 0.057 Uiso 1 1 calc R . . H17B H 0.1640 0.0901 0.7518 0.057 Uiso 1 1 calc R . . C18 C 0.0309(10) 0.0574(5) 0.7891(4) 0.094(4) Uani 1 1 d . . . H18A H 0.0318 0.0250 0.7717 0.113 Uiso 1 1 calc R . . H18B H -0.0335 0.0792 0.7763 0.113 Uiso 1 1 calc R . . H18C H 0.0185 0.0501 0.8219 0.113 Uiso 1 1 calc R . . C19 C 0.2604(6) 0.1689(3) 0.7978(2) 0.0332(19) Uani 1 1 d . . . C20 C 0.2497(6) 0.2204(3) 0.7902(2) 0.036(2) Uani 1 1 d . . . C21 C 0.3486(7) 0.2497(3) 0.7782(2) 0.041(2) Uani 1 1 d . . . H21A H 0.3400 0.2855 0.7724 0.049 Uiso 1 1 calc R . . C22 C 0.4564(7) 0.2269(3) 0.7748(3) 0.037(2) Uani 1 1 d . . . C23 C 0.4713(6) 0.1744(3) 0.7840(3) 0.038(2) Uani 1 1 d . . . C24 C 0.3722(6) 0.1473(3) 0.7958(2) 0.0298(19) Uani 1 1 d . . . H24A H 0.3812 0.1118 0.8029 0.036 Uiso 1 1 calc R . . C25 C 0.5934(7) 0.1501(3) 0.7844(2) 0.040(2) Uani 1 1 d . B . H25A H 0.6410 0.1701 0.7624 0.048 Uiso 1 1 calc R . . C26 C 0.5953(8) 0.0928(3) 0.7685(3) 0.049(2) Uani 1 1 d . . . H26A H 0.5530 0.0720 0.7911 0.059 Uiso 1 1 calc R A 1 H26B H 0.5508 0.0900 0.7381 0.059 Uiso 1 1 calc R A 1 C27A C 0.7148(12) 0.0707(6) 0.7641(5) 0.050(4) Uani 0.60 1 d P B 1 H27A H 0.7074 0.0354 0.7526 0.060 Uiso 0.60 1 calc PR B 1 H27B H 0.7579 0.0708 0.7945 0.060 Uiso 0.60 1 calc PR B 1 H27C H 0.7584 0.0913 0.7421 0.060 Uiso 0.60 1 calc PR B 1 C27B C 0.558(2) 0.0887(12) 0.7146(8) 0.084(9) Uani 0.40 1 d P B 2 H27D H 0.5780 0.0544 0.7033 0.100 Uiso 0.40 1 calc PR B 2 H27E H 0.6013 0.1146 0.6974 0.100 Uiso 0.40 1 calc PR B 2 H27F H 0.4727 0.0945 0.7098 0.100 Uiso 0.40 1 calc PR B 2 C28 C 0.6483(6) 0.1587(3) 0.8323(2) 0.0310(19) Uani 1 1 d . . . C29 C 0.7016(6) 0.2062(3) 0.8430(2) 0.035(2) Uani 1 1 d . B . C30 C 0.7432(6) 0.2187(3) 0.8873(3) 0.037(2) Uani 1 1 d . . . H30A H 0.7781 0.2514 0.8936 0.044 Uiso 1 1 calc R B . C31 C 0.7334(6) 0.1832(3) 0.9222(2) 0.0283(18) Uani 1 1 d . B . C32 C 0.6855(5) 0.1353(3) 0.9147(2) 0.0273(18) Uani 1 1 d . . . C33 C 0.6408(6) 0.1244(3) 0.8689(3) 0.037(2) Uani 1 1 d . B . H33A H 0.6038 0.0921 0.8630 0.044 Uiso 1 1 calc R . . C34 C 0.6816(6) 0.0965(3) 0.9534(2) 0.0270(18) Uani 1 1 d . B . H34A H 0.7457 0.1062 0.9771 0.032 Uiso 1 1 calc R . . C35 C 0.7099(6) 0.0418(3) 0.9371(3) 0.0320(19) Uani 1 1 d . . . H35A H 0.6952 0.0174 0.9625 0.038 Uiso 1 1 calc R B . H35B H 0.6554 0.0329 0.9102 0.038 Uiso 1 1 calc R . . C36 C 0.8383(6) 0.0357(3) 0.9230(3) 0.043(2) Uani 1 1 d . B . H36A H 0.8521 -0.0001 0.9142 0.052 Uiso 1 1 calc R . . H36B H 0.8928 0.0450 0.9492 0.052 Uiso 1 1 calc R . . H36C H 0.8520 0.0582 0.8965 0.052 Uiso 1 1 calc R . . C37 C 0.1900(6) 0.1312(3) 1.0618(2) 0.0304(19) Uani 1 1 d . . . C38 C 0.2186(6) 0.1633(3) 1.0988(3) 0.036(2) Uani 1 1 d . . . H38A H 0.2870 0.1568 1.1185 0.043 Uiso 1 1 calc R . . C39 C 0.1462(6) 0.2055(3) 1.1069(2) 0.035(2) Uani 1 1 d . . . C40 C 0.0443(7) 0.2131(3) 1.0792(3) 0.039(2) Uani 1 1 d . . . C41 C 0.0154(6) 0.1789(3) 1.0431(2) 0.038(2) Uani 1 1 d . . . H41A H -0.0563 0.1833 1.0248 0.046 Uiso 1 1 calc R . . C42 C 0.0899(6) 0.1390(3) 1.0338(2) 0.0330(19) Uani 1 1 d . . . C43 C 0.0526(6) 0.2531(3) 0.8646(3) 0.036(2) Uani 1 1 d . . . C44 C 0.0257(7) 0.2827(3) 0.9021(3) 0.040(2) Uani 1 1 d . . . H44A H -0.0201 0.2684 0.9256 0.048 Uiso 1 1 calc R . . C45 C 0.0640(7) 0.3331(3) 0.9062(3) 0.046(2) Uani 1 1 d . . . C46 C 0.1298(8) 0.3533(3) 0.8712(3) 0.050(2) Uani 1 1 d . . . C47 C 0.1551(7) 0.3232(3) 0.8336(3) 0.049(2) Uani 1 1 d . . . H47A H 0.2001 0.3376 0.8098 0.059 Uiso 1 1 calc R . . C48 C 0.1176(7) 0.2730(3) 0.8293(3) 0.037(2) Uani 1 1 d . . . C49 C 0.6330(7) 0.2769(3) 0.7943(3) 0.047(2) Uani 1 1 d . . . H49A H 0.5912 0.2880 0.8224 0.057 Uiso 1 1 calc R . . C50 C 0.6985(8) 0.3209(3) 0.7748(3) 0.049(2) Uani 1 1 d . . . C51 C 0.6620(8) 0.3467(3) 0.7351(3) 0.054(3) Uani 1 1 d . . . H51A H 0.5873 0.3387 0.7201 0.065 Uiso 1 1 calc R . . C52 C 0.7324(8) 0.3842(4) 0.7164(3) 0.056(3) Uani 1 1 d . . . H52A H 0.7058 0.4012 0.6886 0.067 Uiso 1 1 calc R . . C53 C 0.8389(7) 0.3970(3) 0.7372(3) 0.047(2) Uani 1 1 d . . . C54 C 0.8743(9) 0.3737(4) 0.7779(3) 0.078(3) Uani 1 1 d . . . H54A H 0.9471 0.3835 0.7934 0.093 Uiso 1 1 calc R . . C55 C 0.8059(9) 0.3358(4) 0.7970(4) 0.089(4) Uani 1 1 d . . . H55A H 0.8321 0.3199 0.8254 0.107 Uiso 1 1 calc R . . C56 C 0.9226(7) 0.4341(3) 0.7157(3) 0.043(2) Uani 1 1 d . . . C57 C 0.9190(8) 0.4449(3) 0.6684(3) 0.053(2) Uani 1 1 d . . . H57A H 0.8564 0.4320 0.6483 0.063 Uiso 1 1 calc R . . C58 C 1.0058(8) 0.4739(3) 0.6513(3) 0.053(2) Uani 1 1 d . . . H58A H 1.0035 0.4777 0.6185 0.063 Uiso 1 1 calc R . . C59 C 1.0947(9) 0.4882(4) 0.7199(4) 0.074(3) Uani 1 1 d . . . H59A H 1.1561 0.5039 0.7386 0.089 Uiso 1 1 calc R . . C60 C 1.0137(9) 0.4569(4) 0.7431(3) 0.068(3) Uani 1 1 d . . . H60A H 1.0211 0.4517 0.7758 0.081 Uiso 1 1 calc R . . C61 C 0.7126(6) 0.2287(3) 0.9931(3) 0.0321(19) Uani 1 1 d . . . C62 C 0.7122(7) 0.2797(3) 0.9840(3) 0.041(2) Uani 1 1 d . . . H62A H 0.7587 0.2927 0.9600 0.049 Uiso 1 1 calc R . . C63 C 0.6450(7) 0.3130(3) 1.0090(3) 0.041(2) Uani 1 1 d . . . C64 C 0.5819(6) 0.2930(3) 1.0453(3) 0.039(2) Uani 1 1 d . . . C65 C 0.5857(7) 0.2408(3) 1.0548(3) 0.039(2) Uani 1 1 d . . . H65A H 0.5450 0.2276 1.0803 0.047 Uiso 1 1 calc R . . C66 C 0.6481(6) 0.2079(3) 1.0276(2) 0.0310(19) Uani 1 1 d . . . C67 C 0.2827(8) 0.2598(4) 1.1523(3) 0.053(2) Uani 1 1 d . . . C68 C 0.2991(7) 0.2904(4) 1.1969(3) 0.057(3) Uani 1 1 d . . . H68A H 0.2872 0.3273 1.1898 0.069 Uiso 1 1 calc R . . H68B H 0.2378 0.2800 1.2184 0.069 Uiso 1 1 calc R . . C69 C 0.4180(8) 0.2833(5) 1.2203(4) 0.092(4) Uani 1 1 d . . . H69A H 0.4225 0.3025 1.2496 0.110 Uiso 1 1 calc R . . H69B H 0.4789 0.2960 1.2001 0.110 Uiso 1 1 calc R . . H69C H 0.4313 0.2467 1.2267 0.110 Uiso 1 1 calc R . . C70 C -0.0832(7) 0.2662(3) 1.1262(3) 0.042(2) Uani 1 1 d . . . C71 C -0.1573(7) 0.3150(4) 1.1265(3) 0.053(2) Uani 1 1 d . . . H71A H -0.1040 0.3448 1.1319 0.064 Uiso 1 1 calc R . . H71B H -0.1985 0.3194 1.0956 0.064 Uiso 1 1 calc R . . C72 C -0.2463(9) 0.3146(5) 1.1622(4) 0.090(4) Uani 1 1 d . . . H72A H -0.2799 0.3491 1.1651 0.107 Uiso 1 1 calc R . . H72B H -0.2084 0.3042 1.1921 0.107 Uiso 1 1 calc R . . H72C H -0.3097 0.2903 1.1532 0.107 Uiso 1 1 calc R . . C73 C 0.0032(8) 0.3500(4) 0.9866(4) 0.058(3) Uani 1 1 d . D . C74 C -0.0250(9) 0.3947(4) 1.0188(4) 0.073(3) Uani 1 1 d . . . H74A H -0.1120 0.3947 1.0221 0.088 Uiso 1 1 calc R C 1 H74B H 0.0121 0.3867 1.0499 0.088 Uiso 1 1 calc R C 1 C75A C 0.010(2) 0.4472(8) 1.0071(8) 0.110(8) Uani 0.60 1 d P D 1 H75A H -0.0604 0.4663 0.9952 0.132 Uiso 0.60 1 calc PR D 1 H75B H 0.0686 0.4462 0.9833 0.132 Uiso 0.60 1 calc PR D 1 H75C H 0.0440 0.4643 1.0350 0.132 Uiso 0.60 1 calc PR D 1 C75B C 0.071(2) 0.3993(11) 1.0575(10) 0.118(12) Uani 0.40 1 d P D 2 H75D H 0.1467 0.4071 1.0441 0.142 Uiso 0.40 1 calc PR D 2 H75E H 0.0771 0.3669 1.0746 0.142 Uiso 0.40 1 calc PR D 2 H75F H 0.0500 0.4270 1.0786 0.142 Uiso 0.40 1 calc PR D 2 C76 C 0.1423(11) 0.4485(5) 0.8817(5) 0.093(4) Uani 1 1 d . . . C77 C 0.2209(12) 0.4938(4) 0.8771(6) 0.136(6) Uani 1 1 d . . . H77A H 0.2524 0.5041 0.9085 0.163 Uiso 1 1 calc R . . H77B H 0.2891 0.4838 0.8589 0.163 Uiso 1 1 calc R . . C78 C 0.1624(16) 0.5377(6) 0.8549(6) 0.155(7) Uani 1 1 d . . . H78A H 0.2223 0.5618 0.8445 0.186 Uiso 1 1 calc R . . H78B H 0.1128 0.5549 0.8772 0.186 Uiso 1 1 calc R . . H78C H 0.1126 0.5261 0.8281 0.186 Uiso 1 1 calc R . . C79 C 0.6494(13) 0.3877(4) 0.9544(4) 0.092(4) Uani 1 1 d . F . C80 C 0.6445(16) 0.4446(5) 0.9535(6) 0.133(6) Uani 1 1 d . . . H80A H 0.5629 0.4556 0.9439 0.159 Uiso 1 1 calc R E 1 H80B H 0.6630 0.4578 0.9853 0.159 Uiso 1 1 calc R E 1 C81A C 0.730(3) 0.4674(13) 0.9211(12) 0.206(15) Uiso 0.60 1 d P F 1 H81A H 0.7241 0.5050 0.9222 0.247 Uiso 0.75 1 calc PR F 1 H81B H 0.7097 0.4555 0.8893 0.247 Uiso 0.75 1 calc PR F 1 H81C H 0.8106 0.4568 0.9305 0.247 Uiso 0.75 1 calc PR F 1 C81B C 0.652(5) 0.475(2) 0.995(2) 0.21(2) Uiso 0.40 1 d P F 2 H81D H 0.5725 0.4847 1.0034 0.250 Uiso 0.25 1 calc PR F 2 H81E H 0.6980 0.5065 0.9890 0.250 Uiso 0.25 1 calc PR F 2 H81F H 0.6923 0.4556 1.0200 0.250 Uiso 0.25 1 calc PR F 2 C82 C 0.5257(9) 0.3722(4) 1.0914(3) 0.058(3) Uani 1 1 d . . . C83 C 0.4332(11) 0.3906(5) 1.1205(5) 0.105(4) Uani 1 1 d . . . H83A H 0.3635 0.3999 1.0999 0.126 Uiso 1 1 calc R . . H83B H 0.4090 0.3617 1.1402 0.126 Uiso 1 1 calc R . . C84 C 0.4601(18) 0.4336(6) 1.1504(6) 0.188(8) Uani 1 1 d . . . H84A H 0.3877 0.4450 1.1647 0.226 Uiso 1 1 calc R . . H84B H 0.4918 0.4618 1.1322 0.226 Uiso 1 1 calc R . . H84C H 0.5193 0.4233 1.1748 0.226 Uiso 1 1 calc R . . O15 O 0.2324(14) 0.3201(6) 1.0502(5) 0.238(6) Uiso 1 1 d D . . O16 O 0.4106(15) 0.3980(6) 0.9254(6) 0.264(7) Uiso 1 1 d D . . N8 N 0.3097(9) 0.3884(4) 1.0020(4) 0.107(3) Uiso 1 1 d . . . H8C H 0.3006 0.4184 1.0153 0.128 Uiso 1 1 calc R . . C85 C 0.3617(8) 0.3194(4) 0.9484(3) 0.065(3) Uiso 1 1 d D . . C86 C 0.4038(10) 0.2885(5) 0.9145(4) 0.086(3) Uiso 1 1 d . . . H86A H 0.4406 0.3036 0.8889 0.103 Uiso 1 1 calc R . . C87 C 0.3938(10) 0.2370(4) 0.9169(4) 0.082(3) Uiso 1 1 d . . . H87A H 0.4251 0.2167 0.8931 0.099 Uiso 1 1 calc R . . C88 C 0.3433(9) 0.2143(5) 0.9506(4) 0.078(3) Uiso 1 1 d . . . H88A H 0.3387 0.1778 0.9511 0.094 Uiso 1 1 calc R . . C89 C 0.2962(9) 0.2424(4) 0.9857(4) 0.076(3) Uiso 1 1 d . . . H89A H 0.2584 0.2256 1.0102 0.091 Uiso 1 1 calc R . . C90 C 0.3046(9) 0.2975(4) 0.9850(4) 0.069(3) Uiso 1 1 d D . . C91 C 0.2763(16) 0.3450(7) 1.0173(6) 0.166(7) Uiso 1 1 d D . . C92 C 0.362(2) 0.3797(7) 0.9608(7) 0.228(10) Uiso 1 1 d D . . O17 O 0.1602(9) 0.8492(4) 0.7990(4) 0.041(3) Uiso 0.50 1 d P . . H17C H 0.1530 0.8738 0.7802 0.050 Uiso 0.50 1 calc PR . . C93 C 0.2759(15) 0.8587(7) 0.8343(6) 0.052(5) Uiso 0.50 1 d P . . H93A H 0.2979 0.8955 0.8348 0.062 Uiso 0.50 1 calc PR . . H93B H 0.2585 0.8481 0.8663 0.062 Uiso 0.50 1 calc PR . . C94 C 0.3642(17) 0.8304(8) 0.8187(7) 0.067(6) Uiso 0.50 1 d P . . H94A H 0.4387 0.8395 0.8357 0.081 Uiso 0.50 1 calc PR . . H94B H 0.3714 0.8370 0.7855 0.081 Uiso 0.50 1 calc PR . . H94C H 0.3472 0.7939 0.8235 0.081 Uiso 0.50 1 calc PR . . O18 O 0.4441(14) 0.3968(6) 0.8550(6) 0.096(5) Uiso 0.50 1 d P G 1 O20 O 0.090(3) 0.9149(11) 0.7387(11) 0.083(8) Uiso 0.25 1 d P H 1 O19 O 0.3801(18) 0.4047(8) 0.8023(8) 0.133(7) Uiso 0.50 1 d P I 2 O21 O 0.602(2) 0.4158(11) 0.8386(10) 0.081(8) Uiso 0.25 1 d P J 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 O1 0.030(3) 0.036(3) 0.024(3) 0.005(2) 0.009(2) 0.004(2) O2 0.035(3) 0.037(3) 0.021(3) -0.004(2) 0.004(2) -0.002(2) O3 0.032(3) 0.038(3) 0.026(3) 0.008(2) 0.000(2) 0.001(2) O4 0.034(3) 0.049(3) 0.041(3) 0.016(3) -0.002(2) -0.001(3) O5 0.032(3) 0.054(4) 0.035(3) 0.011(3) 0.003(2) -0.006(3) O6 0.037(3) 0.060(4) 0.034(3) 0.020(3) 0.013(2) -0.003(3) O7 0.031(3) 0.036(3) 0.025(3) 0.000(2) 0.003(2) -0.002(2) O8 0.032(3) 0.036(3) 0.024(3) 0.012(2) 0.000(2) 0.001(2) O9 0.056(4) 0.106(5) 0.074(4) -0.050(4) 0.048(3) -0.030(4) O10 0.042(3) 0.080(4) 0.030(3) 0.000(3) 0.008(3) 0.017(3) O11 0.066(4) 0.048(4) 0.054(4) -0.003(3) 0.006(3) 0.001(3) O12 0.112(6) 0.045(4) 0.158(8) 0.021(5) 0.045(6) 0.004(4) O13 0.224(10) 0.067(5) 0.059(5) 0.016(4) 0.030(6) 0.010(6) O14 0.091(5) 0.062(5) 0.068(5) -0.014(4) 0.007(4) -0.009(4) N1 0.034(4) 0.066(5) 0.031(4) -0.013(3) 0.006(3) 0.000(3) N2 0.054(4) 0.045(4) 0.029(4) 0.002(3) -0.001(3) 0.014(3) N3 0.063(5) 0.040(4) 0.064(5) -0.007(4) -0.001(4) -0.009(4) N4 0.078(6) 0.034(5) 0.140(9) -0.005(5) 0.038(6) 0.004(4) N5 0.071(5) 0.071(6) 0.055(5) -0.007(4) 0.016(4) -0.023(5) N6 0.069(5) 0.040(5) 0.072(6) 0.001(4) 0.011(4) 0.002(4) N7 0.051(4) 0.047(5) 0.056(5) -0.016(4) 0.014(4) -0.004(4) C1 0.025(4) 0.031(4) 0.028(4) 0.008(3) 0.002(3) 0.014(3) C2 0.033(4) 0.021(4) 0.022(4) 0.007(3) -0.008(3) 0.004(3) C3 0.035(4) 0.033(4) 0.012(4) 0.006(3) 0.010(3) 0.014(4) C4 0.020(4) 0.022(4) 0.024(4) 0.003(3) 0.001(3) 0.006(3) C5 0.033(4) 0.025(4) 0.020(4) 0.006(3) -0.002(3) 0.006(3) C6 0.032(4) 0.030(4) 0.029(4) 0.001(3) 0.011(3) 0.004(3) C7 0.027(4) 0.033(4) 0.024(4) 0.001(3) 0.012(3) 0.000(3) C8 0.037(4) 0.033(4) 0.026(4) -0.002(3) 0.010(3) 0.005(4) C9 0.046(5) 0.042(5) 0.060(6) -0.011(4) 0.014(4) 0.003(4) C10 0.032(4) 0.014(4) 0.031(4) 0.005(3) 0.001(3) -0.005(3) C11 0.029(4) 0.035(4) 0.016(4) 0.002(3) 0.010(3) -0.005(3) C12 0.028(4) 0.031(4) 0.035(5) -0.003(4) 0.003(3) -0.002(3) C13 0.027(4) 0.037(5) 0.024(4) 0.000(3) -0.001(3) -0.011(4) C14 0.018(3) 0.046(5) 0.025(4) -0.004(4) 0.006(3) -0.008(3) C15 0.022(4) 0.031(4) 0.025(4) 0.004(3) 0.000(3) 0.005(3) C16 0.028(4) 0.057(5) 0.025(4) 0.003(4) -0.004(3) -0.007(4) C17 0.053(5) 0.051(6) 0.038(5) -0.014(4) 0.001(4) -0.021(4) C18 0.109(9) 0.119(10) 0.054(7) -0.018(6) 0.007(6) -0.043(8) C19 0.038(4) 0.049(5) 0.011(4) 0.012(3) 0.000(3) -0.009(4) C20 0.029(4) 0.052(5) 0.026(4) 0.007(4) 0.001(3) 0.001(4) C21 0.049(5) 0.051(5) 0.022(4) 0.008(4) -0.004(4) 0.000(4) C22 0.035(4) 0.046(5) 0.029(4) 0.012(4) 0.005(3) -0.009(4) C23 0.031(4) 0.056(6) 0.029(4) -0.004(4) 0.007(3) -0.003(4) C24 0.030(4) 0.038(5) 0.020(4) 0.004(3) -0.002(3) 0.005(4) C25 0.049(5) 0.050(5) 0.023(4) 0.008(4) 0.015(4) -0.010(4) C26 0.062(6) 0.052(6) 0.034(5) -0.006(4) 0.009(4) 0.003(5) C27A 0.054(9) 0.062(10) 0.033(8) -0.005(7) 0.012(7) 0.011(8) C27B 0.085(19) 0.14(3) 0.029(14) -0.013(15) 0.002(13) 0.013(18) C28 0.025(4) 0.042(5) 0.027(4) -0.002(4) 0.013(3) -0.004(4) C29 0.030(4) 0.053(5) 0.024(4) 0.015(4) 0.006(3) 0.007(4) C30 0.025(4) 0.040(5) 0.045(5) 0.005(4) 0.009(4) -0.006(4) C31 0.019(3) 0.039(5) 0.027(4) 0.010(4) 0.006(3) -0.002(3) C32 0.014(3) 0.031(4) 0.038(5) -0.001(3) 0.012(3) 0.003(3) C33 0.026(4) 0.052(5) 0.032(5) 0.007(4) 0.011(3) 0.001(4) C34 0.023(4) 0.031(4) 0.028(4) 0.000(3) 0.007(3) 0.006(3) C35 0.029(4) 0.040(5) 0.029(4) 0.003(3) 0.011(3) 0.007(4) C36 0.039(4) 0.047(5) 0.045(5) 0.004(4) 0.009(4) 0.011(4) C37 0.033(4) 0.036(5) 0.022(4) 0.006(3) 0.001(3) 0.006(4) C38 0.034(4) 0.047(5) 0.027(4) 0.000(4) 0.001(3) 0.003(4) C39 0.032(4) 0.048(5) 0.024(4) -0.004(4) 0.003(3) 0.003(4) C40 0.035(4) 0.044(5) 0.037(5) -0.007(4) 0.004(4) 0.013(4) C41 0.034(4) 0.054(5) 0.026(4) -0.013(4) -0.001(3) 0.008(4) C42 0.039(4) 0.042(5) 0.019(4) -0.005(4) 0.009(3) -0.005(4) C43 0.027(4) 0.036(5) 0.045(5) 0.002(4) -0.005(4) 0.000(4) C44 0.039(4) 0.039(5) 0.042(5) 0.005(4) -0.010(4) -0.003(4) C45 0.045(5) 0.039(5) 0.054(6) -0.006(4) -0.010(4) 0.003(4) C46 0.053(5) 0.025(5) 0.070(7) -0.001(4) -0.004(5) -0.002(4) C47 0.046(5) 0.045(6) 0.056(6) 0.021(5) 0.004(4) 0.000(4) C48 0.035(4) 0.033(5) 0.041(5) 0.004(4) -0.003(4) 0.006(4) C49 0.055(5) 0.041(5) 0.048(5) 0.009(4) 0.020(4) 0.002(4) C50 0.055(5) 0.053(6) 0.040(5) 0.009(4) 0.008(4) -0.005(5) C51 0.059(5) 0.062(6) 0.042(6) 0.008(5) 0.002(4) -0.016(5) C52 0.060(6) 0.076(7) 0.033(5) 0.014(5) -0.001(4) -0.016(5) C53 0.049(5) 0.055(6) 0.036(5) 0.009(4) 0.003(4) -0.001(4) C54 0.068(6) 0.094(8) 0.069(7) 0.035(6) -0.020(5) -0.041(6) C55 0.087(7) 0.098(8) 0.079(8) 0.048(6) -0.039(6) -0.039(7) C56 0.049(5) 0.030(5) 0.051(6) 0.005(4) 0.009(4) -0.001(4) C57 0.050(5) 0.060(6) 0.049(6) 0.006(5) 0.006(4) 0.001(5) C58 0.054(5) 0.058(6) 0.048(6) 0.014(5) 0.025(5) 0.001(5) C59 0.071(7) 0.078(8) 0.073(8) -0.001(6) 0.011(6) -0.026(6) C60 0.075(7) 0.085(7) 0.043(6) 0.003(5) 0.010(5) -0.027(6) C61 0.023(4) 0.041(5) 0.032(4) -0.001(4) -0.001(3) 0.004(4) C62 0.038(4) 0.045(5) 0.040(5) -0.004(4) 0.005(4) -0.003(4) C63 0.045(5) 0.033(5) 0.043(5) 0.005(4) -0.004(4) -0.011(4) C64 0.028(4) 0.041(5) 0.049(5) -0.007(4) 0.006(4) 0.004(4) C65 0.039(4) 0.044(5) 0.035(5) -0.004(4) -0.002(4) -0.006(4) C66 0.025(4) 0.043(5) 0.025(4) 0.002(4) -0.006(3) -0.002(4) C67 0.044(5) 0.066(6) 0.049(6) -0.014(5) 0.012(4) -0.006(5) C68 0.044(5) 0.073(7) 0.056(6) -0.033(5) 0.012(4) -0.009(5) C69 0.046(6) 0.131(10) 0.096(9) -0.061(7) -0.018(6) 0.004(6) C70 0.044(5) 0.051(5) 0.030(5) -0.011(4) -0.003(4) 0.013(4) C71 0.043(5) 0.066(6) 0.050(6) -0.014(5) 0.001(4) 0.015(5) C72 0.083(7) 0.126(10) 0.062(7) 0.011(6) 0.022(6) 0.054(7) C73 0.039(5) 0.060(7) 0.075(7) 0.001(6) 0.006(5) -0.001(5) C74 0.077(7) 0.072(7) 0.072(7) -0.033(6) 0.014(6) -0.002(6) C75A 0.137(19) 0.093(17) 0.102(18) -0.009(13) 0.024(15) -0.014(15) C75B 0.094(19) 0.14(2) 0.13(2) -0.13(2) 0.050(17) -0.082(18) C76 0.075(8) 0.071(9) 0.136(11) 0.003(7) 0.030(8) -0.006(7) C77 0.115(11) 0.037(7) 0.26(2) 0.000(9) 0.032(12) -0.020(7) C78 0.219(18) 0.091(11) 0.154(15) 0.004(10) 0.001(13) -0.055(12) C79 0.172(13) 0.036(7) 0.068(8) 0.009(6) -0.002(8) 0.005(7) C80 0.208(17) 0.059(9) 0.134(13) 0.024(8) 0.031(12) 0.014(9) C82 0.068(6) 0.049(6) 0.057(6) -0.019(5) 0.017(5) -0.010(5) C83 0.091(8) 0.091(9) 0.136(11) -0.050(8) 0.048(8) 0.002(7) C84 0.228(19) 0.155(15) 0.190(17) -0.097(13) 0.089(15) -0.013(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C37 1.398(8) . ? O1 C4 1.411(8) . ? O2 C42 1.371(8) . ? O2 C11 1.403(8) . ? O3 C43 1.394(9) . ? O3 C13 1.411(8) . ? O4 C48 1.380(9) . ? O4 C20 1.392(9) . ? O5 C22 1.399(9) . ? O5 C49 1.435(10) . ? O6 C29 1.387(8) . ? O6 C49 1.437(9) . ? O7 C61 1.412(8) . ? O7 C31 1.419(8) . ? O8 C2 1.406(8) . ? O8 C66 1.404(9) . ? O9 C67 1.213(10) . ? O10 C70 1.222(9) . ? O11 C73 1.199(11) . ? O12 C76 1.247(13) . ? O13 C79 1.231(12) . ? O14 C82 1.216(11) . ? N1 C67 1.350(10) . ? N1 C39 1.409(9) . ? N2 C70 1.350(10) . ? N2 C40 1.425(9) . ? N3 C73 1.363(12) . ? N3 C45 1.417(11) . ? N4 C76 1.329(13) . ? N4 C46 1.432(11) . ? N5 C58 1.320(11) . ? N5 C59 1.329(12) . ? N6 C79 1.366(13) . ? N6 C63 1.425(10) . ? N7 C82 1.382(11) . ? N7 C64 1.426(10) . ? C1 C6 1.391(10) . ? C1 C2 1.403(10) . ? C1 C34 1.516(9) . ? C2 C3 1.392(9) . ? C3 C4 1.360(9) . ? C4 C5 1.403(9) . ? C5 C6 1.387(10) . ? C5 C7 1.521(9) . ? C7 C10 1.515(9) . ? C7 C8 1.538(10) . ? C8 C9 1.536(10) . ? C10 C15 1.394(9) . ? C10 C11 1.393(9) . ? C11 C12 1.376(10) . ? C12 C13 1.364(10) . ? C13 C14 1.400(10) . ? C14 C15 1.388(10) . ? C14 C16 1.509(10) . ? C16 C17 1.516(11) . ? C16 C19 1.540(10) . ? C17 C18 1.526(13) . ? C19 C20 1.364(11) . ? C19 C24 1.385(10) . ? C20 C21 1.409(11) . ? C21 C22 1.362(11) . ? C22 C23 1.402(11) . ? C23 C24 1.379(10) . ? C23 C25 1.516(11) . ? C25 C28 1.499(10) . ? C25 C26 1.559(11) . ? C26 C27A 1.478(15) . ? C26 C27B 1.59(2) . ? C28 C33 1.389(10) . ? C28 C29 1.404(10) . ? C29 C30 1.374(10) . ? C30 C31 1.375(10) . ? C31 C32 1.371(10) . ? C32 C33 1.416(10) . ? C32 C34 1.506(10) . ? C34 C35 1.538(10) . ? C35 C36 1.534(10) . ? C37 C42 1.368(10) . ? C37 C38 1.379(10) . ? C38 C39 1.395(10) . ? C39 C40 1.381(10) . ? C40 C41 1.394(10) . ? C41 C42 1.371(10) . ? C43 C44 1.374(11) . ? C43 C48 1.383(11) . ? C44 C45 1.383(11) . ? C45 C46 1.386(12) . ? C46 C47 1.379(12) . ? C47 C48 1.376(11) . ? C49 C50 1.487(11) . ? C50 C51 1.371(11) . ? C50 C55 1.396(13) . ? C51 C52 1.386(12) . ? C52 C53 1.356(11) . ? C53 C54 1.361(12) . ? C53 C56 1.507(11) . ? C54 C55 1.384(13) . ? C56 C57 1.391(11) . ? C56 C60 1.395(12) . ? C57 C58 1.349(11) . ? C59 C60 1.417(13) . ? C61 C62 1.352(11) . ? C61 C66 1.374(10) . ? C62 C63 1.381(11) . ? C63 C64 1.394(11) . ? C64 C65 1.386(11) . ? C65 C66 1.377(10) . ? C67 C68 1.515(12) . ? C68 C69 1.482(12) . ? C70 C71 1.520(11) . ? C71 C72 1.474(12) . ? C73 C74 1.532(13) . ? C74 C75A 1.47(2) . ? C74 C75B 1.51(3) . ? C76 C77 1.486(16) . ? C77 C78 1.451(19) . ? C79 C80 1.481(15) . ? C80 C81A 1.50(3) . ? C80 C81B 1.43(6) . ? C82 C83 1.454(13) . ? C83 C84 1.434(18) . ? O15 C91 1.270(14) . ? O16 C92 1.274(15) . ? N8 C91 1.277(17) . ? N8 C92 1.37(2) . ? C85 C86 1.370(14) . ? C85 C90 1.387(13) . ? C85 C92 1.61(2) . ? C86 C87 1.346(15) . ? C87 C88 1.293(14) . ? C88 C89 1.379(14) . ? C89 C90 1.436(14) . ? C90 C91 1.589(17) . ? O17 C93 1.632(19) . ? C93 C94 1.34(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 C37 O1 C4 117.0(5) . . ? C42 O2 C11 117.5(5) . . ? C43 O3 C13 116.4(5) . . ? C48 O4 C20 116.3(5) . . ? C22 O5 C49 117.4(6) . . ? C29 O6 C49 117.7(5) . . ? C61 O7 C31 114.7(5) . . ? C2 O8 C66 114.3(5) . . ? C67 N1 C39 122.8(6) . . ? C70 N2 C40 124.3(7) . . ? C73 N3 C45 126.9(8) . . ? C76 N4 C46 129.8(9) . . ? C58 N5 C59 112.2(8) . . ? C79 N6 C63 127.6(8) . . ? C82 N7 C64 130.7(7) . . ? C6 C1 C2 116.6(6) . . ? C6 C1 C34 122.1(6) . . ? C2 C1 C34 121.3(6) . . ? C3 C2 C1 120.6(6) . . ? C3 C2 O8 119.6(6) . . ? C1 C2 O8 119.5(6) . . ? C4 C3 C2 120.0(6) . . ? C3 C4 C5 122.2(6) . . ? C3 C4 O1 119.4(6) . . ? C5 C4 O1 118.1(6) . . ? C4 C5 C6 116.1(6) . . ? C4 C5 C7 120.0(6) . . ? C6 C5 C7 123.7(6) . . ? C1 C6 C5 124.3(7) . . ? C10 C7 C5 108.5(6) . . ? C10 C7 C8 113.5(6) . . ? C5 C7 C8 113.3(6) . . ? C7 C8 C9 112.1(6) . . ? C15 C10 C11 116.1(6) . . ? C15 C10 C7 123.1(6) . . ? C11 C10 C7 120.8(6) . . ? C12 C11 O2 119.6(6) . . ? C12 C11 C10 121.9(6) . . ? O2 C11 C10 118.4(6) . . ? C13 C12 C11 119.6(7) . . ? C12 C13 C14 121.8(7) . . ? C12 C13 O3 120.0(6) . . ? C14 C13 O3 118.0(6) . . ? C15 C14 C13 116.4(6) . . ? C15 C14 C16 122.4(6) . . ? C13 C14 C16 121.2(7) . . ? C14 C15 C10 123.8(6) . . ? C14 C16 C17 112.5(7) . . ? C14 C16 C19 112.0(6) . . ? C17 C16 C19 112.2(6) . . ? C16 C17 C18 112.0(7) . . ? C20 C19 C24 117.7(7) . . ? C20 C19 C16 120.5(7) . . ? C24 C19 C16 121.8(7) . . ? C19 C20 O4 120.2(7) . . ? C19 C20 C21 120.5(7) . . ? O4 C20 C21 119.1(7) . . ? C22 C21 C20 120.2(8) . . ? C21 C22 O5 117.8(7) . . ? C21 C22 C23 120.7(7) . . ? O5 C22 C23 121.5(7) . . ? C24 C23 C22 117.1(7) . . ? C24 C23 C25 122.2(7) . . ? C22 C23 C25 120.5(7) . . ? C23 C24 C19 123.7(7) . . ? C23 C25 C28 106.1(6) . . ? C23 C25 C26 115.0(7) . . ? C28 C25 C26 113.7(6) . . ? C27A C26 C25 115.1(9) . . ? C27A C26 C27B 94.8(12) . . ? C25 C26 C27B 110.1(13) . . ? C33 C28 C29 116.2(7) . . ? C33 C28 C25 124.4(7) . . ? C29 C28 C25 119.1(6) . . ? C30 C29 O6 118.9(7) . . ? C30 C29 C28 122.3(7) . . ? O6 C29 C28 118.5(6) . . ? C29 C30 C31 118.9(7) . . ? C32 C31 C30 122.9(7) . . ? C32 C31 O7 118.6(6) . . ? C30 C31 O7 118.4(6) . . ? C31 C32 C33 116.6(7) . . ? C31 C32 C34 121.4(6) . . ? C33 C32 C34 122.1(7) . . ? C28 C33 C32 123.1(7) . . ? C1 C34 C32 111.9(5) . . ? C1 C34 C35 112.0(6) . . ? C32 C34 C35 112.4(6) . . ? C36 C35 C34 113.1(6) . . ? C42 C37 O1 119.2(6) . . ? C42 C37 C38 121.2(7) . . ? O1 C37 C38 119.5(6) . . ? C39 C38 C37 119.4(7) . . ? C40 C39 C38 119.6(7) . . ? C40 C39 N1 121.1(7) . . ? C38 C39 N1 119.2(6) . . ? C39 C40 C41 119.7(7) . . ? C39 C40 N2 122.0(7) . . ? C41 C40 N2 118.3(7) . . ? C42 C41 C40 120.5(7) . . ? O2 C42 C37 119.7(7) . . ? O2 C42 C41 120.5(6) . . ? C37 C42 C41 119.5(7) . . ? C44 C43 O3 120.3(7) . . ? C44 C43 C48 120.9(7) . . ? O3 C43 C48 118.5(7) . . ? C43 C44 C45 121.2(8) . . ? C46 C45 C44 118.3(8) . . ? C46 C45 N3 118.7(8) . . ? C44 C45 N3 123.0(8) . . ? C45 C46 C47 119.7(8) . . ? C45 C46 N4 125.4(8) . . ? C47 C46 N4 114.6(8) . . ? C48 C47 C46 122.3(8) . . ? O4 C48 C47 121.8(7) . . ? O4 C48 C43 120.7(7) . . ? C47 C48 C43 117.5(8) . . ? O6 C49 O5 111.2(6) . . ? O6 C49 C50 104.8(6) . . ? O5 C49 C50 109.6(7) . . ? C51 C50 C55 117.5(8) . . ? C51 C50 C49 124.0(8) . . ? C55 C50 C49 118.5(8) . . ? C50 C51 C52 121.1(8) . . ? C53 C52 C51 120.8(8) . . ? C52 C53 C54 119.1(8) . . ? C52 C53 C56 122.3(8) . . ? C54 C53 C56 118.5(8) . . ? C53 C54 C55 121.0(9) . . ? C54 C55 C50 120.3(9) . . ? C57 C56 C60 116.8(8) . . ? C57 C56 C53 123.1(8) . . ? C60 C56 C53 120.0(8) . . ? C58 C57 C56 119.0(9) . . ? N5 C58 C57 128.2(9) . . ? N5 C59 C60 126.7(10) . . ? C56 C60 C59 116.9(9) . . ? C62 C61 C66 122.0(7) . . ? C62 C61 O7 119.7(7) . . ? C66 C61 O7 118.2(7) . . ? C61 C62 C63 120.7(8) . . ? C62 C63 C64 118.2(7) . . ? C62 C63 N6 120.3(8) . . ? C64 C63 N6 121.5(8) . . ? C65 C64 C63 120.2(7) . . ? C65 C64 N7 116.7(7) . . ? C63 C64 N7 123.1(7) . . ? C64 C65 C66 120.5(7) . . ? C61 C66 C65 118.2(7) . . ? C61 C66 O8 120.5(7) . . ? C65 C66 O8 121.1(7) . . ? O9 C67 N1 122.6(8) . . ? O9 C67 C68 122.3(8) . . ? N1 C67 C68 115.1(7) . . ? C69 C68 C67 112.8(8) . . ? O10 C70 N2 121.6(7) . . ? O10 C70 C71 122.7(7) . . ? N2 C70 C71 115.7(7) . . ? C72 C71 C70 113.2(8) . . ? O11 C73 N3 125.2(9) . . ? O11 C73 C74 120.9(9) . . ? N3 C73 C74 113.8(9) . . ? C75A C74 C75B 84.6(16) . . ? C75A C74 C73 120.1(12) . . ? C75B C74 C73 110.1(13) . . ? O12 C76 N4 122.6(11) . . ? O12 C76 C77 119.6(11) . . ? N4 C76 C77 117.7(11) . . ? C78 C77 C76 113.8(13) . . ? O13 C79 N6 121.9(10) . . ? O13 C79 C80 122.8(11) . . ? N6 C79 C80 114.9(11) . . ? C81A C80 C79 112.5(18) . . ? C81A C80 C81B 106(3) . . ? C79 C80 C81B 123(3) . . ? O14 C82 N7 121.9(8) . . ? O14 C82 C83 122.6(9) . . ? N7 C82 C83 115.5(9) . . ? C84 C83 C82 117.9(12) . . ? C91 N8 C92 107.7(13) . . ? C86 C85 C90 119.5(10) . . ? C86 C85 C92 137.2(11) . . ? C90 C85 C92 103.3(10) . . ? C87 C86 C85 120.9(11) . . ? C88 C87 C86 122.4(12) . . ? C87 C88 C89 120.6(12) . . ? C88 C89 C90 119.4(10) . . ? C85 C90 C89 117.1(10) . . ? C85 C90 C91 103.8(10) . . ? C89 C90 C91 138.8(11) . . ? O15 C91 N8 147.5(18) . . ? O15 C91 C90 97.9(14) . . ? N8 C91 C90 114.4(12) . . ? O16 C92 N8 149(2) . . ? O16 C92 C85 100.5(16) . . ? N8 C92 C85 110.7(12) . . ? C94 C93 O17 107.0(15) . . ? 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 7.7(10) . . . . ? C34 C1 C2 C3 -170.9(6) . . . . ? C6 C1 C2 O8 -178.9(6) . . . . ? C34 C1 C2 O8 2.5(9) . . . . ? C66 O8 C2 C3 -85.8(7) . . . . ? C66 O8 C2 C1 100.7(7) . . . . ? C1 C2 C3 C4 -6.1(10) . . . . ? O8 C2 C3 C4 -179.5(6) . . . . ? C2 C3 C4 C5 0.7(10) . . . . ? C2 C3 C4 O1 175.0(6) . . . . ? C37 O1 C4 C3 70.7(8) . . . . ? C37 O1 C4 C5 -114.8(7) . . . . ? C3 C4 C5 C6 2.6(10) . . . . ? O1 C4 C5 C6 -171.8(6) . . . . ? C3 C4 C5 C7 -172.5(6) . . . . ? O1 C4 C5 C7 13.2(9) . . . . ? C2 C1 C6 C5 -4.4(10) . . . . ? C34 C1 C6 C5 174.2(6) . . . . ? C4 C5 C6 C1 -0.6(10) . . . . ? C7 C5 C6 C1 174.2(6) . . . . ? C4 C5 C7 C10 88.3(7) . . . . ? C6 C5 C7 C10 -86.3(8) . . . . ? C4 C5 C7 C8 -144.6(6) . . . . ? C6 C5 C7 C8 40.7(9) . . . . ? C10 C7 C8 C9 -69.3(8) . . . . ? C5 C7 C8 C9 166.3(6) . . . . ? C5 C7 C10 C15 88.3(8) . . . . ? C8 C7 C10 C15 -38.6(9) . . . . ? C5 C7 C10 C11 -90.5(7) . . . . ? C8 C7 C10 C11 142.6(6) . . . . ? C42 O2 C11 C12 -69.5(8) . . . . ? C42 O2 C11 C10 113.8(7) . . . . ? C15 C10 C11 C12 -5.9(10) . . . . ? C7 C10 C11 C12 172.9(6) . . . . ? C15 C10 C11 O2 170.8(6) . . . . ? C7 C10 C11 O2 -10.4(9) . . . . ? O2 C11 C12 C13 -172.6(6) . . . . ? C10 C11 C12 C13 4.0(10) . . . . ? C11 C12 C13 C14 1.9(10) . . . . ? C11 C12 C13 O3 177.3(6) . . . . ? C43 O3 C13 C12 82.6(8) . . . . ? C43 O3 C13 C14 -101.9(7) . . . . ? C12 C13 C14 C15 -5.3(10) . . . . ? O3 C13 C14 C15 179.3(6) . . . . ? C12 C13 C14 C16 171.7(6) . . . . ? O3 C13 C14 C16 -3.7(9) . . . . ? C13 C14 C15 C10 3.2(10) . . . . ? C16 C14 C15 C10 -173.8(6) . . . . ? C11 C10 C15 C14 2.2(10) . . . . ? C7 C10 C15 C14 -176.6(6) . . . . ? C15 C14 C16 C17 40.9(9) . . . . ? C13 C14 C16 C17 -135.9(7) . . . . ? C15 C14 C16 C19 -86.6(9) . . . . ? C13 C14 C16 C19 96.6(8) . . . . ? C14 C16 C17 C18 63.4(9) . . . . ? C19 C16 C17 C18 -169.2(7) . . . . ? C14 C16 C19 C20 -92.8(8) . . . . ? C17 C16 C19 C20 139.5(7) . . . . ? C14 C16 C19 C24 85.8(8) . . . . ? C17 C16 C19 C24 -41.9(9) . . . . ? C24 C19 C20 O4 178.3(6) . . . . ? C16 C19 C20 O4 -3.0(10) . . . . ? C24 C19 C20 C21 3.4(10) . . . . ? C16 C19 C20 C21 -178.0(6) . . . . ? C48 O4 C20 C19 105.2(8) . . . . ? C48 O4 C20 C21 -79.8(8) . . . . ? C19 C20 C21 C22 -1.0(11) . . . . ? O4 C20 C21 C22 -176.0(7) . . . . ? C20 C21 C22 O5 175.6(6) . . . . ? C20 C21 C22 C23 -1.3(11) . . . . ? C49 O5 C22 C21 99.9(8) . . . . ? C49 O5 C22 C23 -83.2(9) . . . . ? C21 C22 C23 C24 1.0(11) . . . . ? O5 C22 C23 C24 -175.8(6) . . . . ? C21 C22 C23 C25 -174.5(7) . . . . ? O5 C22 C23 C25 8.7(11) . . . . ? C22 C23 C24 C19 1.5(11) . . . . ? C25 C23 C24 C19 177.0(7) . . . . ? C20 C19 C24 C23 -3.7(10) . . . . ? C16 C19 C24 C23 177.7(7) . . . . ? C24 C23 C25 C28 -90.3(8) . . . . ? C22 C23 C25 C28 85.0(8) . . . . ? C24 C23 C25 C26 36.3(10) . . . . ? C22 C23 C25 C26 -148.4(7) . . . . ? C23 C25 C26 C27A 173.7(8) . . . . ? C28 C25 C26 C27A -63.7(10) . . . . ? C23 C25 C26 C27B 68.1(13) . . . . ? C28 C25 C26 C27B -169.3(12) . . . . ? C23 C25 C28 C33 91.9(8) . . . . ? C26 C25 C28 C33 -35.5(10) . . . . ? C23 C25 C28 C29 -81.6(8) . . . . ? C26 C25 C28 C29 151.0(7) . . . . ? C49 O6 C29 C30 -93.9(8) . . . . ? C49 O6 C29 C28 92.1(8) . . . . ? C33 C28 C29 C30 -0.6(10) . . . . ? C25 C28 C29 C30 173.4(7) . . . . ? C33 C28 C29 O6 173.1(6) . . . . ? C25 C28 C29 O6 -12.8(10) . . . . ? O6 C29 C30 C31 -173.0(6) . . . . ? C28 C29 C30 C31 0.7(11) . . . . ? C29 C30 C31 C32 1.1(11) . . . . ? C29 C30 C31 O7 176.5(6) . . . . ? C61 O7 C31 C32 -105.6(7) . . . . ? C61 O7 C31 C30 78.7(8) . . . . ? C30 C31 C32 C33 -2.7(10) . . . . ? O7 C31 C32 C33 -178.2(6) . . . . ? C30 C31 C32 C34 177.0(6) . . . . ? O7 C31 C32 C34 1.6(9) . . . . ? C29 C28 C33 C32 -1.2(10) . . . . ? C25 C28 C33 C32 -174.9(7) . . . . ? C31 C32 C33 C28 2.8(10) . . . . ? C34 C32 C33 C28 -176.9(6) . . . . ? C6 C1 C34 C32 84.9(8) . . . . ? C2 C1 C34 C32 -96.5(8) . . . . ? C6 C1 C34 C35 -42.3(9) . . . . ? C2 C1 C34 C35 136.2(7) . . . . ? C31 C32 C34 C1 92.9(8) . . . . ? C33 C32 C34 C1 -87.4(8) . . . . ? C31 C32 C34 C35 -140.0(6) . . . . ? C33 C32 C34 C35 39.7(8) . . . . ? C1 C34 C35 C36 -166.6(6) . . . . ? C32 C34 C35 C36 66.5(8) . . . . ? C4 O1 C37 C42 95.9(8) . . . . ? C4 O1 C37 C38 -87.8(8) . . . . ? C42 C37 C38 C39 -2.1(11) . . . . ? O1 C37 C38 C39 -178.4(6) . . . . ? C37 C38 C39 C40 2.9(11) . . . . ? C37 C38 C39 N1 179.2(7) . . . . ? C67 N1 C39 C40 -130.3(9) . . . . ? C67 N1 C39 C38 53.5(11) . . . . ? C38 C39 C40 C41 -0.6(12) . . . . ? N1 C39 C40 C41 -176.8(7) . . . . ? C38 C39 C40 N2 -179.9(7) . . . . ? N1 C39 C40 N2 3.9(12) . . . . ? C70 N2 C40 C39 -55.9(11) . . . . ? C70 N2 C40 C41 124.7(8) . . . . ? C39 C40 C41 C42 -2.6(12) . . . . ? N2 C40 C41 C42 176.7(7) . . . . ? C11 O2 C42 C37 -96.5(8) . . . . ? C11 O2 C42 C41 88.5(8) . . . . ? O1 C37 C42 O2 0.2(10) . . . . ? C38 C37 C42 O2 -176.0(6) . . . . ? O1 C37 C42 C41 175.2(6) . . . . ? C38 C37 C42 C41 -1.0(11) . . . . ? C40 C41 C42 O2 178.4(7) . . . . ? C40 C41 C42 C37 3.4(11) . . . . ? C13 O3 C43 C44 -82.0(8) . . . . ? C13 O3 C43 C48 104.1(7) . . . . ? O3 C43 C44 C45 -174.7(7) . . . . ? C48 C43 C44 C45 -1.0(11) . . . . ? C43 C44 C45 C46 0.5(11) . . . . ? C43 C44 C45 N3 178.7(7) . . . . ? C73 N3 C45 C46 -160.2(8) . . . . ? C73 N3 C45 C44 21.7(13) . . . . ? C44 C45 C46 C47 0.0(12) . . . . ? N3 C45 C46 C47 -178.2(7) . . . . ? C44 C45 C46 N4 -173.2(8) . . . . ? N3 C45 C46 N4 8.6(13) . . . . ? C76 N4 C46 C45 -50.7(16) . . . . ? C76 N4 C46 C47 135.8(12) . . . . ? C45 C46 C47 C48 -0.2(13) . . . . ? N4 C46 C47 C48 173.7(8) . . . . ? C20 O4 C48 C47 83.4(9) . . . . ? C20 O4 C48 C43 -99.4(8) . . . . ? C46 C47 C48 O4 177.1(7) . . . . ? C46 C47 C48 C43 -0.2(12) . . . . ? C44 C43 C48 O4 -176.5(7) . . . . ? O3 C43 C48 O4 -2.6(10) . . . . ? C44 C43 C48 C47 0.8(11) . . . . ? O3 C43 C48 C47 174.7(6) . . . . ? C29 O6 C49 O5 -89.6(8) . . . . ? C29 O6 C49 C50 152.1(7) . . . . ? C22 O5 C49 O6 83.6(8) . . . . ? C22 O5 C49 C50 -160.9(7) . . . . ? O6 C49 C50 C51 135.8(9) . . . . ? O5 C49 C50 C51 16.4(12) . . . . ? O6 C49 C50 C55 -41.6(11) . . . . ? O5 C49 C50 C55 -161.1(9) . . . . ? C55 C50 C51 C52 3.5(14) . . . . ? C49 C50 C51 C52 -174.0(8) . . . . ? C50 C51 C52 C53 -0.9(14) . . . . ? C51 C52 C53 C54 -2.3(15) . . . . ? C51 C52 C53 C56 174.4(8) . . . . ? C52 C53 C54 C55 2.8(16) . . . . ? C56 C53 C54 C55 -174.0(10) . . . . ? C53 C54 C55 C50 -0.2(18) . . . . ? C51 C50 C55 C54 -2.9(16) . . . . ? C49 C50 C55 C54 174.7(10) . . . . ? C52 C53 C56 C57 -22.0(13) . . . . ? C54 C53 C56 C57 154.7(9) . . . . ? C52 C53 C56 C60 162.2(9) . . . . ? C54 C53 C56 C60 -21.1(13) . . . . ? C60 C56 C57 C58 3.6(13) . . . . ? C53 C56 C57 C58 -172.3(8) . . . . ? C59 N5 C58 C57 3.7(14) . . . . ? C56 C57 C58 N5 -5.4(15) . . . . ? C58 N5 C59 C60 -0.5(15) . . . . ? C57 C56 C60 C59 -0.9(13) . . . . ? C53 C56 C60 C59 175.1(8) . . . . ? N5 C59 C60 C56 -0.6(16) . . . . ? C31 O7 C61 C62 -78.1(8) . . . . ? C31 O7 C61 C66 102.9(7) . . . . ? C66 C61 C62 C63 -0.7(11) . . . . ? O7 C61 C62 C63 -179.7(6) . . . . ? C61 C62 C63 C64 2.8(11) . . . . ? C61 C62 C63 N6 -175.9(7) . . . . ? C79 N6 C63 C62 29.2(14) . . . . ? C79 N6 C63 C64 -149.5(10) . . . . ? C62 C63 C64 C65 -1.2(11) . . . . ? N6 C63 C64 C65 177.4(7) . . . . ? C62 C63 C64 N7 -179.1(7) . . . . ? N6 C63 C64 N7 -0.4(12) . . . . ? C82 N7 C64 C65 140.9(9) . . . . ? C82 N7 C64 C63 -41.2(13) . . . . ? C63 C64 C65 C66 -2.4(11) . . . . ? N7 C64 C65 C66 175.6(7) . . . . ? C62 C61 C66 C65 -2.9(11) . . . . ? O7 C61 C66 C65 176.1(6) . . . . ? C62 C61 C66 O8 -177.9(6) . . . . ? O7 C61 C66 O8 1.1(9) . . . . ? C64 C65 C66 C61 4.4(10) . . . . ? C64 C65 C66 O8 179.4(6) . . . . ? C2 O8 C66 C61 -101.8(7) . . . . ? C2 O8 C66 C65 83.3(8) . . . . ? C39 N1 C67 O9 3.4(14) . . . . ? C39 N1 C67 C68 -176.2(7) . . . . ? O9 C67 C68 C69 -39.5(14) . . . . ? N1 C67 C68 C69 140.1(9) . . . . ? C40 N2 C70 O10 -2.8(12) . . . . ? C40 N2 C70 C71 176.9(7) . . . . ? O10 C70 C71 C72 -23.4(12) . . . . ? N2 C70 C71 C72 156.9(8) . . . . ? C45 N3 C73 O11 -1.1(14) . . . . ? C45 N3 C73 C74 -177.9(8) . . . . ? O11 C73 C74 C75A 169.1(14) . . . . ? N3 C73 C74 C75A -13.9(17) . . . . ? O11 C73 C74 C75B 73.6(17) . . . . ? N3 C73 C74 C75B -109.4(15) . . . . ? C46 N4 C76 O12 2(2) . . . . ? C46 N4 C76 C77 -176.1(12) . . . . ? O12 C76 C77 C78 -40(2) . . . . ? N4 C76 C77 C78 137.5(14) . . . . ? C63 N6 C79 O13 9(2) . . . . ? C63 N6 C79 C80 -177.4(11) . . . . ? O13 C79 C80 C81A -45(3) . . . . ? N6 C79 C80 C81A 141.3(19) . . . . ? O13 C79 C80 C81B -174(3) . . . . ? N6 C79 C80 C81B 12(4) . . . . ? C64 N7 C82 O14 2.5(15) . . . . ? C64 N7 C82 C83 -176.7(10) . . . . ? O14 C82 C83 C84 -16(2) . . . . ? N7 C82 C83 C84 163.3(13) . . . . ? C90 C85 C86 C87 -2.1(16) . . . . ? C92 C85 C86 C87 175.0(16) . . . . ? C85 C86 C87 C88 0.9(18) . . . . ? C86 C87 C88 C89 0.5(18) . . . . ? C87 C88 C89 C90 -0.7(16) . . . . ? C86 C85 C90 C89 1.8(15) . . . . ? C92 C85 C90 C89 -176.2(12) . . . . ? C86 C85 C90 C91 177.2(11) . . . . ? C92 C85 C90 C91 -0.8(14) . . . . ? C88 C89 C90 C85 -0.5(15) . . . . ? C88 C89 C90 C91 -173.6(14) . . . . ? C92 N8 C91 O15 174(3) . . . . ? C92 N8 C91 C90 0(2) . . . . ? C85 C90 C91 O15 -176.0(13) . . . . ? C89 C90 C91 O15 -2(2) . . . . ? C85 C90 C91 N8 0.9(17) . . . . ? C89 C90 C91 N8 174.6(13) . . . . ? C91 N8 C92 O16 176(4) . . . . ? C91 N8 C92 C85 0(2) . . . . ? C86 C85 C92 O16 5(3) . . . . ? C90 C85 C92 O16 -177.2(15) . . . . ? C86 C85 C92 N8 -176.7(13) . . . . ? C90 C85 C92 N8 0.7(19) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.980 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.115