# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_s3833na #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H56.50 N7 O9 S' _chemical_formula_weight 763.44 _chemical_absolute_configuration ad 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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5236(2) _cell_length_b 14.2240(3) _cell_length_c 16.8220(4) _cell_angle_alpha 109.168(2) _cell_angle_beta 92.395(2) _cell_angle_gamma 100.881(2) _cell_volume 2100.47(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3082 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 69.29 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 819 _exptl_absorpt_coefficient_mu 1.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.736912 _exptl_absorpt_correction_T_max 0.8733 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19488 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 66.59 _reflns_number_total 9306 _reflns_number_gt 7249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 9306 _refine_ls_number_parameters 986 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5035(5) 0.7135(4) 0.0746(3) 0.0322(11) Uani 1 1 d . . . C2 C 0.6496(5) 0.7359(4) 0.0981(3) 0.0402(12) Uani 1 1 d . . . H2 H 0.6916 0.7930 0.1467 0.048 Uiso 1 1 calc R . . C3 C 0.7349(6) 0.6750(6) 0.0509(4) 0.0574(17) Uani 1 1 d . . . H3 H 0.8358 0.6915 0.0672 0.069 Uiso 1 1 calc R . . C4 C 0.6777(7) 0.5922(5) -0.0181(4) 0.0637(19) Uani 1 1 d . . . H4 H 0.7375 0.5504 -0.0495 0.076 Uiso 1 1 calc R . . C5 C 0.5321(7) 0.5696(4) -0.0421(4) 0.0510(14) Uani 1 1 d . . . H5 H 0.4909 0.5122 -0.0906 0.061 Uiso 1 1 calc R . . C6 C 0.4455(6) 0.6298(4) 0.0040(3) 0.0394(12) Uani 1 1 d . . . H6 H 0.3450 0.6135 -0.0130 0.047 Uiso 1 1 calc R . . C7 C 0.4033(5) 0.7782(4) 0.1195(3) 0.0367(11) Uani 1 1 d . . . H7A H 0.3787 0.8191 0.0854 0.044 Uiso 1 1 calc R . . H7B H 0.3131 0.7332 0.1237 0.044 Uiso 1 1 calc R . . C8 C 0.4658(5) 0.8014(4) 0.2637(3) 0.0296(10) Uani 1 1 d . . . C9 C 0.5591(4) 0.8425(3) 0.4120(3) 0.0268(9) Uani 1 1 d . . . H9 H 0.6446 0.8956 0.4454 0.032 Uiso 1 1 calc R . . C10 C 0.4407(4) 0.8496(3) 0.4719(3) 0.0329(9) Uani 1 1 d . . . H10 H 0.4717 0.8269 0.5188 0.040 Uiso 1 1 calc R . . C11 C 0.4309(5) 0.9610(3) 0.5111(3) 0.0370(11) Uani 1 1 d . . . H11A H 0.5246 1.0016 0.5410 0.055 Uiso 1 1 calc R . . H11B H 0.3584 0.9667 0.5511 0.055 Uiso 1 1 calc R . . H11C H 0.4035 0.9862 0.4663 0.055 Uiso 1 1 calc R . . C12 C 0.2956(4) 0.7804(3) 0.4288(3) 0.0385(10) Uani 1 1 d . . . H12A H 0.2618 0.8011 0.3825 0.058 Uiso 1 1 calc R . . H12B H 0.2254 0.7862 0.4702 0.058 Uiso 1 1 calc R . . H12C H 0.3064 0.7096 0.4060 0.058 Uiso 1 1 calc R . . C13 C 0.6079(4) 0.7401(3) 0.3900(3) 0.0265(9) Uani 1 1 d . . . C14 C 0.7727(5) 0.6364(3) 0.3158(3) 0.0311(10) Uani 1 1 d . . . C15 C 0.8615(5) 0.6349(4) 0.2422(4) 0.0427(12) Uani 1 1 d . . . H15A H 0.7987 0.6304 0.1928 0.064 Uiso 1 1 calc R . . H15B H 0.9066 0.5759 0.2281 0.064 Uiso 1 1 calc R . . H15C H 0.9362 0.6976 0.2584 0.064 Uiso 1 1 calc R . . C16 C 0.8669(5) 0.6376(4) 0.3926(3) 0.0434(13) Uani 1 1 d . . . H16A H 0.9443 0.6988 0.4109 0.065 Uiso 1 1 calc R . . H16B H 0.9085 0.5769 0.3770 0.065 Uiso 1 1 calc R . . H16C H 0.8079 0.6378 0.4390 0.065 Uiso 1 1 calc R . . C17 C 0.6538(4) 0.5367(4) 0.2848(3) 0.0282(10) Uani 1 1 d . . . C18 C 0.4155(5) 0.4516(4) 0.2062(3) 0.0303(10) Uani 1 1 d . . . C19 C 0.2834(5) 0.4881(4) 0.1810(3) 0.0360(12) Uani 1 1 d . . . H19A H 0.2558 0.5361 0.2314 0.054 Uiso 1 1 calc R . . H19B H 0.2031 0.4294 0.1560 0.054 Uiso 1 1 calc R . . H19C H 0.3073 0.5220 0.1397 0.054 Uiso 1 1 calc R . . C20 C 0.4552(6) 0.3736(4) 0.1286(3) 0.0419(12) Uani 1 1 d . . . H20A H 0.4886 0.4069 0.0882 0.063 Uiso 1 1 calc R . . H20B H 0.3705 0.3189 0.1018 0.063 Uiso 1 1 calc R . . H20C H 0.5319 0.3448 0.1459 0.063 Uiso 1 1 calc R . . C21 C 0.3699(5) 0.4043(4) 0.2736(3) 0.0300(10) Uani 1 1 d . . . C22 C 0.3244(5) 0.4343(4) 0.4216(3) 0.0310(10) Uani 1 1 d . . . C23 C 0.3729(6) 0.5231(4) 0.5043(3) 0.0417(12) Uani 1 1 d . . . H23A H 0.4783 0.5415 0.5132 0.062 Uiso 1 1 calc R . . H23B H 0.3363 0.5032 0.5514 0.062 Uiso 1 1 calc R . . H23C H 0.3353 0.5817 0.5017 0.062 Uiso 1 1 calc R . . C24 C 0.1601(5) 0.4033(4) 0.4072(4) 0.0454(13) Uani 1 1 d . . . H24A H 0.1207 0.4611 0.4043 0.068 Uiso 1 1 calc R . . H24B H 0.1240 0.3829 0.4541 0.068 Uiso 1 1 calc R . . H24C H 0.1304 0.3459 0.3539 0.068 Uiso 1 1 calc R . . C25 C 0.3879(5) 0.3433(3) 0.4266(3) 0.0308(10) Uani 1 1 d . . . C26 C 0.6003(5) 0.2658(4) 0.4124(3) 0.0321(11) Uani 1 1 d . . . C27 C 0.7465(5) 0.2885(4) 0.3796(4) 0.0425(13) Uani 1 1 d . . . H27A H 0.7315 0.2945 0.3236 0.064 Uiso 1 1 calc R . . H27B H 0.7962 0.2330 0.3753 0.064 Uiso 1 1 calc R . . H27C H 0.8050 0.3526 0.4189 0.064 Uiso 1 1 calc R . . C28 C 0.6203(6) 0.2640(4) 0.5020(4) 0.0444(13) Uani 1 1 d . . . H28A H 0.6784 0.3296 0.5392 0.067 Uiso 1 1 calc R . . H28B H 0.6694 0.2093 0.5021 0.067 Uiso 1 1 calc R . . H28C H 0.5261 0.2518 0.5225 0.067 Uiso 1 1 calc R . . C29 C 0.5211(5) 0.1593(3) 0.3522(3) 0.0303(10) Uani 1 1 d . . . C30 C 0.3503(5) 0.0594(4) 0.2266(4) 0.0391(12) Uani 1 1 d . . . H30A H 0.4131 0.0095 0.2171 0.047 Uiso 1 1 calc R . . H30B H 0.3310 0.0700 0.1722 0.047 Uiso 1 1 calc R . . C31 C 0.2091(5) 0.0139(4) 0.2511(4) 0.0411(13) Uani 1 1 d . . . C32 C 0.0445(5) 0.0280(4) 0.3628(4) 0.0386(12) Uani 1 1 d . . . C33 C 0.0211(6) 0.1172(4) 0.4367(4) 0.0474(13) Uani 1 1 d . . . H33A H 0.1021 0.1380 0.4811 0.071 Uiso 1 1 calc R . . H33B H -0.0683 0.0968 0.4594 0.071 Uiso 1 1 calc R . . H33C H 0.0145 0.1744 0.4175 0.071 Uiso 1 1 calc R . . C34 C 0.0653(6) -0.0598(4) 0.3915(5) 0.0625(18) Uani 1 1 d . . . H34A H 0.0885 -0.1140 0.3438 0.094 Uiso 1 1 calc R . . H34B H -0.0234 -0.0864 0.4117 0.094 Uiso 1 1 calc R . . H34C H 0.1443 -0.0356 0.4374 0.094 Uiso 1 1 calc R . . C35 C -0.0910(5) -0.0076(4) 0.2994(3) 0.0341(11) Uani 1 1 d . . . C36 C -0.2278(5) 0.0331(5) 0.2007(4) 0.0467(13) Uani 1 1 d . . . H36A H -0.2174 -0.0229 0.1501 0.070 Uiso 1 1 calc R . . H36B H -0.2369 0.0925 0.1850 0.070 Uiso 1 1 calc R . . H36C H -0.3139 0.0118 0.2256 0.070 Uiso 1 1 calc R . . C37 C -0.0489(5) 0.1350(4) 1.0590(3) 0.0369(12) Uani 1 1 d . . . C38 C -0.1904(5) 0.1277(4) 1.0301(3) 0.0402(12) Uani 1 1 d . . . H38 H -0.2350 0.0738 0.9800 0.048 Uiso 1 1 calc R . . C39 C -0.2675(6) 0.1982(5) 1.0738(4) 0.0508(14) Uani 1 1 d . . . H39 H -0.3650 0.1918 1.0541 0.061 Uiso 1 1 calc R . . C40 C -0.2016(6) 0.2788(5) 1.1469(4) 0.0500(14) Uani 1 1 d . . . H40 H -0.2536 0.3273 1.1774 0.060 Uiso 1 1 calc R . . C41 C -0.0597(6) 0.2867(5) 1.1739(4) 0.0516(15) Uani 1 1 d . . . H41 H -0.0134 0.3423 1.2225 0.062 Uiso 1 1 calc R . . C42 C 0.0158(5) 0.2159(4) 1.1318(4) 0.0432(13) Uani 1 1 d . . . H42 H 0.1128 0.2219 1.1523 0.052 Uiso 1 1 calc R . . C43 C 0.0380(5) 0.0585(4) 1.0181(4) 0.0426(13) Uani 1 1 d . . . H43A H 0.1371 0.0948 1.0172 0.051 Uiso 1 1 calc R . . H43B H 0.0437 0.0146 1.0527 0.051 Uiso 1 1 calc R . . C44 C 0.0017(5) 0.0408(4) 0.8739(3) 0.0340(11) Uani 1 1 d . . . C45 C -0.0372(5) 0.0123(4) 0.7246(3) 0.0421(12) Uani 1 1 d . . . H45 H 0.0680 0.0372 0.7237 0.050 Uiso 1 1 calc R A 1 C47 C -0.2440(5) -0.1266(3) 0.6330(3) 0.0440(11) Uani 1 1 d . . . H47A H -0.3054 -0.0781 0.6346 0.066 Uiso 1 1 calc R B 1 H47B H -0.2601 -0.1526 0.6798 0.066 Uiso 1 1 calc R B 1 H47C H -0.2675 -0.1835 0.5790 0.066 Uiso 1 1 calc R B 1 C49 C -0.1093(5) 0.1011(4) 0.7328(3) 0.0363(11) Uani 1 1 d . C . C50 C -0.2957(5) 0.1956(4) 0.7941(3) 0.0334(11) Uani 1 1 d . C . C51 C -0.3761(6) 0.1939(4) 0.7137(4) 0.0492(14) Uani 1 1 d . . . H51A H -0.3092 0.1938 0.6709 0.074 Uiso 1 1 calc R . . H51B H -0.4179 0.2544 0.7259 0.074 Uiso 1 1 calc R . . H51C H -0.4530 0.1324 0.6923 0.074 Uiso 1 1 calc R . . C52 C -0.3984(5) 0.1904(4) 0.8604(3) 0.0421(12) Uani 1 1 d . . . H52A H -0.4687 0.1254 0.8395 0.063 Uiso 1 1 calc R . . H52B H -0.4489 0.2467 0.8712 0.063 Uiso 1 1 calc R . . H52C H -0.3438 0.1960 0.9130 0.063 Uiso 1 1 calc R . . C53 C -0.1844(5) 0.2984(3) 0.8338(3) 0.0295(10) Uani 1 1 d . . . C54 C 0.0459(5) 0.3898(3) 0.9220(3) 0.0291(10) Uani 1 1 d . . . C55 C 0.1787(5) 0.3573(4) 0.9487(3) 0.0359(11) Uani 1 1 d . . . H55A H 0.1554 0.3230 0.9899 0.054 Uiso 1 1 calc R . . H55B H 0.2564 0.4176 0.9746 0.054 Uiso 1 1 calc R . . H55C H 0.2096 0.3105 0.8989 0.054 Uiso 1 1 calc R . . C56 C -0.0054(6) 0.4611(4) 0.9986(3) 0.0410(12) Uani 1 1 d . . . H56A H -0.0903 0.4817 0.9805 0.062 Uiso 1 1 calc R . . H56B H 0.0714 0.5216 1.0257 0.062 Uiso 1 1 calc R . . H56C H -0.0303 0.4260 1.0390 0.062 Uiso 1 1 calc R . . C57 C 0.0895(5) 0.4426(4) 0.8582(3) 0.0296(10) Uani 1 1 d . . . C58 C 0.1452(5) 0.4205(4) 0.7118(3) 0.0307(10) Uani 1 1 d . . . C59 C 0.3075(5) 0.4593(5) 0.7308(4) 0.0472(14) Uani 1 1 d . . . H59A H 0.3299 0.5164 0.7846 0.071 Uiso 1 1 calc R . . H59B H 0.3445 0.4822 0.6853 0.071 Uiso 1 1 calc R . . H59C H 0.3527 0.4043 0.7348 0.071 Uiso 1 1 calc R . . C60 C 0.1062(6) 0.3310(4) 0.6273(3) 0.0409(12) Uani 1 1 d . . . H60A H 0.1453 0.2736 0.6315 0.061 Uiso 1 1 calc R . . H60B H 0.1472 0.3524 0.5819 0.061 Uiso 1 1 calc R . . H60C H 0.0013 0.3100 0.6146 0.061 Uiso 1 1 calc R . . C61 C 0.0725(5) 0.5053(3) 0.7043(3) 0.0266(10) Uani 1 1 d . . . C62 C -0.1471(5) 0.5757(3) 0.7154(3) 0.0299(10) Uani 1 1 d . . . C63 C -0.1630(6) 0.5793(4) 0.6243(3) 0.0399(12) Uani 1 1 d . . . H63A H -0.0674 0.5971 0.6071 0.060 Uiso 1 1 calc R . . H63B H -0.2180 0.6306 0.6231 0.060 Uiso 1 1 calc R . . H63C H -0.2136 0.5123 0.5852 0.060 Uiso 1 1 calc R . . C64 C -0.2948(5) 0.5486(4) 0.7436(4) 0.0392(12) Uani 1 1 d . . . H64A H -0.3470 0.4823 0.7043 0.059 Uiso 1 1 calc R . . H64B H -0.3490 0.6008 0.7439 0.059 Uiso 1 1 calc R . . H64C H -0.2833 0.5454 0.8007 0.059 Uiso 1 1 calc R . . C65 C -0.0736(5) 0.6831(4) 0.7773(3) 0.0292(10) Uani 1 1 d . . . C66 C 0.0934(5) 0.7841(4) 0.9046(3) 0.0317(10) Uani 1 1 d . . . H66A H 0.1176 0.7719 0.9576 0.038 Uiso 1 1 calc R . . H66B H 0.0274 0.8319 0.9169 0.038 Uiso 1 1 calc R . . C67 C 0.2299(5) 0.8350(4) 0.8795(3) 0.0332(11) Uani 1 1 d . . . C68 C 0.3843(5) 0.8310(4) 0.7627(3) 0.0410(12) Uani 1 1 d . . . C69 C 0.3498(7) 0.9203(5) 0.7395(4) 0.0621(18) Uani 1 1 d . . . H69A H 0.2624 0.8964 0.6993 0.093 Uiso 1 1 calc R . . H69B H 0.4302 0.9481 0.7136 0.093 Uiso 1 1 calc R . . H69C H 0.3346 0.9735 0.7908 0.093 Uiso 1 1 calc R . . C70 C 0.4018(6) 0.7441(4) 0.6842(3) 0.0529(15) Uani 1 1 d . . . H70A H 0.4228 0.6879 0.7009 0.079 Uiso 1 1 calc R . . H70B H 0.4812 0.7683 0.6557 0.079 Uiso 1 1 calc R . . H70C H 0.3126 0.7201 0.6455 0.079 Uiso 1 1 calc R . . C71 C 0.5224(5) 0.8638(4) 0.8220(3) 0.0357(11) Uani 1 1 d . . . C72 C 0.6622(5) 0.8203(5) 0.9173(4) 0.0491(14) Uani 1 1 d . . . H72A H 0.7485 0.8345 0.8899 0.074 Uiso 1 1 calc R . . H72B H 0.6657 0.7629 0.9368 0.074 Uiso 1 1 calc R . . H72C H 0.6582 0.8807 0.9659 0.074 Uiso 1 1 calc R . . N1 N 0.5264(4) 0.8698(3) 0.3383(2) 0.0285(8) Uani 1 1 d . . . H1 H 0.5476 0.9345 0.3431 0.034 Uiso 1 1 calc R . . N2 N 0.7082(4) 0.7269(3) 0.3374(2) 0.0285(8) Uani 1 1 d . . . H2A H 0.7373 0.7738 0.3147 0.034 Uiso 1 1 calc R . . N3 N 0.5337(4) 0.5400(3) 0.2415(3) 0.0308(9) Uani 1 1 d . . . H3A H 0.5264 0.5975 0.2342 0.037 Uiso 1 1 calc R . . N4 N 0.3802(4) 0.4681(3) 0.3532(2) 0.0287(8) Uani 1 1 d . . . H4A H 0.4217 0.5326 0.3651 0.034 Uiso 1 1 calc R . . N5 N 0.5238(4) 0.3447(3) 0.4084(2) 0.0275(8) Uani 1 1 d . . . H5A H 0.5690 0.3951 0.3935 0.033 Uiso 1 1 calc R . . N6 N 0.4278(4) 0.1555(3) 0.2883(3) 0.0338(9) Uani 1 1 d . . . H6A H 0.4134 0.2129 0.2837 0.041 Uiso 1 1 calc R . . N7 N 0.1703(4) 0.0631(3) 0.3250(3) 0.0412(11) Uani 1 1 d . . . H7 H 0.2253 0.1228 0.3543 0.049 Uiso 1 1 calc R . . N8 N -0.0526(4) -0.0235(3) 0.7956(3) 0.0385(10) Uani 1 1 d . C . H8 H -0.0969 -0.0866 0.7877 0.046 Uiso 1 1 calc R . . N9 N -0.2220(4) 0.1099(3) 0.7785(3) 0.0314(9) Uani 1 1 d . . . H9A H -0.2531 0.0623 0.8002 0.038 Uiso 1 1 calc R C . N10 N -0.0669(4) 0.2980(3) 0.8807(2) 0.0261(8) Uani 1 1 d . . . H10A H -0.0573 0.2404 0.8869 0.031 Uiso 1 1 calc R . . N11 N 0.0897(4) 0.3824(3) 0.7778(2) 0.0276(8) Uani 1 1 d . . . H11 H 0.0547 0.3166 0.7640 0.033 Uiso 1 1 calc R . . N12 N -0.0657(4) 0.4996(3) 0.7201(2) 0.0272(8) Uani 1 1 d . . . H12 H -0.1091 0.4477 0.7339 0.033 Uiso 1 1 calc R . . N13 N 0.0172(4) 0.6878(3) 0.8419(2) 0.0292(8) Uani 1 1 d . . . H13 H 0.0315 0.6305 0.8469 0.035 Uiso 1 1 calc R . . N14 N 0.2633(4) 0.7896(3) 0.8027(3) 0.0333(9) Uani 1 1 d . . . H14 H 0.2092 0.7297 0.7729 0.040 Uiso 1 1 calc R . . O1 O 0.4645(4) 0.8463(2) 0.2039(2) 0.0347(7) Uani 1 1 d . . . O2 O 0.4180(3) 0.7115(2) 0.2488(2) 0.0337(7) Uani 1 1 d . . . O3 O 0.5605(3) 0.6778(2) 0.4236(2) 0.0309(7) Uani 1 1 d . . . O4 O 0.6731(3) 0.4599(2) 0.2968(2) 0.0324(7) Uani 1 1 d . . . O5 O 0.3195(3) 0.3118(2) 0.2528(2) 0.0359(8) Uani 1 1 d . . . O6 O 0.3161(3) 0.2772(3) 0.4490(2) 0.0367(8) Uani 1 1 d . . . O7 O 0.5493(4) 0.0833(2) 0.3623(2) 0.0422(9) Uani 1 1 d . . . O8 O -0.1840(3) -0.0819(3) 0.2917(3) 0.0438(9) Uani 1 1 d . . . O9 O -0.1021(3) 0.0599(3) 0.2619(2) 0.0366(8) Uani 1 1 d . . . O10 O -0.0211(3) -0.0054(3) 0.9323(2) 0.0398(8) Uani 1 1 d . . . O11 O 0.0615(3) 0.1296(2) 0.8906(2) 0.0408(8) Uani 1 1 d . . . O12 O -0.0611(4) 0.1650(3) 0.7000(2) 0.0470(9) Uani 1 1 d . . . O13 O -0.2082(3) 0.3765(2) 0.8244(2) 0.0341(7) Uani 1 1 d . . . O14 O 0.1311(3) 0.5362(2) 0.8810(2) 0.0339(8) Uani 1 1 d . . . O15 O 0.1392(3) 0.5744(2) 0.6825(2) 0.0339(8) Uani 1 1 d . . . O16 O -0.1023(4) 0.7592(2) 0.7666(2) 0.0368(8) Uani 1 1 d . . . O17 O 0.6150(4) 0.9380(3) 0.8289(2) 0.0417(8) Uani 1 1 d . . . O18 O 0.5361(3) 0.7951(2) 0.8576(2) 0.0366(8) Uani 1 1 d . . . S1 S 0.11188(13) -0.09600(10) 0.18235(11) 0.0608(5) Uani 1 1 d . . . S2 S 0.32738(13) 0.94271(10) 0.94869(9) 0.0497(4) Uani 1 1 d . . . C46S C -0.0914(5) -0.0748(4) 0.6413(3) 0.0619(17) Uani 0.441(7) 1 d PD C 2 C48S C -0.0228(12) -0.0534(8) 0.5701(5) 0.0490(18) Uani 0.441(7) 1 d PD C 2 H48D H -0.0209 -0.1178 0.5253 0.073 Uiso 0.441(7) 1 calc PR C 2 H48E H 0.0759 -0.0140 0.5901 0.073 Uiso 0.441(7) 1 calc PR C 2 H48F H -0.0777 -0.0142 0.5476 0.073 Uiso 0.441(7) 1 calc PR C 2 C46 C -0.0914(5) -0.0748(4) 0.6413(3) 0.0619(17) Uani 0.559(7) 1 d PD C 1 C48 C 0.0110(10) -0.1415(7) 0.6079(6) 0.0490(18) Uani 0.559(7) 1 d PD C 1 H48A H 0.1017 -0.0999 0.6020 0.073 Uiso 0.559(7) 1 calc PR C 1 H48B H -0.0304 -0.1918 0.5525 0.073 Uiso 0.559(7) 1 calc PR C 1 H48C H 0.0290 -0.1768 0.6473 0.073 Uiso 0.559(7) 1 calc PR C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(3) 0.027(2) 0.033(3) 0.013(2) 0.000(2) 0.008(2) C2 0.041(3) 0.041(3) 0.036(3) 0.011(2) 0.000(2) 0.008(2) C3 0.045(3) 0.096(5) 0.039(3) 0.027(3) 0.004(2) 0.029(3) C4 0.080(4) 0.086(5) 0.038(3) 0.016(3) 0.007(3) 0.056(4) C5 0.080(4) 0.040(3) 0.033(3) 0.008(2) 0.004(3) 0.019(3) C6 0.045(3) 0.031(3) 0.040(3) 0.012(2) -0.006(2) 0.004(2) C7 0.045(3) 0.034(3) 0.029(2) 0.007(2) -0.0026(19) 0.012(2) C8 0.032(2) 0.027(2) 0.035(3) 0.013(2) 0.0063(17) 0.012(2) C9 0.027(2) 0.024(2) 0.028(2) 0.0113(16) -0.0001(16) 0.0009(18) C10 0.032(2) 0.036(2) 0.034(2) 0.0134(19) 0.0044(17) 0.0107(19) C11 0.039(2) 0.031(2) 0.038(3) 0.006(2) 0.0074(19) 0.013(2) C12 0.029(2) 0.040(2) 0.051(3) 0.022(2) 0.0074(18) 0.008(2) C13 0.025(2) 0.020(2) 0.032(2) 0.0090(18) 0.0014(16) -0.0011(17) C14 0.034(2) 0.021(2) 0.036(2) 0.0063(19) 0.0010(18) 0.0077(19) C15 0.034(2) 0.036(3) 0.060(3) 0.019(2) 0.019(2) 0.007(2) C16 0.036(3) 0.030(2) 0.059(3) 0.011(2) -0.012(2) 0.005(2) C17 0.026(2) 0.028(2) 0.028(2) 0.0068(19) 0.0090(16) 0.0038(19) C18 0.028(2) 0.023(2) 0.036(3) 0.008(2) -0.0027(18) 0.003(2) C19 0.037(3) 0.030(3) 0.037(3) 0.010(2) -0.009(2) 0.003(2) C20 0.050(3) 0.034(3) 0.035(3) 0.000(2) 0.004(2) 0.012(2) C21 0.025(2) 0.025(3) 0.039(3) 0.012(2) -0.0018(18) 0.002(2) C22 0.030(2) 0.026(2) 0.042(3) 0.019(2) 0.0068(19) 0.0049(19) C23 0.064(3) 0.034(3) 0.034(3) 0.016(2) 0.014(2) 0.019(2) C24 0.037(3) 0.052(3) 0.062(4) 0.035(3) 0.014(2) 0.016(2) C25 0.036(2) 0.018(2) 0.033(3) 0.006(2) -0.0034(19) 0.003(2) C26 0.031(2) 0.027(2) 0.042(3) 0.017(2) -0.001(2) 0.006(2) C27 0.026(2) 0.029(3) 0.073(4) 0.021(3) -0.003(2) 0.002(2) C28 0.050(3) 0.034(3) 0.047(3) 0.016(3) -0.013(2) 0.003(3) C29 0.026(2) 0.018(2) 0.047(3) 0.012(2) 0.0024(19) 0.0027(19) C30 0.032(2) 0.025(2) 0.050(3) 0.000(2) -0.006(2) 0.006(2) C31 0.026(2) 0.021(2) 0.065(4) 0.003(2) -0.009(2) 0.004(2) C32 0.028(2) 0.023(2) 0.063(3) 0.016(2) -0.008(2) -0.0001(19) C33 0.038(3) 0.046(3) 0.055(3) 0.017(3) 0.003(2) 0.002(2) C34 0.051(3) 0.042(3) 0.093(5) 0.029(3) -0.030(3) 0.003(3) C35 0.020(2) 0.028(2) 0.054(3) 0.014(2) 0.0040(18) 0.002(2) C36 0.032(3) 0.053(3) 0.061(3) 0.030(3) -0.002(2) 0.004(2) C37 0.035(3) 0.029(3) 0.046(3) 0.014(2) -0.004(2) 0.005(2) C38 0.036(3) 0.047(3) 0.034(3) 0.009(2) -0.001(2) 0.012(2) C39 0.045(3) 0.068(4) 0.043(3) 0.014(3) 0.002(2) 0.029(3) C40 0.060(3) 0.050(3) 0.044(3) 0.014(3) 0.008(2) 0.026(3) C41 0.053(3) 0.041(3) 0.050(4) 0.005(3) -0.002(3) 0.004(3) C42 0.031(3) 0.039(3) 0.053(3) 0.012(3) -0.003(2) 0.004(2) C43 0.038(3) 0.033(3) 0.056(3) 0.013(2) -0.009(2) 0.012(2) C44 0.026(2) 0.021(2) 0.052(3) 0.009(2) 0.0029(19) 0.0069(19) C45 0.033(2) 0.029(2) 0.051(3) 0.001(2) 0.015(2) -0.006(2) C47 0.045(3) 0.035(2) 0.042(3) 0.002(2) 0.001(2) 0.009(2) C49 0.044(3) 0.023(2) 0.031(2) 0.0016(19) 0.0081(19) -0.004(2) C50 0.032(2) 0.028(2) 0.041(3) 0.016(2) 0.0046(18) 0.000(2) C51 0.049(3) 0.037(3) 0.058(3) 0.018(3) -0.011(2) 0.001(2) C52 0.034(2) 0.034(3) 0.060(3) 0.017(2) 0.011(2) 0.007(2) C53 0.034(2) 0.022(2) 0.034(2) 0.012(2) 0.0081(18) 0.0034(19) C54 0.034(2) 0.021(2) 0.028(2) 0.008(2) -0.0029(18) -0.002(2) C55 0.041(3) 0.023(2) 0.041(3) 0.015(2) -0.009(2) -0.004(2) C56 0.052(3) 0.030(3) 0.038(3) 0.008(2) 0.003(2) 0.007(2) C57 0.028(2) 0.024(2) 0.034(3) 0.012(2) -0.0077(18) -0.001(2) C58 0.034(2) 0.026(2) 0.032(3) 0.012(2) 0.0061(18) 0.004(2) C59 0.026(2) 0.056(3) 0.068(4) 0.036(3) 0.006(2) 0.002(2) C60 0.057(3) 0.026(2) 0.044(3) 0.016(2) 0.018(2) 0.012(2) C61 0.026(2) 0.024(2) 0.027(2) 0.0094(19) 0.0022(17) -0.0040(19) C62 0.029(2) 0.017(2) 0.040(3) 0.010(2) -0.0015(19) -0.0022(19) C63 0.055(3) 0.025(3) 0.035(3) 0.009(2) -0.008(2) 0.003(2) C64 0.026(2) 0.035(3) 0.059(3) 0.022(3) 0.003(2) 0.001(2) C65 0.028(2) 0.024(2) 0.034(3) 0.011(2) 0.0062(18) 0.001(2) C66 0.029(2) 0.023(2) 0.040(3) 0.007(2) 0.0013(18) 0.006(2) C67 0.032(2) 0.026(2) 0.042(3) 0.010(2) 0.002(2) 0.010(2) C68 0.041(3) 0.029(3) 0.046(3) 0.014(2) -0.002(2) -0.011(2) C69 0.059(4) 0.054(3) 0.081(4) 0.049(3) -0.014(3) -0.012(3) C70 0.055(3) 0.046(3) 0.037(3) 0.006(2) 0.011(2) -0.025(3) C71 0.039(3) 0.024(2) 0.041(3) 0.011(2) 0.010(2) -0.002(2) C72 0.037(3) 0.056(3) 0.061(4) 0.030(3) 0.001(2) 0.008(3) N1 0.0342(19) 0.0177(17) 0.033(2) 0.0094(16) 0.0004(15) 0.0035(15) N2 0.0283(18) 0.0208(17) 0.038(2) 0.0137(16) 0.0042(15) 0.0023(15) N3 0.0324(19) 0.026(2) 0.036(2) 0.0114(17) 0.0015(15) 0.0086(17) N4 0.0325(19) 0.0183(18) 0.034(2) 0.0092(16) 0.0021(15) 0.0023(16) N5 0.0293(19) 0.0173(18) 0.038(2) 0.0150(17) 0.0009(15) 0.0010(16) N6 0.0277(19) 0.021(2) 0.051(3) 0.0114(19) -0.0068(17) 0.0050(17) N7 0.028(2) 0.023(2) 0.061(3) 0.001(2) -0.0043(18) 0.0041(18) N8 0.034(2) 0.0198(19) 0.055(3) 0.0072(19) 0.0082(18) -0.0020(17) N9 0.033(2) 0.0223(18) 0.037(2) 0.0129(17) 0.0054(15) -0.0019(16) N10 0.0308(18) 0.0160(17) 0.030(2) 0.0104(16) -0.0001(14) -0.0022(15) N11 0.0343(19) 0.0182(18) 0.032(2) 0.0131(16) 0.0027(15) 0.0001(16) N12 0.0272(18) 0.0188(18) 0.034(2) 0.0118(17) -0.0018(15) -0.0027(16) N13 0.033(2) 0.0192(19) 0.033(2) 0.0078(17) -0.0018(15) 0.0022(16) N14 0.035(2) 0.0228(19) 0.036(2) 0.0091(17) -0.0031(16) -0.0058(17) O1 0.0479(19) 0.0234(16) 0.0334(18) 0.0115(14) 0.0029(14) 0.0057(15) O2 0.0375(17) 0.0179(15) 0.0430(18) 0.0096(13) -0.0068(13) 0.0038(13) O3 0.0343(16) 0.0235(15) 0.0367(17) 0.0145(14) 0.0011(12) 0.0032(13) O4 0.0349(17) 0.0220(16) 0.044(2) 0.0126(14) 0.0024(13) 0.0118(14) O5 0.0348(17) 0.0198(16) 0.048(2) 0.0117(15) -0.0088(14) -0.0029(14) O6 0.0380(18) 0.0259(17) 0.048(2) 0.0186(16) 0.0068(15) -0.0005(15) O7 0.049(2) 0.0225(17) 0.058(2) 0.0185(17) -0.0013(17) 0.0070(16) O8 0.0288(17) 0.0365(19) 0.066(2) 0.0242(18) -0.0060(15) -0.0021(16) O9 0.0251(15) 0.0311(17) 0.058(2) 0.0236(16) 0.0002(13) 0.0030(14) O10 0.0360(18) 0.0251(17) 0.054(2) 0.0081(16) -0.0021(15) 0.0074(15) O11 0.0353(17) 0.0225(16) 0.057(2) 0.0096(15) -0.0039(14) -0.0012(14) O12 0.062(2) 0.0337(18) 0.0374(19) 0.0108(16) 0.0155(16) -0.0086(17) O13 0.0372(17) 0.0241(16) 0.042(2) 0.0148(15) 0.0050(13) 0.0030(14) O14 0.0378(18) 0.0200(16) 0.040(2) 0.0119(15) -0.0104(14) -0.0034(14) O15 0.0347(17) 0.0264(17) 0.041(2) 0.0174(16) 0.0038(14) -0.0033(15) O16 0.0426(18) 0.0234(17) 0.043(2) 0.0105(16) -0.0043(15) 0.0079(15) O17 0.0401(18) 0.0270(16) 0.050(2) 0.0130(15) 0.0059(15) -0.0118(15) O18 0.0325(17) 0.0283(17) 0.047(2) 0.0146(15) 0.0046(14) -0.0016(14) S1 0.0291(6) 0.0311(7) 0.0912(12) -0.0142(7) -0.0032(6) -0.0012(6) S2 0.0348(6) 0.0324(7) 0.0592(9) -0.0089(6) 0.0037(6) -0.0019(6) C46S 0.046(3) 0.043(3) 0.063(3) -0.018(3) 0.026(2) -0.009(3) C48S 0.063(5) 0.040(4) 0.040(4) 0.009(3) 0.010(3) 0.011(4) C46 0.046(3) 0.043(3) 0.063(3) -0.018(3) 0.026(2) -0.009(3) C48 0.063(5) 0.040(4) 0.040(4) 0.009(3) 0.010(3) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.378(7) . ? C1 C6 1.379(7) . ? C1 C7 1.504(7) . ? C2 C3 1.382(8) . ? C2 H2 0.9500 . ? C3 C4 1.356(9) . ? C3 H3 0.9500 . ? C4 C5 1.375(9) . ? C4 H4 0.9500 . ? C5 C6 1.378(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.452(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.211(6) . ? C8 N1 1.334(6) . ? C8 O1 1.358(6) . ? C9 N1 1.455(6) . ? C9 C10 1.538(6) . ? C9 C13 1.546(6) . ? C9 H9 1.0000 . ? C10 C11 1.526(6) . ? C10 C12 1.529(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O3 1.227(6) . ? C13 N2 1.327(6) . ? C14 N2 1.475(6) . ? C14 C15 1.525(7) . ? C14 C16 1.535(7) . ? C14 C17 1.557(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O4 1.221(6) . ? C17 N3 1.346(6) . ? C18 N3 1.456(6) . ? C18 C20 1.526(7) . ? C18 C21 1.536(7) . ? C18 C19 1.542(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 O5 1.236(6) . ? C21 N4 1.335(6) . ? C22 N4 1.467(6) . ? C22 C23 1.523(7) . ? C22 C24 1.530(6) . ? C22 C25 1.553(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 O6 1.227(6) . ? C25 N5 1.339(6) . ? C26 N5 1.466(6) . ? C26 C28 1.521(7) . ? C26 C27 1.535(7) . ? C26 C29 1.545(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O7 1.223(6) . ? C29 N6 1.346(6) . ? C30 N6 1.455(6) . ? C30 C31 1.513(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N7 1.318(7) . ? C31 S1 1.678(5) . ? C32 N7 1.462(7) . ? C32 C33 1.516(8) . ? C32 C34 1.522(7) . ? C32 C35 1.530(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 O8 1.210(6) . ? C35 O9 1.327(6) . ? C36 O9 1.451(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.386(7) . ? C37 C42 1.395(7) . ? C37 C43 1.496(7) . ? C38 C39 1.388(7) . ? C38 H38 0.9500 . ? C39 C40 1.400(8) . ? C39 H39 0.9500 . ? C40 C41 1.379(8) . ? C40 H40 0.9500 . ? C41 C42 1.372(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 O10 1.451(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O11 1.217(6) . ? C44 N8 1.346(6) . ? C44 O10 1.353(7) . ? C45 N8 1.448(7) . ? C45 C49 1.519(7) . ? C45 C46S 1.524(6) . ? C45 H45 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C49 O12 1.238(6) . ? C49 N9 1.348(6) . ? C50 N9 1.475(6) . ? C50 C51 1.517(7) . ? C50 C52 1.524(7) . ? C50 C53 1.557(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 O13 1.233(6) . ? C53 N10 1.343(6) . ? C54 N10 1.468(6) . ? C54 C56 1.520(7) . ? C54 C55 1.525(6) . ? C54 C57 1.528(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 O14 1.236(6) . ? C57 N11 1.344(6) . ? C58 N11 1.462(6) . ? C58 C59 1.522(7) . ? C58 C61 1.537(7) . ? C58 C60 1.540(7) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 O15 1.234(6) . ? C61 N12 1.347(6) . ? C62 N12 1.465(6) . ? C62 C64 1.524(7) . ? C62 C65 1.548(6) . ? C62 C63 1.553(7) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 O16 1.231(6) . ? C65 N13 1.337(6) . ? C66 N13 1.458(6) . ? C66 C67 1.511(7) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 N14 1.323(6) . ? C67 S2 1.663(5) . ? C68 N14 1.482(7) . ? C68 C71 1.515(7) . ? C68 C70 1.526(7) . ? C68 C69 1.531(8) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 O17 1.211(6) . ? C71 O18 1.326(6) . ? C72 O18 1.442(6) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N1 H1 0.8800 . ? N2 H2A 0.8800 . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? N5 H5A 0.8800 . ? N6 H6A 0.8800 . ? N7 H7 0.8800 . ? N8 H8 0.8800 . ? N9 H9A 0.8800 . ? N10 H10A 0.8800 . ? N11 H11 0.8800 . ? N12 H12 0.8800 . ? N13 H13 0.8800 . ? N14 H14 0.8800 . ? C46S C48S 1.479(4) . ? C48S H48D 0.9800 . ? C48S H48E 0.9800 . ? C48S H48F 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.7(5) . . ? C2 C1 C7 123.6(5) . . ? C6 C1 C7 117.6(4) . . ? C1 C2 C3 119.9(5) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 121.3(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 119.1(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.6(5) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? O1 C7 C1 112.9(4) . . ? O1 C7 H7A 109.0 . . ? C1 C7 H7A 109.0 . . ? O1 C7 H7B 109.0 . . ? C1 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O2 C8 N1 126.5(5) . . ? O2 C8 O1 123.0(4) . . ? N1 C8 O1 110.4(4) . . ? N1 C9 C10 113.8(3) . . ? N1 C9 C13 113.5(3) . . ? C10 C9 C13 112.4(3) . . ? N1 C9 H9 105.4 . . ? C10 C9 H9 105.4 . . ? C13 C9 H9 105.4 . . ? C11 C10 C12 112.3(3) . . ? C11 C10 C9 108.8(4) . . ? C12 C10 C9 113.0(3) . . ? C11 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C9 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 N2 122.8(4) . . ? O3 C13 C9 120.7(4) . . ? N2 C13 C9 116.3(4) . . ? N2 C14 C15 108.8(4) . . ? N2 C14 C16 110.8(4) . . ? C15 C14 C16 110.6(4) . . ? N2 C14 C17 110.8(3) . . ? C15 C14 C17 106.7(4) . . ? C16 C14 C17 109.2(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 N3 123.1(4) . . ? O4 C17 C14 120.8(4) . . ? N3 C17 C14 116.1(4) . . ? N3 C18 C20 110.9(4) . . ? N3 C18 C21 110.8(4) . . ? C20 C18 C21 111.5(4) . . ? N3 C18 C19 108.2(4) . . ? C20 C18 C19 109.7(4) . . ? C21 C18 C19 105.6(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 N4 122.7(5) . . ? O5 C21 C18 120.2(5) . . ? N4 C21 C18 117.0(4) . . ? N4 C22 C23 107.4(4) . . ? N4 C22 C24 110.2(4) . . ? C23 C22 C24 110.3(4) . . ? N4 C22 C25 110.5(4) . . ? C23 C22 C25 108.5(4) . . ? C24 C22 C25 109.9(4) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O6 C25 N5 123.8(4) . . ? O6 C25 C22 120.0(4) . . ? N5 C25 C22 116.2(4) . . ? N5 C26 C28 111.6(4) . . ? N5 C26 C27 107.3(4) . . ? C28 C26 C27 110.8(4) . . ? N5 C26 C29 111.3(4) . . ? C28 C26 C29 109.5(4) . . ? C27 C26 C29 106.2(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O7 C29 N6 123.2(4) . . ? O7 C29 C26 119.4(4) . . ? N6 C29 C26 117.3(4) . . ? N6 C30 C31 115.1(4) . . ? N6 C30 H30A 108.5 . . ? C31 C30 H30A 108.5 . . ? N6 C30 H30B 108.5 . . ? C31 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? N7 C31 C30 117.9(4) . . ? N7 C31 S1 124.2(4) . . ? C30 C31 S1 117.9(4) . . ? N7 C32 C33 108.4(4) . . ? N7 C32 C34 110.7(4) . . ? C33 C32 C34 110.9(5) . . ? N7 C32 C35 110.9(5) . . ? C33 C32 C35 107.2(4) . . ? C34 C32 C35 108.6(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O8 C35 O9 124.2(4) . . ? O8 C35 C32 124.0(5) . . ? O9 C35 C32 111.3(4) . . ? O9 C36 H36A 109.5 . . ? O9 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O9 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 118.9(5) . . ? C38 C37 C43 123.6(5) . . ? C42 C37 C43 117.5(4) . . ? C37 C38 C39 120.7(5) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C40 119.9(5) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C41 C40 C39 118.9(5) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C42 C41 C40 121.2(5) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C41 C42 C37 120.4(5) . . ? C41 C42 H42 119.8 . . ? C37 C42 H42 119.8 . . ? O10 C43 C37 113.2(4) . . ? O10 C43 H43A 108.9 . . ? C37 C43 H43A 108.9 . . ? O10 C43 H43B 108.9 . . ? C37 C43 H43B 108.9 . . ? H43A C43 H43B 107.8 . . ? O11 C44 N8 124.6(5) . . ? O11 C44 O10 124.1(5) . . ? N8 C44 O10 111.3(4) . . ? N8 C45 C49 112.7(4) . . ? N8 C45 C46S 110.7(4) . . ? C49 C45 C46S 111.3(4) . . ? N8 C45 H45 107.3 . . ? C49 C45 H45 107.3 . . ? C46S C45 H45 107.3 . . ? O12 C49 N9 121.7(5) . . ? O12 C49 C45 119.8(4) . . ? N9 C49 C45 118.5(4) . . ? N9 C50 C51 112.0(4) . . ? N9 C50 C52 108.4(4) . . ? C51 C50 C52 110.7(4) . . ? N9 C50 C53 109.8(4) . . ? C51 C50 C53 109.8(4) . . ? C52 C50 C53 106.1(4) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O13 C53 N10 122.7(4) . . ? O13 C53 C50 120.1(4) . . ? N10 C53 C50 117.1(4) . . ? N10 C54 C56 110.5(4) . . ? N10 C54 C55 108.4(4) . . ? C56 C54 C55 110.3(4) . . ? N10 C54 C57 109.6(4) . . ? C56 C54 C57 111.1(4) . . ? C55 C54 C57 106.8(4) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O14 C57 N11 121.6(5) . . ? O14 C57 C54 121.2(4) . . ? N11 C57 C54 117.0(4) . . ? N11 C58 C59 109.9(4) . . ? N11 C58 C61 111.2(4) . . ? C59 C58 C61 110.3(4) . . ? N11 C58 C60 107.1(4) . . ? C59 C58 C60 110.8(4) . . ? C61 C58 C60 107.5(4) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O15 C61 N12 122.1(5) . . ? O15 C61 C58 120.2(4) . . ? N12 C61 C58 117.6(4) . . ? N12 C62 C64 108.3(4) . . ? N12 C62 C65 111.1(4) . . ? C64 C62 C65 106.8(4) . . ? N12 C62 C63 111.3(4) . . ? C64 C62 C63 110.3(4) . . ? C65 C62 C63 109.0(4) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O16 C65 N13 123.0(4) . . ? O16 C65 C62 119.9(4) . . ? N13 C65 C62 117.1(4) . . ? N13 C66 C67 115.5(4) . . ? N13 C66 H66A 108.4 . . ? C67 C66 H66A 108.4 . . ? N13 C66 H66B 108.4 . . ? C67 C66 H66B 108.4 . . ? H66A C66 H66B 107.5 . . ? N14 C67 C66 116.8(4) . . ? N14 C67 S2 124.5(4) . . ? C66 C67 S2 118.8(4) . . ? N14 C68 C71 110.1(4) . . ? N14 C68 C70 106.8(4) . . ? C71 C68 C70 107.9(4) . . ? N14 C68 C69 109.5(5) . . ? C71 C68 C69 111.2(4) . . ? C70 C68 C69 111.3(5) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O17 C71 O18 124.3(5) . . ? O17 C71 C68 123.9(5) . . ? O18 C71 C68 111.4(4) . . ? O18 C72 H72A 109.5 . . ? O18 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? O18 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C8 N1 C9 123.1(4) . . ? C8 N1 H1 118.4 . . ? C9 N1 H1 118.4 . . ? C13 N2 C14 122.3(4) . . ? C13 N2 H2A 118.9 . . ? C14 N2 H2A 118.9 . . ? C17 N3 C18 122.2(4) . . ? C17 N3 H3A 118.9 . . ? C18 N3 H3A 118.9 . . ? C21 N4 C22 122.2(4) . . ? C21 N4 H4A 118.9 . . ? C22 N4 H4A 118.9 . . ? C25 N5 C26 122.8(4) . . ? C25 N5 H5A 118.6 . . ? C26 N5 H5A 118.6 . . ? C29 N6 C30 121.9(4) . . ? C29 N6 H6A 119.0 . . ? C30 N6 H6A 119.0 . . ? C31 N7 C32 126.2(4) . . ? C31 N7 H7 116.9 . . ? C32 N7 H7 116.9 . . ? C44 N8 C45 119.2(4) . . ? C44 N8 H8 120.4 . . ? C45 N8 H8 120.4 . . ? C49 N9 C50 123.1(4) . . ? C49 N9 H9A 118.4 . . ? C50 N9 H9A 118.4 . . ? C53 N10 C54 122.6(4) . . ? C53 N10 H10A 118.7 . . ? C54 N10 H10A 118.7 . . ? C57 N11 C58 123.5(4) . . ? C57 N11 H11 118.3 . . ? C58 N11 H11 118.3 . . ? C61 N12 C62 123.0(4) . . ? C61 N12 H12 118.5 . . ? C62 N12 H12 118.5 . . ? C65 N13 C66 122.6(4) . . ? C65 N13 H13 118.7 . . ? C66 N13 H13 118.7 . . ? C67 N14 C68 125.5(4) . . ? C67 N14 H14 117.3 . . ? C68 N14 H14 117.3 . . ? C8 O1 C7 115.1(4) . . ? C35 O9 C36 115.5(4) . . ? C44 O10 C43 114.5(4) . . ? C71 O18 C72 115.9(4) . . ? C48S C46S C45 111.1(6) . . ? C46S C48S H48D 109.5 . . ? C46S C48S H48E 109.5 . . ? H48D C48S H48E 109.5 . . ? C46S C48S H48F 109.5 . . ? H48D C48S H48F 109.5 . . ? H48E C48S H48F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.2(8) . . . . ? C7 C1 C2 C3 -176.9(5) . . . . ? C1 C2 C3 C4 -0.8(10) . . . . ? C2 C3 C4 C5 1.0(10) . . . . ? C3 C4 C5 C6 -0.6(10) . . . . ? C4 C5 C6 C1 0.0(9) . . . . ? C2 C1 C6 C5 0.1(8) . . . . ? C7 C1 C6 C5 177.4(5) . . . . ? C2 C1 C7 O1 -18.5(7) . . . . ? C6 C1 C7 O1 164.4(5) . . . . ? N1 C9 C10 C11 -66.0(4) . . . . ? C13 C9 C10 C11 163.1(3) . . . . ? N1 C9 C10 C12 59.5(5) . . . . ? C13 C9 C10 C12 -71.4(4) . . . . ? N1 C9 C13 O3 -135.7(4) . . . . ? C10 C9 C13 O3 -4.8(5) . . . . ? N1 C9 C13 N2 47.9(5) . . . . ? C10 C9 C13 N2 178.9(4) . . . . ? N2 C14 C17 O4 -149.3(4) . . . . ? C15 C14 C17 O4 92.5(5) . . . . ? C16 C14 C17 O4 -27.1(6) . . . . ? N2 C14 C17 N3 33.4(6) . . . . ? C15 C14 C17 N3 -84.7(5) . . . . ? C16 C14 C17 N3 155.7(4) . . . . ? N3 C18 C21 O5 -149.9(4) . . . . ? C20 C18 C21 O5 -25.9(6) . . . . ? C19 C18 C21 O5 93.1(5) . . . . ? N3 C18 C21 N4 33.7(5) . . . . ? C20 C18 C21 N4 157.7(4) . . . . ? C19 C18 C21 N4 -83.2(5) . . . . ? N4 C22 C25 O6 -147.6(4) . . . . ? C23 C22 C25 O6 94.9(5) . . . . ? C24 C22 C25 O6 -25.8(6) . . . . ? N4 C22 C25 N5 34.8(6) . . . . ? C23 C22 C25 N5 -82.7(5) . . . . ? C24 C22 C25 N5 156.6(4) . . . . ? N5 C26 C29 O7 -162.3(4) . . . . ? C28 C26 C29 O7 -38.4(6) . . . . ? C27 C26 C29 O7 81.3(6) . . . . ? N5 C26 C29 N6 20.6(6) . . . . ? C28 C26 C29 N6 144.5(4) . . . . ? C27 C26 C29 N6 -95.8(5) . . . . ? N6 C30 C31 N7 -0.9(7) . . . . ? N6 C30 C31 S1 178.9(4) . . . . ? N7 C32 C35 O8 139.9(5) . . . . ? C33 C32 C35 O8 -102.0(6) . . . . ? C34 C32 C35 O8 18.0(8) . . . . ? N7 C32 C35 O9 -47.9(5) . . . . ? C33 C32 C35 O9 70.2(6) . . . . ? C34 C32 C35 O9 -169.9(5) . . . . ? C42 C37 C38 C39 -1.4(9) . . . . ? C43 C37 C38 C39 176.4(6) . . . . ? C37 C38 C39 C40 1.2(10) . . . . ? C38 C39 C40 C41 0.4(10) . . . . ? C39 C40 C41 C42 -1.7(10) . . . . ? C40 C41 C42 C37 1.5(10) . . . . ? C38 C37 C42 C41 0.1(9) . . . . ? C43 C37 C42 C41 -177.8(6) . . . . ? C38 C37 C43 O10 18.1(8) . . . . ? C42 C37 C43 O10 -164.1(5) . . . . ? N8 C45 C49 O12 150.7(4) . . . . ? C46S C45 C49 O12 -84.2(5) . . . . ? N8 C45 C49 N9 -27.0(6) . . . . ? C46S C45 C49 N9 98.1(5) . . . . ? N9 C50 C53 O13 153.8(4) . . . . ? C51 C50 C53 O13 30.3(6) . . . . ? C52 C50 C53 O13 -89.3(5) . . . . ? N9 C50 C53 N10 -28.8(6) . . . . ? C51 C50 C53 N10 -152.3(4) . . . . ? C52 C50 C53 N10 88.1(5) . . . . ? N10 C54 C57 O14 148.8(4) . . . . ? C56 C54 C57 O14 26.3(6) . . . . ? C55 C54 C57 O14 -94.0(5) . . . . ? N10 C54 C57 N11 -35.6(5) . . . . ? C56 C54 C57 N11 -158.1(4) . . . . ? C55 C54 C57 N11 81.6(5) . . . . ? N11 C58 C61 O15 148.8(4) . . . . ? C59 C58 C61 O15 26.6(6) . . . . ? C60 C58 C61 O15 -94.3(5) . . . . ? N11 C58 C61 N12 -32.8(6) . . . . ? C59 C58 C61 N12 -155.0(4) . . . . ? C60 C58 C61 N12 84.1(5) . . . . ? N12 C62 C65 O16 160.4(4) . . . . ? C64 C62 C65 O16 -81.7(5) . . . . ? C63 C62 C65 O16 37.4(6) . . . . ? N12 C62 C65 N13 -21.1(6) . . . . ? C64 C62 C65 N13 96.7(5) . . . . ? C63 C62 C65 N13 -144.2(4) . . . . ? N13 C66 C67 N14 2.5(6) . . . . ? N13 C66 C67 S2 -177.5(3) . . . . ? N14 C68 C71 O17 -143.1(5) . . . . ? C70 C68 C71 O17 100.7(6) . . . . ? C69 C68 C71 O17 -21.6(7) . . . . ? N14 C68 C71 O18 44.0(6) . . . . ? C70 C68 C71 O18 -72.2(5) . . . . ? C69 C68 C71 O18 165.5(5) . . . . ? O2 C8 N1 C9 7.5(7) . . . . ? O1 C8 N1 C9 -172.3(4) . . . . ? C10 C9 N1 C8 -94.6(5) . . . . ? C13 C9 N1 C8 35.6(6) . . . . ? O3 C13 N2 C14 -0.8(7) . . . . ? C9 C13 N2 C14 175.4(4) . . . . ? C15 C14 N2 C13 169.3(4) . . . . ? C16 C14 N2 C13 -68.9(5) . . . . ? C17 C14 N2 C13 52.4(6) . . . . ? O4 C17 N3 C18 0.8(7) . . . . ? C14 C17 N3 C18 177.9(4) . . . . ? C20 C18 N3 C17 -73.5(6) . . . . ? C21 C18 N3 C17 50.9(6) . . . . ? C19 C18 N3 C17 166.2(4) . . . . ? O5 C21 N4 C22 -3.6(7) . . . . ? C18 C21 N4 C22 172.7(4) . . . . ? C23 C22 N4 C21 172.4(4) . . . . ? C24 C22 N4 C21 -67.4(6) . . . . ? C25 C22 N4 C21 54.2(5) . . . . ? O6 C25 N5 C26 0.9(7) . . . . ? C22 C25 N5 C26 178.4(4) . . . . ? C28 C26 N5 C25 -63.6(6) . . . . ? C27 C26 N5 C25 174.9(4) . . . . ? C29 C26 N5 C25 59.1(6) . . . . ? O7 C29 N6 C30 1.3(8) . . . . ? C26 C29 N6 C30 178.4(4) . . . . ? C31 C30 N6 C29 87.8(6) . . . . ? C30 C31 N7 C32 -174.9(5) . . . . ? S1 C31 N7 C32 5.2(7) . . . . ? C33 C32 N7 C31 -166.9(5) . . . . ? C34 C32 N7 C31 71.2(6) . . . . ? C35 C32 N7 C31 -49.4(6) . . . . ? O11 C44 N8 C45 1.8(7) . . . . ? O10 C44 N8 C45 -179.4(4) . . . . ? C49 C45 N8 C44 -60.6(5) . . . . ? C46S C45 N8 C44 174.0(4) . . . . ? O12 C49 N9 C50 -0.6(7) . . . . ? C45 C49 N9 C50 177.0(4) . . . . ? C51 C50 N9 C49 67.7(6) . . . . ? C52 C50 N9 C49 -170.0(4) . . . . ? C53 C50 N9 C49 -54.6(6) . . . . ? O13 C53 N10 C54 -2.4(7) . . . . ? C50 C53 N10 C54 -179.7(4) . . . . ? C56 C54 N10 C53 74.1(6) . . . . ? C55 C54 N10 C53 -164.9(4) . . . . ? C57 C54 N10 C53 -48.7(6) . . . . ? O14 C57 N11 C58 3.3(7) . . . . ? C54 C57 N11 C58 -172.3(4) . . . . ? C59 C58 N11 C57 67.6(6) . . . . ? C61 C58 N11 C57 -54.8(5) . . . . ? C60 C58 N11 C57 -172.0(4) . . . . ? O15 C61 N12 C62 -1.9(7) . . . . ? C58 C61 N12 C62 179.7(4) . . . . ? C64 C62 N12 C61 -175.8(4) . . . . ? C65 C62 N12 C61 -58.9(6) . . . . ? C63 C62 N12 C61 62.8(5) . . . . ? O16 C65 N13 C66 -1.7(7) . . . . ? C62 C65 N13 C66 179.9(4) . . . . ? C67 C66 N13 C65 -83.2(5) . . . . ? C66 C67 N14 C68 174.1(4) . . . . ? S2 C67 N14 C68 -5.9(7) . . . . ? C71 C68 N14 C67 50.8(6) . . . . ? C70 C68 N14 C67 167.6(5) . . . . ? C69 C68 N14 C67 -71.8(6) . . . . ? O2 C8 O1 C7 -1.0(6) . . . . ? N1 C8 O1 C7 178.8(4) . . . . ? C1 C7 O1 C8 -76.4(5) . . . . ? O8 C35 O9 C36 -7.6(8) . . . . ? C32 C35 O9 C36 -179.7(4) . . . . ? O11 C44 O10 C43 -2.8(7) . . . . ? N8 C44 O10 C43 178.4(4) . . . . ? C37 C43 O10 C44 76.0(6) . . . . ? O17 C71 O18 C72 8.9(7) . . . . ? C68 C71 O18 C72 -178.2(4) . . . . ? N8 C45 C46S C48S -155.5(6) . . . . ? C49 C45 C46S C48S 78.4(7) . . . . ? 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 H1 O7 0.88 2.03 2.893(5) 166.6 1_565 N2 H2A O8 0.88 2.21 3.071(5) 165.2 1_665 N3 H3A O2 0.88 2.04 2.829(5) 149.4 . N4 H4A O3 0.88 2.12 2.971(5) 161.6 . N5 H5A O4 0.88 2.29 3.097(5) 152.4 . N6 H6A O5 0.88 1.99 2.838(5) 160.8 . N7 H7 O6 0.88 2.23 3.090(5) 164.9 . N7 H7 N6 0.88 2.31 2.751(6) 110.8 . N8 H8 O16 0.88 2.09 2.907(5) 153.3 1_545 N9 H9A O17 0.88 2.17 3.024(5) 163.4 1_445 N10 H10A O11 0.88 2.12 2.934(5) 153.5 . N11 H11 O12 0.88 2.12 2.974(5) 162.8 . N12 H12 O13 0.88 2.24 3.050(5) 153.5 . N13 H13 O14 0.88 1.99 2.831(5) 158.7 . N14 H14 O15 0.88 2.19 3.037(5) 161.7 . N14 H14 N13 0.88 2.30 2.739(5) 111.2 . _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 66.59 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.237 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.041 _database_code_depnum_ccdc_archive 'CCDC 969434' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_s3839na #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H53 N7 O9 S' _chemical_formula_weight 735.89 _chemical_absolute_configuration ad 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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5005(2) _cell_length_b 14.2234(3) _cell_length_c 15.3975(3) _cell_angle_alpha 89.612(2) _cell_angle_beta 84.6750(10) _cell_angle_gamma 78.797(2) _cell_volume 2032.07(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4151 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 69.89 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.688175 _exptl_absorpt_correction_T_max 0.9011 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13502 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.26 _diffrn_reflns_theta_max 70.15 _reflns_number_total 9113 _reflns_number_gt 7762 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+0.0299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(2) _refine_ls_number_reflns 9113 _refine_ls_number_parameters 943 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 C1 C 0.7708(5) 0.5893(4) 0.4823(3) 0.0311(10) Uani 1 1 d . . . C2 C 0.6344(6) 0.5826(4) 0.5144(3) 0.0371(11) Uani 1 1 d . . . H2 H 0.5926 0.6172 0.5660 0.045 Uiso 1 1 calc R . . C3 C 0.5532(7) 0.5252(5) 0.4724(4) 0.0490(14) Uani 1 1 d . . . H3 H 0.4570 0.5229 0.4939 0.059 Uiso 1 1 calc R . . C4 C 0.6198(8) 0.4728(5) 0.3990(4) 0.0518(15) Uani 1 1 d . . . H4 H 0.5698 0.4320 0.3706 0.062 Uiso 1 1 calc R . . C5 C 0.7569(6) 0.4794(5) 0.3673(4) 0.0436(13) Uani 1 1 d . . . H5 H 0.8005 0.4433 0.3168 0.052 Uiso 1 1 calc R . . C6 C 0.8345(5) 0.5385(4) 0.4079(3) 0.0360(11) Uani 1 1 d . . . H6 H 0.9290 0.5434 0.3847 0.043 Uiso 1 1 calc R . . C7 C 0.8577(5) 0.6549(4) 0.5210(3) 0.0300(10) Uani 1 1 d . . . H7A H 0.9589 0.6207 0.5211 0.036 Uiso 1 1 calc R . . H7B H 0.8570 0.7117 0.4834 0.036 Uiso 1 1 calc R . . C8 C 0.8369(4) 0.6192(3) 0.6700(3) 0.0228(8) Uani 1 1 d . . . C9 C 0.8148(5) 0.5937(3) 0.8251(3) 0.0276(9) Uani 1 1 d . . . H9 H 0.9212 0.5700 0.8245 0.033 Uiso 1 1 calc R . . C10 C 0.7642(6) 0.6519(4) 0.9077(3) 0.0402(11) Uani 1 1 d . . . H10A H 0.8246 0.6997 0.9132 0.060 Uiso 1 1 calc R . . H10B H 0.7714 0.6093 0.9581 0.060 Uiso 1 1 calc R . . H10C H 0.6637 0.6844 0.9055 0.060 Uiso 1 1 calc R . . C11 C 0.7426(5) 0.5061(3) 0.8225(3) 0.0264(9) Uani 1 1 d . . . C12 C 0.5453(5) 0.4382(3) 0.7695(3) 0.0260(9) Uani 1 1 d . . . C13 C 0.4740(6) 0.4112(4) 0.8569(4) 0.0437(13) Uani 1 1 d . . . H13A H 0.5467 0.3962 0.8987 0.066 Uiso 1 1 calc R . . H13B H 0.4308 0.3551 0.8487 0.066 Uiso 1 1 calc R . . H13C H 0.3989 0.4651 0.8792 0.066 Uiso 1 1 calc R . . C14 C 0.4281(5) 0.4719(4) 0.7064(4) 0.0375(11) Uani 1 1 d . . . H14A H 0.3585 0.5268 0.7324 0.056 Uiso 1 1 calc R . . H14B H 0.3782 0.4194 0.6961 0.056 Uiso 1 1 calc R . . H14C H 0.4734 0.4908 0.6510 0.056 Uiso 1 1 calc R . . C15 C 0.6452(4) 0.3494(3) 0.7272(3) 0.0236(9) Uani 1 1 d . . . C16 C 0.8722(5) 0.2862(3) 0.6354(3) 0.0230(9) Uani 1 1 d . . . C17 C 0.8130(6) 0.2446(4) 0.5575(3) 0.0356(11) Uani 1 1 d . . . H17A H 0.7250 0.2214 0.5777 0.053 Uiso 1 1 calc R . . H17B H 0.8853 0.1912 0.5313 0.053 Uiso 1 1 calc R . . H17C H 0.7909 0.2945 0.5140 0.053 Uiso 1 1 calc R . . C18 C 1.0080(5) 0.3260(4) 0.6052(3) 0.0325(10) Uani 1 1 d . . . H18A H 0.9827 0.3798 0.5659 0.049 Uiso 1 1 calc R . . H18B H 1.0798 0.2754 0.5745 0.049 Uiso 1 1 calc R . . H18C H 1.0480 0.3480 0.6561 0.049 Uiso 1 1 calc R . . C19 C 0.9150(4) 0.2085(3) 0.7033(3) 0.0213(8) Uani 1 1 d . . . C20 C 0.9665(5) 0.1726(3) 0.8549(3) 0.0247(9) Uani 1 1 d . . . C21 C 0.9223(5) 0.2270(4) 0.9415(3) 0.0326(10) Uani 1 1 d . . . H21A H 0.9669 0.2836 0.9414 0.049 Uiso 1 1 calc R . . H21B H 0.9543 0.1851 0.9896 0.049 Uiso 1 1 calc R . . H21C H 0.8172 0.2472 0.9491 0.049 Uiso 1 1 calc R . . C22 C 1.1297(5) 0.1386(4) 0.8412(4) 0.0377(11) Uani 1 1 d . . . H22A H 1.1555 0.1065 0.7842 0.056 Uiso 1 1 calc R . . H22B H 1.1613 0.0938 0.8873 0.056 Uiso 1 1 calc R . . H22C H 1.1769 0.1939 0.8432 0.056 Uiso 1 1 calc R . . C23 C 0.8921(4) 0.0847(3) 0.8590(3) 0.0215(8) Uani 1 1 d . . . C24 C 0.6713(4) 0.0231(3) 0.8415(3) 0.0226(9) Uani 1 1 d . . . C25 C 0.6446(6) -0.0113(4) 0.9344(3) 0.0392(12) Uani 1 1 d . . . H25A H 0.7368 -0.0302 0.9596 0.059 Uiso 1 1 calc R . . H25B H 0.5969 -0.0665 0.9337 0.059 Uiso 1 1 calc R . . H25C H 0.5830 0.0405 0.9696 0.059 Uiso 1 1 calc R . . C26 C 0.5273(5) 0.0621(4) 0.8050(4) 0.0364(12) Uani 1 1 d . . . H26A H 0.4682 0.1097 0.8457 0.055 Uiso 1 1 calc R . . H26B H 0.4766 0.0094 0.7972 0.055 Uiso 1 1 calc R . . H26C H 0.5447 0.0922 0.7486 0.055 Uiso 1 1 calc R . . C27 C 0.7483(4) -0.0633(3) 0.7828(3) 0.0235(9) Uani 1 1 d . . . C28 C 0.9198(5) -0.1169(3) 0.6557(3) 0.0256(9) Uani 1 1 d . . . H28A H 0.9477 -0.0852 0.6011 0.031 Uiso 1 1 calc R . . H28B H 0.8538 -0.1594 0.6414 0.031 Uiso 1 1 calc R . . C29 C 1.0547(5) -0.1790(3) 0.6865(3) 0.0294(10) Uani 1 1 d . . . C30 C 1.2128(5) -0.2121(4) 0.8065(3) 0.0328(11) Uani 1 1 d . . . C31 C 1.1819(6) -0.3090(4) 0.8369(4) 0.0444(13) Uani 1 1 d . . . H31A H 1.1054 -0.2992 0.8851 0.067 Uiso 1 1 calc R . . H31B H 1.2695 -0.3481 0.8568 0.067 Uiso 1 1 calc R . . H31C H 1.1511 -0.3418 0.7885 0.067 Uiso 1 1 calc R . . C32 C 1.2362(6) -0.1528(4) 0.8850(4) 0.0433(12) Uani 1 1 d . . . H32A H 1.2604 -0.0920 0.8647 0.065 Uiso 1 1 calc R . . H32B H 1.3152 -0.1887 0.9157 0.065 Uiso 1 1 calc R . . H32C H 1.1478 -0.1400 0.9248 0.065 Uiso 1 1 calc R . . C33 C 1.3509(5) -0.2242(4) 0.7444(4) 0.0347(11) Uani 1 1 d . . . C34 C 1.4832(6) -0.1479(5) 0.6386(4) 0.0448(13) Uani 1 1 d . . . H34A H 1.5707 -0.1791 0.6643 0.067 Uiso 1 1 calc R . . H34B H 1.4919 -0.0827 0.6213 0.067 Uiso 1 1 calc R . . H34C H 1.4706 -0.1846 0.5872 0.067 Uiso 1 1 calc R . . C35 C 0.3158(5) 0.0159(4) 0.4765(3) 0.0298(10) Uani 1 1 d . . . C36 C 0.4630(6) 0.0067(4) 0.4489(4) 0.0414(13) Uani 1 1 d . . . H36 H 0.5061 -0.0325 0.4001 0.050 Uiso 1 1 calc R . . C37 C 0.5417(7) 0.0561(6) 0.4945(4) 0.063(2) Uani 1 1 d . . . H37 H 0.6406 0.0523 0.4751 0.075 Uiso 1 1 calc R . . C38 C 0.4867(8) 0.1104(6) 0.5661(4) 0.062(2) Uani 1 1 d . . . H38 H 0.5466 0.1424 0.5964 0.074 Uiso 1 1 calc R . . C39 C 0.3425(8) 0.1188(5) 0.5945(4) 0.0533(16) Uani 1 1 d . . . H39 H 0.3017 0.1570 0.6443 0.064 Uiso 1 1 calc R . . C40 C 0.2592(6) 0.0710(4) 0.5496(3) 0.0383(12) Uani 1 1 d . . . H40 H 0.1602 0.0760 0.5692 0.046 Uiso 1 1 calc R . . C41 C 0.2180(6) -0.0361(4) 0.4321(3) 0.0360(11) Uani 1 1 d . . . H41A H 0.1991 -0.0906 0.4687 0.043 Uiso 1 1 calc R . . H41B H 0.1247 0.0080 0.4273 0.043 Uiso 1 1 calc R . . C42 C 0.2668(5) -0.0062(3) 0.2821(3) 0.0254(9) Uani 1 1 d . . . C43 C 0.3359(5) 0.0110(3) 0.1275(3) 0.0318(9) Uani 1 1 d . . . H43 H 0.4068 -0.0288 0.0838 0.038 Uiso 1 1 calc R . . C44 C 0.1911(7) 0.0357(4) 0.0874(4) 0.0580(16) Uani 1 1 d . . . H44A H 0.1630 -0.0235 0.0695 0.087 Uiso 1 1 calc R . . H44B H 0.2008 0.0764 0.0364 0.087 Uiso 1 1 calc R . . H44C H 0.1171 0.0699 0.1307 0.087 Uiso 1 1 calc R . . C45 C 0.3915(5) 0.1035(3) 0.1433(3) 0.0295(10) Uani 1 1 d . . . C46 C 0.5696(5) 0.1767(3) 0.2113(3) 0.0283(10) Uani 1 1 d . . . C47 C 0.6715(6) 0.1472(4) 0.2817(4) 0.0414(12) Uani 1 1 d . . . H47A H 0.6180 0.1262 0.3334 0.062 Uiso 1 1 calc R . . H47B H 0.7132 0.2019 0.2973 0.062 Uiso 1 1 calc R . . H47C H 0.7488 0.0944 0.2597 0.062 Uiso 1 1 calc R . . C48 C 0.6512(6) 0.2046(4) 0.1275(4) 0.0418(13) Uani 1 1 d . . . H48A H 0.7196 0.1483 0.1032 0.063 Uiso 1 1 calc R . . H48B H 0.7036 0.2548 0.1408 0.063 Uiso 1 1 calc R . . H48C H 0.5824 0.2284 0.0850 0.063 Uiso 1 1 calc R . . C49 C 0.4558(5) 0.2644(3) 0.2468(3) 0.0252(9) Uani 1 1 d . . . C50 C 0.2244(5) 0.3229(3) 0.3315(3) 0.0268(10) Uani 1 1 d . . . C51 C 0.2720(7) 0.3699(4) 0.4087(3) 0.0432(13) Uani 1 1 d . . . H51A H 0.3090 0.3206 0.4500 0.065 Uiso 1 1 calc R . . H51B H 0.1898 0.4147 0.4375 0.065 Uiso 1 1 calc R . . H51C H 0.3481 0.4047 0.3884 0.065 Uiso 1 1 calc R . . C52 C 0.0919(5) 0.2785(4) 0.3612(3) 0.0329(11) Uani 1 1 d . . . H52A H 0.0638 0.2460 0.3116 0.049 Uiso 1 1 calc R . . H52B H 0.0117 0.3293 0.3834 0.049 Uiso 1 1 calc R . . H52C H 0.1163 0.2322 0.4075 0.049 Uiso 1 1 calc R . . C53 C 0.1755(4) 0.3987(3) 0.2624(3) 0.0261(10) Uani 1 1 d . . . C54 C 0.1344(4) 0.4314(3) 0.1088(3) 0.0264(9) Uani 1 1 d . . . C55 C 0.1898(6) 0.3788(4) 0.0230(3) 0.0340(11) Uani 1 1 d . . . H55A H 0.2953 0.3676 0.0162 0.051 Uiso 1 1 calc R . . H55B H 0.1516 0.4176 -0.0254 0.051 Uiso 1 1 calc R . . H55C H 0.1581 0.3172 0.0230 0.051 Uiso 1 1 calc R . . C56 C -0.0306(5) 0.4581(4) 0.1167(4) 0.0423(13) Uani 1 1 d . . . H56A H -0.0706 0.3996 0.1164 0.063 Uiso 1 1 calc R . . H56B H -0.0620 0.4982 0.0674 0.063 Uiso 1 1 calc R . . H56C H -0.0647 0.4936 0.1714 0.063 Uiso 1 1 calc R . . C57 C 0.1983(5) 0.5232(3) 0.1094(3) 0.0251(9) Uani 1 1 d . . . C58 C 0.4131(5) 0.5906(3) 0.1302(3) 0.0255(9) Uani 1 1 d . . . C59 C 0.5575(5) 0.5514(4) 0.1666(4) 0.0357(12) Uani 1 1 d . . . H59A H 0.5400 0.5319 0.2272 0.054 Uiso 1 1 calc R . . H59B H 0.6157 0.6013 0.1643 0.054 Uiso 1 1 calc R . . H59C H 0.6089 0.4959 0.1315 0.054 Uiso 1 1 calc R . . C60 C 0.4360(6) 0.6274(4) 0.0374(3) 0.0386(12) Uani 1 1 d . . . H60A H 0.4947 0.5759 0.0003 0.058 Uiso 1 1 calc R . . H60B H 0.4856 0.6816 0.0382 0.058 Uiso 1 1 calc R . . H60C H 0.3425 0.6481 0.0142 0.058 Uiso 1 1 calc R . . C61 C 0.3332(5) 0.6727(3) 0.1908(3) 0.0249(9) Uani 1 1 d . . . C62 C 0.1671(4) 0.7229(3) 0.3188(3) 0.0261(9) Uani 1 1 d . . . H62A H 0.2313 0.7676 0.3302 0.031 Uiso 1 1 calc R . . H62B H 0.1467 0.6904 0.3743 0.031 Uiso 1 1 calc R . . C63 C 0.0239(5) 0.7822(4) 0.2922(3) 0.0277(10) Uani 1 1 d . . . C64 C -0.1392(5) 0.8152(4) 0.1747(3) 0.0306(10) Uani 1 1 d . . . C65 C -0.1663(6) 0.7542(4) 0.0986(3) 0.0410(12) Uani 1 1 d . . . H65A H -0.0865 0.7499 0.0527 0.061 Uiso 1 1 calc R . . H65B H -0.2567 0.7840 0.0751 0.061 Uiso 1 1 calc R . . H65C H -0.1731 0.6898 0.1192 0.061 Uiso 1 1 calc R . . C66 C -0.1116(6) 0.9117(4) 0.1440(4) 0.0424(12) Uani 1 1 d . . . H66A H -0.0946 0.9491 0.1940 0.064 Uiso 1 1 calc R . . H66B H -0.1955 0.9462 0.1167 0.064 Uiso 1 1 calc R . . H66C H -0.0266 0.9025 0.1014 0.064 Uiso 1 1 calc R . . C67 C -0.2728(5) 0.8271(4) 0.2394(3) 0.0284(10) Uani 1 1 d . . . C68 C -0.4113(5) 0.7497(4) 0.3412(4) 0.0394(12) Uani 1 1 d . . . H68A H -0.4055 0.7926 0.3898 0.059 Uiso 1 1 calc R . . H68B H -0.4153 0.6855 0.3636 0.059 Uiso 1 1 calc R . . H68C H -0.4983 0.7743 0.3121 0.059 Uiso 1 1 calc R . . N1 N 0.7891(4) 0.6556(3) 0.7507(2) 0.0254(7) Uani 1 1 d . . . H1 H 0.7433 0.7154 0.7578 0.031 Uiso 1 1 calc R . . N2 N 0.6224(4) 0.5171(3) 0.7801(2) 0.0271(8) Uani 1 1 d . . . H2A H 0.5890 0.5733 0.7580 0.033 Uiso 1 1 calc R . . N3 N 0.7631(4) 0.3649(3) 0.6772(2) 0.0245(8) Uani 1 1 d . . . H3A H 0.7753 0.4242 0.6694 0.029 Uiso 1 1 calc R . . N4 N 0.9156(4) 0.2371(3) 0.7853(2) 0.0227(7) Uani 1 1 d . . . H4A H 0.8836 0.2981 0.7983 0.027 Uiso 1 1 calc R . . N5 N 0.7544(4) 0.0999(3) 0.8385(2) 0.0217(7) Uani 1 1 d . . . H5A H 0.7134 0.1577 0.8229 0.026 Uiso 1 1 calc R . . N6 N 0.8413(4) -0.0440(3) 0.7163(2) 0.0236(7) Uani 1 1 d . . . H6A H 0.8546 0.0153 0.7098 0.028 Uiso 1 1 calc R . . N7 N 1.0912(4) -0.1583(3) 0.7641(3) 0.0307(9) Uani 1 1 d . . . H7 H 1.0380 -0.1083 0.7923 0.037 Uiso 1 1 calc R . . N8 N 0.3271(4) -0.0449(3) 0.2062(3) 0.0292(8) Uani 1 1 d . . . H8 H 0.3631 -0.1067 0.2035 0.035 Uiso 1 1 calc R . . N9 N 0.4996(4) 0.0963(3) 0.1939(3) 0.0272(8) Uani 1 1 d . . . H9A H 0.5303 0.0407 0.2180 0.033 Uiso 1 1 calc R . . N10 N 0.3389(4) 0.2468(3) 0.2928(2) 0.0249(8) Uani 1 1 d . . . H10 H 0.3297 0.1868 0.3004 0.030 Uiso 1 1 calc R . . N11 N 0.1830(4) 0.3670(3) 0.1801(2) 0.0247(8) Uani 1 1 d . . . H11 H 0.2179 0.3060 0.1682 0.030 Uiso 1 1 calc R . . N12 N 0.3354(4) 0.5110(3) 0.1305(2) 0.0229(8) Uani 1 1 d . . . H12 H 0.3795 0.4535 0.1448 0.028 Uiso 1 1 calc R . . N13 N 0.2439(4) 0.6513(3) 0.2561(2) 0.0235(7) Uani 1 1 d . . . H13 H 0.2309 0.5918 0.2613 0.028 Uiso 1 1 calc R . . N14 N -0.0117(4) 0.7614(3) 0.2150(3) 0.0280(8) Uani 1 1 d . . . H14 H 0.0431 0.7129 0.1855 0.034 Uiso 1 1 calc R . . O1 O 0.8041(3) 0.6865(2) 0.6081(2) 0.0282(7) Uani 1 1 d . . . O2 O 0.8964(3) 0.5372(2) 0.6541(2) 0.0297(7) Uani 1 1 d . . . O3 O 0.7960(4) 0.4318(2) 0.8573(2) 0.0334(7) Uani 1 1 d . . . O4 O 0.6164(3) 0.2696(2) 0.7369(2) 0.0272(7) Uani 1 1 d . . . O5 O 0.9564(3) 0.1240(2) 0.6793(2) 0.0296(7) Uani 1 1 d . . . O6 O 0.9538(3) 0.0071(3) 0.8840(2) 0.0311(7) Uani 1 1 d . . . O7 O 0.7206(4) -0.1424(2) 0.7952(2) 0.0324(7) Uani 1 1 d . . . O8 O 1.4455(4) -0.2946(3) 0.7419(3) 0.0433(9) Uani 1 1 d . . . O9 O 1.3597(3) -0.1439(3) 0.7020(2) 0.0341(8) Uani 1 1 d . . . O10 O 0.2766(4) -0.0717(2) 0.3468(2) 0.0303(7) Uani 1 1 d . . . O11 O 0.2118(3) 0.0781(2) 0.2952(2) 0.0318(7) Uani 1 1 d . . . O12 O 0.3404(4) 0.1786(2) 0.1082(2) 0.0333(7) Uani 1 1 d . . . O13 O 0.4806(4) 0.3464(2) 0.2358(2) 0.0295(7) Uani 1 1 d . . . O14 O 0.1275(3) 0.4827(2) 0.2838(2) 0.0312(7) Uani 1 1 d . . . O15 O 0.1292(4) 0.5997(3) 0.0873(2) 0.0315(7) Uani 1 1 d . . . O16 O 0.3626(4) 0.7529(3) 0.1798(2) 0.0360(8) Uani 1 1 d . . . O17 O -0.3661(4) 0.8992(3) 0.2454(3) 0.0379(8) Uani 1 1 d . . . O18 O -0.2853(4) 0.7448(3) 0.2794(2) 0.0333(7) Uani 1 1 d . . . S1 S 1.14904(12) -0.26448(10) 0.61958(9) 0.0415(3) Uani 1 1 d . . . S2 S -0.06859(11) 0.86623(9) 0.36045(8) 0.0351(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(2) 0.026(3) 0.031(2) 0.0017(18) -0.0052(17) -0.004(2) C2 0.037(2) 0.042(3) 0.033(2) -0.005(2) 0.0037(18) -0.013(2) C3 0.050(3) 0.065(4) 0.041(3) 0.002(3) -0.003(2) -0.033(3) C4 0.078(4) 0.047(3) 0.037(3) 0.000(2) -0.016(3) -0.025(3) C5 0.041(3) 0.048(4) 0.043(3) -0.013(2) -0.008(2) -0.008(2) C6 0.033(2) 0.034(3) 0.036(2) -0.003(2) 0.0010(18) 0.004(2) C7 0.031(2) 0.031(3) 0.031(2) 0.0030(18) 0.0028(16) -0.0154(19) C8 0.0263(18) 0.012(2) 0.031(2) 0.0001(16) -0.0015(15) -0.0063(16) C9 0.035(2) 0.020(2) 0.028(2) 0.0009(16) -0.0071(16) -0.0050(17) C10 0.058(3) 0.033(3) 0.032(2) -0.0015(18) -0.0007(19) -0.018(2) C11 0.034(2) 0.018(2) 0.0255(19) -0.0015(16) -0.0011(15) -0.0004(17) C12 0.0273(19) 0.016(2) 0.034(2) 0.0030(17) 0.0015(15) -0.0028(17) C13 0.059(3) 0.024(3) 0.045(3) -0.004(2) 0.020(2) -0.014(2) C14 0.029(2) 0.016(2) 0.067(3) 0.004(2) -0.005(2) 0.0002(18) C15 0.0263(19) 0.015(2) 0.030(2) 0.0055(17) -0.0072(16) -0.0041(17) C16 0.034(2) 0.012(2) 0.0208(19) 0.0000(16) 0.0027(16) -0.0008(17) C17 0.049(3) 0.023(3) 0.035(2) -0.005(2) -0.005(2) -0.007(2) C18 0.039(2) 0.018(3) 0.037(2) 0.0002(19) 0.0098(19) -0.004(2) C19 0.0248(19) 0.009(2) 0.028(2) 0.0028(16) 0.0050(15) -0.0017(16) C20 0.026(2) 0.017(2) 0.031(2) -0.0004(17) -0.0033(16) -0.0029(17) C21 0.040(2) 0.028(3) 0.033(2) 0.0064(19) -0.0101(18) -0.012(2) C22 0.027(2) 0.035(3) 0.050(3) 0.012(2) -0.0065(19) -0.004(2) C23 0.0239(18) 0.013(2) 0.026(2) 0.0002(16) -0.0051(15) 0.0011(17) C24 0.0220(19) 0.012(2) 0.032(2) 0.0016(17) 0.0037(15) -0.0025(16) C25 0.055(3) 0.027(3) 0.035(3) 0.001(2) 0.014(2) -0.012(2) C26 0.023(2) 0.026(3) 0.060(3) -0.005(2) 0.001(2) -0.006(2) C27 0.0222(18) 0.016(2) 0.032(2) 0.0015(17) -0.0044(15) -0.0019(17) C28 0.027(2) 0.016(2) 0.033(2) -0.0004(17) -0.0008(16) -0.0051(18) C29 0.029(2) 0.019(2) 0.040(2) -0.0033(19) -0.0033(18) -0.0037(18) C30 0.0223(19) 0.027(3) 0.047(3) 0.000(2) -0.0057(18) 0.0025(18) C31 0.046(3) 0.020(3) 0.061(3) 0.003(2) -0.006(2) 0.009(2) C32 0.040(3) 0.033(3) 0.053(3) -0.003(2) -0.018(2) 0.009(2) C33 0.034(2) 0.020(3) 0.049(3) -0.003(2) -0.010(2) 0.001(2) C34 0.035(3) 0.045(4) 0.053(3) 0.003(3) -0.003(2) -0.005(2) C35 0.034(2) 0.023(3) 0.032(2) 0.0041(18) 0.0031(17) -0.0084(19) C36 0.038(3) 0.043(3) 0.040(3) 0.000(2) 0.007(2) -0.007(2) C37 0.050(3) 0.107(6) 0.045(3) 0.013(3) -0.008(2) -0.047(4) C38 0.075(4) 0.092(5) 0.040(3) 0.009(3) -0.015(3) -0.063(4) C39 0.081(4) 0.047(4) 0.036(3) -0.002(3) -0.006(3) -0.022(3) C40 0.047(3) 0.034(3) 0.035(2) 0.000(2) 0.001(2) -0.011(2) C41 0.041(2) 0.034(3) 0.034(2) -0.0037(19) 0.0075(18) -0.016(2) C42 0.0293(19) 0.011(2) 0.035(2) 0.0013(16) -0.0014(16) -0.0028(17) C43 0.039(2) 0.028(2) 0.031(2) 0.0029(17) -0.0031(17) -0.0130(19) C44 0.082(4) 0.049(4) 0.055(3) 0.016(3) -0.033(3) -0.033(3) C45 0.040(2) 0.013(2) 0.031(2) -0.0037(16) 0.0076(17) 0.0000(17) C46 0.0262(19) 0.014(2) 0.042(2) 0.0009(18) 0.0052(16) -0.0016(17) C47 0.037(2) 0.027(3) 0.058(3) -0.002(2) -0.009(2) 0.000(2) C48 0.040(2) 0.029(3) 0.054(3) -0.004(2) 0.017(2) -0.011(2) C49 0.028(2) 0.017(2) 0.031(2) -0.0013(17) 0.0016(16) -0.0070(18) C50 0.026(2) 0.018(2) 0.034(2) 0.0001(18) 0.0065(16) -0.0043(18) C51 0.055(3) 0.038(3) 0.034(3) -0.008(2) 0.002(2) -0.005(3) C52 0.034(2) 0.017(3) 0.042(3) 0.0029(19) 0.0137(19) -0.0008(19) C53 0.0224(19) 0.019(3) 0.036(2) 0.0007(18) 0.0054(16) -0.0070(17) C54 0.0232(19) 0.022(3) 0.034(2) 0.0072(18) -0.0051(16) -0.0038(17) C55 0.049(3) 0.026(3) 0.032(2) -0.0020(19) -0.0116(19) -0.016(2) C56 0.029(2) 0.037(3) 0.064(3) 0.010(3) -0.010(2) -0.013(2) C57 0.029(2) 0.017(3) 0.026(2) -0.0011(17) 0.0024(16) -0.0012(19) C58 0.029(2) 0.015(2) 0.032(2) 0.0016(17) -0.0012(17) -0.0043(18) C59 0.023(2) 0.018(3) 0.066(3) 0.001(2) -0.007(2) -0.0026(18) C60 0.053(3) 0.026(3) 0.039(3) 0.000(2) 0.006(2) -0.018(2) C61 0.025(2) 0.014(2) 0.037(2) 0.0018(17) -0.0068(16) -0.0057(17) C62 0.0246(19) 0.021(3) 0.031(2) -0.0059(18) -0.0041(16) 0.0001(18) C63 0.0217(19) 0.026(3) 0.036(2) 0.0007(19) -0.0004(16) -0.0080(18) C64 0.034(2) 0.019(2) 0.036(2) -0.0027(18) -0.0069(18) 0.0051(18) C65 0.040(3) 0.040(3) 0.039(3) -0.008(2) -0.013(2) 0.007(2) C66 0.043(3) 0.036(3) 0.045(3) 0.007(2) 0.004(2) -0.003(2) C67 0.024(2) 0.023(3) 0.039(2) -0.0012(19) -0.0091(17) -0.0042(19) C68 0.027(2) 0.037(3) 0.053(3) 0.010(2) -0.003(2) -0.004(2) N1 0.0370(18) 0.0112(19) 0.0278(17) -0.0006(13) -0.0024(14) -0.0042(14) N2 0.0320(18) 0.015(2) 0.0335(19) 0.0035(14) 0.0021(14) -0.0044(15) N3 0.0295(17) 0.014(2) 0.0300(18) 0.0029(15) 0.0007(14) -0.0050(15) N4 0.0287(17) 0.0069(18) 0.0309(18) 0.0048(14) -0.0027(14) 0.0001(14) N5 0.0259(16) 0.0093(19) 0.0285(18) 0.0022(14) 0.0000(13) -0.0013(14) N6 0.0283(18) 0.0095(19) 0.0325(19) -0.0010(14) -0.0020(14) -0.0027(14) N7 0.0332(19) 0.016(2) 0.040(2) -0.0054(16) -0.0054(16) 0.0039(16) N8 0.0357(18) 0.019(2) 0.034(2) -0.0003(15) -0.0032(14) -0.0074(15) N9 0.0296(17) 0.0142(19) 0.0373(19) 0.0036(14) 0.0015(14) -0.0051(14) N10 0.0344(18) 0.0099(19) 0.0286(18) -0.0003(14) 0.0017(14) -0.0022(15) N11 0.0272(17) 0.016(2) 0.0312(18) -0.0007(15) 0.0003(14) -0.0054(15) N12 0.0214(16) 0.014(2) 0.0324(19) 0.0006(14) 0.0011(13) -0.0030(14) N13 0.0225(16) 0.014(2) 0.0327(19) 0.0028(15) -0.0026(13) -0.0020(14) N14 0.0197(16) 0.027(2) 0.035(2) -0.0045(16) -0.0022(14) -0.0008(15) O1 0.0386(16) 0.0159(16) 0.0305(15) 0.0024(12) -0.0021(12) -0.0073(13) O2 0.0324(15) 0.0155(17) 0.0393(17) -0.0018(12) 0.0012(12) -0.0017(12) O3 0.0484(18) 0.0180(17) 0.0321(16) 0.0032(12) -0.0056(13) -0.0013(14) O4 0.0249(14) 0.0166(17) 0.0412(17) 0.0041(13) -0.0049(12) -0.0059(12) O5 0.0342(16) 0.0170(18) 0.0338(16) -0.0013(13) 0.0082(12) -0.0012(13) O6 0.0338(16) 0.0216(19) 0.0363(17) 0.0024(14) -0.0076(13) 0.0009(14) O7 0.0394(17) 0.0146(18) 0.0433(19) -0.0030(14) 0.0033(14) -0.0086(14) O8 0.0219(15) 0.025(2) 0.079(3) 0.0028(17) -0.0091(15) 0.0084(13) O9 0.0250(15) 0.0212(19) 0.055(2) 0.0019(15) -0.0080(13) 0.0011(13) O10 0.0419(17) 0.0153(17) 0.0333(16) 0.0002(12) 0.0016(12) -0.0073(13) O11 0.0325(15) 0.0162(18) 0.0454(18) -0.0028(13) 0.0059(13) -0.0058(13) O12 0.0458(18) 0.0180(17) 0.0334(16) 0.0026(12) -0.0019(13) -0.0003(13) O13 0.0353(16) 0.0144(17) 0.0392(17) 0.0011(13) -0.0011(12) -0.0068(13) O14 0.0325(16) 0.0146(18) 0.0438(18) -0.0015(13) 0.0107(13) -0.0043(13) O15 0.0370(17) 0.0183(19) 0.0382(17) 0.0002(14) -0.0107(13) 0.0007(14) O16 0.049(2) 0.0154(19) 0.0437(19) -0.0002(14) 0.0002(15) -0.0092(15) O17 0.0339(17) 0.024(2) 0.052(2) 0.0014(15) -0.0028(14) 0.0032(15) O18 0.0318(16) 0.0216(18) 0.0451(19) 0.0030(14) -0.0063(13) -0.0007(13) S1 0.0288(5) 0.0346(7) 0.0572(8) -0.0229(6) -0.0052(5) 0.0047(5) S2 0.0297(5) 0.0310(7) 0.0418(6) -0.0130(5) -0.0015(4) 0.0007(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 C1 C2 1.364(7) . ? C1 C6 1.383(7) . ? C1 C7 1.519(7) . ? C2 C3 1.421(8) . ? C2 H2 0.9500 . ? C3 C4 1.389(9) . ? C3 H3 0.9500 . ? C4 C5 1.369(9) . ? C4 H4 0.9500 . ? C5 C6 1.405(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.433(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.210(6) . ? C8 N1 1.352(6) . ? C8 O1 1.359(5) . ? C9 N1 1.451(6) . ? C9 C10 1.510(6) . ? C9 C11 1.537(6) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O3 1.223(6) . ? C11 N2 1.349(6) . ? C12 N2 1.472(5) . ? C12 C13 1.530(6) . ? C12 C15 1.533(6) . ? C12 C14 1.549(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O4 1.224(6) . ? C15 N3 1.352(5) . ? C16 N3 1.476(6) . ? C16 C18 1.539(6) . ? C16 C19 1.539(6) . ? C16 C17 1.539(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O5 1.238(6) . ? C19 N4 1.330(6) . ? C20 N4 1.462(6) . ? C20 C22 1.526(6) . ? C20 C21 1.529(7) . ? C20 C23 1.549(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 O6 1.223(6) . ? C23 N5 1.350(6) . ? C24 N5 1.465(5) . ? C24 C25 1.523(6) . ? C24 C26 1.530(7) . ? C24 C27 1.551(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O7 1.215(5) . ? C27 N6 1.351(6) . ? C28 N6 1.445(6) . ? C28 C29 1.521(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 N7 1.325(7) . ? C29 S1 1.663(5) . ? C30 N7 1.461(6) . ? C30 C31 1.526(7) . ? C30 C33 1.532(7) . ? C30 C32 1.535(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 O8 1.207(7) . ? C33 O9 1.324(6) . ? C34 O9 1.448(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C40 1.380(7) . ? C35 C36 1.405(7) . ? C35 C41 1.506(7) . ? C36 C37 1.362(9) . ? C36 H36 0.9500 . ? C37 C38 1.353(10) . ? C37 H37 0.9500 . ? C38 C39 1.382(10) . ? C38 H38 0.9500 . ? C39 C40 1.373(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 O10 1.433(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 O11 1.220(6) . ? C42 N8 1.327(6) . ? C42 O10 1.356(5) . ? C43 N8 1.449(6) . ? C43 C45 1.538(6) . ? C43 C44 1.538(7) . ? C43 H43 1.0000 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 O12 1.229(6) . ? C45 N9 1.333(7) . ? C46 N9 1.469(6) . ? C46 C47 1.523(7) . ? C46 C48 1.532(6) . ? C46 C49 1.549(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 O13 1.242(6) . ? C49 N10 1.326(5) . ? C50 N10 1.463(6) . ? C50 C51 1.513(7) . ? C50 C52 1.546(6) . ? C50 C53 1.547(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 O14 1.229(6) . ? C53 N11 1.339(6) . ? C54 N11 1.474(6) . ? C54 C55 1.522(7) . ? C54 C56 1.533(6) . ? C54 C57 1.544(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 O15 1.221(6) . ? C57 N12 1.350(6) . ? C58 N12 1.467(5) . ? C58 C60 1.529(7) . ? C58 C59 1.532(7) . ? C58 C61 1.534(6) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 O16 1.232(6) . ? C61 N13 1.327(6) . ? C62 N13 1.448(6) . ? C62 C63 1.543(6) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 N14 1.318(6) . ? C63 S2 1.656(5) . ? C64 N14 1.487(6) . ? C64 C66 1.512(7) . ? C64 C67 1.522(6) . ? C64 C65 1.533(7) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 O17 1.215(6) . ? C67 O18 1.340(6) . ? C68 O18 1.449(6) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? N1 H1 0.8800 . ? N2 H2A 0.8800 . ? N3 H3A 0.8800 . ? N4 H4A 0.8800 . ? N5 H5A 0.8800 . ? N6 H6A 0.8800 . ? N7 H7 0.8800 . ? N8 H8 0.8800 . ? N9 H9A 0.8800 . ? N10 H10 0.8800 . ? N11 H11 0.8800 . ? N12 H12 0.8800 . ? N13 H13 0.8800 . ? N14 H14 0.8800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120.1(5) . . ? C2 C1 C7 123.6(5) . . ? C6 C1 C7 116.2(4) . . ? C1 C2 C3 121.7(5) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C4 C3 C2 117.6(5) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C5 C4 C3 120.5(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 118.7(5) . . ? C1 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? O1 C7 C1 113.4(3) . . ? O1 C7 H7A 108.9 . . ? C1 C7 H7A 108.9 . . ? O1 C7 H7B 108.9 . . ? C1 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O2 C8 N1 125.1(4) . . ? O2 C8 O1 124.0(4) . . ? N1 C8 O1 110.8(4) . . ? N1 C9 C10 108.9(4) . . ? N1 C9 C11 112.6(3) . . ? C10 C9 C11 111.1(4) . . ? N1 C9 H9 108.0 . . ? C10 C9 H9 108.0 . . ? C11 C9 H9 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O3 C11 N2 124.2(4) . . ? O3 C11 C9 119.4(4) . . ? N2 C11 C9 116.4(4) . . ? N2 C12 C13 111.3(4) . . ? N2 C12 C15 111.7(3) . . ? C13 C12 C15 109.7(4) . . ? N2 C12 C14 107.9(4) . . ? C13 C12 C14 109.4(4) . . ? C15 C12 C14 106.7(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C15 N3 122.5(4) . . ? O4 C15 C12 121.0(4) . . ? N3 C15 C12 116.4(4) . . ? N3 C16 C18 108.4(3) . . ? N3 C16 C19 109.2(3) . . ? C18 C16 C19 107.3(4) . . ? N3 C16 C17 110.2(4) . . ? C18 C16 C17 110.7(4) . . ? C19 C16 C17 111.0(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 N4 122.6(4) . . ? O5 C19 C16 119.6(4) . . ? N4 C19 C16 117.6(4) . . ? N4 C20 C22 110.7(4) . . ? N4 C20 C21 107.7(4) . . ? C22 C20 C21 111.1(4) . . ? N4 C20 C23 110.8(4) . . ? C22 C20 C23 109.6(4) . . ? C21 C20 C23 107.0(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O6 C23 N5 122.4(4) . . ? O6 C23 C20 120.9(4) . . ? N5 C23 C20 116.6(4) . . ? N5 C24 C25 111.4(4) . . ? N5 C24 C26 108.0(4) . . ? C25 C24 C26 109.7(4) . . ? N5 C24 C27 111.5(3) . . ? C25 C24 C27 109.2(4) . . ? C26 C24 C27 106.9(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O7 C27 N6 123.1(4) . . ? O7 C27 C24 120.7(4) . . ? N6 C27 C24 116.2(4) . . ? N6 C28 C29 116.1(4) . . ? N6 C28 H28A 108.3 . . ? C29 C28 H28A 108.3 . . ? N6 C28 H28B 108.3 . . ? C29 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? N7 C29 C28 117.1(4) . . ? N7 C29 S1 124.7(4) . . ? C28 C29 S1 118.2(4) . . ? N7 C30 C31 110.5(4) . . ? N7 C30 C33 110.1(4) . . ? C31 C30 C33 111.2(4) . . ? N7 C30 C32 108.2(4) . . ? C31 C30 C32 110.0(5) . . ? C33 C30 C32 106.8(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O8 C33 O9 124.8(5) . . ? O8 C33 C30 123.6(5) . . ? O9 C33 C30 111.2(4) . . ? O9 C34 H34A 109.5 . . ? O9 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O9 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 119.1(5) . . ? C40 C35 C41 118.3(4) . . ? C36 C35 C41 122.5(5) . . ? C37 C36 C35 117.6(5) . . ? C37 C36 H36 121.2 . . ? C35 C36 H36 121.2 . . ? C38 C37 C36 123.6(6) . . ? C38 C37 H37 118.2 . . ? C36 C37 H37 118.2 . . ? C37 C38 C39 119.2(5) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 118.9(6) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 C35 121.6(5) . . ? C39 C40 H40 119.2 . . ? C35 C40 H40 119.2 . . ? O10 C41 C35 113.3(4) . . ? O10 C41 H41A 108.9 . . ? C35 C41 H41A 108.9 . . ? O10 C41 H41B 108.9 . . ? C35 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? O11 C42 N8 125.8(4) . . ? O11 C42 O10 122.4(4) . . ? N8 C42 O10 111.7(4) . . ? N8 C43 C45 111.9(4) . . ? N8 C43 C44 112.4(4) . . ? C45 C43 C44 109.7(4) . . ? N8 C43 H43 107.5 . . ? C45 C43 H43 107.5 . . ? C44 C43 H43 107.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O12 C45 N9 122.8(4) . . ? O12 C45 C43 120.6(4) . . ? N9 C45 C43 116.5(4) . . ? N9 C46 C47 108.6(4) . . ? N9 C46 C48 110.2(4) . . ? C47 C46 C48 111.0(4) . . ? N9 C46 C49 110.3(3) . . ? C47 C46 C49 107.5(4) . . ? C48 C46 C49 109.3(4) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O13 C49 N10 123.1(4) . . ? O13 C49 C46 119.6(4) . . ? N10 C49 C46 117.2(4) . . ? N10 C50 C51 111.5(4) . . ? N10 C50 C52 108.3(4) . . ? C51 C50 C52 109.7(4) . . ? N10 C50 C53 110.5(3) . . ? C51 C50 C53 110.3(4) . . ? C52 C50 C53 106.4(4) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O14 C53 N11 122.7(5) . . ? O14 C53 C50 120.7(4) . . ? N11 C53 C50 116.6(4) . . ? N11 C54 C55 107.7(4) . . ? N11 C54 C56 110.1(4) . . ? C55 C54 C56 110.3(4) . . ? N11 C54 C57 111.3(4) . . ? C55 C54 C57 107.6(4) . . ? C56 C54 C57 109.8(4) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O15 C57 N12 123.8(4) . . ? O15 C57 C54 120.6(4) . . ? N12 C57 C54 115.5(4) . . ? N12 C58 C60 110.2(4) . . ? N12 C58 C59 106.6(4) . . ? C60 C58 C59 111.1(4) . . ? N12 C58 C61 111.7(3) . . ? C60 C58 C61 110.1(4) . . ? C59 C58 C61 107.2(4) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O16 C61 N13 123.9(4) . . ? O16 C61 C58 118.4(4) . . ? N13 C61 C58 117.5(4) . . ? N13 C62 C63 115.9(4) . . ? N13 C62 H62A 108.3 . . ? C63 C62 H62A 108.3 . . ? N13 C62 H62B 108.3 . . ? C63 C62 H62B 108.3 . . ? H62A C62 H62B 107.4 . . ? N14 C63 C62 115.6(4) . . ? N14 C63 S2 126.0(4) . . ? C62 C63 S2 118.5(3) . . ? N14 C64 C66 110.1(4) . . ? N14 C64 C67 110.4(4) . . ? C66 C64 C67 110.7(4) . . ? N14 C64 C65 107.4(4) . . ? C66 C64 C65 111.3(4) . . ? C67 C64 C65 106.8(4) . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O17 C67 O18 123.9(4) . . ? O17 C67 C64 123.6(4) . . ? O18 C67 C64 111.9(4) . . ? O18 C68 H68A 109.5 . . ? O18 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? O18 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C8 N1 C9 118.5(4) . . ? C8 N1 H1 120.7 . . ? C9 N1 H1 120.7 . . ? C11 N2 C12 122.3(4) . . ? C11 N2 H2A 118.9 . . ? C12 N2 H2A 118.9 . . ? C15 N3 C16 122.6(4) . . ? C15 N3 H3A 118.7 . . ? C16 N3 H3A 118.7 . . ? C19 N4 C20 123.5(4) . . ? C19 N4 H4A 118.2 . . ? C20 N4 H4A 118.2 . . ? C23 N5 C24 121.9(4) . . ? C23 N5 H5A 119.1 . . ? C24 N5 H5A 119.1 . . ? C27 N6 C28 122.5(4) . . ? C27 N6 H6A 118.8 . . ? C28 N6 H6A 118.8 . . ? C29 N7 C30 125.2(4) . . ? C29 N7 H7 117.4 . . ? C30 N7 H7 117.4 . . ? C42 N8 C43 122.4(4) . . ? C42 N8 H8 118.8 . . ? C43 N8 H8 118.8 . . ? C45 N9 C46 123.1(4) . . ? C45 N9 H9A 118.5 . . ? C46 N9 H9A 118.5 . . ? C49 N10 C50 122.7(4) . . ? C49 N10 H10 118.6 . . ? C50 N10 H10 118.6 . . ? C53 N11 C54 121.8(4) . . ? C53 N11 H11 119.1 . . ? C54 N11 H11 119.1 . . ? C57 N12 C58 122.0(4) . . ? C57 N12 H12 119.0 . . ? C58 N12 H12 119.0 . . ? C61 N13 C62 121.9(4) . . ? C61 N13 H13 119.1 . . ? C62 N13 H13 119.1 . . ? C63 N14 C64 123.7(4) . . ? C63 N14 H14 118.1 . . ? C64 N14 H14 118.1 . . ? C8 O1 C7 114.3(4) . . ? C33 O9 C34 116.2(4) . . ? C42 O10 C41 115.9(4) . . ? C67 O18 C68 115.3(4) . . ? 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(9) . . . . ? C7 C1 C2 C3 175.5(6) . . . . ? C1 C2 C3 C4 2.4(10) . . . . ? C2 C3 C4 C5 -2.1(10) . . . . ? C3 C4 C5 C6 0.4(10) . . . . ? C2 C1 C6 C5 -0.9(8) . . . . ? C7 C1 C6 C5 -177.6(5) . . . . ? C4 C5 C6 C1 1.2(9) . . . . ? C2 C1 C7 O1 18.2(7) . . . . ? C6 C1 C7 O1 -165.2(5) . . . . ? N1 C9 C11 O3 151.3(4) . . . . ? C10 C9 C11 O3 -86.2(5) . . . . ? N1 C9 C11 N2 -28.1(5) . . . . ? C10 C9 C11 N2 94.4(5) . . . . ? N2 C12 C15 O4 157.3(4) . . . . ? C13 C12 C15 O4 33.3(6) . . . . ? C14 C12 C15 O4 -85.0(5) . . . . ? N2 C12 C15 N3 -24.6(5) . . . . ? C13 C12 C15 N3 -148.6(4) . . . . ? C14 C12 C15 N3 93.0(4) . . . . ? N3 C16 C19 O5 151.4(4) . . . . ? C18 C16 C19 O5 -91.4(5) . . . . ? C17 C16 C19 O5 29.6(5) . . . . ? N3 C16 C19 N4 -33.4(5) . . . . ? C18 C16 C19 N4 83.8(4) . . . . ? C17 C16 C19 N4 -155.2(4) . . . . ? N4 C20 C23 O6 149.9(4) . . . . ? C22 C20 C23 O6 27.6(6) . . . . ? C21 C20 C23 O6 -92.9(5) . . . . ? N4 C20 C23 N5 -33.8(5) . . . . ? C22 C20 C23 N5 -156.1(4) . . . . ? C21 C20 C23 N5 83.4(5) . . . . ? N5 C24 C27 O7 158.5(4) . . . . ? C25 C24 C27 O7 35.0(6) . . . . ? C26 C24 C27 O7 -83.7(5) . . . . ? N5 C24 C27 N6 -24.1(5) . . . . ? C25 C24 C27 N6 -147.6(4) . . . . ? C26 C24 C27 N6 93.7(4) . . . . ? N6 C28 C29 N7 -2.6(6) . . . . ? N6 C28 C29 S1 179.8(3) . . . . ? N7 C30 C33 O8 -145.0(5) . . . . ? C31 C30 C33 O8 -22.3(8) . . . . ? C32 C30 C33 O8 97.7(6) . . . . ? N7 C30 C33 O9 42.2(6) . . . . ? C31 C30 C33 O9 165.0(4) . . . . ? C32 C30 C33 O9 -75.0(5) . . . . ? C40 C35 C36 C37 -2.3(9) . . . . ? C41 C35 C36 C37 -179.2(6) . . . . ? C35 C36 C37 C38 2.2(11) . . . . ? C36 C37 C38 C39 -1.4(12) . . . . ? C37 C38 C39 C40 0.6(11) . . . . ? C38 C39 C40 C35 -0.7(10) . . . . ? C36 C35 C40 C39 1.6(9) . . . . ? C41 C35 C40 C39 178.6(5) . . . . ? C40 C35 C41 O10 165.9(5) . . . . ? C36 C35 C41 O10 -17.1(7) . . . . ? N8 C43 C45 O12 -141.1(4) . . . . ? C44 C43 C45 O12 -15.7(6) . . . . ? N8 C43 C45 N9 41.0(5) . . . . ? C44 C43 C45 N9 166.5(4) . . . . ? N9 C46 C49 O13 -153.7(4) . . . . ? C47 C46 C49 O13 88.1(5) . . . . ? C48 C46 C49 O13 -32.5(6) . . . . ? N9 C46 C49 N10 30.4(6) . . . . ? C47 C46 C49 N10 -87.8(5) . . . . ? C48 C46 C49 N10 151.7(4) . . . . ? N10 C50 C53 O14 -150.9(4) . . . . ? C51 C50 C53 O14 -27.3(5) . . . . ? C52 C50 C53 O14 91.7(5) . . . . ? N10 C50 C53 N11 31.7(5) . . . . ? C51 C50 C53 N11 155.4(4) . . . . ? C52 C50 C53 N11 -85.7(4) . . . . ? N11 C54 C57 O15 -146.2(4) . . . . ? C55 C54 C57 O15 96.1(5) . . . . ? C56 C54 C57 O15 -24.0(6) . . . . ? N11 C54 C57 N12 37.7(5) . . . . ? C55 C54 C57 N12 -80.1(5) . . . . ? C56 C54 C57 N12 159.9(4) . . . . ? N12 C58 C61 O16 -160.4(4) . . . . ? C60 C58 C61 O16 -37.7(6) . . . . ? C59 C58 C61 O16 83.2(5) . . . . ? N12 C58 C61 N13 24.3(6) . . . . ? C60 C58 C61 N13 147.0(4) . . . . ? C59 C58 C61 N13 -92.1(5) . . . . ? N13 C62 C63 N14 -0.6(6) . . . . ? N13 C62 C63 S2 -179.3(3) . . . . ? N14 C64 C67 O17 142.3(5) . . . . ? C66 C64 C67 O17 20.1(7) . . . . ? C65 C64 C67 O17 -101.2(6) . . . . ? N14 C64 C67 O18 -46.6(5) . . . . ? C66 C64 C67 O18 -168.8(4) . . . . ? C65 C64 C67 O18 69.9(5) . . . . ? O2 C8 N1 C9 2.5(6) . . . . ? O1 C8 N1 C9 -179.9(3) . . . . ? C10 C9 N1 C8 175.0(4) . . . . ? C11 C9 N1 C8 -61.3(5) . . . . ? O3 C11 N2 C12 -1.8(7) . . . . ? C9 C11 N2 C12 177.6(4) . . . . ? C13 C12 N2 C11 68.4(5) . . . . ? C15 C12 N2 C11 -54.6(5) . . . . ? C14 C12 N2 C11 -171.6(4) . . . . ? O4 C15 N3 C16 -4.5(7) . . . . ? C12 C15 N3 C16 177.4(4) . . . . ? C18 C16 N3 C15 -165.1(4) . . . . ? C19 C16 N3 C15 -48.5(5) . . . . ? C17 C16 N3 C15 73.7(5) . . . . ? O5 C19 N4 C20 0.9(6) . . . . ? C16 C19 N4 C20 -174.1(4) . . . . ? C22 C20 N4 C19 69.6(5) . . . . ? C21 C20 N4 C19 -168.8(4) . . . . ? C23 C20 N4 C19 -52.1(5) . . . . ? O6 C23 N5 C24 -2.5(6) . . . . ? C20 C23 N5 C24 -178.8(3) . . . . ? C25 C24 N5 C23 65.7(5) . . . . ? C26 C24 N5 C23 -173.8(4) . . . . ? C27 C24 N5 C23 -56.6(5) . . . . ? O7 C27 N6 C28 -2.0(7) . . . . ? C24 C27 N6 C28 -179.4(4) . . . . ? C29 C28 N6 C27 -81.2(5) . . . . ? C28 C29 N7 C30 177.1(4) . . . . ? S1 C29 N7 C30 -5.5(7) . . . . ? C31 C30 N7 C29 -71.5(6) . . . . ? C33 C30 N7 C29 51.7(6) . . . . ? C32 C30 N7 C29 168.1(4) . . . . ? O11 C42 N8 C43 0.6(7) . . . . ? O10 C42 N8 C43 -177.5(4) . . . . ? C45 C43 N8 C42 47.5(6) . . . . ? C44 C43 N8 C42 -76.4(6) . . . . ? O12 C45 N9 C46 -1.2(7) . . . . ? C43 C45 N9 C46 176.6(4) . . . . ? C47 C46 N9 C45 171.6(4) . . . . ? C48 C46 N9 C45 -66.7(5) . . . . ? C49 C46 N9 C45 54.1(6) . . . . ? O13 C49 N10 C50 3.0(7) . . . . ? C46 C49 N10 C50 178.7(4) . . . . ? C51 C50 N10 C49 -72.1(6) . . . . ? C52 C50 N10 C49 167.1(4) . . . . ? C53 C50 N10 C49 50.9(6) . . . . ? O14 C53 N11 C54 0.4(6) . . . . ? C50 C53 N11 C54 177.7(3) . . . . ? C55 C54 N11 C53 166.9(4) . . . . ? C56 C54 N11 C53 -72.8(5) . . . . ? C57 C54 N11 C53 49.2(5) . . . . ? O15 C57 N12 C58 1.3(7) . . . . ? C54 C57 N12 C58 177.3(4) . . . . ? C60 C58 N12 C57 -65.3(5) . . . . ? C59 C58 N12 C57 174.1(4) . . . . ? C61 C58 N12 C57 57.3(5) . . . . ? O16 C61 N13 C62 2.8(7) . . . . ? C58 C61 N13 C62 177.8(4) . . . . ? C63 C62 N13 C61 85.2(5) . . . . ? C62 C63 N14 C64 -175.1(4) . . . . ? S2 C63 N14 C64 3.5(6) . . . . ? C66 C64 N14 C63 73.5(5) . . . . ? C67 C64 N14 C63 -49.0(6) . . . . ? C65 C64 N14 C63 -165.1(4) . . . . ? O2 C8 O1 C7 -5.4(6) . . . . ? N1 C8 O1 C7 177.0(3) . . . . ? C1 C7 O1 C8 76.3(5) . . . . ? O8 C33 O9 C34 9.8(8) . . . . ? C30 C33 O9 C34 -177.5(4) . . . . ? O11 C42 O10 C41 0.1(6) . . . . ? N8 C42 O10 C41 178.3(4) . . . . ? C35 C41 O10 C42 -78.5(6) . . . . ? O17 C67 O18 C68 -8.0(7) . . . . ? C64 C67 O18 C68 -179.1(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 N14 H14 N13 0.88 2.30 2.746(6) 111.1 . N14 H14 O15 0.88 2.20 3.053(5) 163.4 . N13 H13 O14 0.88 2.00 2.843(5) 158.9 . N12 H12 O13 0.88 2.20 3.020(5) 154.1 . N11 H11 O12 0.88 2.12 2.969(5) 161.8 . N10 H10 O11 0.88 2.08 2.886(5) 151.2 . N9 H9A O17 0.88 2.12 2.981(6) 165.7 1_645 N8 H8 O16 0.88 2.03 2.859(5) 155.7 1_545 N7 H7 N6 0.88 2.33 2.762(6) 110.4 . N7 H7 O6 0.88 2.15 3.011(5) 164.6 . N6 H6A O5 0.88 2.01 2.848(5) 159.1 . N5 H5A O4 0.88 2.18 3.015(5) 157.6 . N4 H4A O3 0.88 2.10 2.963(5) 167.2 . N3 H3A O2 0.88 2.15 2.974(5) 155.7 . N2 H2A O8 0.88 2.12 2.959(5) 158.3 1_465 N1 H1 O7 0.88 2.07 2.892(5) 155.0 1_565 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 66.60 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.273 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.054 _database_code_depnum_ccdc_archive 'CCDC 969435'