data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Volker Boehmer' _publ_contact_author_email VBOEHMER@MAIL.UNI-MAINZ.DE _publ_section_title ; Cyclic tetraureas with variable flexibility - s ynthesis, crystal structures and properties ; loop_ _publ_author_name 'Volker Boehmer' 'Francoise Arnaud-Neu' 'Michael Bolte' 'Veronique Hubscher-Bruder' ; D.Meshcheryakov ; 'Iris Thondorf' 'Sabine Werner' # Attachment 'Article_Boehmer_Tetraureas.cif' #============================================================================== data_boeh19 _database_code_depnum_ccdc_archive 'CCDC 687873' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H80 N8 O13' _chemical_formula_weight 1265.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.808(2) _cell_length_b 19.667(2) _cell_length_c 25.792(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.206(7) _cell_angle_gamma 90.00 _cell_volume 13071(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23300 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 23.6 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5376 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9720 _exptl_absorpt_correction_T_max 0.9885 _exptl_absorpt_process_details ? _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 112990 _diffrn_reflns_av_R_equivalents 0.1890 _diffrn_reflns_av_sigmaI/netI 0.2556 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.96 _reflns_number_total 24137 _reflns_number_gt 5702 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0000P)^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_number_reflns 24137 _refine_ls_number_parameters 1675 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2012 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 0.562 _refine_ls_restrained_S_all 0.562 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.15722(13) 0.94915(13) 0.18438(10) 0.0516(8) Uani 1 1 d . . . N1 N 0.18070(15) 0.85041(15) 0.14409(12) 0.0473(10) Uani 1 1 d . . . H1 H 0.1882 0.8074 0.1502 0.057 Uiso 1 1 calc R . . C1 C 0.16295(19) 0.8875(2) 0.18463(16) 0.0456(12) Uani 1 1 d . . . O2 O 0.16878(12) 0.76760(13) 0.31070(10) 0.0548(8) Uani 1 1 d . . . N2 N 0.15335(15) 0.84641(16) 0.22638(12) 0.0513(10) Uani 1 1 d . . . H2 H 0.1620 0.8033 0.2242 0.062 Uiso 1 1 calc R . . C2 C 0.2739(2) 0.6365(2) 0.37126(16) 0.0484(12) Uani 1 1 d . . . O3 O 0.27215(13) 0.57475(13) 0.37682(10) 0.0555(9) Uani 1 1 d . . . N3 N 0.23321(17) 0.67535(16) 0.35089(12) 0.0497(10) Uani 1 1 d . . . H3 H 0.2395 0.7190 0.3473 0.060 Uiso 1 1 calc R . . C3 C 0.3322(2) 0.6429(2) 0.07773(16) 0.0485(12) Uani 1 1 d . . . O4 O 0.40453(12) 0.74558(12) 0.36889(9) 0.0507(8) Uani 1 1 d . . . N4 N 0.31770(17) 0.67501(16) 0.38356(12) 0.0513(10) Uani 1 1 d . . . H4 H 0.3162 0.7187 0.3762 0.062 Uiso 1 1 calc R . . C4 C 0.4436(2) 0.8831(2) 0.26607(17) 0.0496(13) Uani 1 1 d . . . O5 O 0.45098(13) 0.94407(13) 0.26952(10) 0.0521(9) Uani 1 1 d . . . N5 N 0.42394(15) 0.84275(16) 0.30464(12) 0.0506(10) Uani 1 1 d . . . H5 H 0.4144 0.8011 0.2959 0.061 Uiso 1 1 calc R . . O6 O 0.43924(12) 0.77276(13) 0.13460(10) 0.0532(8) Uani 1 1 d . . . N6 N 0.45425(15) 0.84507(15) 0.22251(12) 0.0506(10) Uani 1 1 d . . . H6 H 0.4453 0.8019 0.2227 0.061 Uiso 1 1 calc R . . O7 O 0.33392(13) 0.58141(14) 0.07138(10) 0.0545(9) Uani 1 1 d . . . N7 N 0.37375(16) 0.68222(16) 0.09634(12) 0.0483(10) Uani 1 1 d . . . H7 H 0.3683 0.7262 0.0992 0.058 Uiso 1 1 calc R . . O8 O 0.20671(12) 0.76091(13) 0.07766(9) 0.0554(8) Uani 1 1 d . . . N8 N 0.28865(17) 0.68179(16) 0.06691(12) 0.0533(10) Uani 1 1 d . . . H8 H 0.2907 0.7250 0.0755 0.064 Uiso 1 1 calc R . . C11 C 0.1309(2) 0.8677(2) 0.27203(16) 0.0497(12) Uani 1 1 d . . . C12 C 0.1360(2) 0.8242(2) 0.31504(16) 0.0503(12) Uani 1 1 d . . . C13 C 0.1140(2) 0.8382(2) 0.36155(16) 0.0559(13) Uani 1 1 d . . . H13 H 0.1186 0.8080 0.3901 0.067 Uiso 1 1 calc R . . C14 C 0.0852(2) 0.8970(2) 0.36564(16) 0.0593(14) Uani 1 1 d . . . H14 H 0.0688 0.9064 0.3969 0.071 Uiso 1 1 calc R . . C15 C 0.08004(19) 0.9423(2) 0.32438(16) 0.0541(13) Uani 1 1 d . . . H15 H 0.0610 0.9832 0.3277 0.065 Uiso 1 1 calc R . . C16 C 0.1031(2) 0.9274(2) 0.27777(16) 0.0524(13) Uani 1 1 d . . . H16 H 0.0996 0.9587 0.2497 0.063 Uiso 1 1 calc R . . C21 C 0.1474(2) 0.7022(2) 0.31609(15) 0.0484(12) Uani 1 1 d . . . C22 C 0.1830(2) 0.6535(2) 0.33526(15) 0.0463(12) Uani 1 1 d . . . C23 C 0.1662(2) 0.5862(2) 0.33902(15) 0.0530(14) Uani 1 1 d . . . H23 H 0.1891 0.5518 0.3525 0.064 Uiso 1 1 calc R . . C24 C 0.1147(2) 0.5701(2) 0.32246(16) 0.0558(13) Uani 1 1 d . . . H24 H 0.1034 0.5242 0.3238 0.067 Uiso 1 1 calc R . . C25 C 0.0804(2) 0.6192(2) 0.30438(14) 0.0531(13) Uani 1 1 d . . . H25 H 0.0454 0.6077 0.2946 0.064 Uiso 1 1 calc R . . C26 C 0.0976(2) 0.6854(2) 0.30059(15) 0.0514(12) Uani 1 1 d . . . H26 H 0.0745 0.7195 0.2871 0.062 Uiso 1 1 calc R . . C31 C 0.3645(2) 0.64997(19) 0.40691(14) 0.0448(12) Uani 1 1 d . . . C32 C 0.4088(2) 0.6887(2) 0.40125(16) 0.0465(12) Uani 1 1 d . . . C33 C 0.4561(2) 0.6696(2) 0.42437(15) 0.0550(13) Uani 1 1 d . . . H33 H 0.4859 0.6971 0.4206 0.066 Uiso 1 1 calc R . . C34 C 0.4597(2) 0.6103(2) 0.45298(15) 0.0565(13) Uani 1 1 d . . . H34 H 0.4922 0.5964 0.4686 0.068 Uiso 1 1 calc R . . C35 C 0.4159(2) 0.5712(2) 0.45884(16) 0.0560(13) Uani 1 1 d . . . H35 H 0.4183 0.5307 0.4790 0.067 Uiso 1 1 calc R . . C36 C 0.3686(2) 0.5904(2) 0.43566(15) 0.0486(12) Uani 1 1 d . . . H36 H 0.3389 0.5627 0.4394 0.058 Uiso 1 1 calc R . . C41 C 0.4089(2) 0.81045(19) 0.39168(16) 0.0468(12) Uani 1 1 d . . . C42 C 0.41791(19) 0.86235(19) 0.35608(15) 0.0481(12) Uani 1 1 d . . . C43 C 0.41937(18) 0.9289(2) 0.37456(16) 0.0503(12) Uani 1 1 d . . . H43 H 0.4227 0.9658 0.3512 0.060 Uiso 1 1 calc R . . C44 C 0.4160(2) 0.9411(2) 0.42729(17) 0.0540(13) Uani 1 1 d . . . H44 H 0.4196 0.9863 0.4400 0.065 Uiso 1 1 calc R . . C45 C 0.40742(19) 0.8885(2) 0.46206(16) 0.0526(13) Uani 1 1 d . . . H45 H 0.4045 0.8978 0.4979 0.063 Uiso 1 1 calc R . . C46 C 0.4033(2) 0.8224(2) 0.44348(15) 0.0517(13) Uani 1 1 d . . . H46 H 0.3966 0.7859 0.4663 0.062 Uiso 1 1 calc R . . C51 C 0.47792(18) 0.86872(19) 0.17812(15) 0.0436(11) Uani 1 1 d . . . C52 C 0.4727(2) 0.8293(2) 0.13362(18) 0.0531(13) Uani 1 1 d . . . C53 C 0.4954(2) 0.8468(2) 0.08835(16) 0.0568(13) Uani 1 1 d . . . H53 H 0.4910 0.8189 0.0584 0.068 Uiso 1 1 calc R . . C54 C 0.52430(19) 0.9055(2) 0.08725(16) 0.0542(13) Uani 1 1 d . . . H54 H 0.5405 0.9180 0.0565 0.065 Uiso 1 1 calc R . . C55 C 0.5299(2) 0.9463(2) 0.13079(16) 0.0581(14) Uani 1 1 d . . . H55 H 0.5499 0.9868 0.1298 0.070 Uiso 1 1 calc R . . C56 C 0.50647(19) 0.9282(2) 0.17632(16) 0.0527(13) Uani 1 1 d . . . H56 H 0.5101 0.9567 0.2060 0.063 Uiso 1 1 calc R . . C61 C 0.4591(2) 0.7073(2) 0.13006(16) 0.0492(12) Uani 1 1 d . . . C62 C 0.4236(2) 0.6585(2) 0.11104(15) 0.0477(12) Uani 1 1 d . . . C63 C 0.4403(2) 0.5915(2) 0.10826(15) 0.0523(13) Uani 1 1 d . . . H63 H 0.4171 0.5574 0.0952 0.063 Uiso 1 1 calc R . . C64 C 0.4904(2) 0.5744(2) 0.12439(16) 0.0554(14) Uani 1 1 d . . . H64 H 0.5010 0.5282 0.1230 0.067 Uiso 1 1 calc R . . C65 C 0.5254(2) 0.6229(2) 0.14241(16) 0.0530(12) Uani 1 1 d . . . H65 H 0.5599 0.6103 0.1530 0.064 Uiso 1 1 calc R . . C66 C 0.5099(2) 0.6904(2) 0.14500(16) 0.0557(14) Uani 1 1 d . . . H66 H 0.5337 0.7245 0.1569 0.067 Uiso 1 1 calc R . . C71 C 0.2410(2) 0.6594(2) 0.04340(15) 0.0453(11) Uani 1 1 d . . . C72 C 0.1986(2) 0.7034(2) 0.04593(16) 0.0516(13) Uani 1 1 d . . . C73 C 0.1510(2) 0.6892(2) 0.02340(16) 0.0552(13) Uani 1 1 d . . . H73 H 0.1232 0.7205 0.0256 0.066 Uiso 1 1 calc R . . C74 C 0.1438(2) 0.6282(2) -0.00291(15) 0.0558(13) Uani 1 1 d . . . H74 H 0.1108 0.6172 -0.0189 0.067 Uiso 1 1 calc R . . C75 C 0.1851(2) 0.5830(2) -0.00574(17) 0.0583(13) Uani 1 1 d . . . H75 H 0.1803 0.5411 -0.0238 0.070 Uiso 1 1 calc R . . C76 C 0.2329(2) 0.5987(2) 0.01751(16) 0.0542(12) Uani 1 1 d . . . H76 H 0.2607 0.5673 0.0157 0.065 Uiso 1 1 calc R . . C81 C 0.20030(19) 0.8257(2) 0.05701(16) 0.0493(12) Uani 1 1 d . . . C82 C 0.18810(18) 0.87488(19) 0.09347(15) 0.0451(11) Uani 1 1 d . . . C83 C 0.18456(19) 0.94193(19) 0.07716(16) 0.0509(12) Uani 1 1 d . . . H83 H 0.1779 0.9768 0.1014 0.061 Uiso 1 1 calc R . . C84 C 0.1907(2) 0.9585(2) 0.02569(17) 0.0547(13) Uani 1 1 d . . . H84 H 0.1868 1.0043 0.0146 0.066 Uiso 1 1 calc R . . C85 C 0.2025(2) 0.9090(2) -0.00971(16) 0.0554(13) Uani 1 1 d . . . H85 H 0.2078 0.9210 -0.0447 0.066 Uiso 1 1 calc R . . C86 C 0.2066(2) 0.8422(2) 0.00589(17) 0.0565(13) Uani 1 1 d . . . H86 H 0.2137 0.8076 -0.0185 0.068 Uiso 1 1 calc R . . O1A O 0.65765(14) 0.93300(13) 0.67652(10) 0.0564(9) Uani 1 1 d . . . N1A N 0.68267(15) 0.83882(15) 0.63171(12) 0.0492(10) Uani 1 1 d . . . H1A H 0.6899 0.7953 0.6352 0.059 Uiso 1 1 calc R . . C1A C 0.6648(2) 0.8720(2) 0.67474(16) 0.0489(12) Uani 1 1 d . . . O2A O 0.66931(12) 0.74187(13) 0.79464(10) 0.0537(8) Uani 1 1 d . . . N2A N 0.65588(15) 0.82731(15) 0.71459(11) 0.0487(10) Uani 1 1 d . . . H2A H 0.6643 0.7843 0.7105 0.058 Uiso 1 1 calc R . . O3A O 0.77242(13) 0.55375(13) 0.86821(10) 0.0563(9) Uani 1 1 d . . . N3A N 0.73295(16) 0.65487(16) 0.84495(12) 0.0509(10) Uani 1 1 d . . . H3A H 0.7388 0.6987 0.8415 0.061 Uiso 1 1 calc R . . C3A C 0.7732(2) 0.6162(2) 0.86539(16) 0.0488(13) Uani 1 1 d . . . N4A N 0.81537(16) 0.65477(16) 0.88265(12) 0.0483(10) Uani 1 1 d . . . H4A H 0.8141 0.6984 0.8753 0.058 Uiso 1 1 calc R . . O4A O 0.90088(12) 0.73092(13) 0.88060(9) 0.0552(8) Uani 1 1 d . . . O5A O 0.94919(13) 0.92417(13) 0.77818(10) 0.0502(8) Uani 1 1 d . . . N5A N 0.91914(15) 0.82526(15) 0.81398(12) 0.0479(10) Uani 1 1 d . . . H5A H 0.9089 0.7838 0.8056 0.057 Uiso 1 1 calc R . . C5A C 0.9413(2) 0.8637(2) 0.77551(16) 0.0482(12) Uani 1 1 d . . . O6A O 0.94467(13) 0.73911(14) 0.65446(10) 0.0580(8) Uani 1 1 d . . . N6A N 0.95285(15) 0.82219(15) 0.73375(12) 0.0493(10) Uani 1 1 d . . . H6A H 0.9440 0.7791 0.7357 0.059 Uiso 1 1 calc R . . O7A O 0.83285(12) 0.56013(13) 0.58102(10) 0.0532(8) Uani 1 1 d . . . N7A N 0.87815(16) 0.65694(16) 0.60519(12) 0.0484(10) Uani 1 1 d . . . H7A H 0.8744 0.7011 0.6091 0.058 Uiso 1 1 calc R . . C7A C 0.8344(2) 0.6221(2) 0.58684(16) 0.0459(12) Uani 1 1 d . . . N8A N 0.79323(16) 0.66517(16) 0.57653(12) 0.0497(10) Uani 1 1 d . . . H8A H 0.7973 0.7074 0.5873 0.060 Uiso 1 1 calc R . . O8A O 0.73127(13) 0.76539(13) 0.56297(10) 0.0589(8) Uani 1 1 d . . . C11A C 0.63412(19) 0.8465(2) 0.76149(15) 0.0472(12) Uani 1 1 d . . . C12A C 0.6386(2) 0.8000(2) 0.80268(16) 0.0524(13) Uani 1 1 d . . . C13A C 0.6162(2) 0.8108(2) 0.84961(16) 0.0563(13) Uani 1 1 d . . . H13A H 0.6193 0.7777 0.8764 0.068 Uiso 1 1 calc R . . C14A C 0.5893(2) 0.8706(2) 0.85658(17) 0.0604(14) Uani 1 1 d . . . H14A H 0.5738 0.8792 0.8885 0.073 Uiso 1 1 calc R . . C15A C 0.5851(2) 0.9178(2) 0.81703(16) 0.0580(13) Uani 1 1 d . . . H15A H 0.5668 0.9590 0.8221 0.070 Uiso 1 1 calc R . . C16A C 0.6071(2) 0.9063(2) 0.77001(16) 0.0557(14) Uani 1 1 d . . . H16A H 0.6038 0.9396 0.7433 0.067 Uiso 1 1 calc R . . C21A C 0.6488(2) 0.6777(2) 0.80471(16) 0.0511(12) Uani 1 1 d . . . C22A C 0.6828(2) 0.6312(2) 0.82878(15) 0.0474(12) Uani 1 1 d . . . C23A C 0.6647(2) 0.5652(2) 0.83695(14) 0.0493(13) Uani 1 1 d . . . H23A H 0.6870 0.5320 0.8530 0.059 Uiso 1 1 calc R . . C24A C 0.6139(2) 0.5487(2) 0.82142(16) 0.0574(14) Uani 1 1 d . . . H24A H 0.6017 0.5038 0.8269 0.069 Uiso 1 1 calc R . . C25A C 0.5807(2) 0.5958(2) 0.79823(15) 0.0566(13) Uani 1 1 d . . . H25A H 0.5458 0.5838 0.7885 0.068 Uiso 1 1 calc R . . C26A C 0.5986(2) 0.6610(2) 0.78924(15) 0.0552(13) Uani 1 1 d . . . H26A H 0.5764 0.6938 0.7725 0.066 Uiso 1 1 calc R . . C31A C 0.8602(2) 0.63153(19) 0.91078(15) 0.0470(12) Uani 1 1 d . . . C32A C 0.9037(2) 0.6725(2) 0.91219(16) 0.0509(13) Uani 1 1 d . . . C33A C 0.9484(2) 0.6570(2) 0.94073(16) 0.0577(13) Uani 1 1 d . . . H33A H 0.9768 0.6878 0.9426 0.069 Uiso 1 1 calc R . . C34A C 0.9515(2) 0.5956(2) 0.96678(16) 0.0631(13) Uani 1 1 d . . . H34A H 0.9823 0.5835 0.9865 0.076 Uiso 1 1 calc R . . C35A C 0.9090(2) 0.5517(2) 0.96381(16) 0.0601(14) Uani 1 1 d . . . H35A H 0.9113 0.5090 0.9811 0.072 Uiso 1 1 calc R . . C36A C 0.8638(2) 0.5694(2) 0.93611(15) 0.0532(13) Uani 1 1 d . . . H36A H 0.8351 0.5390 0.9344 0.064 Uiso 1 1 calc R . . C41A C 0.90390(19) 0.79623(19) 0.90202(16) 0.0455(12) Uani 1 1 d . . . C42A C 0.91175(18) 0.84687(19) 0.86501(15) 0.0461(12) Uani 1 1 d . . . C43A C 0.91128(17) 0.9144(2) 0.88113(15) 0.0471(11) Uani 1 1 d . . . H43A H 0.9143 0.9500 0.8566 0.057 Uiso 1 1 calc R . . C44A C 0.90634(19) 0.9294(2) 0.93342(16) 0.0510(13) Uani 1 1 d . . . H44A H 0.9074 0.9755 0.9445 0.061 Uiso 1 1 calc R . . C45A C 0.90000(19) 0.8787(2) 0.96910(16) 0.0537(13) Uani 1 1 d . . . H45A H 0.8958 0.8897 1.0045 0.064 Uiso 1 1 calc R . . C46A C 0.89972(19) 0.81063(19) 0.95310(15) 0.0515(12) Uani 1 1 d . . . H46A H 0.8966 0.7750 0.9776 0.062 Uiso 1 1 calc R . . C51A C 0.97729(19) 0.84284(19) 0.68882(15) 0.0470(12) Uani 1 1 d . . . C52A C 0.9748(2) 0.7971(2) 0.64749(16) 0.0502(13) Uani 1 1 d . . . C53A C 0.9986(2) 0.8106(2) 0.60203(16) 0.0574(13) Uani 1 1 d . . . H53A H 0.9972 0.7784 0.5746 0.069 Uiso 1 1 calc R . . C54A C 1.0243(2) 0.8709(2) 0.59673(16) 0.0559(13) Uani 1 1 d . . . H54A H 1.0410 0.8803 0.5656 0.067 Uiso 1 1 calc R . . C55A C 1.0262(2) 0.9178(2) 0.63637(16) 0.0587(14) Uani 1 1 d . . . H55A H 1.0437 0.9598 0.6323 0.070 Uiso 1 1 calc R . . C56A C 1.00220(19) 0.9040(2) 0.68281(15) 0.0513(13) Uani 1 1 d . . . H56A H 1.0032 0.9367 0.7099 0.062 Uiso 1 1 calc R . . C61A C 0.9640(2) 0.6746(2) 0.64223(16) 0.0505(12) Uani 1 1 d . . . C62A C 0.92733(19) 0.6311(2) 0.61832(15) 0.0452(11) Uani 1 1 d . . . C63A C 0.9425(2) 0.56456(19) 0.60646(15) 0.0496(12) Uani 1 1 d . . . H63A H 0.9190 0.5343 0.5886 0.060 Uiso 1 1 calc R . . C64A C 0.9924(2) 0.5440(2) 0.62128(17) 0.0552(13) Uani 1 1 d . . . H64A H 1.0026 0.4986 0.6145 0.066 Uiso 1 1 calc R . . C65A C 1.0285(2) 0.5885(2) 0.64601(16) 0.0577(13) Uani 1 1 d . . . H65A H 1.0627 0.5737 0.6556 0.069 Uiso 1 1 calc R . . C66A C 1.0131(2) 0.6543(2) 0.65619(15) 0.0550(13) Uani 1 1 d . . . H66A H 1.0369 0.6852 0.6729 0.066 Uiso 1 1 calc R . . C71A C 0.7456(2) 0.6494(2) 0.55084(15) 0.0490(12) Uani 1 1 d . . . C72A C 0.7120(2) 0.7048(2) 0.54059(15) 0.0487(12) Uani 1 1 d . . . C73A C 0.6659(2) 0.6986(2) 0.51309(15) 0.0594(14) Uani 1 1 d . . . H73A H 0.6451 0.7375 0.5054 0.071 Uiso 1 1 calc R . . C74A C 0.6498(2) 0.6350(2) 0.49643(16) 0.0580(13) Uani 1 1 d . . . H74A H 0.6172 0.6299 0.4777 0.070 Uiso 1 1 calc R . . C75A C 0.6805(2) 0.5788(2) 0.50674(16) 0.0571(13) Uani 1 1 d . . . H75A H 0.6693 0.5354 0.4945 0.068 Uiso 1 1 calc R . . C76A C 0.7281(2) 0.5852(2) 0.53506(15) 0.0541(13) Uani 1 1 d . . . H76A H 0.7484 0.5460 0.5435 0.065 Uiso 1 1 calc R . . C81A C 0.7123(2) 0.8281(2) 0.54553(17) 0.0552(13) Uani 1 1 d . . . C82A C 0.69030(19) 0.86842(19) 0.58273(15) 0.0461(11) Uani 1 1 d . . . C83A C 0.67663(19) 0.93420(19) 0.56915(16) 0.0518(12) Uani 1 1 d . . . H83A H 0.6627 0.9634 0.5942 0.062 Uiso 1 1 calc R . . C84A C 0.6831(2) 0.9580(2) 0.51924(16) 0.0581(13) Uani 1 1 d . . . H84A H 0.6726 1.0029 0.5101 0.070 Uiso 1 1 calc R . . C85A C 0.7049(2) 0.9165(2) 0.48268(17) 0.0584(13) Uani 1 1 d . . . H85A H 0.7096 0.9329 0.4486 0.070 Uiso 1 1 calc R . . C86A C 0.7192(2) 0.8520(2) 0.49641(17) 0.0620(14) Uani 1 1 d . . . H86A H 0.7342 0.8233 0.4717 0.074 Uiso 1 1 calc R . . O101 O 1.04364(13) 0.77664(14) 0.98750(12) 0.0644(9) Uani 1 1 d . . . C102 C 1.0385(2) 0.8325(2) 1.02264(16) 0.0687(15) Uani 1 1 d . . . H10A H 1.0619 0.8263 1.0540 0.082 Uiso 1 1 calc R . . H10B H 1.0023 0.8355 1.0335 0.082 Uiso 1 1 calc R . . C103 C 1.0527(2) 0.8963(2) 0.99389(18) 0.0664(15) Uani 1 1 d . . . H10C H 1.0288 0.9341 1.0010 0.080 Uiso 1 1 calc R . . H10D H 1.0887 0.9106 1.0038 0.080 Uiso 1 1 calc R . . C104 C 1.0475(2) 0.8754(2) 0.93790(17) 0.0624(14) Uani 1 1 d . . . H10E H 1.0113 0.8809 0.9235 0.075 Uiso 1 1 calc R . . H10F H 1.0710 0.9019 0.9166 0.075 Uiso 1 1 calc R . . C105 C 1.0627(2) 0.8025(2) 0.94052(17) 0.0689(16) Uani 1 1 d . . . H10G H 1.0472 0.7774 0.9102 0.083 Uiso 1 1 calc R . . H10H H 1.1009 0.7979 0.9409 0.083 Uiso 1 1 calc R . . O111 O 0.18341(14) 0.71203(14) 0.19039(10) 0.0581(9) Uani 1 1 d . . . C112 C 0.1432(2) 0.6653(2) 0.17068(17) 0.0628(14) Uani 1 1 d . . . H11A H 0.1295 0.6798 0.1358 0.075 Uiso 1 1 calc R . . H11B H 0.1141 0.6644 0.1942 0.075 Uiso 1 1 calc R . . C113 C 0.1672(3) 0.5978(3) 0.1680(3) 0.119(3) Uani 1 1 d . . . H11C H 0.1456 0.5636 0.1849 0.143 Uiso 1 1 calc R . . H11D H 0.1704 0.5843 0.1314 0.143 Uiso 1 1 calc R . . C114 C 0.2181(3) 0.6014(2) 0.1946(2) 0.087(2) Uani 1 1 d . . . H11E H 0.2443 0.5789 0.1738 0.104 Uiso 1 1 calc R . . H11F H 0.2179 0.5786 0.2288 0.104 Uiso 1 1 calc R . . C115 C 0.2307(2) 0.6753(2) 0.20138(18) 0.0619(14) Uani 1 1 d . . . H11G H 0.2442 0.6844 0.2374 0.074 Uiso 1 1 calc R . . H11H H 0.2572 0.6892 0.1772 0.074 Uiso 1 1 calc R . . O121 O 0.28300(13) 0.81087(13) 0.34751(10) 0.0569(9) Uani 1 1 d . . . C122 C 0.2709(2) 0.8619(2) 0.38582(18) 0.0686(15) Uani 1 1 d . . . H12A H 0.3025 0.8749 0.4071 0.082 Uiso 1 1 calc R . . H12B H 0.2447 0.8445 0.4091 0.082 Uiso 1 1 calc R . . C123 C 0.2498(2) 0.9220(2) 0.3549(2) 0.0760(16) Uani 1 1 d . . . H12C H 0.2571 0.9652 0.3737 0.091 Uiso 1 1 calc R . . H12D H 0.2119 0.9177 0.3474 0.091 Uiso 1 1 calc R . . C124 C 0.2788(2) 0.9187(2) 0.3052(2) 0.0868(18) Uani 1 1 d . . . H12E H 0.3134 0.9405 0.3098 0.104 Uiso 1 1 calc R . . H12F H 0.2588 0.9406 0.2759 0.104 Uiso 1 1 calc R . . C125 C 0.2837(2) 0.8423(2) 0.29682(16) 0.0609(14) Uani 1 1 d . . . H12G H 0.2544 0.8254 0.2739 0.073 Uiso 1 1 calc R . . H12H H 0.3166 0.8316 0.2805 0.073 Uiso 1 1 calc R . . O131 O 0.42128(14) 0.70998(14) 0.25223(10) 0.0605(9) Uani 1 1 d . . . C132 C 0.3717(3) 0.6769(3) 0.24446(18) 0.0849(19) Uani 1 1 d . . . H13B H 0.3603 0.6761 0.2072 0.102 Uiso 1 1 calc R . . H13C H 0.3450 0.7004 0.2640 0.102 Uiso 1 1 calc R . . C133 C 0.3809(4) 0.6040(3) 0.2653(4) 0.184(6) Uani 1 1 d . . . H13D H 0.3674 0.5989 0.3003 0.221 Uiso 1 1 calc R . . H13E H 0.3638 0.5701 0.2418 0.221 Uiso 1 1 calc R . . C134 C 0.4350(5) 0.5959(3) 0.2673(2) 0.172(5) Uani 1 1 d . . . H13F H 0.4453 0.5722 0.2356 0.206 Uiso 1 1 calc R . . H13G H 0.4460 0.5676 0.2977 0.206 Uiso 1 1 calc R . . C135 C 0.4612(3) 0.6633(3) 0.2714(2) 0.100(2) Uani 1 1 d . . . H13H H 0.4726 0.6737 0.3078 0.119 Uiso 1 1 calc R . . H13I H 0.4917 0.6649 0.2497 0.119 Uiso 1 1 calc R . . O141 O 0.32388(13) 0.81735(13) 0.10602(10) 0.0588(9) Uani 1 1 d . . . C142 C 0.3204(2) 0.8407(2) 0.15889(16) 0.0595(14) Uani 1 1 d . . . H14B H 0.3502 0.8238 0.1810 0.071 Uiso 1 1 calc R . . H14C H 0.2880 0.8240 0.1733 0.071 Uiso 1 1 calc R . . C143 C 0.3206(2) 0.9175(2) 0.15727(19) 0.0715(15) Uani 1 1 d . . . H14D H 0.3380 0.9369 0.1891 0.086 Uiso 1 1 calc R . . H14E H 0.2849 0.9360 0.1529 0.086 Uiso 1 1 calc R . . C144 C 0.3512(2) 0.9314(2) 0.10997(18) 0.0712(15) Uani 1 1 d . . . H14F H 0.3416 0.9760 0.0945 0.085 Uiso 1 1 calc R . . H14G H 0.3890 0.9312 0.1193 0.085 Uiso 1 1 calc R . . C145 C 0.3370(2) 0.8753(2) 0.07332(17) 0.0668(15) Uani 1 1 d . . . H14H H 0.3069 0.8883 0.0499 0.080 Uiso 1 1 calc R . . H14I H 0.3665 0.8639 0.0520 0.080 Uiso 1 1 calc R . . O151 O 0.68891(14) 0.69534(13) 0.67344(10) 0.0567(9) Uani 1 1 d . . . C152 C 0.7347(2) 0.6637(2) 0.69739(16) 0.0579(14) Uani 1 1 d . . . H15B H 0.7371 0.6726 0.7352 0.069 Uiso 1 1 calc R . . H15C H 0.7663 0.6817 0.6822 0.069 Uiso 1 1 calc R . . C153 C 0.7292(2) 0.5873(2) 0.68676(17) 0.0621(15) Uani 1 1 d . . . H15D H 0.7451 0.5745 0.6541 0.074 Uiso 1 1 calc R . . H15E H 0.7453 0.5602 0.7157 0.074 Uiso 1 1 calc R . . C154 C 0.6708(2) 0.5774(2) 0.68237(17) 0.0613(15) Uani 1 1 d . . . H15F H 0.6568 0.5716 0.7170 0.074 Uiso 1 1 calc R . . H15G H 0.6613 0.5373 0.6606 0.074 Uiso 1 1 calc R . . C155 C 0.6510(2) 0.6437(2) 0.65639(17) 0.0584(13) Uani 1 1 d . . . H15H H 0.6492 0.6392 0.6181 0.070 Uiso 1 1 calc R . . H15I H 0.6161 0.6554 0.6677 0.070 Uiso 1 1 calc R . . O161 O 0.77661(13) 0.79188(13) 0.85229(11) 0.0608(9) Uani 1 1 d . . . C162 C 0.7801(2) 0.8306(2) 0.80463(18) 0.0728(16) Uani 1 1 d . . . H16B H 0.7539 0.8143 0.7780 0.087 Uiso 1 1 calc R . . H16C H 0.8149 0.8253 0.7910 0.087 Uiso 1 1 calc R . . C163 C 0.7704(3) 0.9037(2) 0.8172(3) 0.107(2) Uani 1 1 d . . . H16D H 0.8035 0.9288 0.8225 0.128 Uiso 1 1 calc R . . H16E H 0.7491 0.9259 0.7889 0.128 Uiso 1 1 calc R . . C164 C 0.7428(3) 0.9022(3) 0.8647(3) 0.119(3) Uani 1 1 d . . . H16F H 0.7049 0.8986 0.8569 0.143 Uiso 1 1 calc R . . H16G H 0.7501 0.9436 0.8856 0.143 Uiso 1 1 calc R . . C165 C 0.7633(2) 0.8399(3) 0.89287(18) 0.0846(18) Uani 1 1 d . . . H16H H 0.7944 0.8512 0.9155 0.102 Uiso 1 1 calc R . . H16I H 0.7366 0.8203 0.9146 0.102 Uiso 1 1 calc R . . O171 O 0.91920(14) 0.68977(13) 0.76697(10) 0.0568(9) Uani 1 1 d . . . C172 C 0.8707(2) 0.6568(2) 0.75175(17) 0.0606(14) Uani 1 1 d . . . H17A H 0.8631 0.6609 0.7138 0.073 Uiso 1 1 calc R . . H17B H 0.8418 0.6773 0.7699 0.073 Uiso 1 1 calc R . . C173 C 0.8779(3) 0.5826(2) 0.7672(2) 0.089(2) Uani 1 1 d . . . H17C H 0.8586 0.5521 0.7424 0.107 Uiso 1 1 calc R . . H17D H 0.8663 0.5742 0.8026 0.107 Uiso 1 1 calc R . . C174 C 0.9366(3) 0.5726(2) 0.7650(2) 0.0799(19) Uani 1 1 d . . . H17E H 0.9491 0.5348 0.7878 0.096 Uiso 1 1 calc R . . H17F H 0.9466 0.5637 0.7292 0.096 Uiso 1 1 calc R . . C175 C 0.9569(2) 0.6393(2) 0.78444(19) 0.0723(17) Uani 1 1 d . . . H17G H 0.9611 0.6391 0.8228 0.087 Uiso 1 1 calc R . . H17H H 0.9910 0.6490 0.7703 0.087 Uiso 1 1 calc R . . O181 O 0.83996(14) 0.79803(13) 0.60946(12) 0.0657(10) Uani 1 1 d . . . C182 C 0.8543(2) 0.8524(2) 0.5745(2) 0.0775(16) Uani 1 1 d . . . H18A H 0.8915 0.8492 0.5674 0.093 Uiso 1 1 calc R . . H18B H 0.8334 0.8497 0.5412 0.093 Uiso 1 1 calc R . . C183 C 0.8438(4) 0.9155(3) 0.6012(2) 0.158(4) Uani 1 1 d . . . H18C H 0.8738 0.9466 0.5991 0.190 Uiso 1 1 calc R . . H18D H 0.8131 0.9379 0.5841 0.190 Uiso 1 1 calc R . . C184 C 0.8348(3) 0.9031(2) 0.6536(3) 0.103(2) Uani 1 1 d . . . H18E H 0.8040 0.9287 0.6641 0.124 Uiso 1 1 calc R . . H18F H 0.8652 0.9168 0.6763 0.124 Uiso 1 1 calc R . . C185 C 0.8256(2) 0.8273(2) 0.65758(18) 0.0666(15) Uani 1 1 d . . . H18G H 0.8470 0.8080 0.6870 0.080 Uiso 1 1 calc R . . H18H H 0.7886 0.8180 0.6631 0.080 Uiso 1 1 calc R . . O191 O 0.56111(14) 0.77507(14) 0.45653(11) 0.0662(10) Uani 1 1 d . . . C192 C 0.5716(3) 0.8310(2) 0.42520(19) 0.0859(19) Uani 1 1 d . . . H19A H 0.5536 0.8253 0.3906 0.103 Uiso 1 1 calc R . . H19B H 0.6094 0.8335 0.4205 0.103 Uiso 1 1 calc R . . C193 C 0.5542(2) 0.8944(2) 0.44922(18) 0.0714(16) Uani 1 1 d . . . H19C H 0.5201 0.9091 0.4336 0.086 Uiso 1 1 calc R . . H19D H 0.5797 0.9315 0.4455 0.086 Uiso 1 1 calc R . . C194 C 0.5503(2) 0.8750(2) 0.50543(17) 0.0684(15) Uani 1 1 d . . . H19E H 0.5832 0.8846 0.5258 0.082 Uiso 1 1 calc R . . H19F H 0.5217 0.8996 0.5212 0.082 Uiso 1 1 calc R . . C195 C 0.5397(2) 0.8001(2) 0.50270(17) 0.0647(14) Uani 1 1 d . . . H19G H 0.5560 0.7770 0.5336 0.078 Uiso 1 1 calc R . . H19H H 0.5019 0.7915 0.5017 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.056(3) 0.0366(16) 0.0634(18) -0.0016(13) 0.0100(16) 0.0022(15) N1 0.058(3) 0.0294(17) 0.055(2) 0.0045(15) 0.0066(19) 0.0049(17) C1 0.038(4) 0.036(2) 0.062(3) -0.001(2) 0.000(2) 0.001(2) O2 0.047(3) 0.0420(17) 0.0766(19) 0.0085(14) 0.0091(16) 0.0008(15) N2 0.061(3) 0.0371(19) 0.056(2) 0.0024(17) 0.008(2) 0.0046(18) C2 0.048(4) 0.042(3) 0.056(3) 0.001(2) 0.010(2) 0.001(2) O3 0.048(3) 0.0398(17) 0.0783(19) 0.0050(14) 0.0053(17) 0.0001(15) N3 0.048(3) 0.0366(19) 0.064(2) 0.0029(16) 0.001(2) 0.0002(19) C3 0.047(4) 0.043(3) 0.056(3) -0.007(2) 0.006(2) 0.000(2) O4 0.054(3) 0.0425(16) 0.0563(16) -0.0006(13) 0.0095(15) -0.0035(14) N4 0.052(3) 0.0400(19) 0.062(2) 0.0036(16) 0.007(2) 0.000(2) C4 0.046(4) 0.043(3) 0.060(3) -0.001(2) 0.006(2) -0.001(2) O5 0.056(3) 0.0370(16) 0.0643(18) -0.0050(13) 0.0102(16) -0.0036(15) N5 0.056(3) 0.0402(19) 0.055(2) -0.0049(17) 0.003(2) -0.0076(18) O6 0.043(2) 0.0429(17) 0.0743(18) -0.0099(14) 0.0071(16) 0.0006(15) N6 0.058(3) 0.0384(18) 0.056(2) -0.0026(16) 0.008(2) -0.0105(18) O7 0.051(3) 0.0412(18) 0.0720(19) -0.0079(14) 0.0084(17) 0.0049(15) N7 0.043(3) 0.0336(18) 0.068(2) -0.0084(16) 0.001(2) 0.0034(18) O8 0.065(3) 0.0448(16) 0.0571(16) -0.0014(14) 0.0047(16) 0.0046(15) N8 0.046(3) 0.041(2) 0.073(2) -0.0060(17) 0.005(2) 0.0010(19) C11 0.051(4) 0.042(2) 0.057(3) -0.005(2) 0.004(2) -0.005(2) C12 0.047(4) 0.044(3) 0.059(3) 0.002(2) -0.005(2) 0.000(2) C13 0.060(4) 0.051(3) 0.056(3) 0.004(2) 0.005(3) 0.000(3) C14 0.063(4) 0.063(3) 0.052(3) 0.005(2) 0.003(2) -0.004(3) C15 0.049(4) 0.051(3) 0.063(3) -0.012(2) 0.006(2) 0.009(2) C16 0.057(4) 0.041(2) 0.059(3) 0.000(2) -0.001(2) 0.005(2) C21 0.049(4) 0.038(2) 0.059(3) 0.004(2) 0.008(2) -0.001(2) C22 0.040(4) 0.048(3) 0.051(2) -0.003(2) 0.005(2) 0.000(2) C23 0.069(5) 0.039(3) 0.052(3) 0.000(2) 0.010(3) 0.000(2) C24 0.054(4) 0.049(3) 0.065(3) -0.006(2) 0.011(3) -0.007(3) C25 0.052(4) 0.052(3) 0.055(3) -0.001(2) 0.007(2) -0.005(3) C26 0.040(4) 0.053(3) 0.060(3) 0.001(2) -0.003(2) -0.002(2) C31 0.048(4) 0.041(2) 0.045(2) 0.0019(19) 0.000(2) 0.005(2) C32 0.050(4) 0.042(3) 0.048(3) -0.0008(19) 0.006(2) 0.001(2) C33 0.059(4) 0.055(3) 0.051(2) 0.000(2) 0.006(3) 0.001(3) C34 0.061(4) 0.055(3) 0.052(3) -0.001(2) -0.003(2) 0.010(3) C35 0.063(5) 0.046(3) 0.059(3) -0.001(2) 0.006(3) 0.001(3) C36 0.049(4) 0.043(2) 0.054(3) 0.007(2) 0.003(2) 0.001(2) C41 0.046(4) 0.038(2) 0.057(3) -0.007(2) 0.009(2) -0.001(2) C42 0.043(4) 0.040(2) 0.061(3) -0.006(2) -0.001(2) 0.003(2) C43 0.043(4) 0.042(2) 0.067(3) -0.002(2) 0.002(2) 0.004(2) C44 0.054(4) 0.041(2) 0.067(3) -0.012(2) 0.001(3) 0.002(2) C45 0.046(4) 0.055(3) 0.057(3) -0.003(2) 0.007(2) 0.005(2) C46 0.054(4) 0.045(2) 0.057(3) -0.003(2) 0.006(2) -0.002(2) C51 0.035(3) 0.041(2) 0.055(2) 0.000(2) 0.003(2) -0.003(2) C52 0.047(4) 0.035(2) 0.078(3) -0.008(2) 0.006(3) -0.013(2) C53 0.061(4) 0.054(3) 0.056(3) -0.002(2) 0.004(3) 0.001(3) C54 0.046(4) 0.061(3) 0.056(3) 0.001(2) 0.010(2) -0.014(2) C55 0.076(5) 0.044(2) 0.055(3) 0.004(2) 0.009(3) -0.005(2) C56 0.054(4) 0.042(2) 0.062(3) -0.001(2) 0.001(2) 0.000(2) C61 0.042(4) 0.048(3) 0.058(3) -0.001(2) 0.003(2) 0.004(2) C62 0.046(4) 0.047(3) 0.051(2) 0.003(2) 0.004(2) 0.004(2) C63 0.051(4) 0.043(3) 0.062(3) 0.000(2) 0.002(3) -0.002(2) C64 0.058(5) 0.045(3) 0.063(3) 0.007(2) 0.003(3) 0.005(3) C65 0.041(4) 0.047(3) 0.071(3) -0.001(2) 0.004(2) 0.001(2) C66 0.053(4) 0.048(3) 0.066(3) 0.000(2) 0.009(3) -0.013(3) C71 0.038(4) 0.043(2) 0.055(2) 0.000(2) 0.007(2) -0.001(2) C72 0.056(4) 0.041(2) 0.059(3) -0.003(2) 0.008(3) 0.000(2) C73 0.048(4) 0.054(3) 0.064(3) 0.001(2) 0.009(3) 0.002(2) C74 0.049(4) 0.057(3) 0.061(3) 0.004(2) 0.003(2) -0.011(3) C75 0.054(4) 0.053(3) 0.067(3) -0.004(2) 0.006(3) -0.004(3) C76 0.040(4) 0.051(3) 0.072(3) -0.011(2) 0.004(3) 0.005(2) C81 0.043(4) 0.043(2) 0.062(3) 0.003(2) -0.001(2) 0.001(2) C82 0.038(3) 0.040(2) 0.057(3) 0.003(2) 0.000(2) -0.002(2) C83 0.052(4) 0.037(2) 0.064(3) -0.001(2) 0.005(2) 0.005(2) C84 0.051(4) 0.044(2) 0.069(3) 0.010(2) 0.011(2) -0.007(2) C85 0.057(4) 0.051(3) 0.060(3) 0.001(2) 0.013(2) -0.004(2) C86 0.047(4) 0.055(3) 0.068(3) -0.003(2) 0.006(3) 0.010(2) O1A 0.068(3) 0.0361(16) 0.0656(18) -0.0018(13) 0.0116(17) 0.0032(15) N1A 0.050(3) 0.0364(18) 0.061(2) 0.0018(17) 0.0037(19) 0.0032(17) C1A 0.041(4) 0.054(3) 0.051(3) -0.004(2) -0.007(2) 0.001(2) O2A 0.047(2) 0.0483(17) 0.0665(18) 0.0080(14) 0.0100(15) -0.0018(15) N2A 0.059(3) 0.0359(18) 0.052(2) 0.0045(16) 0.0105(19) 0.0085(18) O3A 0.061(3) 0.0383(17) 0.0697(18) -0.0006(14) 0.0070(16) -0.0020(15) N3A 0.051(3) 0.0352(19) 0.065(2) 0.0097(16) -0.006(2) -0.0054(19) C3A 0.051(4) 0.042(3) 0.055(3) 0.006(2) 0.011(2) 0.001(2) N4A 0.047(3) 0.0369(19) 0.060(2) 0.0030(16) -0.0058(19) -0.0041(19) O4A 0.063(3) 0.0416(16) 0.0614(16) 0.0009(14) 0.0107(16) -0.0066(15) O5A 0.048(3) 0.0382(17) 0.0654(18) -0.0008(13) 0.0110(16) 0.0009(14) N5A 0.047(3) 0.0356(18) 0.062(2) -0.0065(16) 0.0055(19) -0.0112(17) C5A 0.039(4) 0.050(3) 0.055(3) 0.001(2) -0.001(2) 0.001(2) O6A 0.045(3) 0.0548(18) 0.0758(19) -0.0140(15) 0.0161(16) 0.0011(16) N6A 0.052(3) 0.0395(18) 0.057(2) 0.0018(16) 0.0078(19) -0.0051(17) O7A 0.046(2) 0.0401(17) 0.0741(19) -0.0026(14) 0.0038(16) 0.0031(14) N7A 0.047(3) 0.0368(19) 0.061(2) -0.0045(16) 0.003(2) 0.0040(19) C7A 0.037(4) 0.045(3) 0.056(3) -0.001(2) 0.008(2) 0.005(2) N8A 0.044(3) 0.0369(19) 0.068(2) -0.0048(16) 0.003(2) 0.0042(19) O8A 0.063(3) 0.0478(17) 0.0651(17) -0.0019(14) -0.0021(16) 0.0137(16) C11A 0.043(4) 0.043(2) 0.055(3) 0.002(2) -0.001(2) -0.001(2) C12A 0.044(4) 0.049(3) 0.064(3) -0.001(2) 0.003(2) 0.002(2) C13A 0.053(4) 0.062(3) 0.054(3) -0.002(2) 0.005(2) -0.004(3) C14A 0.059(4) 0.062(3) 0.062(3) -0.011(2) 0.015(3) 0.004(3) C15A 0.061(4) 0.052(3) 0.062(3) -0.009(2) 0.010(3) 0.003(2) C16A 0.067(4) 0.042(2) 0.058(3) 0.002(2) 0.002(3) 0.003(2) C21A 0.054(4) 0.045(3) 0.055(3) 0.003(2) 0.008(2) -0.005(2) C22A 0.049(4) 0.041(2) 0.052(3) -0.003(2) 0.000(2) -0.003(2) C23A 0.062(4) 0.041(2) 0.045(2) 0.0008(18) 0.002(2) -0.007(2) C24A 0.066(5) 0.053(3) 0.053(3) -0.009(2) 0.010(3) -0.011(3) C25A 0.040(4) 0.070(3) 0.060(3) 0.000(2) 0.004(2) -0.007(3) C26A 0.049(4) 0.058(3) 0.059(3) 0.004(2) 0.002(2) -0.005(3) C31A 0.053(4) 0.036(2) 0.053(2) 0.0019(19) 0.008(2) 0.001(2) C32A 0.063(4) 0.044(3) 0.046(2) 0.007(2) 0.007(2) 0.002(3) C33A 0.058(4) 0.053(3) 0.062(3) 0.007(2) 0.000(3) -0.010(3) C34A 0.042(4) 0.076(3) 0.070(3) 0.001(3) 0.001(3) 0.006(3) C35A 0.067(5) 0.049(3) 0.065(3) 0.011(2) 0.004(3) 0.003(3) C36A 0.057(4) 0.045(3) 0.058(3) 0.002(2) 0.006(3) -0.003(2) C41A 0.042(4) 0.038(2) 0.057(3) -0.007(2) 0.004(2) 0.001(2) C42A 0.042(4) 0.039(2) 0.057(3) -0.008(2) 0.002(2) -0.005(2) C43A 0.034(3) 0.047(2) 0.061(3) -0.001(2) 0.003(2) -0.003(2) C44A 0.041(4) 0.045(3) 0.067(3) -0.007(2) 0.008(2) 0.005(2) C45A 0.055(4) 0.051(3) 0.056(3) -0.006(2) 0.008(2) 0.003(2) C46A 0.050(4) 0.043(2) 0.062(3) 0.002(2) 0.005(2) 0.000(2) C51A 0.047(4) 0.042(2) 0.052(2) 0.009(2) 0.006(2) 0.002(2) C52A 0.045(4) 0.045(3) 0.060(3) -0.005(2) 0.003(2) -0.005(2) C53A 0.059(4) 0.058(3) 0.055(3) -0.003(2) 0.002(2) 0.006(3) C54A 0.056(4) 0.061(3) 0.052(3) 0.003(2) 0.006(2) 0.001(3) C55A 0.059(4) 0.058(3) 0.060(3) 0.009(2) 0.006(3) -0.003(2) C56A 0.054(4) 0.046(3) 0.054(2) 0.003(2) -0.002(2) 0.002(2) C61A 0.048(4) 0.045(3) 0.059(3) -0.003(2) 0.006(3) 0.001(2) C62A 0.032(4) 0.050(3) 0.052(2) -0.002(2) 0.001(2) 0.004(2) C63A 0.047(4) 0.042(2) 0.059(3) -0.001(2) 0.000(2) 0.004(2) C64A 0.048(4) 0.047(3) 0.070(3) 0.006(2) 0.006(3) 0.008(3) C65A 0.043(4) 0.061(3) 0.068(3) 0.000(2) 0.003(2) 0.006(3) C66A 0.043(4) 0.062(3) 0.060(3) -0.007(2) 0.001(2) -0.002(3) C71A 0.053(4) 0.048(3) 0.046(2) 0.003(2) 0.006(2) 0.004(2) C72A 0.047(4) 0.051(3) 0.048(2) 0.002(2) 0.001(2) 0.005(2) C73A 0.065(5) 0.057(3) 0.056(3) 0.012(2) -0.001(3) 0.004(3) C74A 0.041(4) 0.064(3) 0.069(3) 0.008(2) 0.000(2) -0.001(3) C75A 0.054(4) 0.050(3) 0.067(3) 0.002(2) -0.002(3) -0.006(2) C76A 0.056(4) 0.048(3) 0.059(3) -0.001(2) 0.007(3) 0.003(2) C81A 0.054(4) 0.045(3) 0.066(3) 0.008(2) 0.005(3) 0.013(2) C82A 0.045(4) 0.039(2) 0.054(2) 0.007(2) 0.001(2) -0.001(2) C83A 0.047(4) 0.043(2) 0.065(3) -0.001(2) 0.009(2) 0.002(2) C84A 0.058(4) 0.051(3) 0.066(3) 0.010(2) 0.011(3) -0.002(2) C85A 0.049(4) 0.060(3) 0.068(3) 0.009(2) 0.012(3) 0.006(2) C86A 0.063(4) 0.059(3) 0.066(3) 0.006(2) 0.019(3) 0.016(3) O101 0.056(3) 0.0528(19) 0.085(2) 0.0095(17) 0.0107(18) -0.0001(16) C102 0.067(5) 0.080(3) 0.061(3) 0.004(3) 0.015(3) 0.005(3) C103 0.054(4) 0.058(3) 0.089(4) -0.014(3) 0.017(3) -0.011(3) C104 0.061(4) 0.059(3) 0.068(3) 0.000(2) 0.007(3) 0.000(3) C105 0.086(5) 0.057(3) 0.065(3) -0.007(2) 0.017(3) -0.004(3) O111 0.055(3) 0.0461(17) 0.0734(19) -0.0020(14) 0.0046(17) 0.0033(16) C112 0.060(4) 0.055(3) 0.074(3) -0.002(2) 0.010(3) -0.006(3) C113 0.093(7) 0.050(3) 0.213(7) -0.033(4) 0.005(6) 0.004(3) C114 0.111(7) 0.048(3) 0.101(4) -0.004(3) 0.006(4) 0.009(3) C115 0.060(5) 0.055(3) 0.072(3) 0.008(2) 0.011(3) 0.007(3) O121 0.060(3) 0.0432(16) 0.0671(18) 0.0038(14) -0.0001(17) 0.0034(15) C122 0.067(5) 0.048(3) 0.090(3) -0.010(3) -0.002(3) 0.003(3) C123 0.054(4) 0.051(3) 0.120(4) -0.019(3) -0.015(3) 0.003(3) C124 0.078(5) 0.053(3) 0.129(5) 0.021(3) -0.006(4) -0.007(3) C125 0.058(4) 0.043(3) 0.080(3) 0.004(2) -0.009(3) 0.000(2) O131 0.061(3) 0.0495(18) 0.0721(19) -0.0004(15) 0.0088(18) 0.0060(17) C132 0.096(6) 0.080(4) 0.079(3) -0.006(3) 0.008(3) -0.045(3) C133 0.233(11) 0.049(4) 0.296(11) -0.044(5) 0.231(10) -0.044(5) C134 0.391(17) 0.054(4) 0.066(4) -0.006(3) -0.035(6) 0.021(7) C135 0.113(7) 0.100(4) 0.087(4) 0.022(3) 0.024(4) 0.067(4) O141 0.062(3) 0.0458(17) 0.0681(18) -0.0035(14) 0.0011(17) -0.0058(15) C142 0.060(4) 0.050(3) 0.068(3) -0.007(2) -0.002(3) 0.001(2) C143 0.069(5) 0.051(3) 0.093(3) -0.011(2) 0.000(3) 0.005(3) C144 0.077(5) 0.038(3) 0.098(4) 0.005(2) 0.002(3) 0.001(2) C145 0.068(5) 0.059(3) 0.074(3) 0.004(2) 0.001(3) -0.015(3) O151 0.058(3) 0.0454(17) 0.0660(18) 0.0037(14) 0.0004(17) -0.0030(16) C152 0.063(5) 0.051(3) 0.060(3) 0.007(2) 0.006(3) 0.000(3) C153 0.074(5) 0.047(3) 0.067(3) 0.005(2) 0.022(3) 0.007(3) C154 0.070(5) 0.046(3) 0.071(3) -0.005(2) 0.023(3) 0.000(3) C155 0.049(4) 0.049(3) 0.079(3) -0.006(2) 0.011(3) -0.005(2) O161 0.065(3) 0.0453(16) 0.0720(19) 0.0020(15) 0.0026(17) -0.0005(16) C162 0.053(5) 0.074(3) 0.091(4) 0.021(3) -0.003(3) -0.002(3) C163 0.082(6) 0.050(3) 0.182(7) 0.019(4) -0.052(5) -0.013(3) C164 0.107(7) 0.048(3) 0.208(7) -0.015(4) 0.066(6) 0.010(3) C165 0.071(5) 0.102(4) 0.080(3) -0.020(3) -0.005(3) 0.022(3) O171 0.058(3) 0.0413(17) 0.0716(19) -0.0024(14) 0.0041(17) -0.0044(16) C172 0.056(4) 0.058(3) 0.069(3) -0.005(2) 0.010(3) -0.004(3) C173 0.122(7) 0.046(3) 0.106(4) -0.021(3) 0.061(4) -0.024(3) C174 0.110(6) 0.045(3) 0.086(4) 0.005(2) 0.025(4) 0.015(3) C175 0.081(5) 0.062(3) 0.074(3) 0.000(3) 0.004(3) 0.021(3) O181 0.068(3) 0.0396(16) 0.090(2) -0.0050(16) 0.0085(19) 0.0010(16) C182 0.068(5) 0.055(3) 0.111(4) 0.019(3) 0.015(3) -0.002(3) C183 0.344(14) 0.045(3) 0.083(4) 0.009(3) -0.005(6) -0.034(5) C184 0.086(6) 0.052(3) 0.172(6) -0.030(4) 0.023(5) 0.001(3) C185 0.063(4) 0.048(3) 0.088(3) -0.005(2) 0.000(3) 0.008(2) O191 0.069(3) 0.0564(19) 0.0745(19) -0.0007(16) 0.0117(18) 0.0049(17) C192 0.113(6) 0.067(3) 0.081(3) 0.001(3) 0.037(4) -0.005(3) C193 0.061(5) 0.064(3) 0.090(4) 0.006(3) 0.012(3) 0.004(3) C194 0.058(5) 0.075(3) 0.074(3) -0.007(3) 0.012(3) 0.003(3) C195 0.053(4) 0.076(3) 0.065(3) 0.016(3) 0.007(3) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.221(4) . ? N1 C1 1.374(5) . ? N1 C82 1.414(4) . ? N1 H1 0.8800 . ? C1 N2 1.380(5) . ? O2 C12 1.407(5) . ? O2 C21 1.410(5) . ? N2 C11 1.405(5) . ? N2 H2 0.8800 . ? C2 O3 1.224(4) . ? C2 N3 1.378(6) . ? C2 N4 1.383(6) . ? N3 C22 1.402(6) . ? N3 H3 0.8800 . ? C3 O7 1.222(4) . ? C3 N8 1.374(6) . ? C3 N7 1.386(6) . ? O4 C32 1.396(4) . ? O4 C41 1.406(4) . ? N4 C31 1.407(6) . ? N4 H4 0.8800 . ? C4 O5 1.216(4) . ? C4 N5 1.391(5) . ? C4 N6 1.390(5) . ? N5 C42 1.399(4) . ? N5 H5 0.8800 . ? O6 C61 1.394(5) . ? O6 C52 1.409(5) . ? N6 C51 1.407(4) . ? N6 H6 0.8800 . ? N7 C62 1.400(6) . ? N7 H7 0.8800 . ? O8 C81 1.388(4) . ? O8 C72 1.405(5) . ? N8 C71 1.411(6) . ? N8 H8 0.8800 . ? C11 C16 1.389(6) . ? C11 C12 1.401(5) . ? C12 C13 1.383(5) . ? C13 C14 1.381(6) . ? C13 H13 0.9500 . ? C14 C15 1.389(5) . ? C14 H14 0.9500 . ? C15 C16 1.401(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.366(6) . ? C21 C22 1.400(6) . ? C22 C23 1.399(6) . ? C23 C24 1.409(7) . ? C23 H23 0.9500 . ? C24 C25 1.374(6) . ? C24 H24 0.9500 . ? C25 C26 1.381(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C36 1.388(5) . ? C31 C32 1.391(6) . ? C32 C33 1.379(7) . ? C33 C34 1.380(5) . ? C33 H33 0.9500 . ? C34 C35 1.385(6) . ? C34 H34 0.9500 . ? C35 C36 1.380(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C46 1.372(5) . ? C41 C42 1.401(5) . ? C42 C43 1.393(5) . ? C43 C44 1.389(5) . ? C43 H43 0.9500 . ? C44 C45 1.394(5) . ? C44 H44 0.9500 . ? C45 C46 1.388(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.385(6) . ? C51 C52 1.386(5) . ? C52 C53 1.378(5) . ? C53 C54 1.376(6) . ? C53 H53 0.9500 . ? C54 C55 1.381(5) . ? C54 H54 0.9500 . ? C55 C56 1.397(5) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C66 1.384(6) . ? C61 C62 1.397(6) . ? C62 C63 1.389(6) . ? C63 C64 1.377(7) . ? C63 H63 0.9500 . ? C64 C65 1.376(6) . ? C64 H64 0.9500 . ? C65 C66 1.389(6) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C76 1.378(5) . ? C71 C72 1.398(6) . ? C72 C73 1.359(6) . ? C73 C74 1.386(6) . ? C73 H73 0.9500 . ? C74 C75 1.394(7) . ? C74 H74 0.9500 . ? C75 C76 1.376(7) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C86 1.376(5) . ? C81 C82 1.397(5) . ? C82 C83 1.386(5) . ? C83 C84 1.384(5) . ? C83 H83 0.9500 . ? C84 C85 1.380(5) . ? C84 H84 0.9500 . ? C85 C86 1.377(5) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? O1A C1A 1.215(5) . ? N1A C1A 1.388(5) . ? N1A C82A 1.415(4) . ? N1A H1A 0.8800 . ? C1A N2A 1.381(5) . ? O2A C21A 1.398(5) . ? O2A C12A 1.413(5) . ? N2A C11A 1.413(5) . ? N2A H2A 0.8800 . ? O3A C3A 1.230(4) . ? N3A C3A 1.370(6) . ? N3A C22A 1.416(6) . ? N3A H3A 0.8800 . ? C3A N4A 1.379(6) . ? N4A C31A 1.407(6) . ? N4A H4A 0.8800 . ? O4A C41A 1.399(4) . ? O4A C32A 1.408(4) . ? O5A C5A 1.207(5) . ? N5A C5A 1.395(5) . ? N5A C42A 1.406(4) . ? N5A H5A 0.8800 . ? C5A N6A 1.397(5) . ? O6A C52A 1.397(5) . ? O6A C61A 1.405(5) . ? N6A C51A 1.410(4) . ? N6A H6A 0.8800 . ? O7A C7A 1.228(5) . ? N7A C7A 1.382(6) . ? N7A C62A 1.391(6) . ? N7A H7A 0.8800 . ? C7A N8A 1.373(6) . ? N8A C71A 1.399(6) . ? N8A H8A 0.8800 . ? O8A C81A 1.393(5) . ? O8A C72A 1.403(5) . ? C11A C16A 1.390(6) . ? C11A C12A 1.401(5) . ? C12A C13A 1.386(5) . ? C13A C14A 1.383(6) . ? C13A H13A 0.9500 . ? C14A C15A 1.379(5) . ? C14A H14A 0.9500 . ? C15A C16A 1.387(5) . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? C21A C26A 1.374(6) . ? C21A C22A 1.391(6) . ? C22A C23A 1.400(5) . ? C23A C24A 1.388(6) . ? C23A H23A 0.9500 . ? C24A C25A 1.376(6) . ? C24A H24A 0.9500 . ? C25A C26A 1.387(6) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? C31A C32A 1.381(7) . ? C31A C36A 1.386(5) . ? C32A C33A 1.369(7) . ? C33A C34A 1.382(6) . ? C33A H33A 0.9500 . ? C34A C35A 1.396(7) . ? C34A H34A 0.9500 . ? C35A C36A 1.380(6) . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? C41A C46A 1.358(5) . ? C41A C42A 1.402(5) . ? C42A C43A 1.391(5) . ? C43A C44A 1.393(5) . ? C43A H43A 0.9500 . ? C44A C45A 1.373(5) . ? C44A H44A 0.9500 . ? C45A C46A 1.400(5) . ? C45A H45A 0.9500 . ? C46A H46A 0.9500 . ? C51A C56A 1.377(5) . ? C51A C52A 1.394(5) . ? C52A C53A 1.380(5) . ? C53A C54A 1.369(6) . ? C53A H53A 0.9500 . ? C54A C55A 1.376(5) . ? C54A H54A 0.9500 . ? C55A C56A 1.405(5) . ? C55A H55A 0.9500 . ? C56A H56A 0.9500 . ? C61A C66A 1.359(7) . ? C61A C62A 1.393(6) . ? C62A C63A 1.405(5) . ? C63A C64A 1.384(6) . ? C63A H63A 0.9500 . ? C64A C65A 1.404(6) . ? C64A H64A 0.9500 . ? C65A C66A 1.383(6) . ? C65A H65A 0.9500 . ? C66A H66A 0.9500 . ? C71A C76A 1.395(6) . ? C71A C72A 1.406(6) . ? C72A C73A 1.356(6) . ? C73A C74A 1.380(6) . ? C73A H73A 0.9500 . ? C74A C75A 1.377(6) . ? C74A H74A 0.9500 . ? C75A C76A 1.400(6) . ? C75A H75A 0.9500 . ? C76A H76A 0.9500 . ? C81A C86A 1.372(5) . ? C81A C82A 1.390(5) . ? C82A C83A 1.381(5) . ? C83A C84A 1.389(5) . ? C83A H83A 0.9500 . ? C84A C85A 1.389(5) . ? C84A H84A 0.9500 . ? C85A C86A 1.363(5) . ? C85A H85A 0.9500 . ? C86A H86A 0.9500 . ? O101 C105 1.427(4) . ? O101 C102 1.435(5) . ? C102 C103 1.514(6) . ? C102 H10A 0.9900 . ? C102 H10B 0.9900 . ? C103 C104 1.501(6) . ? C103 H10C 0.9900 . ? C103 H10D 0.9900 . ? C104 C105 1.487(6) . ? C104 H10E 0.9900 . ? C104 H10F 0.9900 . ? C105 H10G 0.9900 . ? C105 H10H 0.9900 . ? O111 C115 1.432(6) . ? O111 C112 1.456(5) . ? C112 C113 1.469(7) . ? C112 H11A 0.9900 . ? C112 H11B 0.9900 . ? C113 C114 1.449(8) . ? C113 H11C 0.9900 . ? C113 H11D 0.9900 . ? C114 C115 1.497(6) . ? C114 H11E 0.9900 . ? C114 H11F 0.9900 . ? C115 H11G 0.9900 . ? C115 H11H 0.9900 . ? O121 C125 1.447(4) . ? O121 C122 1.455(5) . ? C122 C123 1.510(6) . ? C122 H12A 0.9900 . ? C122 H12B 0.9900 . ? C123 C124 1.522(6) . ? C123 H12C 0.9900 . ? C123 H12D 0.9900 . ? C124 C125 1.524(6) . ? C124 H12E 0.9900 . ? C124 H12F 0.9900 . ? C125 H12G 0.9900 . ? C125 H12H 0.9900 . ? O131 C132 1.441(6) . ? O131 C135 1.446(6) . ? C132 C133 1.545(9) . ? C132 H13B 0.9900 . ? C132 H13C 0.9900 . ? C133 C134 1.402(13) . ? C133 H13D 0.9900 . ? C133 H13E 0.9900 . ? C134 C135 1.489(10) . ? C134 H13F 0.9900 . ? C134 H13G 0.9900 . ? C135 H13H 0.9900 . ? C135 H13I 0.9900 . ? O141 C142 1.447(4) . ? O141 C145 1.469(4) . ? C142 C143 1.511(6) . ? C142 H14B 0.9900 . ? C142 H14C 0.9900 . ? C143 C144 1.515(6) . ? C143 H14D 0.9900 . ? C143 H14E 0.9900 . ? C144 C145 1.486(6) . ? C144 H14F 0.9900 . ? C144 H14G 0.9900 . ? C145 H14H 0.9900 . ? C145 H14I 0.9900 . ? O151 C152 1.444(6) . ? O151 C155 1.462(5) . ? C152 C153 1.533(6) . ? C152 H15B 0.9900 . ? C152 H15C 0.9900 . ? C153 C154 1.516(7) . ? C153 H15D 0.9900 . ? C153 H15E 0.9900 . ? C154 C155 1.541(6) . ? C154 H15F 0.9900 . ? C154 H15G 0.9900 . ? C155 H15H 0.9900 . ? C155 H15I 0.9900 . ? O161 C162 1.454(5) . ? O161 C165 1.464(5) . ? C162 C163 1.498(7) . ? C162 H16B 0.9900 . ? C162 H16C 0.9900 . ? C163 C164 1.449(7) . ? C163 H16D 0.9900 . ? C163 H16E 0.9900 . ? C164 C165 1.505(7) . ? C164 H16F 0.9900 . ? C164 H16G 0.9900 . ? C165 H16H 0.9900 . ? C165 H16I 0.9900 . ? O171 C172 1.444(6) . ? O171 C175 1.445(6) . ? C172 C173 1.521(6) . ? C172 H17A 0.9900 . ? C172 H17B 0.9900 . ? C173 C174 1.532(8) . ? C173 H17C 0.9900 . ? C173 H17D 0.9900 . ? C174 C175 1.489(7) . ? C174 H17E 0.9900 . ? C174 H17F 0.9900 . ? C175 H17G 0.9900 . ? C175 H17H 0.9900 . ? O181 C185 1.436(4) . ? O181 C182 1.460(5) . ? C182 C183 1.452(7) . ? C182 H18A 0.9900 . ? C182 H18B 0.9900 . ? C183 C184 1.406(6) . ? C183 H18C 0.9900 . ? C183 H18D 0.9900 . ? C184 C185 1.512(6) . ? C184 H18E 0.9900 . ? C184 H18F 0.9900 . ? C185 H18G 0.9900 . ? C185 H18H 0.9900 . ? O191 C192 1.400(5) . ? O191 C195 1.428(5) . ? C192 C193 1.475(6) . ? C192 H19A 0.9900 . ? C192 H19B 0.9900 . ? C193 C194 1.508(6) . ? C193 H19C 0.9900 . ? C193 H19D 0.9900 . ? C194 C195 1.499(6) . ? C194 H19E 0.9900 . ? C194 H19F 0.9900 . ? C195 H19G 0.9900 . ? C195 H19H 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C82 126.1(3) . . ? C1 N1 H1 116.9 . . ? C82 N1 H1 116.9 . . ? O1 C1 N1 124.6(4) . . ? O1 C1 N2 124.0(4) . . ? N1 C1 N2 111.4(3) . . ? C12 O2 C21 118.3(4) . . ? C1 N2 C11 125.4(3) . . ? C1 N2 H2 117.3 . . ? C11 N2 H2 117.3 . . ? O3 C2 N3 124.3(5) . . ? O3 C2 N4 123.4(5) . . ? N3 C2 N4 112.3(4) . . ? C2 N3 C22 127.7(4) . . ? C2 N3 H3 116.2 . . ? C22 N3 H3 116.2 . . ? O7 C3 N8 124.0(5) . . ? O7 C3 N7 124.4(5) . . ? N8 C3 N7 111.6(4) . . ? C32 O4 C41 118.3(3) . . ? C2 N4 C31 125.3(4) . . ? C2 N4 H4 117.4 . . ? C31 N4 H4 117.4 . . ? O5 C4 N5 124.9(4) . . ? O5 C4 N6 123.6(4) . . ? N5 C4 N6 111.5(3) . . ? C4 N5 C42 125.8(3) . . ? C4 N5 H5 117.1 . . ? C42 N5 H5 117.1 . . ? C61 O6 C52 119.8(4) . . ? C4 N6 C51 126.5(3) . . ? C4 N6 H6 116.8 . . ? C51 N6 H6 116.8 . . ? C3 N7 C62 126.1(4) . . ? C3 N7 H7 116.9 . . ? C62 N7 H7 116.9 . . ? C81 O8 C72 120.3(3) . . ? C3 N8 C71 126.6(4) . . ? C3 N8 H8 116.7 . . ? C71 N8 H8 116.7 . . ? C16 C11 C12 117.3(4) . . ? C16 C11 N2 125.6(4) . . ? C12 C11 N2 117.1(4) . . ? C13 C12 C11 122.7(4) . . ? C13 C12 O2 120.3(4) . . ? C11 C12 O2 116.8(4) . . ? C14 C13 C12 118.8(4) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 119.8(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.9(4) . . ? C11 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C26 C21 C22 121.8(4) . . ? C26 C21 O2 124.0(4) . . ? C22 C21 O2 114.0(5) . . ? C23 C22 C21 118.2(5) . . ? C23 C22 N3 123.8(4) . . ? C21 C22 N3 118.0(4) . . ? C22 C23 C24 118.8(5) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 121.7(4) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 118.9(5) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 120.5(4) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C36 C31 C32 118.7(5) . . ? C36 C31 N4 124.3(4) . . ? C32 C31 N4 117.1(4) . . ? C33 C32 C31 121.2(4) . . ? C33 C32 O4 121.1(4) . . ? C31 C32 O4 117.6(5) . . ? C34 C33 C32 119.6(5) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 119.8(5) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 120.6(4) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 120.2(5) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C46 C41 C42 122.9(4) . . ? C46 C41 O4 123.5(3) . . ? C42 C41 O4 113.5(3) . . ? C43 C42 N5 125.5(4) . . ? C43 C42 C41 117.6(4) . . ? N5 C42 C41 116.9(3) . . ? C44 C43 C42 119.7(4) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C45 121.5(4) . . ? C43 C44 H44 119.2 . . ? C45 C44 H44 119.2 . . ? C46 C45 C44 119.0(4) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C41 C46 C45 119.1(4) . . ? C41 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C56 C51 C52 118.2(4) . . ? C56 C51 N6 124.2(4) . . ? C52 C51 N6 117.6(4) . . ? C53 C52 C51 122.4(4) . . ? C53 C52 O6 120.1(4) . . ? C51 C52 O6 117.2(4) . . ? C54 C53 C52 118.9(4) . . ? C54 C53 H53 120.5 . . ? C52 C53 H53 120.5 . . ? C53 C54 C55 120.2(4) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C54 C55 C56 120.3(4) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C51 C56 C55 120.0(4) . . ? C51 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C66 C61 O6 123.1(4) . . ? C66 C61 C62 121.6(4) . . ? O6 C61 C62 115.2(5) . . ? C63 C62 C61 118.0(5) . . ? C63 C62 N7 125.8(4) . . ? C61 C62 N7 116.2(4) . . ? C64 C63 C62 120.4(5) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C65 C64 C63 121.3(4) . . ? C65 C64 H64 119.4 . . ? C63 C64 H64 119.4 . . ? C64 C65 C66 119.5(5) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C61 C66 C65 119.2(5) . . ? C61 C66 H66 120.4 . . ? C65 C66 H66 120.4 . . ? C76 C71 C72 117.5(5) . . ? C76 C71 N8 125.7(4) . . ? C72 C71 N8 116.8(4) . . ? C73 C72 C71 122.9(4) . . ? C73 C72 O8 121.1(4) . . ? C71 C72 O8 115.8(5) . . ? C72 C73 C74 118.8(5) . . ? C72 C73 H73 120.6 . . ? C74 C73 H73 120.6 . . ? C73 C74 C75 119.7(5) . . ? C73 C74 H74 120.2 . . ? C75 C74 H74 120.2 . . ? C76 C75 C74 120.2(4) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C75 C76 C71 120.9(5) . . ? C75 C76 H76 119.5 . . ? C71 C76 H76 119.5 . . ? C86 C81 O8 124.5(4) . . ? C86 C81 C82 121.7(4) . . ? O8 C81 C82 113.8(3) . . ? C83 C82 C81 117.9(4) . . ? C83 C82 N1 126.4(4) . . ? C81 C82 N1 115.7(3) . . ? C82 C83 C84 120.4(4) . . ? C82 C83 H83 119.8 . . ? C84 C83 H83 119.8 . . ? C85 C84 C83 120.7(4) . . ? C85 C84 H84 119.7 . . ? C83 C84 H84 119.7 . . ? C86 C85 C84 119.7(4) . . ? C86 C85 H85 120.1 . . ? C84 C85 H85 120.1 . . ? C81 C86 C85 119.6(4) . . ? C81 C86 H86 120.2 . . ? C85 C86 H86 120.2 . . ? C1A N1A C82A 126.1(3) . . ? C1A N1A H1A 116.9 . . ? C82A N1A H1A 116.9 . . ? O1A C1A N2A 124.6(4) . . ? O1A C1A N1A 123.5(4) . . ? N2A C1A N1A 111.9(4) . . ? C21A O2A C12A 118.8(4) . . ? C1A N2A C11A 123.9(3) . . ? C1A N2A H2A 118.0 . . ? C11A N2A H2A 118.0 . . ? C3A N3A C22A 126.3(4) . . ? C3A N3A H3A 116.8 . . ? C22A N3A H3A 116.8 . . ? O3A C3A N3A 124.2(5) . . ? O3A C3A N4A 123.1(5) . . ? N3A C3A N4A 112.7(4) . . ? C3A N4A C31A 126.7(4) . . ? C3A N4A H4A 116.6 . . ? C31A N4A H4A 116.6 . . ? C41A O4A C32A 121.4(3) . . ? C5A N5A C42A 125.7(3) . . ? C5A N5A H5A 117.1 . . ? C42A N5A H5A 117.1 . . ? O5A C5A N5A 124.6(4) . . ? O5A C5A N6A 125.2(4) . . ? N5A C5A N6A 110.2(3) . . ? C52A O6A C61A 120.1(4) . . ? C5A N6A C51A 126.1(3) . . ? C5A N6A H6A 116.9 . . ? C51A N6A H6A 116.9 . . ? C7A N7A C62A 128.3(4) . . ? C7A N7A H7A 115.9 . . ? C62A N7A H7A 115.9 . . ? O7A C7A N8A 124.8(5) . . ? O7A C7A N7A 123.6(4) . . ? N8A C7A N7A 111.6(4) . . ? C7A N8A C71A 127.2(4) . . ? C7A N8A H8A 116.4 . . ? C71A N8A H8A 116.4 . . ? C81A O8A C72A 120.7(4) . . ? C16A C11A C12A 116.9(4) . . ? C16A C11A N2A 126.0(4) . . ? C12A C11A N2A 117.1(4) . . ? C13A C12A C11A 122.8(4) . . ? C13A C12A O2A 121.1(4) . . ? C11A C12A O2A 116.1(3) . . ? C14A C13A C12A 118.7(4) . . ? C14A C13A H13A 120.6 . . ? C12A C13A H13A 120.6 . . ? C15A C14A C13A 119.7(4) . . ? C15A C14A H14A 120.1 . . ? C13A C14A H14A 120.1 . . ? C14A C15A C16A 121.1(4) . . ? C14A C15A H15A 119.4 . . ? C16A C15A H15A 119.4 . . ? C15A C16A C11A 120.7(4) . . ? C15A C16A H16A 119.7 . . ? C11A C16A H16A 119.7 . . ? C26A C21A C22A 122.3(4) . . ? C26A C21A O2A 121.6(4) . . ? C22A C21A O2A 116.1(5) . . ? C21A C22A C23A 118.0(5) . . ? C21A C22A N3A 117.3(4) . . ? C23A C22A N3A 124.6(4) . . ? C24A C23A C22A 119.5(5) . . ? C24A C23A H23A 120.3 . . ? C22A C23A H23A 120.3 . . ? C25A C24A C23A 121.6(4) . . ? C25A C24A H24A 119.2 . . ? C23A C24A H24A 119.2 . . ? C24A C25A C26A 119.3(5) . . ? C24A C25A H25A 120.3 . . ? C26A C25A H25A 120.3 . . ? C21A C26A C25A 119.4(5) . . ? C21A C26A H26A 120.3 . . ? C25A C26A H26A 120.3 . . ? C32A C31A C36A 118.0(5) . . ? C32A C31A N4A 117.9(4) . . ? C36A C31A N4A 124.1(4) . . ? C33A C32A C31A 123.0(4) . . ? C33A C32A O4A 120.5(4) . . ? C31A C32A O4A 116.5(4) . . ? C32A C33A C34A 118.7(5) . . ? C32A C33A H33A 120.6 . . ? C34A C33A H33A 120.6 . . ? C33A C34A C35A 119.4(5) . . ? C33A C34A H34A 120.3 . . ? C35A C34A H34A 120.3 . . ? C36A C35A C34A 120.8(4) . . ? C36A C35A H35A 119.6 . . ? C34A C35A H35A 119.6 . . ? C35A C36A C31A 119.9(5) . . ? C35A C36A H36A 120.0 . . ? C31A C36A H36A 120.0 . . ? C46A C41A O4A 124.7(3) . . ? C46A C41A C42A 122.3(4) . . ? O4A C41A C42A 113.0(3) . . ? C43A C42A C41A 118.1(3) . . ? C43A C42A N5A 124.9(4) . . ? C41A C42A N5A 117.1(3) . . ? C42A C43A C44A 119.6(4) . . ? C42A C43A H43A 120.2 . . ? C44A C43A H43A 120.2 . . ? C45A C44A C43A 121.0(4) . . ? C45A C44A H44A 119.5 . . ? C43A C44A H44A 119.5 . . ? C44A C45A C46A 119.7(4) . . ? C44A C45A H45A 120.1 . . ? C46A C45A H45A 120.1 . . ? C41A C46A C45A 119.1(4) . . ? C41A C46A H46A 120.5 . . ? C45A C46A H46A 120.5 . . ? C56A C51A C52A 118.7(4) . . ? C56A C51A N6A 125.3(4) . . ? C52A C51A N6A 116.0(4) . . ? C53A C52A C51A 121.4(4) . . ? C53A C52A O6A 123.0(4) . . ? C51A C52A O6A 115.5(4) . . ? C54A C53A C52A 119.6(4) . . ? C54A C53A H53A 120.2 . . ? C52A C53A H53A 120.2 . . ? C53A C54A C55A 120.2(4) . . ? C53A C54A H54A 119.9 . . ? C55A C54A H54A 119.9 . . ? C54A C55A C56A 120.3(4) . . ? C54A C55A H55A 119.8 . . ? C56A C55A H55A 119.8 . . ? C51A C56A C55A 119.7(4) . . ? C51A C56A H56A 120.2 . . ? C55A C56A H56A 120.2 . . ? C66A C61A C62A 122.5(4) . . ? C66A C61A O6A 122.9(4) . . ? C62A C61A O6A 114.4(5) . . ? C61A C62A N7A 118.2(4) . . ? C61A C62A C63A 118.5(5) . . ? N7A C62A C63A 123.3(4) . . ? C64A C63A C62A 118.6(4) . . ? C64A C63A H63A 120.7 . . ? C62A C63A H63A 120.7 . . ? C63A C64A C65A 121.8(4) . . ? C63A C64A H64A 119.1 . . ? C65A C64A H64A 119.1 . . ? C66A C65A C64A 118.7(5) . . ? C66A C65A H65A 120.7 . . ? C64A C65A H65A 120.7 . . ? C61A C66A C65A 119.9(5) . . ? C61A C66A H66A 120.1 . . ? C65A C66A H66A 120.1 . . ? C76A C71A N8A 126.9(4) . . ? C76A C71A C72A 117.5(5) . . ? N8A C71A C72A 115.7(4) . . ? C73A C72A O8A 124.8(4) . . ? C73A C72A C71A 122.8(4) . . ? O8A C72A C71A 112.4(4) . . ? C72A C73A C74A 119.0(5) . . ? C72A C73A H73A 120.5 . . ? C74A C73A H73A 120.5 . . ? C75A C74A C73A 120.4(5) . . ? C75A C74A H74A 119.8 . . ? C73A C74A H74A 119.8 . . ? C74A C75A C76A 120.5(4) . . ? C74A C75A H75A 119.7 . . ? C76A C75A H75A 119.7 . . ? C71A C76A C75A 119.6(4) . . ? C71A C76A H76A 120.2 . . ? C75A C76A H76A 120.2 . . ? C86A C81A C82A 121.4(4) . . ? C86A C81A O8A 122.7(4) . . ? C82A C81A O8A 115.6(4) . . ? C83A C82A C81A 117.9(4) . . ? C83A C82A N1A 124.5(4) . . ? C81A C82A N1A 117.7(3) . . ? C82A C83A C84A 120.6(4) . . ? C82A C83A H83A 119.7 . . ? C84A C83A H83A 119.7 . . ? C85A C84A C83A 120.3(4) . . ? C85A C84A H84A 119.8 . . ? C83A C84A H84A 119.8 . . ? C86A C85A C84A 119.0(4) . . ? C86A C85A H85A 120.5 . . ? C84A C85A H85A 120.5 . . ? C85A C86A C81A 120.7(4) . . ? C85A C86A H86A 119.6 . . ? C81A C86A H86A 119.6 . . ? C105 O101 C102 108.2(3) . . ? O101 C102 C103 106.9(3) . . ? O101 C102 H10A 110.3 . . ? C103 C102 H10A 110.3 . . ? O101 C102 H10B 110.3 . . ? C103 C102 H10B 110.3 . . ? H10A C102 H10B 108.6 . . ? C104 C103 C102 103.5(4) . . ? C104 C103 H10C 111.1 . . ? C102 C103 H10C 111.1 . . ? C104 C103 H10D 111.1 . . ? C102 C103 H10D 111.1 . . ? H10C C103 H10D 109.0 . . ? C105 C104 C103 102.2(4) . . ? C105 C104 H10E 111.3 . . ? C103 C104 H10E 111.3 . . ? C105 C104 H10F 111.3 . . ? C103 C104 H10F 111.3 . . ? H10E C104 H10F 109.2 . . ? O101 C105 C104 106.2(4) . . ? O101 C105 H10G 110.5 . . ? C104 C105 H10G 110.5 . . ? O101 C105 H10H 110.5 . . ? C104 C105 H10H 110.5 . . ? H10G C105 H10H 108.7 . . ? C115 O111 C112 109.5(3) . . ? O111 C112 C113 106.9(5) . . ? O111 C112 H11A 110.3 . . ? C113 C112 H11A 110.3 . . ? O111 C112 H11B 110.3 . . ? C113 C112 H11B 110.3 . . ? H11A C112 H11B 108.6 . . ? C114 C113 C112 108.0(5) . . ? C114 C113 H11C 110.1 . . ? C112 C113 H11C 110.1 . . ? C114 C113 H11D 110.1 . . ? C112 C113 H11D 110.1 . . ? H11C C113 H11D 108.4 . . ? C113 C114 C115 106.7(5) . . ? C113 C114 H11E 110.4 . . ? C115 C114 H11E 110.4 . . ? C113 C114 H11F 110.4 . . ? C115 C114 H11F 110.4 . . ? H11E C114 H11F 108.6 . . ? O111 C115 C114 106.9(5) . . ? O111 C115 H11G 110.3 . . ? C114 C115 H11G 110.3 . . ? O111 C115 H11H 110.3 . . ? C114 C115 H11H 110.3 . . ? H11G C115 H11H 108.6 . . ? C125 O121 C122 109.5(3) . . ? O121 C122 C123 105.4(4) . . ? O121 C122 H12A 110.7 . . ? C123 C122 H12A 110.7 . . ? O121 C122 H12B 110.7 . . ? C123 C122 H12B 110.7 . . ? H12A C122 H12B 108.8 . . ? C122 C123 C124 103.3(4) . . ? C122 C123 H12C 111.1 . . ? C124 C123 H12C 111.1 . . ? C122 C123 H12D 111.1 . . ? C124 C123 H12D 111.1 . . ? H12C C123 H12D 109.1 . . ? C123 C124 C125 102.1(4) . . ? C123 C124 H12E 111.3 . . ? C125 C124 H12E 111.3 . . ? C123 C124 H12F 111.3 . . ? C125 C124 H12F 111.3 . . ? H12E C124 H12F 109.2 . . ? O121 C125 C124 106.7(3) . . ? O121 C125 H12G 110.4 . . ? C124 C125 H12G 110.4 . . ? O121 C125 H12H 110.4 . . ? C124 C125 H12H 110.4 . . ? H12G C125 H12H 108.6 . . ? C132 O131 C135 111.8(4) . . ? O131 C132 C133 104.6(6) . . ? O131 C132 H13B 110.8 . . ? C133 C132 H13B 110.8 . . ? O131 C132 H13C 110.8 . . ? C133 C132 H13C 110.8 . . ? H13B C132 H13C 108.9 . . ? C134 C133 C132 104.6(5) . . ? C134 C133 H13D 110.8 . . ? C132 C133 H13D 110.8 . . ? C134 C133 H13E 110.8 . . ? C132 C133 H13E 110.8 . . ? H13D C133 H13E 108.9 . . ? C133 C134 C135 110.4(7) . . ? C133 C134 H13F 109.6 . . ? C135 C134 H13F 109.6 . . ? C133 C134 H13G 109.6 . . ? C135 C134 H13G 109.6 . . ? H13F C134 H13G 108.1 . . ? O131 C135 C134 103.2(7) . . ? O131 C135 H13H 111.1 . . ? C134 C135 H13H 111.1 . . ? O131 C135 H13I 111.1 . . ? C134 C135 H13I 111.1 . . ? H13H C135 H13I 109.1 . . ? C142 O141 C145 108.9(3) . . ? O141 C142 C143 106.9(3) . . ? O141 C142 H14B 110.3 . . ? C143 C142 H14B 110.3 . . ? O141 C142 H14C 110.3 . . ? C143 C142 H14C 110.3 . . ? H14B C142 H14C 108.6 . . ? C142 C143 C144 101.8(3) . . ? C142 C143 H14D 111.4 . . ? C144 C143 H14D 111.4 . . ? C142 C143 H14E 111.4 . . ? C144 C143 H14E 111.4 . . ? H14D C143 H14E 109.3 . . ? C145 C144 C143 104.9(4) . . ? C145 C144 H14F 110.8 . . ? C143 C144 H14F 110.8 . . ? C145 C144 H14G 110.8 . . ? C143 C144 H14G 110.8 . . ? H14F C144 H14G 108.8 . . ? O141 C145 C144 105.5(3) . . ? O141 C145 H14H 110.6 . . ? C144 C145 H14H 110.6 . . ? O141 C145 H14I 110.6 . . ? C144 C145 H14I 110.6 . . ? H14H C145 H14I 108.8 . . ? C152 O151 C155 110.4(3) . . ? O151 C152 C153 106.2(4) . . ? O151 C152 H15B 110.5 . . ? C153 C152 H15B 110.5 . . ? O151 C152 H15C 110.5 . . ? C153 C152 H15C 110.5 . . ? H15B C152 H15C 108.7 . . ? C154 C153 C152 102.8(4) . . ? C154 C153 H15D 111.2 . . ? C152 C153 H15D 111.2 . . ? C154 C153 H15E 111.2 . . ? C152 C153 H15E 111.2 . . ? H15D C153 H15E 109.1 . . ? C153 C154 C155 103.2(4) . . ? C153 C154 H15F 111.1 . . ? C155 C154 H15F 111.1 . . ? C153 C154 H15G 111.1 . . ? C155 C154 H15G 111.1 . . ? H15F C154 H15G 109.1 . . ? O151 C155 C154 104.9(4) . . ? O151 C155 H15H 110.8 . . ? C154 C155 H15H 110.8 . . ? O151 C155 H15I 110.8 . . ? C154 C155 H15I 110.8 . . ? H15H C155 H15I 108.8 . . ? C162 O161 C165 107.1(3) . . ? O161 C162 C163 107.5(4) . . ? O161 C162 H16B 110.2 . . ? C163 C162 H16B 110.2 . . ? O161 C162 H16C 110.2 . . ? C163 C162 H16C 110.2 . . ? H16B C162 H16C 108.5 . . ? C164 C163 C162 105.0(5) . . ? C164 C163 H16D 110.8 . . ? C162 C163 H16D 110.8 . . ? C164 C163 H16E 110.8 . . ? C162 C163 H16E 110.8 . . ? H16D C163 H16E 108.8 . . ? C163 C164 C165 104.5(5) . . ? C163 C164 H16F 110.9 . . ? C165 C164 H16F 110.9 . . ? C163 C164 H16G 110.9 . . ? C165 C164 H16G 110.9 . . ? H16F C164 H16G 108.9 . . ? O161 C165 C164 105.6(4) . . ? O161 C165 H16H 110.6 . . ? C164 C165 H16H 110.6 . . ? O161 C165 H16I 110.6 . . ? C164 C165 H16I 110.6 . . ? H16H C165 H16I 108.7 . . ? C172 O171 C175 109.5(3) . . ? O171 C172 C173 105.6(4) . . ? O171 C172 H17A 110.6 . . ? C173 C172 H17A 110.6 . . ? O171 C172 H17B 110.6 . . ? C173 C172 H17B 110.6 . . ? H17A C172 H17B 108.8 . . ? C172 C173 C174 102.7(4) . . ? C172 C173 H17C 111.2 . . ? C174 C173 H17C 111.2 . . ? C172 C173 H17D 111.2 . . ? C174 C173 H17D 111.2 . . ? H17C C173 H17D 109.1 . . ? C175 C174 C173 101.8(4) . . ? C175 C174 H17E 111.4 . . ? C173 C174 H17E 111.4 . . ? C175 C174 H17F 111.4 . . ? C173 C174 H17F 111.4 . . ? H17E C174 H17F 109.3 . . ? O171 C175 C174 106.4(5) . . ? O171 C175 H17G 110.4 . . ? C174 C175 H17G 110.4 . . ? O171 C175 H17H 110.4 . . ? C174 C175 H17H 110.4 . . ? H17G C175 H17H 108.6 . . ? C185 O181 C182 109.0(3) . . ? C183 C182 O181 105.9(4) . . ? C183 C182 H18A 110.6 . . ? O181 C182 H18A 110.6 . . ? C183 C182 H18B 110.6 . . ? O181 C182 H18B 110.6 . . ? H18A C182 H18B 108.7 . . ? C184 C183 C182 110.6(5) . . ? C184 C183 H18C 109.5 . . ? C182 C183 H18C 109.5 . . ? C184 C183 H18D 109.5 . . ? C182 C183 H18D 109.5 . . ? H18C C183 H18D 108.1 . . ? C183 C184 C185 105.8(4) . . ? C183 C184 H18E 110.6 . . ? C185 C184 H18E 110.6 . . ? C183 C184 H18F 110.6 . . ? C185 C184 H18F 110.6 . . ? H18E C184 H18F 108.7 . . ? O181 C185 C184 106.8(4) . . ? O181 C185 H18G 110.4 . . ? C184 C185 H18G 110.4 . . ? O181 C185 H18H 110.4 . . ? C184 C185 H18H 110.4 . . ? H18G C185 H18H 108.6 . . ? C192 O191 C195 107.9(3) . . ? O191 C192 C193 110.4(4) . . ? O191 C192 H19A 109.6 . . ? C193 C192 H19A 109.6 . . ? O191 C192 H19B 109.6 . . ? C193 C192 H19B 109.6 . . ? H19A C192 H19B 108.1 . . ? C192 C193 C194 103.1(4) . . ? C192 C193 H19C 111.1 . . ? C194 C193 H19C 111.1 . . ? C192 C193 H19D 111.1 . . ? C194 C193 H19D 111.1 . . ? H19C C193 H19D 109.1 . . ? C195 C194 C193 103.1(4) . . ? C195 C194 H19E 111.2 . . ? C193 C194 H19E 111.2 . . ? C195 C194 H19F 111.2 . . ? C193 C194 H19F 111.2 . . ? H19E C194 H19F 109.1 . . ? O191 C195 C194 107.4(4) . . ? O191 C195 H19G 110.2 . . ? C194 C195 H19G 110.2 . . ? O191 C195 H19H 110.2 . . ? C194 C195 H19H 110.2 . . ? H19G C195 H19H 108.5 . . ? 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 C82 N1 C1 O1 -9.7(7) . . . . ? C82 N1 C1 N2 171.6(4) . . . . ? O1 C1 N2 C11 6.9(8) . . . . ? N1 C1 N2 C11 -174.4(4) . . . . ? O3 C2 N3 C22 3.0(7) . . . . ? N4 C2 N3 C22 -178.6(4) . . . . ? O3 C2 N4 C31 -4.4(6) . . . . ? N3 C2 N4 C31 177.2(3) . . . . ? O5 C4 N5 C42 -11.8(8) . . . . ? N6 C4 N5 C42 168.0(4) . . . . ? O5 C4 N6 C51 4.8(8) . . . . ? N5 C4 N6 C51 -175.0(4) . . . . ? O7 C3 N7 C62 -0.5(7) . . . . ? N8 C3 N7 C62 179.9(3) . . . . ? O7 C3 N8 C71 -5.4(7) . . . . ? N7 C3 N8 C71 174.2(3) . . . . ? C1 N2 C11 C16 17.3(8) . . . . ? C1 N2 C11 C12 -164.2(4) . . . . ? C16 C11 C12 C13 1.1(7) . . . . ? N2 C11 C12 C13 -177.5(4) . . . . ? C16 C11 C12 O2 -173.4(4) . . . . ? N2 C11 C12 O2 7.9(6) . . . . ? C21 O2 C12 C13 64.7(5) . . . . ? C21 O2 C12 C11 -120.7(4) . . . . ? C11 C12 C13 C14 0.9(7) . . . . ? O2 C12 C13 C14 175.2(4) . . . . ? C12 C13 C14 C15 -2.3(7) . . . . ? C13 C14 C15 C16 1.7(7) . . . . ? C12 C11 C16 C15 -1.7(7) . . . . ? N2 C11 C16 C15 176.8(4) . . . . ? C14 C15 C16 C11 0.3(7) . . . . ? C12 O2 C21 C26 33.2(5) . . . . ? C12 O2 C21 C22 -151.6(4) . . . . ? C26 C21 C22 C23 -0.9(6) . . . . ? O2 C21 C22 C23 -176.2(3) . . . . ? C26 C21 C22 N3 -179.2(4) . . . . ? O2 C21 C22 N3 5.5(5) . . . . ? C2 N3 C22 C23 1.0(6) . . . . ? C2 N3 C22 C21 179.2(4) . . . . ? C21 C22 C23 C24 1.3(6) . . . . ? N3 C22 C23 C24 179.5(4) . . . . ? C22 C23 C24 C25 -2.1(6) . . . . ? C23 C24 C25 C26 2.5(6) . . . . ? C22 C21 C26 C25 1.3(6) . . . . ? O2 C21 C26 C25 176.1(3) . . . . ? C24 C25 C26 C21 -2.0(6) . . . . ? C2 N4 C31 C36 -21.7(6) . . . . ? C2 N4 C31 C32 159.6(4) . . . . ? C36 C31 C32 C33 -1.2(6) . . . . ? N4 C31 C32 C33 177.6(4) . . . . ? C36 C31 C32 O4 175.1(3) . . . . ? N4 C31 C32 O4 -6.1(5) . . . . ? C41 O4 C32 C33 -72.6(5) . . . . ? C41 O4 C32 C31 111.1(4) . . . . ? C31 C32 C33 C34 1.1(6) . . . . ? O4 C32 C33 C34 -175.1(3) . . . . ? C32 C33 C34 C35 -1.0(6) . . . . ? C33 C34 C35 C36 1.0(6) . . . . ? C34 C35 C36 C31 -1.2(6) . . . . ? C32 C31 C36 C35 1.3(6) . . . . ? N4 C31 C36 C35 -177.5(4) . . . . ? C32 O4 C41 C46 -18.0(7) . . . . ? C32 O4 C41 C42 163.8(4) . . . . ? C4 N5 C42 C43 15.3(7) . . . . ? C4 N5 C42 C41 -165.7(5) . . . . ? C46 C41 C42 C43 -2.3(7) . . . . ? O4 C41 C42 C43 175.9(4) . . . . ? C46 C41 C42 N5 178.7(5) . . . . ? O4 C41 C42 N5 -3.2(6) . . . . ? N5 C42 C43 C44 -176.1(5) . . . . ? C41 C42 C43 C44 5.0(7) . . . . ? C42 C43 C44 C45 -4.6(7) . . . . ? C43 C44 C45 C46 1.3(7) . . . . ? C42 C41 C46 C45 -0.9(7) . . . . ? O4 C41 C46 C45 -178.9(4) . . . . ? C44 C45 C46 C41 1.5(7) . . . . ? C4 N6 C51 C56 17.9(7) . . . . ? C4 N6 C51 C52 -163.0(5) . . . . ? C56 C51 C52 C53 0.7(7) . . . . ? N6 C51 C52 C53 -178.5(4) . . . . ? C56 C51 C52 O6 -173.7(4) . . . . ? N6 C51 C52 O6 7.1(6) . . . . ? C61 O6 C52 C53 69.3(6) . . . . ? C61 O6 C52 C51 -116.2(4) . . . . ? C51 C52 C53 C54 0.2(8) . . . . ? O6 C52 C53 C54 174.5(4) . . . . ? C52 C53 C54 C55 -0.7(8) . . . . ? C53 C54 C55 C56 0.2(7) . . . . ? C52 C51 C56 C55 -1.2(7) . . . . ? N6 C51 C56 C55 177.9(4) . . . . ? C54 C55 C56 C51 0.8(7) . . . . ? C52 O6 C61 C66 26.8(6) . . . . ? C52 O6 C61 C62 -155.6(4) . . . . ? C66 C61 C62 C63 1.1(6) . . . . ? O6 C61 C62 C63 -176.6(3) . . . . ? C66 C61 C62 N7 -178.9(4) . . . . ? O6 C61 C62 N7 3.5(5) . . . . ? C3 N7 C62 C63 1.7(6) . . . . ? C3 N7 C62 C61 -178.3(4) . . . . ? C61 C62 C63 C64 0.6(6) . . . . ? N7 C62 C63 C64 -179.4(4) . . . . ? C62 C63 C64 C65 -1.5(6) . . . . ? C63 C64 C65 C66 0.8(6) . . . . ? O6 C61 C66 C65 175.6(3) . . . . ? C62 C61 C66 C65 -1.9(7) . . . . ? C64 C65 C66 C61 0.9(6) . . . . ? C3 N8 C71 C76 -14.3(6) . . . . ? C3 N8 C71 C72 166.9(4) . . . . ? C76 C71 C72 C73 -1.2(6) . . . . ? N8 C71 C72 C73 177.7(4) . . . . ? C76 C71 C72 O8 172.8(3) . . . . ? N8 C71 C72 O8 -8.3(5) . . . . ? C81 O8 C72 C73 -64.2(5) . . . . ? C81 O8 C72 C71 121.6(4) . . . . ? C71 C72 C73 C74 0.6(6) . . . . ? O8 C72 C73 C74 -173.1(3) . . . . ? C72 C73 C74 C75 0.0(6) . . . . ? C73 C74 C75 C76 0.1(6) . . . . ? C74 C75 C76 C71 -0.8(6) . . . . ? C72 C71 C76 C75 1.3(6) . . . . ? N8 C71 C76 C75 -177.5(4) . . . . ? C72 O8 C81 C86 -27.1(7) . . . . ? C72 O8 C81 C82 154.7(4) . . . . ? C86 C81 C82 C83 -2.7(7) . . . . ? O8 C81 C82 C83 175.6(4) . . . . ? C86 C81 C82 N1 177.5(4) . . . . ? O8 C81 C82 N1 -4.2(6) . . . . ? C1 N1 C82 C83 7.9(7) . . . . ? C1 N1 C82 C81 -172.3(4) . . . . ? C81 C82 C83 C84 2.9(7) . . . . ? N1 C82 C83 C84 -177.4(5) . . . . ? C82 C83 C84 C85 -2.7(7) . . . . ? C83 C84 C85 C86 2.1(7) . . . . ? O8 C81 C86 C85 -175.8(5) . . . . ? C82 C81 C86 C85 2.2(7) . . . . ? C84 C85 C86 C81 -1.9(7) . . . . ? C82A N1A C1A O1A -6.6(7) . . . . ? C82A N1A C1A N2A 173.0(4) . . . . ? O1A C1A N2A C11A 4.2(7) . . . . ? N1A C1A N2A C11A -175.4(4) . . . . ? C22A N3A C3A O3A 6.7(7) . . . . ? C22A N3A C3A N4A -173.4(4) . . . . ? O3A C3A N4A C31A -7.9(7) . . . . ? N3A C3A N4A C31A 172.2(4) . . . . ? C42A N5A C5A O5A -12.9(8) . . . . ? C42A N5A C5A N6A 167.1(4) . . . . ? O5A C5A N6A C51A 2.6(8) . . . . ? N5A C5A N6A C51A -177.5(4) . . . . ? C62A N7A C7A O7A 2.5(7) . . . . ? C62A N7A C7A N8A -178.0(4) . . . . ? O7A C7A N8A C71A -10.3(7) . . . . ? N7A C7A N8A C71A 170.2(4) . . . . ? C1A N2A C11A C16A 16.9(7) . . . . ? C1A N2A C11A C12A -165.4(4) . . . . ? C16A C11A C12A C13A 2.1(7) . . . . ? N2A C11A C12A C13A -175.9(4) . . . . ? C16A C11A C12A O2A -175.6(4) . . . . ? N2A C11A C12A O2A 6.4(6) . . . . ? C21A O2A C12A C13A 52.8(6) . . . . ? C21A O2A C12A C11A -129.5(4) . . . . ? C11A C12A C13A C14A -1.6(7) . . . . ? O2A C12A C13A C14A 175.9(4) . . . . ? C12A C13A C14A C15A 0.4(7) . . . . ? C13A C14A C15A C16A 0.4(8) . . . . ? C14A C15A C16A C11A 0.1(8) . . . . ? C12A C11A C16A C15A -1.3(7) . . . . ? N2A C11A C16A C15A 176.5(5) . . . . ? C12A O2A C21A C26A 43.4(5) . . . . ? C12A O2A C21A C22A -139.7(4) . . . . ? C26A C21A C22A C23A 0.3(6) . . . . ? O2A C21A C22A C23A -176.5(3) . . . . ? C26A C21A C22A N3A -177.5(4) . . . . ? O2A C21A C22A N3A 5.7(5) . . . . ? C3A N3A C22A C21A -174.4(4) . . . . ? C3A N3A C22A C23A 8.0(6) . . . . ? C21A C22A C23A C24A -0.6(6) . . . . ? N3A C22A C23A C24A 177.1(4) . . . . ? C22A C23A C24A C25A -0.2(6) . . . . ? C23A C24A C25A C26A 1.2(6) . . . . ? C22A C21A C26A C25A 0.7(6) . . . . ? O2A C21A C26A C25A 177.3(3) . . . . ? C24A C25A C26A C21A -1.5(6) . . . . ? C3A N4A C31A C32A 162.4(4) . . . . ? C3A N4A C31A C36A -16.0(6) . . . . ? C36A C31A C32A C33A -5.4(6) . . . . ? N4A C31A C32A C33A 176.1(4) . . . . ? C36A C31A C32A O4A 172.0(3) . . . . ? N4A C31A C32A O4A -6.5(5) . . . . ? C41A O4A C32A C33A -66.0(6) . . . . ? C41A O4A C32A C31A 116.5(4) . . . . ? C31A C32A C33A C34A 4.2(7) . . . . ? O4A C32A C33A C34A -173.1(3) . . . . ? C32A C33A C34A C35A -0.7(6) . . . . ? C33A C34A C35A C36A -1.3(7) . . . . ? C34A C35A C36A C31A 0.0(6) . . . . ? C32A C31A C36A C35A 3.2(6) . . . . ? N4A C31A C36A C35A -178.4(4) . . . . ? C32A O4A C41A C46A -13.2(7) . . . . ? C32A O4A C41A C42A 166.9(4) . . . . ? C46A C41A C42A C43A -4.9(7) . . . . ? O4A C41A C42A C43A 175.0(4) . . . . ? C46A C41A C42A N5A 175.6(4) . . . . ? O4A C41A C42A N5A -4.5(6) . . . . ? C5A N5A C42A C43A 19.4(7) . . . . ? C5A N5A C42A C41A -161.1(5) . . . . ? C41A C42A C43A C44A 3.9(6) . . . . ? N5A C42A C43A C44A -176.6(4) . . . . ? C42A C43A C44A C45A -2.4(7) . . . . ? C43A C44A C45A C46A 1.5(7) . . . . ? O4A C41A C46A C45A -175.8(4) . . . . ? C42A C41A C46A C45A 4.1(7) . . . . ? C44A C45A C46A C41A -2.3(7) . . . . ? C5A N6A C51A C56A 12.6(7) . . . . ? C5A N6A C51A C52A -166.4(4) . . . . ? C56A C51A C52A C53A 3.0(7) . . . . ? N6A C51A C52A C53A -178.0(4) . . . . ? C56A C51A C52A O6A -174.0(4) . . . . ? N6A C51A C52A O6A 5.0(6) . . . . ? C61A O6A C52A C53A 49.7(6) . . . . ? C61A O6A C52A C51A -133.4(4) . . . . ? C51A C52A C53A C54A -1.5(7) . . . . ? O6A C52A C53A C54A 175.3(5) . . . . ? C52A C53A C54A C55A -0.4(7) . . . . ? C53A C54A C55A C56A 0.8(7) . . . . ? C52A C51A C56A C55A -2.6(7) . . . . ? N6A C51A C56A C55A 178.5(4) . . . . ? C54A C55A C56A C51A 0.7(7) . . . . ? C52A O6A C61A C66A 44.8(6) . . . . ? C52A O6A C61A C62A -140.2(4) . . . . ? C66A C61A C62A N7A -179.5(4) . . . . ? O6A C61A C62A N7A 5.4(5) . . . . ? C66A C61A C62A C63A -2.5(6) . . . . ? O6A C61A C62A C63A -177.5(3) . . . . ? C7A N7A C62A C61A -172.0(4) . . . . ? C7A N7A C62A C63A 11.1(6) . . . . ? C61A C62A C63A C64A 3.1(6) . . . . ? N7A C62A C63A C64A 180.0(4) . . . . ? C62A C63A C64A C65A -2.3(6) . . . . ? C63A C64A C65A C66A 0.7(6) . . . . ? C62A C61A C66A C65A 1.0(7) . . . . ? O6A C61A C66A C65A 175.6(3) . . . . ? C64A C65A C66A C61A 0.0(6) . . . . ? C7A N8A C71A C76A 6.9(7) . . . . ? C7A N8A C71A C72A -173.6(4) . . . . ? C81A O8A C72A C73A -20.1(6) . . . . ? C81A O8A C72A C71A 161.3(4) . . . . ? C76A C71A C72A C73A -4.9(6) . . . . ? N8A C71A C72A C73A 175.6(4) . . . . ? C76A C71A C72A O8A 173.6(3) . . . . ? N8A C71A C72A O8A -5.8(5) . . . . ? O8A C72A C73A C74A -175.2(4) . . . . ? C71A C72A C73A C74A 3.2(7) . . . . ? C72A C73A C74A C75A -1.3(7) . . . . ? C73A C74A C75A C76A 1.2(7) . . . . ? N8A C71A C76A C75A -175.9(4) . . . . ? C72A C71A C76A C75A 4.6(6) . . . . ? C74A C75A C76A C71A -2.9(6) . . . . ? C72A O8A C81A C86A -65.2(6) . . . . ? C72A O8A C81A C82A 121.0(5) . . . . ? C86A C81A C82A C83A -1.6(7) . . . . ? O8A C81A C82A C83A 172.4(4) . . . . ? C86A C81A C82A N1A 177.5(4) . . . . ? O8A C81A C82A N1A -8.6(7) . . . . ? C1A N1A C82A C83A -5.9(7) . . . . ? C1A N1A C82A C81A 175.2(5) . . . . ? C81A C82A C83A C84A 2.3(7) . . . . ? N1A C82A C83A C84A -176.7(4) . . . . ? C82A C83A C84A C85A -1.8(7) . . . . ? C83A C84A C85A C86A 0.6(8) . . . . ? C84A C85A C86A C81A 0.1(8) . . . . ? C82A C81A C86A C85A 0.4(8) . . . . ? O8A C81A C86A C85A -173.1(5) . . . . ? C105 O101 C102 C103 3.0(5) . . . . ? O101 C102 C103 C104 19.2(6) . . . . ? C102 C103 C104 C105 -32.8(6) . . . . ? C102 O101 C105 C104 -24.5(6) . . . . ? C103 C104 C105 O101 35.8(6) . . . . ? C115 O111 C112 C113 -1.8(5) . . . . ? O111 C112 C113 C114 10.3(7) . . . . ? C112 C113 C114 C115 -14.5(7) . . . . ? C112 O111 C115 C114 -7.1(5) . . . . ? C113 C114 C115 O111 13.3(6) . . . . ? C125 O121 C122 C123 15.1(5) . . . . ? O121 C122 C123 C124 -31.7(5) . . . . ? C122 C123 C124 C125 35.4(5) . . . . ? C122 O121 C125 C124 7.7(5) . . . . ? C123 C124 C125 O121 -27.0(5) . . . . ? C135 O131 C132 C133 5.2(5) . . . . ? O131 C132 C133 C134 -17.7(8) . . . . ? C132 C133 C134 C135 24.0(9) . . . . ? C132 O131 C135 C134 8.5(6) . . . . ? C133 C134 C135 O131 -20.8(8) . . . . ? C145 O141 C142 C143 11.6(5) . . . . ? O141 C142 C143 C144 -28.3(5) . . . . ? C142 C143 C144 C145 34.5(5) . . . . ? C142 O141 C145 C144 10.6(5) . . . . ? C143 C144 C145 O141 -28.4(5) . . . . ? C155 O151 C152 C153 9.8(4) . . . . ? O151 C152 C153 C154 -28.2(4) . . . . ? C152 C153 C154 C155 35.0(4) . . . . ? C152 O151 C155 C154 12.5(4) . . . . ? C153 C154 C155 O151 -29.8(4) . . . . ? C165 O161 C162 C163 1.9(6) . . . . ? O161 C162 C163 C164 -21.1(7) . . . . ? C162 C163 C164 C165 31.3(7) . . . . ? C162 O161 C165 C164 17.4(6) . . . . ? C163 C164 C165 O161 -30.6(7) . . . . ? C175 O171 C172 C173 7.0(5) . . . . ? O171 C172 C173 C174 -27.2(5) . . . . ? C172 C173 C174 C175 36.5(5) . . . . ? C172 O171 C175 C174 16.9(5) . . . . ? C173 C174 C175 O171 -33.2(5) . . . . ? C185 O181 C182 C183 -4.9(6) . . . . ? O181 C182 C183 C184 12.5(8) . . . . ? C182 C183 C184 C185 -14.7(9) . . . . ? C182 O181 C185 C184 -3.7(5) . . . . ? C183 C184 C185 O181 11.2(7) . . . . ? C195 O191 C192 C193 -3.4(6) . . . . ? O191 C192 C193 C194 19.9(6) . . . . ? C192 C193 C194 C195 -27.3(6) . . . . ? C192 O191 C195 C194 -14.9(6) . . . . ? C193 C194 C195 O191 26.6(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O111 0.88 2.15 2.971(4) 155.1 . N2 H2 O111 0.88 2.08 2.920(4) 158.6 . N3 H3 O121 0.88 2.13 2.962(4) 158.3 . N4 H4 O121 0.88 2.12 2.952(4) 157.1 . N5 H5 O131 0.88 2.13 2.939(4) 152.6 . N6 H6 O131 0.88 2.07 2.906(4) 158.3 . N7 H7 O141 0.88 2.14 2.969(4) 156.7 . N8 H8 O141 0.88 2.14 2.975(4) 158.6 . N1A H1A O151 0.88 2.20 3.021(4) 155.2 . N2A H2A O151 0.88 2.11 2.948(4) 158.9 . N3A H3A O161 0.88 2.09 2.923(4) 158.1 . N4A H4A O161 0.88 2.14 2.966(4) 155.1 . N5A H5A O171 0.88 2.12 2.927(4) 151.4 . N6A H6A O171 0.88 2.05 2.890(4) 159.2 . N7A H7A O181 0.88 2.10 2.949(4) 160.7 . N8A H8A O181 0.88 2.16 2.982(4) 156.1 . _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.199 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.035 data_boeh32 _database_code_depnum_ccdc_archive 'CCDC 687874' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H106 N10 O8' _chemical_formula_weight 1443.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9282(13) _cell_length_b 18.9297(17) _cell_length_c 19.2836(16) _cell_angle_alpha 61.351(6) _cell_angle_beta 86.758(7) _cell_angle_gamma 71.553(7) _cell_volume 4506.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37291 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 25.8 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9672 _exptl_absorpt_correction_T_max 0.9757 _exptl_absorpt_process_details . _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47861 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.82 _reflns_number_total 16476 _reflns_number_gt 9541 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.1720P)^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_number_reflns 16476 _refine_ls_number_parameters 1022 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1361 _refine_ls_R_factor_gt 0.0992 _refine_ls_wR_factor_ref 0.3104 _refine_ls_wR_factor_gt 0.2860 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.189 _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 0.5736(3) 0.4919(2) 0.0962(2) 0.0367(8) Uani 1 1 d . . . O1 O 0.65840(17) 0.47886(17) 0.10918(16) 0.0406(6) Uani 1 1 d . . . N11 N 0.5130(2) 0.5679(2) 0.0397(2) 0.0399(8) Uani 1 1 d . . . H11 H 0.4573 0.5698 0.0250 0.048 Uiso 1 1 calc R . . N12 N 0.5311(2) 0.4315(2) 0.1380(2) 0.0420(8) Uani 1 1 d . . . H12 H 0.4691 0.4498 0.1379 0.050 Uiso 1 1 calc R . . C2 C 0.2846(3) 0.5045(3) 0.3200(3) 0.0485(10) Uani 1 1 d . . . O2 O 0.2060(2) 0.5034(2) 0.3391(2) 0.0678(10) Uani 1 1 d . . . N21 N 0.3558(3) 0.4357(2) 0.3248(3) 0.0580(10) Uani 1 1 d . . . H21 H 0.4067 0.4459 0.3026 0.070 Uiso 1 1 calc R . . N22 N 0.3127(3) 0.5751(2) 0.2893(3) 0.0552(10) Uani 1 1 d . . . H22 H 0.3737 0.5661 0.2843 0.066 Uiso 1 1 calc R . . C3 C 0.5731(3) 0.5359(2) 0.2721(2) 0.0395(9) Uani 1 1 d . . . O3 O 0.5157(2) 0.54036(18) 0.31841(18) 0.0493(7) Uani 1 1 d . . . N31 N 0.5822(2) 0.6066(2) 0.2067(2) 0.0441(8) Uani 1 1 d . . . H31 H 0.6157 0.5983 0.1706 0.053 Uiso 1 1 calc R . . N32 N 0.6331(2) 0.4603(2) 0.2785(2) 0.0425(8) Uani 1 1 d . . . H32 H 0.6576 0.4625 0.2352 0.051 Uiso 1 1 calc R . . C4 C 0.8810(3) 0.4171(3) 0.0690(2) 0.0427(9) Uani 1 1 d . . . O4 O 0.9523(2) 0.3854(2) 0.04645(19) 0.0585(9) Uani 1 1 d . . . N41 N 0.8596(2) 0.3832(2) 0.1457(2) 0.0450(8) Uani 1 1 d . . . H41 H 0.8078 0.4143 0.1551 0.054 Uiso 1 1 calc R . . N42 N 0.8124(2) 0.4931(2) 0.0195(2) 0.0469(8) Uani 1 1 d . . . H42 H 0.7636 0.5117 0.0412 0.056 Uiso 1 1 calc R . . C11 C 0.5782(3) 0.3421(2) 0.1813(2) 0.0392(9) Uani 1 1 d . . . C12 C 0.6514(3) 0.3003(3) 0.1533(2) 0.0417(9) Uani 1 1 d . . . H12A H 0.6770 0.3326 0.1070 0.050 Uiso 1 1 calc R . . C13 C 0.6884(3) 0.2110(3) 0.1923(3) 0.0435(9) Uani 1 1 d . . . C14 C 0.6460(3) 0.1662(3) 0.2579(3) 0.0459(10) Uani 1 1 d . . . H14 H 0.6687 0.1057 0.2834 0.055 Uiso 1 1 calc R . . C15 C 0.5720(3) 0.2059(3) 0.2876(2) 0.0439(10) Uani 1 1 d . . . C16 C 0.5422(3) 0.2948(2) 0.2503(2) 0.0410(9) Uani 1 1 d . . . O16 O 0.47404(19) 0.34131(17) 0.27731(17) 0.0448(7) Uani 1 1 d . . . C17 C 0.7680(3) 0.1616(3) 0.1636(3) 0.0485(10) Uani 1 1 d . . . C171 C 0.7319(4) 0.1042(3) 0.1446(3) 0.0627(13) Uani 1 1 d . . . H17A H 0.7831 0.0721 0.1263 0.094 Uiso 1 1 calc R . . H17B H 0.6780 0.1397 0.1028 0.094 Uiso 1 1 calc R . . H17C H 0.7116 0.0644 0.1926 0.094 Uiso 1 1 calc R . . C172 C 0.8030(4) 0.2202(3) 0.0889(4) 0.0712(15) Uani 1 1 d . . . H17D H 0.8541 0.1857 0.0727 0.107 Uiso 1 1 calc R . . H17E H 0.8271 0.2566 0.1001 0.107 Uiso 1 1 calc R . . H17F H 0.7504 0.2558 0.0460 0.107 Uiso 1 1 calc R . . C173 C 0.8529(3) 0.1050(3) 0.2292(3) 0.0599(12) Uani 1 1 d . . . H17G H 0.9040 0.0731 0.2105 0.090 Uiso 1 1 calc R . . H17H H 0.8326 0.0649 0.2770 0.090 Uiso 1 1 calc R . . H17I H 0.8762 0.1410 0.2418 0.090 Uiso 1 1 calc R . . C18 C 0.5239(3) 0.1536(3) 0.3563(3) 0.0483(10) Uani 1 1 d . . . C181 C 0.4870(4) 0.1004(3) 0.3327(3) 0.0624(13) Uani 1 1 d . . . H18A H 0.5401 0.0629 0.3210 0.094 Uiso 1 1 calc R . . H18B H 0.4403 0.1384 0.2853 0.094 Uiso 1 1 calc R . . H18C H 0.4568 0.0658 0.3766 0.094 Uiso 1 1 calc R . . C182 C 0.5965(4) 0.0953(3) 0.4313(3) 0.0703(16) Uani 1 1 d . . . H18D H 0.6500 0.0569 0.4209 0.105 Uiso 1 1 calc R . . H18E H 0.5660 0.0616 0.4755 0.105 Uiso 1 1 calc R . . H18F H 0.6198 0.1303 0.4453 0.105 Uiso 1 1 calc R . . C21 C 0.3583(3) 0.3512(3) 0.3605(3) 0.0476(10) Uani 1 1 d . . . C22 C 0.2992(3) 0.3180(3) 0.4163(3) 0.0531(11) Uani 1 1 d . . . H22A H 0.2519 0.3540 0.4310 0.064 Uiso 1 1 calc R . . C23 C 0.3095(3) 0.2310(3) 0.4510(3) 0.0545(12) Uani 1 1 d . A . C24 C 0.3810(3) 0.1801(3) 0.4305(3) 0.0523(11) Uani 1 1 d . . . H24 H 0.3895 0.1209 0.4552 0.063 Uiso 1 1 calc R . . C25 C 0.4421(3) 0.2120(3) 0.3743(2) 0.0462(10) Uani 1 1 d . . . C26 C 0.4262(3) 0.2983(3) 0.3387(2) 0.0439(10) Uani 1 1 d . . . C27 C 0.2431(4) 0.1955(4) 0.5113(3) 0.0714(15) Uani 1 1 d . . . C271 C 0.2032(9) 0.1411(9) 0.4917(9) 0.080(4) Uani 0.546(18) 1 d P A 1 H27A H 0.2551 0.1014 0.4815 0.119 Uiso 0.546(18) 1 calc PR A 1 H27B H 0.1565 0.1783 0.4443 0.119 Uiso 0.546(18) 1 calc PR A 1 H27C H 0.1724 0.1089 0.5367 0.119 Uiso 0.546(18) 1 calc PR A 1 C272 C 0.168(3) 0.2634(15) 0.524(2) 0.196(19) Uani 0.546(18) 1 d P A 1 H27D H 0.1280 0.2370 0.5631 0.294 Uiso 0.546(18) 1 calc PR A 1 H27E H 0.1293 0.3072 0.4735 0.294 Uiso 0.546(18) 1 calc PR A 1 H27F H 0.2000 0.2896 0.5436 0.294 Uiso 0.546(18) 1 calc PR A 1 C273 C 0.3103(18) 0.1290(18) 0.5952(8) 0.132(9) Uani 0.546(18) 1 d P A 1 H27G H 0.3594 0.0840 0.5894 0.198 Uiso 0.546(18) 1 calc PR A 1 H27H H 0.2715 0.1033 0.6365 0.198 Uiso 0.546(18) 1 calc PR A 1 H27I H 0.3405 0.1594 0.6103 0.198 Uiso 0.546(18) 1 calc PR A 1 C274 C 0.2577(12) 0.1022(9) 0.5396(10) 0.077(5) Uani 0.454(18) 1 d P A 2 H27J H 0.2466 0.0951 0.4941 0.116 Uiso 0.454(18) 1 calc PR A 2 H27K H 0.2130 0.0837 0.5780 0.116 Uiso 0.454(18) 1 calc PR A 2 H27L H 0.3229 0.0676 0.5651 0.116 Uiso 0.454(18) 1 calc PR A 2 C275 C 0.1392(9) 0.2497(12) 0.4715(12) 0.107(9) Uani 0.454(18) 1 d P A 2 H27M H 0.1290 0.2452 0.4242 0.161 Uiso 0.454(18) 1 calc PR A 2 H27N H 0.1282 0.3095 0.4560 0.161 Uiso 0.454(18) 1 calc PR A 2 H27O H 0.0949 0.2286 0.5093 0.161 Uiso 0.454(18) 1 calc PR A 2 C276 C 0.2609(14) 0.2055(19) 0.5811(11) 0.092(7) Uani 0.454(18) 1 d P A 2 H27P H 0.2192 0.1833 0.6212 0.138 Uiso 0.454(18) 1 calc PR A 2 H27Q H 0.2477 0.2660 0.5638 0.138 Uiso 0.454(18) 1 calc PR A 2 H27R H 0.3274 0.1736 0.6041 0.138 Uiso 0.454(18) 1 calc PR A 2 C31 C 0.2571(3) 0.6590(3) 0.2651(3) 0.0491(10) Uani 1 1 d . . . C32 C 0.1696(4) 0.6845(4) 0.2872(4) 0.0721(16) Uani 1 1 d . . . H32A H 0.1406 0.6431 0.3193 0.087 Uiso 1 1 calc R . . C33 C 0.1216(4) 0.7706(4) 0.2635(5) 0.090(2) Uani 1 1 d . . . C34 C 0.1662(3) 0.8292(4) 0.2176(4) 0.0675(15) Uani 1 1 d . . . H34 H 0.1356 0.8875 0.2030 0.081 Uiso 1 1 calc R . . C35 C 0.2538(3) 0.8059(3) 0.1924(3) 0.0461(10) Uani 1 1 d . . . C36 C 0.2971(3) 0.7205(3) 0.2153(3) 0.0424(9) Uani 1 1 d . . . O36 O 0.38361(18) 0.69052(16) 0.19182(17) 0.0412(6) Uani 1 1 d . . . C37 C 0.0230(6) 0.8010(7) 0.2854(9) 0.189(7) Uani 1 1 d D . . C371 C -0.0295(4) 0.7418(5) 0.3059(5) 0.093(2) Uani 1 1 d . . . H37A H -0.0067 0.7077 0.2791 0.140 Uiso 1 1 calc R . . H37B H -0.0973 0.7739 0.2889 0.140 Uiso 1 1 calc R . . H37C H -0.0197 0.7040 0.3636 0.140 Uiso 1 1 calc R . . C372 C 0.0128(5) 0.8553(5) 0.3161(6) 0.108(3) Uani 1 1 d . . . H37D H 0.0585 0.8860 0.2956 0.162 Uiso 1 1 calc R . . H37E H 0.0245 0.8222 0.3742 0.162 Uiso 1 1 calc R . . H37F H -0.0520 0.8963 0.3002 0.162 Uiso 1 1 calc R . . C373 C -0.0521(8) 0.8842(9) 0.1980(9) 0.212(8) Uani 1 1 d D . . H37G H -0.0583 0.8623 0.1623 0.318 Uiso 1 1 calc R . . H37H H -0.0247 0.9301 0.1713 0.318 Uiso 1 1 calc R . . H37I H -0.1149 0.9064 0.2121 0.318 Uiso 1 1 calc R . . C38 C 0.3033(3) 0.8673(3) 0.1372(3) 0.0453(10) Uani 1 1 d . . . C381 C 0.2718(3) 0.9498(3) 0.1430(3) 0.0568(12) Uani 1 1 d . . . H38A H 0.2029 0.9772 0.1290 0.085 Uiso 1 1 calc R . . H38B H 0.3040 0.9887 0.1063 0.085 Uiso 1 1 calc R . . H38C H 0.2886 0.9361 0.1975 0.085 Uiso 1 1 calc R . . C382 C 0.2754(3) 0.8897(3) 0.0508(3) 0.0630(13) Uani 1 1 d . . . H38D H 0.2068 0.9195 0.0366 0.094 Uiso 1 1 calc R . . H38E H 0.2922 0.8371 0.0473 0.094 Uiso 1 1 calc R . . H38F H 0.3096 0.9266 0.0140 0.094 Uiso 1 1 calc R . . C41 C 0.5426(3) 0.6917(3) 0.1921(2) 0.0421(9) Uani 1 1 d . . . C42 C 0.6043(3) 0.7366(3) 0.1809(3) 0.0472(10) Uani 1 1 d . . . H42A H 0.6707 0.7076 0.1880 0.057 Uiso 1 1 calc R . . C43 C 0.5726(3) 0.8229(3) 0.1596(3) 0.0483(10) Uani 1 1 d . . . C44 C 0.4759(3) 0.8635(3) 0.1478(3) 0.0451(9) Uani 1 1 d . . . H44 H 0.4526 0.9225 0.1323 0.054 Uiso 1 1 calc R . . C45 C 0.4107(3) 0.8212(2) 0.1578(2) 0.0404(9) Uani 1 1 d . . . C46 C 0.4458(3) 0.7345(2) 0.1820(2) 0.0391(9) Uani 1 1 d . . . C47 C 0.6439(4) 0.8695(3) 0.1489(3) 0.0606(13) Uani 1 1 d . . . C471 C 0.7032(8) 0.8287(6) 0.2261(6) 0.157(5) Uani 1 1 d . . . H47A H 0.7491 0.8580 0.2202 0.236 Uiso 1 1 calc R . . H47B H 0.7374 0.7686 0.2425 0.236 Uiso 1 1 calc R . . H47C H 0.6623 0.8325 0.2666 0.236 Uiso 1 1 calc R . . C472 C 0.5965(5) 0.9631(4) 0.1230(6) 0.098(2) Uani 1 1 d . . . H47D H 0.5573 0.9913 0.0720 0.148 Uiso 1 1 calc R . . H47E H 0.6453 0.9896 0.1172 0.148 Uiso 1 1 calc R . . H47F H 0.5563 0.9692 0.1632 0.148 Uiso 1 1 calc R . . C473 C 0.7043(5) 0.8655(5) 0.0847(5) 0.102(3) Uani 1 1 d . . . H47G H 0.6636 0.8932 0.0345 0.154 Uiso 1 1 calc R . . H47H H 0.7384 0.8057 0.0997 0.154 Uiso 1 1 calc R . . H47I H 0.7502 0.8949 0.0783 0.154 Uiso 1 1 calc R . . C51 C 0.6591(3) 0.3797(2) 0.3477(2) 0.0397(9) Uani 1 1 d . . . C52 C 0.6085(3) 0.3618(3) 0.4132(2) 0.0436(9) Uani 1 1 d . . . H52 H 0.5511 0.4036 0.4108 0.052 Uiso 1 1 calc R . . C53 C 0.6410(3) 0.2827(3) 0.4831(2) 0.0461(10) Uani 1 1 d . B . C54 C 0.7241(3) 0.2228(3) 0.4840(2) 0.0448(10) Uani 1 1 d . . . H54 H 0.7470 0.1691 0.5310 0.054 Uiso 1 1 calc R . . C55 C 0.7749(3) 0.2383(2) 0.4188(2) 0.0395(9) Uani 1 1 d . . . C56 C 0.7411(3) 0.3162(2) 0.3500(2) 0.0378(8) Uani 1 1 d . . . O56 O 0.78531(18) 0.33768(16) 0.28171(16) 0.0410(6) Uani 1 1 d . . . C57 C 0.5878(3) 0.2640(3) 0.5564(3) 0.0543(12) Uani 1 1 d . . . C571 C 0.4886(7) 0.2819(9) 0.5362(7) 0.067(3) Uani 0.490(10) 1 d P B 1 H57A H 0.4630 0.3388 0.4898 0.100 Uiso 0.490(10) 1 calc PR B 1 H57B H 0.4536 0.2798 0.5813 0.100 Uiso 0.490(10) 1 calc PR B 1 H57C H 0.4819 0.2393 0.5236 0.100 Uiso 0.490(10) 1 calc PR B 1 C572 C 0.6323(9) 0.1780(9) 0.6273(7) 0.083(5) Uani 0.490(10) 1 d P B 1 H57D H 0.6993 0.1691 0.6385 0.124 Uiso 0.490(10) 1 calc PR B 1 H57E H 0.6275 0.1338 0.6163 0.124 Uiso 0.490(10) 1 calc PR B 1 H57F H 0.5990 0.1748 0.6735 0.124 Uiso 0.490(10) 1 calc PR B 1 C573 C 0.5927(8) 0.3340(8) 0.5843(7) 0.067(3) Uani 0.490(10) 1 d P B 1 H57G H 0.6591 0.3237 0.5993 0.100 Uiso 0.490(10) 1 calc PR B 1 H57H H 0.5566 0.3272 0.6298 0.100 Uiso 0.490(10) 1 calc PR B 1 H57I H 0.5652 0.3921 0.5400 0.100 Uiso 0.490(10) 1 calc PR B 1 C574 C 0.6500(7) 0.2404(9) 0.6251(6) 0.066(3) Uani 0.510(10) 1 d P B 2 H57J H 0.7081 0.1941 0.6318 0.099 Uiso 0.510(10) 1 calc PR B 2 H57K H 0.6173 0.2214 0.6729 0.099 Uiso 0.510(10) 1 calc PR B 2 H57L H 0.6664 0.2899 0.6167 0.099 Uiso 0.510(10) 1 calc PR B 2 C575 C 0.4961(7) 0.3350(8) 0.5427(6) 0.064(3) Uani 0.510(10) 1 d P B 2 H57M H 0.4570 0.3490 0.4958 0.097 Uiso 0.510(10) 1 calc PR B 2 H57N H 0.5104 0.3855 0.5339 0.097 Uiso 0.510(10) 1 calc PR B 2 H57O H 0.4614 0.3166 0.5893 0.097 Uiso 0.510(10) 1 calc PR B 2 C576 C 0.5558(7) 0.1825(7) 0.5766(6) 0.062(3) Uani 0.510(10) 1 d P B 2 H57P H 0.5127 0.1966 0.5319 0.093 Uiso 0.510(10) 1 calc PR B 2 H57Q H 0.5233 0.1678 0.6247 0.093 Uiso 0.510(10) 1 calc PR B 2 H57R H 0.6122 0.1339 0.5854 0.093 Uiso 0.510(10) 1 calc PR B 2 C58 C 0.8679(3) 0.1703(2) 0.4253(2) 0.0415(9) Uani 1 1 d . . . C581 C 0.9361(3) 0.1493(3) 0.4949(3) 0.0574(12) Uani 1 1 d . . . H58A H 0.9960 0.1057 0.4995 0.086 Uiso 1 1 calc R . . H58B H 0.9070 0.1280 0.5444 0.086 Uiso 1 1 calc R . . H58C H 0.9487 0.2010 0.4848 0.086 Uiso 1 1 calc R . . C582 C 0.8470(3) 0.0898(3) 0.4404(3) 0.0537(11) Uani 1 1 d . . . H58D H 0.9065 0.0459 0.4447 0.081 Uiso 1 1 calc R . . H58E H 0.8034 0.1038 0.3961 0.081 Uiso 1 1 calc R . . H58F H 0.8179 0.0683 0.4900 0.081 Uiso 1 1 calc R . . C61 C 0.9101(3) 0.3051(2) 0.2108(2) 0.0407(9) Uani 1 1 d . . . C62 C 0.9982(3) 0.2524(3) 0.2076(3) 0.0442(9) Uani 1 1 d . . . H62 H 1.0266 0.2700 0.1594 0.053 Uiso 1 1 calc R . . C63 C 1.0449(3) 0.1748(3) 0.2736(3) 0.0433(9) Uani 1 1 d . . . C64 C 1.0014(3) 0.1508(3) 0.3430(3) 0.0435(9) Uani 1 1 d . . . H64 H 1.0323 0.0974 0.3884 0.052 Uiso 1 1 calc R . . C65 C 0.9146(3) 0.2018(2) 0.3488(2) 0.0389(9) Uani 1 1 d . . . C66 C 0.8706(2) 0.2796(2) 0.2826(2) 0.0386(9) Uani 1 1 d . . . C67 C 1.1405(3) 0.1150(3) 0.2694(3) 0.0501(11) Uani 1 1 d . . . C671 C 1.2148(3) 0.0944(4) 0.3352(4) 0.0747(16) Uani 1 1 d . . . H67A H 1.1916 0.0690 0.3872 0.112 Uiso 1 1 calc R . . H67B H 1.2247 0.1471 0.3253 0.112 Uiso 1 1 calc R . . H67C H 1.2750 0.0543 0.3347 0.112 Uiso 1 1 calc R . . C672 C 1.1277(4) 0.0313(3) 0.2856(4) 0.0691(14) Uani 1 1 d . . . H67D H 1.1032 0.0063 0.3371 0.104 Uiso 1 1 calc R . . H67E H 1.1890 -0.0086 0.2866 0.104 Uiso 1 1 calc R . . H67F H 1.0825 0.0429 0.2435 0.104 Uiso 1 1 calc R . . C673 C 1.1785(4) 0.1535(4) 0.1909(4) 0.0797(18) Uani 1 1 d . . . H67G H 1.2392 0.1131 0.1916 0.119 Uiso 1 1 calc R . . H67H H 1.1881 0.2061 0.1815 0.119 Uiso 1 1 calc R . . H67I H 1.1329 0.1665 0.1483 0.119 Uiso 1 1 calc R . . C71 C 0.8132(3) 0.5436(3) -0.0621(2) 0.0436(9) Uani 1 1 d . . . C72 C 0.7273(3) 0.5969(3) -0.1077(2) 0.0422(9) Uani 1 1 d . . . C73 C 0.7210(3) 0.6490(3) -0.1888(3) 0.0533(11) Uani 1 1 d . . . H73 H 0.6607 0.6842 -0.2190 0.064 Uiso 1 1 calc R . . C74 C 0.8024(4) 0.6496(3) -0.2254(3) 0.0594(12) Uani 1 1 d . . . H74 H 0.7989 0.6852 -0.2812 0.071 Uiso 1 1 calc R . . C75 C 0.8890(4) 0.5982(3) -0.1807(3) 0.0587(12) Uani 1 1 d . . . H75 H 0.9453 0.5994 -0.2061 0.070 Uiso 1 1 calc R . . C76 C 0.8961(3) 0.5453(3) -0.1003(3) 0.0530(11) Uani 1 1 d . . . H76 H 0.9568 0.5100 -0.0706 0.064 Uiso 1 1 calc R . . O72 O 0.64476(18) 0.59405(16) -0.06961(16) 0.0414(6) Uani 1 1 d . . . C81 C 0.5364(3) 0.6447(2) 0.0034(2) 0.0388(9) Uani 1 1 d . . . C82 C 0.6025(3) 0.6580(2) -0.0498(2) 0.0385(9) Uani 1 1 d . . . C83 C 0.6235(3) 0.7340(3) -0.0832(3) 0.0464(10) Uani 1 1 d . . . H83 H 0.6702 0.7427 -0.1191 0.056 Uiso 1 1 calc R . . C84 C 0.5763(3) 0.7960(3) -0.0636(3) 0.0526(11) Uani 1 1 d . . . H84 H 0.5910 0.8475 -0.0863 0.063 Uiso 1 1 calc R . . C85 C 0.5081(3) 0.7851(3) -0.0119(3) 0.0528(11) Uani 1 1 d . . . H85 H 0.4754 0.8285 0.0009 0.063 Uiso 1 1 calc R . . C86 C 0.4881(3) 0.7087(3) 0.0213(3) 0.0448(10) Uani 1 1 d . . . H86 H 0.4408 0.7005 0.0566 0.054 Uiso 1 1 calc R . . N91 N 0.7719(4) 0.5782(5) 0.1454(5) 0.114(2) Uani 1 1 d . . . C92 C 0.8118(5) 0.6186(6) 0.0927(6) 0.109(3) Uani 1 1 d . . . C93 C 0.8563(4) 0.6680(5) 0.0302(5) 0.093(2) Uani 1 1 d . . . H93A H 0.8959 0.6881 0.0505 0.139 Uiso 1 1 calc R . . H93B H 0.8077 0.7171 -0.0116 0.139 Uiso 1 1 calc R . . H93C H 0.8961 0.6332 0.0082 0.139 Uiso 1 1 calc R . . N101 N 0.3210(3) 0.5722(3) 0.0928(4) 0.0783(14) Uani 1 1 d . . . C102 C 0.2476(4) 0.5889(3) 0.1090(3) 0.0614(13) Uani 1 1 d . . . C103 C 0.1516(4) 0.6127(6) 0.1282(5) 0.101(2) Uani 1 1 d . . . H10A H 0.1396 0.6619 0.1366 0.151 Uiso 1 1 calc R . . H10B H 0.1433 0.5648 0.1768 0.151 Uiso 1 1 calc R . . H10C H 0.1067 0.6277 0.0843 0.151 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0404(19) 0.0377(19) 0.0310(19) -0.0149(16) 0.0086(15) -0.0153(15) O1 0.0364(13) 0.0399(14) 0.0355(14) -0.0099(12) 0.0041(11) -0.0141(11) N11 0.0388(16) 0.0345(16) 0.0379(18) -0.0097(14) 0.0004(13) -0.0138(13) N12 0.0369(16) 0.0353(16) 0.0440(19) -0.0108(15) 0.0076(14) -0.0143(13) C2 0.054(2) 0.053(2) 0.047(2) -0.026(2) 0.0168(19) -0.028(2) O2 0.0570(18) 0.065(2) 0.092(3) -0.040(2) 0.0342(18) -0.0349(16) N21 0.055(2) 0.050(2) 0.069(3) -0.024(2) 0.0285(19) -0.0285(17) N22 0.0474(19) 0.050(2) 0.073(3) -0.029(2) 0.0212(18) -0.0258(16) C3 0.0363(18) 0.039(2) 0.038(2) -0.0155(17) 0.0055(16) -0.0107(15) O3 0.0530(16) 0.0407(15) 0.0421(16) -0.0158(13) 0.0159(13) -0.0093(12) N31 0.0454(17) 0.0371(17) 0.0429(19) -0.0167(15) 0.0143(14) -0.0114(14) N32 0.0476(17) 0.0362(17) 0.0307(17) -0.0120(14) 0.0088(14) -0.0056(14) C4 0.0386(19) 0.043(2) 0.037(2) -0.0134(18) 0.0077(16) -0.0135(16) O4 0.0455(16) 0.0609(19) 0.0433(17) -0.0144(15) 0.0128(13) -0.0050(14) N41 0.0418(17) 0.0424(18) 0.0360(18) -0.0137(15) 0.0079(14) -0.0053(14) N42 0.0442(17) 0.0491(19) 0.0326(18) -0.0122(16) 0.0115(14) -0.0107(15) C11 0.0405(19) 0.0344(19) 0.039(2) -0.0135(17) 0.0030(16) -0.0149(15) C12 0.044(2) 0.041(2) 0.038(2) -0.0152(17) 0.0076(16) -0.0189(17) C13 0.045(2) 0.038(2) 0.044(2) -0.0175(18) 0.0014(17) -0.0129(16) C14 0.050(2) 0.035(2) 0.046(2) -0.0142(18) 0.0030(18) -0.0145(17) C15 0.046(2) 0.039(2) 0.040(2) -0.0118(18) 0.0033(17) -0.0186(17) C16 0.0393(19) 0.0374(19) 0.038(2) -0.0118(17) 0.0053(16) -0.0141(15) O16 0.0459(14) 0.0396(14) 0.0426(16) -0.0119(12) 0.0133(12) -0.0208(12) C17 0.056(2) 0.039(2) 0.049(2) -0.0216(19) 0.0049(19) -0.0132(18) C171 0.064(3) 0.063(3) 0.071(3) -0.041(3) -0.001(2) -0.016(2) C172 0.081(3) 0.055(3) 0.070(3) -0.031(3) 0.033(3) -0.016(2) C173 0.051(2) 0.061(3) 0.069(3) -0.036(3) 0.000(2) -0.011(2) C18 0.051(2) 0.038(2) 0.043(2) -0.0072(18) 0.0040(18) -0.0200(17) C181 0.066(3) 0.051(3) 0.073(3) -0.025(2) 0.019(2) -0.033(2) C182 0.058(3) 0.065(3) 0.048(3) 0.004(2) 0.003(2) -0.022(2) C21 0.053(2) 0.049(2) 0.043(2) -0.0191(19) 0.0103(18) -0.0259(19) C22 0.062(3) 0.058(3) 0.045(2) -0.023(2) 0.020(2) -0.034(2) C23 0.064(3) 0.061(3) 0.041(2) -0.018(2) 0.016(2) -0.038(2) C24 0.062(3) 0.051(2) 0.041(2) -0.013(2) 0.010(2) -0.031(2) C25 0.050(2) 0.047(2) 0.037(2) -0.0126(18) 0.0051(17) -0.0241(18) C26 0.044(2) 0.048(2) 0.036(2) -0.0127(18) 0.0094(16) -0.0232(17) C27 0.092(4) 0.073(3) 0.057(3) -0.026(3) 0.040(3) -0.052(3) C271 0.067(7) 0.078(8) 0.088(10) -0.029(7) 0.027(7) -0.040(6) C272 0.26(3) 0.142(17) 0.26(4) -0.12(2) 0.22(3) -0.14(2) C273 0.20(2) 0.18(2) 0.050(7) -0.039(10) 0.047(10) -0.145(19) C274 0.081(10) 0.065(8) 0.071(10) -0.018(7) 0.036(8) -0.035(7) C275 0.043(6) 0.101(13) 0.104(13) 0.016(10) 0.016(7) -0.043(7) C276 0.094(11) 0.147(19) 0.072(10) -0.061(12) 0.050(9) -0.079(13) C31 0.051(2) 0.057(3) 0.060(3) -0.039(2) 0.020(2) -0.028(2) C32 0.074(3) 0.087(4) 0.111(5) -0.077(4) 0.057(3) -0.055(3) C33 0.072(3) 0.099(4) 0.167(7) -0.108(5) 0.070(4) -0.053(3) C34 0.048(2) 0.068(3) 0.117(5) -0.067(3) 0.027(3) -0.022(2) C35 0.044(2) 0.053(2) 0.055(3) -0.037(2) 0.0118(18) -0.0162(18) C36 0.0401(19) 0.051(2) 0.047(2) -0.031(2) 0.0116(17) -0.0171(17) O36 0.0417(14) 0.0380(14) 0.0466(16) -0.0226(12) 0.0136(12) -0.0149(11) C37 0.125(7) 0.185(10) 0.43(2) -0.250(13) 0.193(11) -0.119(7) C371 0.057(3) 0.095(5) 0.153(7) -0.078(5) 0.045(4) -0.033(3) C372 0.094(5) 0.111(6) 0.165(8) -0.101(6) 0.075(5) -0.044(4) C373 0.106(7) 0.154(11) 0.244(17) -0.043(11) 0.025(9) 0.030(7) C38 0.049(2) 0.042(2) 0.041(2) -0.0217(18) 0.0064(17) -0.0076(17) C381 0.060(3) 0.043(2) 0.065(3) -0.030(2) 0.018(2) -0.011(2) C382 0.057(3) 0.068(3) 0.050(3) -0.028(2) 0.000(2) -0.003(2) C41 0.047(2) 0.038(2) 0.035(2) -0.0139(17) 0.0080(16) -0.0138(16) C42 0.042(2) 0.047(2) 0.044(2) -0.0163(19) 0.0043(17) -0.0140(17) C43 0.055(2) 0.046(2) 0.045(2) -0.0193(19) 0.0075(19) -0.0221(19) C44 0.055(2) 0.041(2) 0.043(2) -0.0228(18) 0.0104(18) -0.0179(18) C45 0.047(2) 0.040(2) 0.036(2) -0.0196(17) 0.0098(16) -0.0138(16) C46 0.0406(19) 0.040(2) 0.037(2) -0.0175(17) 0.0073(16) -0.0155(16) C47 0.062(3) 0.058(3) 0.069(3) -0.031(3) 0.007(2) -0.029(2) C471 0.183(9) 0.149(8) 0.126(7) -0.010(6) -0.060(7) -0.119(7) C472 0.098(4) 0.084(4) 0.159(7) -0.078(5) 0.043(5) -0.060(4) C473 0.111(5) 0.095(5) 0.146(7) -0.075(5) 0.074(5) -0.073(4) C51 0.0408(19) 0.0375(19) 0.033(2) -0.0134(16) 0.0022(15) -0.0099(15) C52 0.0408(19) 0.041(2) 0.039(2) -0.0153(18) 0.0055(16) -0.0080(16) C53 0.045(2) 0.046(2) 0.034(2) -0.0123(18) 0.0049(16) -0.0112(17) C54 0.048(2) 0.040(2) 0.033(2) -0.0092(17) 0.0042(16) -0.0127(17) C55 0.0383(18) 0.0358(19) 0.036(2) -0.0139(17) 0.0015(15) -0.0077(15) C56 0.0386(18) 0.040(2) 0.0306(19) -0.0140(16) 0.0049(15) -0.0137(15) O56 0.0398(13) 0.0375(14) 0.0326(14) -0.0118(12) 0.0065(11) -0.0057(11) C57 0.051(2) 0.060(3) 0.032(2) -0.013(2) 0.0093(18) -0.009(2) C571 0.059(6) 0.071(8) 0.052(6) -0.017(6) 0.015(5) -0.022(5) C572 0.073(7) 0.076(8) 0.044(6) -0.005(6) 0.012(5) 0.004(6) C573 0.070(6) 0.080(7) 0.057(6) -0.038(6) 0.016(5) -0.026(6) C574 0.067(6) 0.089(9) 0.032(5) -0.024(5) 0.013(4) -0.023(6) C575 0.068(6) 0.067(7) 0.040(5) -0.020(5) 0.023(4) -0.012(5) C576 0.063(6) 0.074(7) 0.042(5) -0.023(5) 0.023(4) -0.027(5) C58 0.0367(18) 0.039(2) 0.035(2) -0.0117(17) 0.0009(15) -0.0059(15) C581 0.049(2) 0.066(3) 0.036(2) -0.014(2) -0.0009(18) -0.009(2) C582 0.054(2) 0.039(2) 0.054(3) -0.014(2) 0.014(2) -0.0137(18) C61 0.0378(18) 0.039(2) 0.038(2) -0.0136(17) 0.0056(16) -0.0117(15) C62 0.042(2) 0.044(2) 0.042(2) -0.0180(19) 0.0097(17) -0.0136(17) C63 0.0376(19) 0.040(2) 0.046(2) -0.0178(18) 0.0062(17) -0.0102(16) C64 0.0394(19) 0.0360(19) 0.041(2) -0.0106(17) 0.0010(16) -0.0079(16) C65 0.0368(18) 0.0378(19) 0.037(2) -0.0140(17) 0.0031(15) -0.0127(15) C66 0.0333(17) 0.0367(19) 0.041(2) -0.0166(17) 0.0021(15) -0.0084(15) C67 0.042(2) 0.041(2) 0.054(3) -0.018(2) 0.0099(18) -0.0071(17) C671 0.046(3) 0.070(3) 0.092(4) -0.036(3) 0.004(3) -0.005(2) C672 0.067(3) 0.052(3) 0.083(4) -0.034(3) 0.019(3) -0.013(2) C673 0.061(3) 0.064(3) 0.081(4) -0.021(3) 0.032(3) -0.008(2) C71 0.050(2) 0.041(2) 0.034(2) -0.0136(17) 0.0091(17) -0.0167(17) C72 0.049(2) 0.043(2) 0.034(2) -0.0173(18) 0.0100(16) -0.0191(17) C73 0.065(3) 0.053(2) 0.034(2) -0.014(2) 0.0038(19) -0.022(2) C74 0.079(3) 0.061(3) 0.036(2) -0.018(2) 0.017(2) -0.031(2) C75 0.065(3) 0.067(3) 0.047(3) -0.026(2) 0.025(2) -0.031(2) C76 0.048(2) 0.055(3) 0.048(3) -0.019(2) 0.0140(19) -0.0187(19) O72 0.0441(14) 0.0384(14) 0.0385(15) -0.0148(12) 0.0076(11) -0.0167(11) C81 0.0385(18) 0.0356(19) 0.033(2) -0.0083(16) -0.0004(15) -0.0132(15) C82 0.0407(18) 0.0341(19) 0.033(2) -0.0103(16) 0.0000(15) -0.0117(15) C83 0.051(2) 0.040(2) 0.042(2) -0.0144(18) 0.0069(18) -0.0178(18) C84 0.061(3) 0.040(2) 0.055(3) -0.019(2) 0.011(2) -0.0228(19) C85 0.063(3) 0.041(2) 0.051(3) -0.019(2) 0.008(2) -0.0165(19) C86 0.044(2) 0.044(2) 0.041(2) -0.0171(18) 0.0060(17) -0.0146(17) N91 0.089(4) 0.163(6) 0.177(7) -0.131(6) 0.077(4) -0.079(4) C92 0.084(4) 0.149(7) 0.153(8) -0.114(7) 0.047(5) -0.051(5) C93 0.068(3) 0.112(5) 0.099(5) -0.052(4) 0.033(3) -0.034(3) N101 0.052(2) 0.076(3) 0.110(4) -0.044(3) 0.018(2) -0.029(2) C102 0.057(3) 0.062(3) 0.064(3) -0.026(3) 0.008(2) -0.028(2) C103 0.065(3) 0.175(8) 0.115(6) -0.105(6) 0.035(4) -0.053(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 O1 1.227(4) . ? C1 N11 1.364(5) . ? C1 N12 1.369(5) . ? N11 C81 1.428(5) . ? N11 H11 0.8800 . ? N12 C11 1.420(5) . ? N12 H12 0.8800 . ? C2 O2 1.215(5) . ? C2 N21 1.361(6) . ? C2 N22 1.371(5) . ? N21 C21 1.395(6) . ? N21 H21 0.8800 . ? N22 C31 1.388(6) . ? N22 H22 0.8800 . ? C3 O3 1.216(5) . ? C3 N31 1.369(5) . ? C3 N32 1.378(5) . ? N31 C41 1.416(5) . ? N31 H31 0.8800 . ? N32 C51 1.412(5) . ? N32 H32 0.8800 . ? C4 O4 1.215(5) . ? C4 N41 1.366(5) . ? C4 N42 1.376(5) . ? N41 C61 1.398(5) . ? N41 H41 0.8800 . ? N42 C71 1.397(5) . ? N42 H42 0.8800 . ? C11 C12 1.380(6) . ? C11 C16 1.394(6) . ? C12 C13 1.402(6) . ? C12 H12A 0.9500 . ? C13 C14 1.393(6) . ? C13 C17 1.521(6) . ? C14 C15 1.389(6) . ? C14 H14 0.9500 . ? C15 C16 1.397(6) . ? C15 C18 1.529(6) . ? C16 O16 1.376(5) . ? O16 C26 1.386(5) . ? C17 C172 1.525(7) . ? C17 C173 1.542(6) . ? C17 C171 1.542(6) . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? C18 C25 1.516(7) . ? C18 C181 1.531(7) . ? C18 C182 1.542(6) . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C182 H18F 0.9800 . ? C21 C26 1.385(7) . ? C21 C22 1.387(6) . ? C22 C23 1.407(7) . ? C22 H22A 0.9500 . ? C23 C24 1.376(7) . ? C23 C27 1.525(6) . ? C24 C25 1.407(6) . ? C24 H24 0.9500 . ? C25 C26 1.376(6) . ? C27 C276 1.495(18) . ? C27 C274 1.519(15) . ? C27 C272 1.52(2) . ? C27 C271 1.530(14) . ? C27 C275 1.555(14) . ? C27 C273 1.63(2) . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C273 H27G 0.9800 . ? C273 H27H 0.9800 . ? C273 H27I 0.9800 . ? C274 H27J 0.9800 . ? C274 H27K 0.9800 . ? C274 H27L 0.9800 . ? C275 H27M 0.9800 . ? C275 H27N 0.9800 . ? C275 H27O 0.9800 . ? C276 H27P 0.9800 . ? C276 H27Q 0.9800 . ? C276 H27R 0.9800 . ? C31 C32 1.362(7) . ? C31 C36 1.391(6) . ? C32 C33 1.401(8) . ? C32 H32A 0.9500 . ? C33 C34 1.384(8) . ? C33 C37 1.519(8) . ? C34 C35 1.382(6) . ? C34 H34 0.9500 . ? C35 C36 1.382(6) . ? C35 C38 1.516(6) . ? C36 O36 1.383(5) . ? O36 C46 1.382(4) . ? C37 C372 1.381(11) . ? C37 C371 1.455(9) . ? C37 C373 1.768(17) . ? C371 H37A 0.9800 . ? C371 H37B 0.9800 . ? C371 H37C 0.9800 . ? C372 H37D 0.9800 . ? C372 H37E 0.9800 . ? C372 H37F 0.9800 . ? C373 H37G 0.9800 . ? C373 H37H 0.9800 . ? C373 H37I 0.9800 . ? C38 C45 1.531(6) . ? C38 C381 1.541(6) . ? C38 C382 1.555(7) . ? C381 H38A 0.9800 . ? C381 H38B 0.9800 . ? C381 H38C 0.9800 . ? C382 H38D 0.9800 . ? C382 H38E 0.9800 . ? C382 H38F 0.9800 . ? C41 C42 1.384(6) . ? C41 C46 1.386(6) . ? C42 C43 1.396(6) . ? C42 H42A 0.9500 . ? C43 C44 1.376(6) . ? C43 C47 1.534(6) . ? C44 C45 1.396(6) . ? C44 H44 0.9500 . ? C45 C46 1.391(6) . ? C47 C471 1.487(9) . ? C47 C473 1.507(9) . ? C47 C472 1.513(8) . ? C471 H47A 0.9800 . ? C471 H47B 0.9800 . ? C471 H47C 0.9800 . ? C472 H47D 0.9800 . ? C472 H47E 0.9800 . ? C472 H47F 0.9800 . ? C473 H47G 0.9800 . ? C473 H47H 0.9800 . ? C473 H47I 0.9800 . ? C51 C52 1.388(6) . ? C51 C56 1.404(6) . ? C52 C53 1.404(6) . ? C52 H52 0.9500 . ? C53 C54 1.385(6) . ? C53 C57 1.526(6) . ? C54 C55 1.387(6) . ? C54 H54 0.9500 . ? C55 C56 1.385(5) . ? C55 C58 1.528(5) . ? C56 O56 1.375(5) . ? O56 C66 1.389(5) . ? C57 C571 1.442(11) . ? C57 C574 1.458(11) . ? C57 C572 1.498(12) . ? C57 C575 1.512(11) . ? C57 C576 1.620(12) . ? C57 C573 1.673(13) . ? C571 H57A 0.9800 . ? C571 H57B 0.9800 . ? C571 H57C 0.9800 . ? C572 H57D 0.9800 . ? C572 H57E 0.9800 . ? C572 H57F 0.9800 . ? C573 H57G 0.9800 . ? C573 H57H 0.9800 . ? C573 H57I 0.9800 . ? C574 H57J 0.9800 . ? C574 H57K 0.9800 . ? C574 H57L 0.9800 . ? C575 H57M 0.9800 . ? C575 H57N 0.9800 . ? C575 H57O 0.9800 . ? C576 H57P 0.9800 . ? C576 H57Q 0.9800 . ? C576 H57R 0.9800 . ? C58 C65 1.524(6) . ? C58 C582 1.539(6) . ? C58 C581 1.544(6) . ? C581 H58A 0.9800 . ? C581 H58B 0.9800 . ? C581 H58C 0.9800 . ? C582 H58D 0.9800 . ? C582 H58E 0.9800 . ? C582 H58F 0.9800 . ? C61 C66 1.395(6) . ? C61 C62 1.396(6) . ? C62 C63 1.388(6) . ? C62 H62 0.9500 . ? C63 C64 1.388(6) . ? C63 C67 1.542(6) . ? C64 C65 1.385(6) . ? C64 H64 0.9500 . ? C65 C66 1.381(5) . ? C67 C673 1.501(7) . ? C67 C672 1.533(7) . ? C67 C671 1.550(8) . ? C671 H67A 0.9800 . ? C671 H67B 0.9800 . ? C671 H67C 0.9800 . ? C672 H67D 0.9800 . ? C672 H67E 0.9800 . ? C672 H67F 0.9800 . ? C673 H67G 0.9800 . ? C673 H67H 0.9800 . ? C673 H67I 0.9800 . ? C71 C72 1.377(6) . ? C71 C76 1.406(6) . ? C72 C73 1.380(6) . ? C72 O72 1.401(5) . ? C73 C74 1.371(7) . ? C73 H73 0.9500 . ? C74 C75 1.374(7) . ? C74 H74 0.9500 . ? C75 C76 1.371(7) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? O72 C82 1.394(5) . ? C81 C82 1.373(6) . ? C81 C86 1.389(6) . ? C82 C83 1.399(5) . ? C83 C84 1.374(7) . ? C83 H83 0.9500 . ? C84 C85 1.376(7) . ? C84 H84 0.9500 . ? C85 C86 1.397(6) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? N91 C92 1.203(11) . ? C92 C93 1.410(11) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? N101 C102 1.111(7) . ? C102 C103 1.445(8) . ? C103 H10A 0.9800 . ? C103 H10B 0.9800 . ? C103 H10C 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 O1 C1 N11 123.1(3) . . ? O1 C1 N12 122.8(3) . . ? N11 C1 N12 114.0(3) . . ? C1 N11 C81 122.8(3) . . ? C1 N11 H11 118.6 . . ? C81 N11 H11 118.6 . . ? C1 N12 C11 125.8(3) . . ? C1 N12 H12 117.1 . . ? C11 N12 H12 117.1 . . ? O2 C2 N21 123.9(4) . . ? O2 C2 N22 124.8(4) . . ? N21 C2 N22 111.3(4) . . ? C2 N21 C21 128.2(4) . . ? C2 N21 H21 115.9 . . ? C21 N21 H21 115.9 . . ? C2 N22 C31 128.2(4) . . ? C2 N22 H22 115.9 . . ? C31 N22 H22 115.9 . . ? O3 C3 N31 122.7(4) . . ? O3 C3 N32 123.9(4) . . ? N31 C3 N32 113.4(4) . . ? C3 N31 C41 125.8(4) . . ? C3 N31 H31 117.1 . . ? C41 N31 H31 117.1 . . ? C3 N32 C51 126.3(4) . . ? C3 N32 H32 116.8 . . ? C51 N32 H32 116.8 . . ? O4 C4 N41 124.9(4) . . ? O4 C4 N42 123.3(4) . . ? N41 C4 N42 111.8(4) . . ? C4 N41 C61 127.7(3) . . ? C4 N41 H41 116.2 . . ? C61 N41 H41 116.2 . . ? C4 N42 C71 126.0(4) . . ? C4 N42 H42 117.0 . . ? C71 N42 H42 117.0 . . ? C12 C11 C16 119.5(4) . . ? C12 C11 N12 122.3(4) . . ? C16 C11 N12 117.9(4) . . ? C11 C12 C13 120.9(4) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C14 C13 C12 117.7(4) . . ? C14 C13 C17 119.0(4) . . ? C12 C13 C17 123.2(4) . . ? C15 C14 C13 123.1(4) . . ? C15 C14 H14 118.5 . . ? C13 C14 H14 118.5 . . ? C14 C15 C16 117.1(4) . . ? C14 C15 C18 120.7(4) . . ? C16 C15 C18 122.2(4) . . ? O16 C16 C11 115.9(3) . . ? O16 C16 C15 122.7(4) . . ? C11 C16 C15 121.3(4) . . ? C16 O16 C26 118.1(3) . . ? C13 C17 C172 112.3(4) . . ? C13 C17 C173 109.8(4) . . ? C172 C17 C173 108.1(4) . . ? C13 C17 C171 109.3(4) . . ? C172 C17 C171 108.3(5) . . ? C173 C17 C171 109.0(4) . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C17 C173 H17G 109.5 . . ? C17 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C17 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C25 C18 C15 110.3(3) . . ? C25 C18 C181 110.0(4) . . ? C15 C18 C181 108.6(4) . . ? C25 C18 C182 108.2(4) . . ? C15 C18 C182 109.2(3) . . ? C181 C18 C182 110.6(4) . . ? C18 C181 H18A 109.5 . . ? C18 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C18 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C18 C182 H18D 109.5 . . ? C18 C182 H18E 109.5 . . ? H18D C182 H18E 109.5 . . ? C18 C182 H18F 109.5 . . ? H18D C182 H18F 109.5 . . ? H18E C182 H18F 109.5 . . ? C26 C21 C22 119.6(4) . . ? C26 C21 N21 116.3(4) . . ? C22 C21 N21 124.1(5) . . ? C21 C22 C23 119.9(5) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C24 C23 C22 118.5(4) . . ? C24 C23 C27 122.0(4) . . ? C22 C23 C27 119.5(5) . . ? C23 C24 C25 122.7(4) . . ? C23 C24 H24 118.6 . . ? C25 C24 H24 118.6 . . ? C26 C25 C24 116.8(4) . . ? C26 C25 C18 121.7(4) . . ? C24 C25 C18 121.5(4) . . ? C25 C26 C21 122.4(4) . . ? C25 C26 O16 124.2(4) . . ? C21 C26 O16 113.4(4) . . ? C276 C27 C274 109.0(12) . . ? C276 C27 C272 61.4(16) . . ? C274 C27 C272 132.7(8) . . ? C276 C27 C23 107.1(7) . . ? C274 C27 C23 113.9(7) . . ? C272 C27 C23 113.0(7) . . ? C276 C27 C271 139.2(9) . . ? C274 C27 C271 40.5(7) . . ? C272 C27 C271 114.6(15) . . ? C23 C27 C271 110.7(6) . . ? C276 C27 C275 109.9(13) . . ? C274 C27 C275 109.1(10) . . ? C272 C27 C275 49.4(15) . . ? C23 C27 C275 107.8(6) . . ? C271 C27 C275 72.4(10) . . ? C276 C27 C273 48.9(10) . . ? C274 C27 C273 65.3(10) . . ? C272 C27 C273 107.0(17) . . ? C23 C27 C273 105.6(7) . . ? C271 C27 C273 105.1(9) . . ? C275 C27 C273 145.0(10) . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C27 C273 H27G 109.5 . . ? C27 C273 H27H 109.5 . . ? H27G C273 H27H 109.5 . . ? C27 C273 H27I 109.5 . . ? H27G C273 H27I 109.5 . . ? H27H C273 H27I 109.5 . . ? C27 C274 H27J 109.5 . . ? C27 C274 H27K 109.5 . . ? H27J C274 H27K 109.5 . . ? C27 C274 H27L 109.5 . . ? H27J C274 H27L 109.5 . . ? H27K C274 H27L 109.5 . . ? C27 C275 H27M 109.5 . . ? C27 C275 H27N 109.5 . . ? H27M C275 H27N 109.5 . . ? C27 C275 H27O 109.5 . . ? H27M C275 H27O 109.5 . . ? H27N C275 H27O 109.5 . . ? C27 C276 H27P 109.5 . . ? C27 C276 H27Q 109.5 . . ? H27P C276 H27Q 109.5 . . ? C27 C276 H27R 109.5 . . ? H27P C276 H27R 109.5 . . ? H27Q C276 H27R 109.5 . . ? C32 C31 N22 125.5(4) . . ? C32 C31 C36 118.9(4) . . ? N22 C31 C36 115.6(4) . . ? C31 C32 C33 121.1(5) . . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 119.4 . . ? C34 C33 C32 118.1(5) . . ? C34 C33 C37 119.7(6) . . ? C32 C33 C37 122.2(6) . . ? C35 C34 C33 122.3(5) . . ? C35 C34 H34 118.9 . . ? C33 C34 H34 118.9 . . ? C36 C35 C34 117.5(4) . . ? C36 C35 C38 117.3(4) . . ? C34 C35 C38 125.1(4) . . ? C35 C36 O36 122.3(4) . . ? C35 C36 C31 122.0(4) . . ? O36 C36 C31 115.7(4) . . ? C46 O36 C36 115.4(3) . . ? C372 C37 C371 124.9(7) . . ? C372 C37 C33 114.7(7) . . ? C371 C37 C33 113.7(6) . . ? C372 C37 C373 91.2(9) . . ? C371 C37 C373 96.6(9) . . ? C33 C37 C373 109.0(9) . . ? C37 C371 H37A 109.5 . . ? C37 C371 H37B 109.5 . . ? H37A C371 H37B 109.5 . . ? C37 C371 H37C 109.5 . . ? H37A C371 H37C 109.5 . . ? H37B C371 H37C 109.5 . . ? C37 C372 H37D 109.5 . . ? C37 C372 H37E 109.5 . . ? H37D C372 H37E 109.5 . . ? C37 C372 H37F 109.5 . . ? H37D C372 H37F 109.5 . . ? H37E C372 H37F 109.5 . . ? C37 C373 H37G 109.5 . . ? C37 C373 H37H 109.5 . . ? H37G C373 H37H 109.5 . . ? C37 C373 H37I 109.5 . . ? H37G C373 H37I 109.5 . . ? H37H C373 H37I 109.5 . . ? C35 C38 C45 108.1(3) . . ? C35 C38 C381 111.1(4) . . ? C45 C38 C381 112.4(4) . . ? C35 C38 C382 107.7(4) . . ? C45 C38 C382 108.5(4) . . ? C381 C38 C382 109.1(4) . . ? C38 C381 H38A 109.5 . . ? C38 C381 H38B 109.5 . . ? H38A C381 H38B 109.5 . . ? C38 C381 H38C 109.5 . . ? H38A C381 H38C 109.5 . . ? H38B C381 H38C 109.5 . . ? C38 C382 H38D 109.5 . . ? C38 C382 H38E 109.5 . . ? H38D C382 H38E 109.5 . . ? C38 C382 H38F 109.5 . . ? H38D C382 H38F 109.5 . . ? H38E C382 H38F 109.5 . . ? C42 C41 C46 118.2(4) . . ? C42 C41 N31 117.6(4) . . ? C46 C41 N31 124.0(4) . . ? C41 C42 C43 122.5(4) . . ? C41 C42 H42A 118.8 . . ? C43 C42 H42A 118.8 . . ? C44 C43 C42 117.4(4) . . ? C44 C43 C47 122.2(4) . . ? C42 C43 C47 120.5(4) . . ? C43 C44 C45 122.4(4) . . ? C43 C44 H44 118.8 . . ? C45 C44 H44 118.8 . . ? C46 C45 C44 118.1(4) . . ? C46 C45 C38 118.8(3) . . ? C44 C45 C38 122.9(4) . . ? O36 C46 C41 118.6(3) . . ? O36 C46 C45 119.9(3) . . ? C41 C46 C45 121.4(3) . . ? C471 C47 C473 111.2(7) . . ? C471 C47 C472 108.3(7) . . ? C473 C47 C472 106.3(5) . . ? C471 C47 C43 108.6(5) . . ? C473 C47 C43 109.5(5) . . ? C472 C47 C43 113.0(4) . . ? C47 C471 H47A 109.5 . . ? C47 C471 H47B 109.5 . . ? H47A C471 H47B 109.5 . . ? C47 C471 H47C 109.5 . . ? H47A C471 H47C 109.5 . . ? H47B C471 H47C 109.5 . . ? C47 C472 H47D 109.5 . . ? C47 C472 H47E 109.5 . . ? H47D C472 H47E 109.5 . . ? C47 C472 H47F 109.5 . . ? H47D C472 H47F 109.5 . . ? H47E C472 H47F 109.5 . . ? C47 C473 H47G 109.5 . . ? C47 C473 H47H 109.5 . . ? H47G C473 H47H 109.5 . . ? C47 C473 H47I 109.5 . . ? H47G C473 H47I 109.5 . . ? H47H C473 H47I 109.5 . . ? C52 C51 C56 119.4(3) . . ? C52 C51 N32 122.9(4) . . ? C56 C51 N32 117.7(4) . . ? C51 C52 C53 120.8(4) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C54 C53 C52 118.0(4) . . ? C54 C53 C57 120.9(4) . . ? C52 C53 C57 121.1(4) . . ? C53 C54 C55 122.3(4) . . ? C53 C54 H54 118.8 . . ? C55 C54 H54 118.8 . . ? C56 C55 C54 119.0(4) . . ? C56 C55 C58 121.7(4) . . ? C54 C55 C58 119.3(3) . . ? O56 C56 C55 123.7(4) . . ? O56 C56 C51 116.0(3) . . ? C55 C56 C51 120.3(4) . . ? C56 O56 C66 118.4(3) . . ? C571 C57 C574 138.2(7) . . ? C571 C57 C572 112.8(8) . . ? C574 C57 C572 50.9(8) . . ? C571 C57 C575 44.1(7) . . ? C574 C57 C575 112.4(8) . . ? C572 C57 C575 131.5(7) . . ? C571 C57 C53 110.8(6) . . ? C574 C57 C53 110.7(5) . . ? C572 C57 C53 115.2(6) . . ? C575 C57 C53 113.3(5) . . ? C571 C57 C576 63.8(7) . . ? C574 C57 C576 107.3(7) . . ? C572 C57 C576 57.3(8) . . ? C575 C57 C576 105.0(7) . . ? C53 C57 C576 107.7(5) . . ? C571 C57 C573 106.6(8) . . ? C574 C57 C573 57.0(7) . . ? C572 C57 C573 105.2(9) . . ? C575 C57 C573 63.4(7) . . ? C53 C57 C573 105.4(5) . . ? C576 C57 C573 146.8(6) . . ? C57 C571 H57A 109.5 . . ? C57 C571 H57B 109.5 . . ? H57A C571 H57B 109.5 . . ? C57 C571 H57C 109.5 . . ? H57A C571 H57C 109.5 . . ? H57B C571 H57C 109.5 . . ? C57 C572 H57D 109.5 . . ? C57 C572 H57E 109.5 . . ? H57D C572 H57E 109.5 . . ? C57 C572 H57F 109.5 . . ? H57D C572 H57F 109.5 . . ? H57E C572 H57F 109.5 . . ? C57 C573 H57G 109.5 . . ? C57 C573 H57H 109.5 . . ? H57G C573 H57H 109.5 . . ? C57 C573 H57I 109.5 . . ? H57G C573 H57I 109.5 . . ? H57H C573 H57I 109.5 . . ? C57 C574 H57J 109.5 . . ? C57 C574 H57K 109.5 . . ? H57J C574 H57K 109.5 . . ? C57 C574 H57L 109.5 . . ? H57J C574 H57L 109.5 . . ? H57K C574 H57L 109.5 . . ? C57 C575 H57M 109.5 . . ? C57 C575 H57N 109.5 . . ? H57M C575 H57N 109.5 . . ? C57 C575 H57O 109.5 . . ? H57M C575 H57O 109.5 . . ? H57N C575 H57O 109.5 . . ? C57 C576 H57P 109.5 . . ? C57 C576 H57Q 109.5 . . ? H57P C576 H57Q 109.5 . . ? C57 C576 H57R 109.5 . . ? H57P C576 H57R 109.5 . . ? H57Q C576 H57R 109.5 . . ? C65 C58 C55 110.8(3) . . ? C65 C58 C582 108.7(4) . . ? C55 C58 C582 109.2(3) . . ? C65 C58 C581 109.1(3) . . ? C55 C58 C581 108.9(4) . . ? C582 C58 C581 110.1(4) . . ? C58 C581 H58A 109.5 . . ? C58 C581 H58B 109.5 . . ? H58A C581 H58B 109.5 . . ? C58 C581 H58C 109.5 . . ? H58A C581 H58C 109.5 . . ? H58B C581 H58C 109.5 . . ? C58 C582 H58D 109.5 . . ? C58 C582 H58E 109.5 . . ? H58D C582 H58E 109.5 . . ? C58 C582 H58F 109.5 . . ? H58D C582 H58F 109.5 . . ? H58E C582 H58F 109.5 . . ? C66 C61 C62 118.8(3) . . ? C66 C61 N41 118.0(3) . . ? C62 C61 N41 123.2(4) . . ? C63 C62 C61 121.0(4) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C62 C63 C64 118.1(4) . . ? C62 C63 C67 121.2(4) . . ? C64 C63 C67 120.7(4) . . ? C65 C64 C63 122.5(4) . . ? C65 C64 H64 118.8 . . ? C63 C64 H64 118.8 . . ? C66 C65 C64 118.2(4) . . ? C66 C65 C58 121.6(3) . . ? C64 C65 C58 120.1(3) . . ? C65 C66 O56 123.7(4) . . ? C65 C66 C61 121.3(4) . . ? O56 C66 C61 115.0(3) . . ? C673 C67 C672 109.8(5) . . ? C673 C67 C63 112.9(4) . . ? C672 C67 C63 108.9(4) . . ? C673 C67 C671 108.0(4) . . ? C672 C67 C671 108.4(4) . . ? C63 C67 C671 108.8(4) . . ? C67 C671 H67A 109.5 . . ? C67 C671 H67B 109.5 . . ? H67A C671 H67B 109.5 . . ? C67 C671 H67C 109.5 . . ? H67A C671 H67C 109.5 . . ? H67B C671 H67C 109.5 . . ? C67 C672 H67D 109.5 . . ? C67 C672 H67E 109.5 . . ? H67D C672 H67E 109.5 . . ? C67 C672 H67F 109.5 . . ? H67D C672 H67F 109.5 . . ? H67E C672 H67F 109.5 . . ? C67 C673 H67G 109.5 . . ? C67 C673 H67H 109.5 . . ? H67G C673 H67H 109.5 . . ? C67 C673 H67I 109.5 . . ? H67G C673 H67I 109.5 . . ? H67H C673 H67I 109.5 . . ? C72 C71 N42 117.9(4) . . ? C72 C71 C76 117.8(4) . . ? N42 C71 C76 124.3(4) . . ? C71 C72 C73 122.0(4) . . ? C71 C72 O72 117.6(3) . . ? C73 C72 O72 120.4(4) . . ? C74 C73 C72 119.6(4) . . ? C74 C73 H73 120.2 . . ? C72 C73 H73 120.2 . . ? C73 C74 C75 119.4(4) . . ? C73 C74 H74 120.3 . . ? C75 C74 H74 120.3 . . ? C76 C75 C74 121.6(4) . . ? C76 C75 H75 119.2 . . ? C74 C75 H75 119.2 . . ? C75 C76 C71 119.6(4) . . ? C75 C76 H76 120.2 . . ? C71 C76 H76 120.2 . . ? C82 O72 C72 117.3(3) . . ? C82 C81 C86 119.2(4) . . ? C82 C81 N11 122.5(4) . . ? C86 C81 N11 118.3(4) . . ? C81 C82 O72 117.1(3) . . ? C81 C82 C83 120.3(4) . . ? O72 C82 C83 122.6(4) . . ? C84 C83 C82 119.7(4) . . ? C84 C83 H83 120.2 . . ? C82 C83 H83 120.2 . . ? C83 C84 C85 121.2(4) . . ? C83 C84 H84 119.4 . . ? C85 C84 H84 119.4 . . ? C84 C85 C86 118.6(4) . . ? C84 C85 H85 120.7 . . ? C86 C85 H85 120.7 . . ? C81 C86 C85 121.0(4) . . ? C81 C86 H86 119.5 . . ? C85 C86 H86 119.5 . . ? N91 C92 C93 178.4(9) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? N101 C102 C103 178.5(7) . . ? C102 C103 H10A 109.5 . . ? C102 C103 H10B 109.5 . . ? H10A C103 H10B 109.5 . . ? C102 C103 H10C 109.5 . . ? H10A C103 H10C 109.5 . . ? H10B C103 H10C 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 O1 C1 N11 C81 -15.0(6) . . . . ? N12 C1 N11 C81 164.4(4) . . . . ? O1 C1 N12 C11 -21.2(7) . . . . ? N11 C1 N12 C11 159.3(4) . . . . ? O2 C2 N21 C21 -9.1(8) . . . . ? N22 C2 N21 C21 172.4(5) . . . . ? O2 C2 N22 C31 -8.5(8) . . . . ? N21 C2 N22 C31 170.1(5) . . . . ? O3 C3 N31 C41 13.3(6) . . . . ? N32 C3 N31 C41 -168.4(4) . . . . ? O3 C3 N32 C51 -20.0(6) . . . . ? N31 C3 N32 C51 161.7(4) . . . . ? O4 C4 N41 C61 -4.5(7) . . . . ? N42 C4 N41 C61 176.6(4) . . . . ? O4 C4 N42 C71 1.1(7) . . . . ? N41 C4 N42 C71 -180.0(4) . . . . ? C1 N12 C11 C12 -40.2(6) . . . . ? C1 N12 C11 C16 146.3(4) . . . . ? C16 C11 C12 C13 1.5(6) . . . . ? N12 C11 C12 C13 -171.8(4) . . . . ? C11 C12 C13 C14 2.8(6) . . . . ? C11 C12 C13 C17 179.2(4) . . . . ? C12 C13 C14 C15 -2.5(6) . . . . ? C17 C13 C14 C15 -179.1(4) . . . . ? C13 C14 C15 C16 -2.0(6) . . . . ? C13 C14 C15 C18 175.8(4) . . . . ? C12 C11 C16 O16 175.6(3) . . . . ? N12 C11 C16 O16 -10.8(5) . . . . ? C12 C11 C16 C15 -6.4(6) . . . . ? N12 C11 C16 C15 167.3(4) . . . . ? C14 C15 C16 O16 -175.6(4) . . . . ? C18 C15 C16 O16 6.5(6) . . . . ? C14 C15 C16 C11 6.5(6) . . . . ? C18 C15 C16 C11 -171.3(4) . . . . ? C11 C16 O16 C26 170.9(3) . . . . ? C15 C16 O16 C26 -7.1(5) . . . . ? C14 C13 C17 C172 177.1(4) . . . . ? C12 C13 C17 C172 0.7(6) . . . . ? C14 C13 C17 C173 -62.6(5) . . . . ? C12 C13 C17 C173 121.1(4) . . . . ? C14 C13 C17 C171 56.8(5) . . . . ? C12 C13 C17 C171 -119.5(4) . . . . ? C14 C15 C18 C25 -176.8(4) . . . . ? C16 C15 C18 C25 1.0(6) . . . . ? C14 C15 C18 C181 -56.2(5) . . . . ? C16 C15 C18 C181 121.6(5) . . . . ? C14 C15 C18 C182 64.4(6) . . . . ? C16 C15 C18 C182 -117.8(5) . . . . ? C2 N21 C21 C26 162.8(5) . . . . ? C2 N21 C21 C22 -18.7(8) . . . . ? C26 C21 C22 C23 0.8(7) . . . . ? N21 C21 C22 C23 -177.7(4) . . . . ? C21 C22 C23 C24 2.4(7) . . . . ? C21 C22 C23 C27 -178.9(5) . . . . ? C22 C23 C24 C25 -2.2(7) . . . . ? C27 C23 C24 C25 179.2(4) . . . . ? C23 C24 C25 C26 -1.2(7) . . . . ? C23 C24 C25 C18 176.5(4) . . . . ? C15 C18 C25 C26 -7.9(6) . . . . ? C181 C18 C25 C26 -127.7(4) . . . . ? C182 C18 C25 C26 111.4(4) . . . . ? C15 C18 C25 C24 174.4(4) . . . . ? C181 C18 C25 C24 54.7(5) . . . . ? C182 C18 C25 C24 -66.2(5) . . . . ? C24 C25 C26 C21 4.6(6) . . . . ? C18 C25 C26 C21 -173.2(4) . . . . ? C24 C25 C26 O16 -174.0(4) . . . . ? C18 C25 C26 O16 8.2(6) . . . . ? C22 C21 C26 C25 -4.4(6) . . . . ? N21 C21 C26 C25 174.2(4) . . . . ? C22 C21 C26 O16 174.3(4) . . . . ? N21 C21 C26 O16 -7.1(5) . . . . ? C16 O16 C26 C25 -0.4(6) . . . . ? C16 O16 C26 C21 -179.1(3) . . . . ? C24 C23 C27 C276 115.2(13) . . . . ? C22 C23 C27 C276 -63.4(13) . . . . ? C24 C23 C27 C274 -5.4(11) . . . . ? C22 C23 C27 C274 176.0(10) . . . . ? C24 C23 C27 C272 -179(2) . . . . ? C22 C23 C27 C272 2(2) . . . . ? C24 C23 C27 C271 -49.1(9) . . . . ? C22 C23 C27 C271 132.2(8) . . . . ? C24 C23 C27 C275 -126.5(12) . . . . ? C22 C23 C27 C275 54.9(13) . . . . ? C24 C23 C27 C273 64.1(12) . . . . ? C22 C23 C27 C273 -114.5(12) . . . . ? C2 N22 C31 C32 19.7(9) . . . . ? C2 N22 C31 C36 -161.7(5) . . . . ? N22 C31 C32 C33 175.9(6) . . . . ? C36 C31 C32 C33 -2.7(9) . . . . ? C31 C32 C33 C34 -0.8(11) . . . . ? C31 C32 C33 C37 178.3(9) . . . . ? C32 C33 C34 C35 2.5(11) . . . . ? C37 C33 C34 C35 -176.6(8) . . . . ? C33 C34 C35 C36 -0.7(9) . . . . ? C33 C34 C35 C38 175.2(6) . . . . ? C34 C35 C36 O36 178.4(4) . . . . ? C38 C35 C36 O36 2.2(6) . . . . ? C34 C35 C36 C31 -3.0(7) . . . . ? C38 C35 C36 C31 -179.2(4) . . . . ? C32 C31 C36 C35 4.7(7) . . . . ? N22 C31 C36 C35 -174.0(4) . . . . ? C32 C31 C36 O36 -176.6(5) . . . . ? N22 C31 C36 O36 4.7(6) . . . . ? C35 C36 O36 C46 32.4(5) . . . . ? C31 C36 O36 C46 -146.3(4) . . . . ? C34 C33 C37 C372 -49.2(16) . . . . ? C32 C33 C37 C372 131.7(10) . . . . ? C34 C33 C37 C371 157.9(9) . . . . ? C32 C33 C37 C371 -21.2(16) . . . . ? C34 C33 C37 C373 51.4(11) . . . . ? C32 C33 C37 C373 -127.7(10) . . . . ? C36 C35 C38 C45 -33.8(5) . . . . ? C34 C35 C38 C45 150.3(5) . . . . ? C36 C35 C38 C381 -157.5(4) . . . . ? C34 C35 C38 C381 26.6(6) . . . . ? C36 C35 C38 C382 83.2(5) . . . . ? C34 C35 C38 C382 -92.7(6) . . . . ? C3 N31 C41 C42 122.3(4) . . . . ? C3 N31 C41 C46 -63.1(6) . . . . ? C46 C41 C42 C43 -0.4(7) . . . . ? N31 C41 C42 C43 174.5(4) . . . . ? C41 C42 C43 C44 -1.6(7) . . . . ? C41 C42 C43 C47 179.2(4) . . . . ? C42 C43 C44 C45 1.1(7) . . . . ? C47 C43 C44 C45 -179.7(4) . . . . ? C43 C44 C45 C46 1.2(7) . . . . ? C43 C44 C45 C38 -173.8(4) . . . . ? C35 C38 C45 C46 35.1(5) . . . . ? C381 C38 C45 C46 158.0(4) . . . . ? C382 C38 C45 C46 -81.3(5) . . . . ? C35 C38 C45 C44 -149.9(4) . . . . ? C381 C38 C45 C44 -27.0(6) . . . . ? C382 C38 C45 C44 93.7(5) . . . . ? C36 O36 C46 C41 152.9(4) . . . . ? C36 O36 C46 C45 -30.8(5) . . . . ? C42 C41 C46 O36 179.0(4) . . . . ? N31 C41 C46 O36 4.5(6) . . . . ? C42 C41 C46 C45 2.8(6) . . . . ? N31 C41 C46 C45 -171.7(4) . . . . ? C44 C45 C46 O36 -179.4(4) . . . . ? C38 C45 C46 O36 -4.1(6) . . . . ? C44 C45 C46 C41 -3.2(6) . . . . ? C38 C45 C46 C41 172.0(4) . . . . ? C44 C43 C47 C471 118.9(7) . . . . ? C42 C43 C47 C471 -61.9(8) . . . . ? C44 C43 C47 C473 -119.5(6) . . . . ? C42 C43 C47 C473 59.7(7) . . . . ? C44 C43 C47 C472 -1.2(8) . . . . ? C42 C43 C47 C472 178.0(6) . . . . ? C3 N32 C51 C52 17.5(6) . . . . ? C3 N32 C51 C56 -161.1(4) . . . . ? C56 C51 C52 C53 3.4(6) . . . . ? N32 C51 C52 C53 -175.2(4) . . . . ? C51 C52 C53 C54 -1.1(6) . . . . ? C51 C52 C53 C57 177.6(4) . . . . ? C52 C53 C54 C55 -0.4(7) . . . . ? C57 C53 C54 C55 -179.0(4) . . . . ? C53 C54 C55 C56 -0.5(6) . . . . ? C53 C54 C55 C58 177.8(4) . . . . ? C54 C55 C56 O56 -179.2(4) . . . . ? C58 C55 C56 O56 2.6(6) . . . . ? C54 C55 C56 C51 2.9(6) . . . . ? C58 C55 C56 C51 -175.4(4) . . . . ? C52 C51 C56 O56 177.6(4) . . . . ? N32 C51 C56 O56 -3.7(5) . . . . ? C52 C51 C56 C55 -4.3(6) . . . . ? N32 C51 C56 C55 174.3(4) . . . . ? C55 C56 O56 C66 -2.7(5) . . . . ? C51 C56 O56 C66 175.3(3) . . . . ? C54 C53 C57 C571 -129.2(8) . . . . ? C52 C53 C57 C571 52.2(9) . . . . ? C54 C53 C57 C574 55.8(8) . . . . ? C52 C53 C57 C574 -122.8(7) . . . . ? C54 C53 C57 C572 0.4(10) . . . . ? C52 C53 C57 C572 -178.3(9) . . . . ? C54 C53 C57 C575 -176.9(7) . . . . ? C52 C53 C57 C575 4.5(9) . . . . ? C54 C53 C57 C576 -61.2(6) . . . . ? C52 C53 C57 C576 120.2(6) . . . . ? C54 C53 C57 C573 115.9(6) . . . . ? C52 C53 C57 C573 -62.7(6) . . . . ? C56 C55 C58 C65 1.1(5) . . . . ? C54 C55 C58 C65 -177.1(4) . . . . ? C56 C55 C58 C582 -118.6(4) . . . . ? C54 C55 C58 C582 63.1(5) . . . . ? C56 C55 C58 C581 121.1(4) . . . . ? C54 C55 C58 C581 -57.1(5) . . . . ? C4 N41 C61 C66 -174.2(4) . . . . ? C4 N41 C61 C62 6.5(7) . . . . ? C66 C61 C62 C63 1.7(6) . . . . ? N41 C61 C62 C63 -178.9(4) . . . . ? C61 C62 C63 C64 0.2(6) . . . . ? C61 C62 C63 C67 177.9(4) . . . . ? C62 C63 C64 C65 -0.9(6) . . . . ? C67 C63 C64 C65 -178.6(4) . . . . ? C63 C64 C65 C66 -0.4(6) . . . . ? C63 C64 C65 C58 177.0(4) . . . . ? C55 C58 C65 C66 -4.8(5) . . . . ? C582 C58 C65 C66 115.2(4) . . . . ? C581 C58 C65 C66 -124.7(4) . . . . ? C55 C58 C65 C64 178.0(4) . . . . ? C582 C58 C65 C64 -62.0(5) . . . . ? C581 C58 C65 C64 58.1(5) . . . . ? C64 C65 C66 O56 -177.5(4) . . . . ? C58 C65 C66 O56 5.2(6) . . . . ? C64 C65 C66 C61 2.4(6) . . . . ? C58 C65 C66 C61 -174.9(4) . . . . ? C56 O56 C66 C65 -1.3(5) . . . . ? C56 O56 C66 C61 178.8(3) . . . . ? C62 C61 C66 C65 -3.1(6) . . . . ? N41 C61 C66 C65 177.6(4) . . . . ? C62 C61 C66 O56 176.9(4) . . . . ? N41 C61 C66 O56 -2.5(5) . . . . ? C62 C63 C67 C673 5.1(7) . . . . ? C64 C63 C67 C673 -177.3(5) . . . . ? C62 C63 C67 C672 -117.2(5) . . . . ? C64 C63 C67 C672 60.4(6) . . . . ? C62 C63 C67 C671 124.9(5) . . . . ? C64 C63 C67 C671 -57.5(5) . . . . ? C4 N42 C71 C72 154.8(4) . . . . ? C4 N42 C71 C76 -27.1(7) . . . . ? N42 C71 C72 C73 -179.9(4) . . . . ? C76 C71 C72 C73 1.9(7) . . . . ? N42 C71 C72 O72 -2.7(6) . . . . ? C76 C71 C72 O72 179.1(4) . . . . ? C71 C72 C73 C74 -1.4(7) . . . . ? O72 C72 C73 C74 -178.5(4) . . . . ? C72 C73 C74 C75 0.0(8) . . . . ? C73 C74 C75 C76 1.0(8) . . . . ? C74 C75 C76 C71 -0.5(8) . . . . ? C72 C71 C76 C75 -0.9(7) . . . . ? N42 C71 C76 C75 -179.0(5) . . . . ? C71 C72 O72 C82 100.4(4) . . . . ? C73 C72 O72 C82 -82.4(5) . . . . ? C1 N11 C81 C82 71.4(5) . . . . ? C1 N11 C81 C86 -110.5(4) . . . . ? C86 C81 C82 O72 -176.1(3) . . . . ? N11 C81 C82 O72 2.0(5) . . . . ? C86 C81 C82 C83 2.5(5) . . . . ? N11 C81 C82 C83 -179.4(3) . . . . ? C72 O72 C82 C81 -164.9(3) . . . . ? C72 O72 C82 C83 16.6(5) . . . . ? C81 C82 C83 C84 -1.3(6) . . . . ? O72 C82 C83 C84 177.2(4) . . . . ? C82 C83 C84 C85 -0.2(7) . . . . ? C83 C84 C85 C86 0.5(7) . . . . ? C82 C81 C86 C85 -2.2(6) . . . . ? N11 C81 C86 C85 179.6(4) . . . . ? C84 C85 C86 C81 0.7(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11 H11 N101 0.88 2.36 2.979(6) 128.0 . N12 H12 N101 0.88 2.46 3.238(6) 147.6 . N21 H21 O3 0.88 2.89 3.516(5) 129.3 . N22 H22 O3 0.88 2.09 2.916(5) 156.5 . N31 H31 N91 0.88 2.30 2.996(7) 135.5 . N32 H32 O1 0.88 2.30 3.125(5) 156.8 . N41 H41 O1 0.88 2.17 2.893(4) 138.8 . N42 H42 O1 0.88 2.04 2.801(4) 143.7 . _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.886 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.110 data_boeh58 _database_code_depnum_ccdc_archive 'CCDC 687875' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C95 H130 N8 O13' _chemical_formula_weight 1592.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 29.7280(13) _cell_length_b 16.1350(5) _cell_length_c 20.0431(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.696(3) _cell_angle_gamma 90.00 _cell_volume 9159.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 44893 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.4 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9642 _exptl_absorpt_correction_T_max 0.9819 _exptl_absorpt_process_details 'MULABS (Spek, 2003; Blessing, 1995)' _exptl_special_details ; ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 73886 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0531 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.19 _reflns_number_total 16079 _reflns_number_gt 10965 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.1418P)^2^+9.9584P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0059(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16079 _refine_ls_number_parameters 1049 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0873 _refine_ls_wR_factor_ref 0.2593 _refine_ls_wR_factor_gt 0.2404 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.020 _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 0.72593(12) 0.56073(18) 0.37047(18) 0.0303(7) Uani 1 1 d . . . O1 O 0.73429(8) 0.51137(13) 0.32755(13) 0.0332(5) Uani 1 1 d . . . N11 N 0.68161(10) 0.57452(18) 0.37346(17) 0.0385(7) Uani 1 1 d . . . H11 H 0.6773 0.6139 0.4013 0.046 Uiso 1 1 calc R . . N12 N 0.76024(10) 0.60555(16) 0.41594(16) 0.0333(7) Uani 1 1 d . . . H12 H 0.7513 0.6432 0.4411 0.040 Uiso 1 1 calc R . . C2 C 0.71764(14) 0.9115(2) 0.3263(2) 0.0383(8) Uani 1 1 d . . . O2 O 0.71999(13) 0.98525(19) 0.3272(3) 0.0971(15) Uani 1 1 d . . . N21 N 0.75447(12) 0.86228(18) 0.3605(2) 0.0500(9) Uani 1 1 d . . . H21 H 0.7474 0.8096 0.3630 0.060 Uiso 1 1 calc R . . N22 N 0.67766(11) 0.86724(18) 0.29383(18) 0.0453(8) Uani 1 1 d . . . H22 H 0.6791 0.8134 0.3014 0.054 Uiso 1 1 calc R . . C3 C 0.71449(13) 0.6871(2) 0.20629(19) 0.0335(8) Uani 1 1 d . . . O3 O 0.71019(10) 0.76076(15) 0.18864(15) 0.0471(7) Uani 1 1 d . . . N31 N 0.67769(11) 0.63285(17) 0.18835(17) 0.0401(7) Uani 1 1 d . . . H31 H 0.6806 0.5839 0.2085 0.048 Uiso 1 1 calc R . . N32 N 0.75629(10) 0.65368(17) 0.24736(16) 0.0358(7) Uani 1 1 d . . . H32 H 0.7554 0.6154 0.2782 0.043 Uiso 1 1 calc R . . C4 C 0.77078(12) 0.31932(19) 0.30206(19) 0.0332(8) Uani 1 1 d . . . O4 O 0.78129(10) 0.24786(14) 0.29151(17) 0.0492(7) Uani 1 1 d . . . N41 N 0.79151(10) 0.38873(16) 0.28477(16) 0.0327(6) Uani 1 1 d . . . H41 H 0.7785 0.4366 0.2889 0.039 Uiso 1 1 calc R . . N42 N 0.73636(11) 0.33870(17) 0.33241(17) 0.0384(7) Uani 1 1 d . . . H42 H 0.7287 0.3914 0.3320 0.046 Uiso 1 1 calc R . . C11 C 0.80930(12) 0.59688(19) 0.42642(18) 0.0308(7) Uani 1 1 d . . . C12 C 0.83220(12) 0.52118(19) 0.44151(18) 0.0323(7) Uani 1 1 d . . . H12A H 0.8143 0.4721 0.4401 0.039 Uiso 1 1 calc R . . C13 C 0.88137(12) 0.51621(19) 0.45884(18) 0.0314(7) Uani 1 1 d . . . C14 C 0.90647(12) 0.59004(19) 0.46267(18) 0.0328(7) Uani 1 1 d . . . H14 H 0.9399 0.5875 0.4755 0.039 Uiso 1 1 calc R . . C15 C 0.88461(12) 0.66783(18) 0.44839(17) 0.0291(7) Uani 1 1 d . . . C16 C 0.83577(12) 0.66859(18) 0.42817(18) 0.0296(7) Uani 1 1 d . . . O16 O 0.80904(8) 0.74005(13) 0.40882(13) 0.0343(6) Uani 1 1 d . . . C17 C 0.90828(13) 0.43380(19) 0.47861(19) 0.0358(8) Uani 1 1 d . . . C171 C 0.93972(14) 0.4389(2) 0.5546(2) 0.0453(9) Uani 1 1 d . . . H17A H 0.9615 0.4858 0.5599 0.068 Uiso 1 1 calc R . . H17B H 0.9578 0.3874 0.5673 0.068 Uiso 1 1 calc R . . H17C H 0.9200 0.4468 0.5854 0.068 Uiso 1 1 calc R . . C172 C 0.87486(15) 0.3594(2) 0.4723(3) 0.0513(11) Uani 1 1 d . . . H17D H 0.8545 0.3545 0.4238 0.077 Uiso 1 1 calc R . . H17E H 0.8553 0.3678 0.5033 0.077 Uiso 1 1 calc R . . H17F H 0.8935 0.3086 0.4859 0.077 Uiso 1 1 calc R . . C173 C 0.93863(15) 0.4178(2) 0.4299(2) 0.0481(10) Uani 1 1 d . . . H17G H 0.9603 0.4644 0.4330 0.072 Uiso 1 1 calc R . . H17H H 0.9181 0.4123 0.3816 0.072 Uiso 1 1 calc R . . H17I H 0.9568 0.3667 0.4442 0.072 Uiso 1 1 calc R . . C18 C 0.91372(12) 0.74807(19) 0.45947(19) 0.0321(7) Uani 1 1 d . . . C181 C 0.94452(13) 0.7532(2) 0.5365(2) 0.0382(8) Uani 1 1 d . . . H18A H 0.9657 0.7052 0.5479 0.057 Uiso 1 1 calc R . . H18B H 0.9242 0.7535 0.5670 0.057 Uiso 1 1 calc R . . H18C H 0.9633 0.8042 0.5439 0.057 Uiso 1 1 calc R . . C182 C 0.94571(14) 0.7483(2) 0.4118(2) 0.0403(9) Uani 1 1 d . . . H18D H 0.9670 0.7005 0.4230 0.060 Uiso 1 1 calc R . . H18E H 0.9643 0.7995 0.4192 0.060 Uiso 1 1 calc R . . H18F H 0.9262 0.7450 0.3627 0.060 Uiso 1 1 calc R . . C21 C 0.80194(13) 0.8826(2) 0.39242(19) 0.0358(8) Uani 1 1 d . . . C22 C 0.82102(14) 0.9623(2) 0.4014(2) 0.0408(9) Uani 1 1 d . . . H22A H 0.8008 1.0090 0.3878 0.049 Uiso 1 1 calc R . . C23 C 0.86942(15) 0.9739(2) 0.4302(2) 0.0434(9) Uani 1 1 d . A . C24 C 0.89847(14) 0.90471(19) 0.4496(2) 0.0371(8) Uani 1 1 d . . . H24 H 0.9316 0.9128 0.4688 0.045 Uiso 1 1 calc R . . C25 C 0.88080(13) 0.82341(19) 0.44185(18) 0.0324(8) Uani 1 1 d . . . C26 C 0.83252(12) 0.81487(19) 0.41525(18) 0.0320(7) Uani 1 1 d . . . C27 C 0.88959(15) 1.0627(2) 0.4413(2) 0.0624(13) Uani 1 1 d D . . C271 C 0.9404(2) 1.0689(5) 0.4828(4) 0.058(2) Uiso 0.566(9) 1 d PD A 1 H27A H 0.9465 1.0344 0.5249 0.087 Uiso 0.566(9) 1 calc PR A 1 H27B H 0.9482 1.1267 0.4965 0.087 Uiso 0.566(9) 1 calc PR A 1 H27C H 0.9600 1.0496 0.4544 0.087 Uiso 0.566(9) 1 calc PR A 1 C272 C 0.8738(3) 1.1100(5) 0.3743(3) 0.057(2) Uiso 0.566(9) 1 d PD A 1 H27D H 0.8400 1.1003 0.3516 0.085 Uiso 0.566(9) 1 calc PR A 1 H27E H 0.8916 1.0915 0.3432 0.085 Uiso 0.566(9) 1 calc PR A 1 H27F H 0.8793 1.1693 0.3839 0.085 Uiso 0.566(9) 1 calc PR A 1 C273 C 0.8648(3) 1.1069(5) 0.4892(4) 0.062(2) Uiso 0.566(9) 1 d PD A 1 H27G H 0.8306 1.1069 0.4664 0.093 Uiso 0.566(9) 1 calc PR A 1 H27H H 0.8761 1.1641 0.4975 0.093 Uiso 0.566(9) 1 calc PR A 1 H27I H 0.8719 1.0774 0.5340 0.093 Uiso 0.566(9) 1 calc PR A 1 C274 C 0.8595(3) 1.1269(5) 0.3957(5) 0.048(3) Uiso 0.434(9) 1 d PD A 2 H27J H 0.8425 1.1025 0.3503 0.072 Uiso 0.434(9) 1 calc PR A 2 H27K H 0.8793 1.1726 0.3889 0.072 Uiso 0.434(9) 1 calc PR A 2 H27L H 0.8366 1.1480 0.4181 0.072 Uiso 0.434(9) 1 calc PR A 2 C275 C 0.9292(4) 1.0607(9) 0.4070(7) 0.086(4) Uiso 0.434(9) 1 d PD A 2 H27M H 0.9157 1.0487 0.3569 0.129 Uiso 0.434(9) 1 calc PR A 2 H27N H 0.9520 1.0174 0.4291 0.129 Uiso 0.434(9) 1 calc PR A 2 H27O H 0.9451 1.1145 0.4131 0.129 Uiso 0.434(9) 1 calc PR A 2 C276 C 0.9206(4) 1.0815(7) 0.5133(4) 0.062(3) Uiso 0.434(9) 1 d PD A 2 H27P H 0.9378 1.0314 0.5341 0.093 Uiso 0.434(9) 1 calc PR A 2 H27Q H 0.9012 1.1006 0.5420 0.093 Uiso 0.434(9) 1 calc PR A 2 H27R H 0.9431 1.1251 0.5111 0.093 Uiso 0.434(9) 1 calc PR A 2 C31 C 0.63452(13) 0.8979(2) 0.2497(2) 0.0390(8) Uani 1 1 d . . . C32 C 0.62137(14) 0.9807(2) 0.2438(2) 0.0434(9) Uani 1 1 d . . . H32A H 0.6418 1.0207 0.2725 0.052 Uiso 1 1 calc R . . C33 C 0.57863(15) 1.0066(2) 0.1964(2) 0.0461(10) Uani 1 1 d . . . C34 C 0.54848(15) 0.9472(2) 0.1566(2) 0.0459(10) Uani 1 1 d . . . H34 H 0.5191 0.9643 0.1250 0.055 Uiso 1 1 calc R . . C35 C 0.55996(14) 0.8633(2) 0.1617(2) 0.0421(9) Uani 1 1 d . . . C36 C 0.60313(13) 0.8401(2) 0.20766(19) 0.0371(8) Uani 1 1 d . . . O36 O 0.61758(9) 0.75698(14) 0.21280(13) 0.0373(6) Uani 1 1 d . . . C37 C 0.56730(18) 1.0996(3) 0.1878(3) 0.0600(12) Uani 1 1 d . . . C371 C 0.5173(2) 1.1167(3) 0.1429(4) 0.096(2) Uani 1 1 d . . . H37A H 0.4951 1.0923 0.1649 0.143 Uiso 1 1 calc R . . H37B H 0.5121 1.0922 0.0964 0.143 Uiso 1 1 calc R . . H37C H 0.5121 1.1767 0.1383 0.143 Uiso 1 1 calc R . . C372 C 0.6003(3) 1.1388(4) 0.1528(6) 0.163(5) Uani 1 1 d . . . H37D H 0.5936 1.1983 0.1467 0.245 Uiso 1 1 calc R . . H37E H 0.5957 1.1131 0.1070 0.245 Uiso 1 1 calc R . . H37F H 0.6330 1.1307 0.1820 0.245 Uiso 1 1 calc R . . C373 C 0.5720(3) 1.1379(3) 0.2589(4) 0.105(3) Uani 1 1 d . . . H37G H 0.5498 1.1110 0.2795 0.157 Uiso 1 1 calc R . . H37H H 0.5650 1.1973 0.2533 0.157 Uiso 1 1 calc R . . H37I H 0.6043 1.1300 0.2898 0.157 Uiso 1 1 calc R . . C38 C 0.52847(14) 0.7939(3) 0.1197(2) 0.0460(9) Uani 1 1 d . . . C381 C 0.48968(16) 0.8274(3) 0.0566(3) 0.0636(13) Uani 1 1 d . . . H38A H 0.4703 0.7813 0.0316 0.095 Uiso 1 1 calc R . . H38B H 0.5041 0.8562 0.0251 0.095 Uiso 1 1 calc R . . H38C H 0.4698 0.8662 0.0726 0.095 Uiso 1 1 calc R . . C382 C 0.50540(16) 0.7478(3) 0.1682(3) 0.0578(12) Uani 1 1 d . . . H38D H 0.4851 0.7035 0.1419 0.087 Uiso 1 1 calc R . . H38E H 0.4864 0.7868 0.1858 0.087 Uiso 1 1 calc R . . H38F H 0.5300 0.7239 0.2077 0.087 Uiso 1 1 calc R . . C41 C 0.63427(13) 0.6550(2) 0.1370(2) 0.0392(8) Uani 1 1 d . . . C42 C 0.62238(15) 0.6147(2) 0.0721(2) 0.0459(9) Uani 1 1 d . . . H42A H 0.6428 0.5731 0.0643 0.055 Uiso 1 1 calc R . . C43 C 0.58118(16) 0.6345(3) 0.0185(2) 0.0508(10) Uani 1 1 d . . . C44 C 0.55072(15) 0.6931(3) 0.0338(2) 0.0504(10) Uani 1 1 d . . . H44 H 0.5219 0.7059 -0.0012 0.061 Uiso 1 1 calc R . . C45 C 0.56133(14) 0.7330(2) 0.0985(2) 0.0426(9) Uani 1 1 d . . . C46 C 0.60425(13) 0.7150(2) 0.1490(2) 0.0384(8) Uani 1 1 d . . . C47 C 0.57046(19) 0.5955(3) -0.0552(3) 0.0654(13) Uani 1 1 d . . . C471 C 0.5650(3) 0.6645(4) -0.1097(3) 0.110(3) Uani 1 1 d . . . H47A H 0.5944 0.6964 -0.0992 0.165 Uiso 1 1 calc R . . H47B H 0.5391 0.7014 -0.1083 0.165 Uiso 1 1 calc R . . H47C H 0.5581 0.6399 -0.1565 0.165 Uiso 1 1 calc R . . C472 C 0.5246(3) 0.5471(6) -0.0715(4) 0.124(3) Uani 1 1 d . . . H47D H 0.4994 0.5834 -0.0665 0.186 Uiso 1 1 calc R . . H47E H 0.5286 0.5004 -0.0389 0.186 Uiso 1 1 calc R . . H47F H 0.5162 0.5261 -0.1196 0.186 Uiso 1 1 calc R . . C473 C 0.6104(2) 0.5412(4) -0.0625(3) 0.0819(17) Uani 1 1 d . . . H47G H 0.6395 0.5740 -0.0523 0.123 Uiso 1 1 calc R . . H47H H 0.6023 0.5197 -0.1104 0.123 Uiso 1 1 calc R . . H47I H 0.6152 0.4948 -0.0295 0.123 Uiso 1 1 calc R . . C51 C 0.80064(12) 0.67870(19) 0.24175(18) 0.0310(7) Uani 1 1 d . . . C52 C 0.81196(13) 0.7606(2) 0.2320(2) 0.0366(8) Uani 1 1 d . . . H52 H 0.7908 0.8036 0.2349 0.044 Uiso 1 1 calc R . . C53 C 0.85408(13) 0.78083(19) 0.21813(19) 0.0348(8) Uani 1 1 d . . . C54 C 0.88451(13) 0.7164(2) 0.21551(19) 0.0357(8) Uani 1 1 d . . . H54 H 0.9129 0.7291 0.2051 0.043 Uiso 1 1 calc R . . C55 C 0.87507(12) 0.63324(19) 0.22760(18) 0.0307(7) Uani 1 1 d . . . C56 C 0.83343(12) 0.61621(18) 0.24187(17) 0.0293(7) Uani 1 1 d . . . O56 O 0.81974(8) 0.53663(12) 0.25537(12) 0.0300(5) Uani 1 1 d . . . C57 C 0.86505(15) 0.8711(2) 0.2019(2) 0.0429(9) Uani 1 1 d . . . C571 C 0.8492(4) 0.8821(3) 0.1229(3) 0.124(3) Uani 1 1 d . . . H57A H 0.8154 0.8703 0.1042 0.186 Uiso 1 1 calc R . . H57B H 0.8668 0.8438 0.1021 0.186 Uiso 1 1 calc R . . H57C H 0.8553 0.9392 0.1114 0.186 Uiso 1 1 calc R . . C572 C 0.9161(2) 0.8895(3) 0.2300(6) 0.168(5) Uani 1 1 d . . . H57D H 0.9340 0.8494 0.2114 0.252 Uiso 1 1 calc R . . H57E H 0.9261 0.8857 0.2813 0.252 Uiso 1 1 calc R . . H57F H 0.9222 0.9456 0.2161 0.252 Uiso 1 1 calc R . . C573 C 0.8378(3) 0.9333(3) 0.2302(4) 0.099(2) Uani 1 1 d . . . H57G H 0.8039 0.9211 0.2117 0.149 Uiso 1 1 calc R . . H57H H 0.8439 0.9891 0.2158 0.149 Uiso 1 1 calc R . . H57I H 0.8477 0.9300 0.2814 0.149 Uiso 1 1 calc R . . C58 C 0.90949(13) 0.56511(19) 0.22275(19) 0.0339(8) Uani 1 1 d . . . C581 C 0.91969(16) 0.5711(2) 0.1526(2) 0.0475(10) Uani 1 1 d . . . H58A H 0.9418 0.5272 0.1496 0.071 Uiso 1 1 calc R . . H58B H 0.9337 0.6253 0.1488 0.071 Uiso 1 1 calc R . . H58C H 0.8902 0.5647 0.1143 0.071 Uiso 1 1 calc R . . C582 C 0.95566(13) 0.5753(2) 0.2835(2) 0.0447(9) Uani 1 1 d . . . H58D H 0.9779 0.5316 0.2807 0.067 Uiso 1 1 calc R . . H58E H 0.9489 0.5712 0.3282 0.067 Uiso 1 1 calc R . . H58F H 0.9695 0.6296 0.2800 0.067 Uiso 1 1 calc R . . C61 C 0.83158(12) 0.39133(19) 0.26102(17) 0.0284(7) Uani 1 1 d . . . C62 C 0.85692(12) 0.32207(19) 0.25199(18) 0.0318(7) Uani 1 1 d . . . H62 H 0.8464 0.2686 0.2603 0.038 Uiso 1 1 calc R . . C63 C 0.89738(12) 0.32914(19) 0.23112(18) 0.0315(7) Uani 1 1 d . . . C64 C 0.91304(13) 0.40837(19) 0.22170(18) 0.0329(8) Uani 1 1 d . . . H64 H 0.9413 0.4140 0.2093 0.039 Uiso 1 1 calc R . . C65 C 0.88873(12) 0.47985(19) 0.22985(17) 0.0297(7) Uani 1 1 d . . . C66 C 0.84785(12) 0.47065(18) 0.24767(17) 0.0291(7) Uani 1 1 d . . . C67 C 0.92640(13) 0.2526(2) 0.2242(2) 0.0355(8) Uani 1 1 d . . . C671 C 0.96402(17) 0.2385(3) 0.2941(2) 0.0586(12) Uani 1 1 d . . . H67A H 0.9830 0.1900 0.2907 0.088 Uiso 1 1 calc R . . H67B H 0.9488 0.2292 0.3305 0.088 Uiso 1 1 calc R . . H67C H 0.9845 0.2874 0.3060 0.088 Uiso 1 1 calc R . . C672 C 0.95055(16) 0.2657(2) 0.1672(2) 0.0481(10) Uani 1 1 d . . . H67D H 0.9689 0.2163 0.1639 0.072 Uiso 1 1 calc R . . H67E H 0.9716 0.3138 0.1793 0.072 Uiso 1 1 calc R . . H67F H 0.9265 0.2755 0.1221 0.072 Uiso 1 1 calc R . . C673 C 0.89532(17) 0.1755(2) 0.2042(3) 0.0592(12) Uani 1 1 d . . . H67G H 0.9148 0.1279 0.2003 0.089 Uiso 1 1 calc R . . H67H H 0.8711 0.1848 0.1591 0.089 Uiso 1 1 calc R . . H67I H 0.8801 0.1643 0.2403 0.089 Uiso 1 1 calc R . . C71 C 0.71202(13) 0.2841(2) 0.3641(2) 0.0366(8) Uani 1 1 d . . . C72 C 0.68131(13) 0.3205(2) 0.3964(2) 0.0372(8) Uani 1 1 d . . . C73 C 0.65727(15) 0.2747(3) 0.4327(2) 0.0488(10) Uani 1 1 d . . . H73 H 0.6373 0.3013 0.4552 0.059 Uiso 1 1 calc R . . C74 C 0.66261(17) 0.1892(3) 0.4360(2) 0.0544(11) Uani 1 1 d . . . H74 H 0.6463 0.1567 0.4608 0.065 Uiso 1 1 calc R . . C75 C 0.69152(16) 0.1519(2) 0.4032(2) 0.0532(11) Uani 1 1 d . . . H75 H 0.6946 0.0933 0.4050 0.064 Uiso 1 1 calc R . . C76 C 0.71656(15) 0.1977(2) 0.3672(2) 0.0462(10) Uani 1 1 d . . . H76 H 0.7365 0.1705 0.3449 0.055 Uiso 1 1 calc R . . O72 O 0.67759(9) 0.40759(14) 0.39418(13) 0.0372(6) Uani 1 1 d . . . C81 C 0.64166(13) 0.5281(2) 0.33354(19) 0.0363(8) Uani 1 1 d . . . C82 C 0.63962(13) 0.4422(2) 0.34444(19) 0.0366(8) Uani 1 1 d . . . C83 C 0.60029(15) 0.3982(3) 0.3068(2) 0.0494(10) Uani 1 1 d . . . H83 H 0.5988 0.3400 0.3131 0.059 Uiso 1 1 calc R . . C84 C 0.56272(16) 0.4393(3) 0.2597(3) 0.0620(13) Uani 1 1 d . . . H84 H 0.5354 0.4091 0.2344 0.074 Uiso 1 1 calc R . . C85 C 0.56493(16) 0.5241(3) 0.2494(3) 0.0603(12) Uani 1 1 d . . . H85 H 0.5394 0.5519 0.2168 0.072 Uiso 1 1 calc R . . C86 C 0.60440(14) 0.5678(3) 0.2868(2) 0.0469(9) Uani 1 1 d . . . H86 H 0.6058 0.6260 0.2803 0.056 Uiso 1 1 calc R . . O1A O 0.6906(3) 0.6187(3) 0.5865(4) 0.163(3) Uani 1 1 d . . . H1A H 0.6861 0.6694 0.5772 0.244 Uiso 1 1 calc R . . C2A C 0.6459(4) 0.5769(7) 0.5712(6) 0.183(6) Uani 1 1 d . . . H2A1 H 0.6522 0.5248 0.5986 0.220 Uiso 1 1 calc R . . H2A2 H 0.6261 0.6115 0.5920 0.220 Uiso 1 1 calc R . . C3A C 0.6169(5) 0.5549(12) 0.5041(5) 0.284(11) Uani 1 1 d . . . H3A1 H 0.5882 0.5279 0.5079 0.426 Uiso 1 1 calc R . . H3A2 H 0.6339 0.5166 0.4824 0.426 Uiso 1 1 calc R . . H3A3 H 0.6083 0.6048 0.4751 0.426 Uiso 1 1 calc R . . O1B O 0.7067(2) 0.7089(4) 0.4764(3) 0.124(2) Uani 1 1 d . . . H1B H 0.6855 0.6881 0.4910 0.186 Uiso 1 1 calc R . . C2B C 0.7134(4) 0.7880(5) 0.4969(5) 0.135(3) Uani 1 1 d . . . H2B1 H 0.6896 0.8040 0.5199 0.162 Uiso 1 1 calc R . . H2B2 H 0.7090 0.8239 0.4553 0.162 Uiso 1 1 calc R . . C3B C 0.7613(4) 0.8010(6) 0.5460(4) 0.142(4) Uani 1 1 d . . . H3B1 H 0.7668 0.8605 0.5551 0.212 Uiso 1 1 calc R . . H3B2 H 0.7849 0.7791 0.5254 0.212 Uiso 1 1 calc R . . H3B3 H 0.7641 0.7722 0.5902 0.212 Uiso 1 1 calc R . . O1C O 0.7418(2) 0.3514(3) 0.1054(3) 0.1072(15) Uani 1 1 d . . . H1C H 0.7435 0.3000 0.1123 0.161 Uiso 1 1 calc R . . C2C C 0.7772(3) 0.3767(4) 0.0729(4) 0.101(2) Uani 1 1 d . . . H2C1 H 0.7729 0.3460 0.0287 0.122 Uiso 1 1 calc R . . H2C2 H 0.8093 0.3649 0.1047 0.122 Uiso 1 1 calc R . . C3C C 0.7712(4) 0.4685(5) 0.0587(4) 0.138(3) Uani 1 1 d . . . H3C1 H 0.7947 0.4875 0.0368 0.206 Uiso 1 1 calc R . . H3C2 H 0.7757 0.4982 0.1029 0.206 Uiso 1 1 calc R . . H3C3 H 0.7394 0.4794 0.0272 0.206 Uiso 1 1 calc R . . O1D O 0.7580(4) 0.3052(3) 0.6540(3) 0.175(3) Uani 1 1 d . . . H1D H 0.7644 0.2989 0.6975 0.263 Uiso 1 1 calc R . . C2D C 0.7454(3) 0.3865(5) 0.6368(6) 0.146(4) Uani 1 1 d . . . H2D1 H 0.7633 0.4235 0.6751 0.176 Uiso 1 1 calc R . . H2D2 H 0.7113 0.3940 0.6303 0.176 Uiso 1 1 calc R . . C3D C 0.7558(4) 0.4072(5) 0.5728(5) 0.149(4) Uani 1 1 d . . . H3D1 H 0.7463 0.4646 0.5598 0.223 Uiso 1 1 calc R . . H3D2 H 0.7383 0.3699 0.5353 0.223 Uiso 1 1 calc R . . H3D3 H 0.7897 0.4011 0.5800 0.223 Uiso 1 1 calc R . . O1E O 0.68960(14) 0.4602(2) 0.1565(2) 0.0801(11) Uani 1 1 d . . . H1E H 0.7085 0.4310 0.1428 0.120 Uiso 1 1 calc R . . C2E C 0.6553(3) 0.4096(4) 0.1694(4) 0.096(2) Uani 1 1 d . . . H2E1 H 0.6401 0.4407 0.1993 0.115 Uiso 1 1 calc R . . H2E2 H 0.6713 0.3611 0.1967 0.115 Uiso 1 1 calc R . . C3E C 0.6179(3) 0.3789(5) 0.1081(4) 0.117(3) Uani 1 1 d . . . H3E1 H 0.5957 0.3450 0.1238 0.175 Uiso 1 1 calc R . . H3E2 H 0.6320 0.3453 0.0790 0.175 Uiso 1 1 calc R . . H3E3 H 0.6012 0.4260 0.0808 0.175 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0247(19) 0.0209(15) 0.0455(19) 0.0015(14) 0.0111(15) 0.0007(13) O1 0.0297(13) 0.0239(11) 0.0480(14) -0.0024(10) 0.0144(11) -0.0018(9) N11 0.0251(17) 0.0344(15) 0.0563(19) -0.0127(13) 0.0125(14) -0.0035(12) N12 0.0270(16) 0.0238(13) 0.0487(17) -0.0062(12) 0.0110(13) -0.0008(11) C2 0.039(2) 0.0262(18) 0.048(2) 0.0005(15) 0.0112(17) 0.0112(15) O2 0.057(2) 0.0329(17) 0.163(4) 0.002(2) -0.025(2) 0.0091(15) N21 0.0326(19) 0.0259(15) 0.082(2) 0.0103(15) 0.0028(17) 0.0048(13) N22 0.0352(19) 0.0281(15) 0.064(2) 0.0035(14) 0.0029(15) 0.0106(13) C3 0.031(2) 0.0278(17) 0.0432(19) 0.0018(14) 0.0131(15) 0.0059(14) O3 0.0381(16) 0.0306(13) 0.0703(18) 0.0129(12) 0.0130(13) 0.0077(11) N31 0.0306(18) 0.0256(14) 0.061(2) 0.0081(13) 0.0095(14) 0.0054(12) N32 0.0287(17) 0.0270(14) 0.0532(18) 0.0116(13) 0.0148(14) 0.0045(12) C4 0.0264(19) 0.0236(16) 0.050(2) 0.0044(14) 0.0131(16) 0.0007(13) O4 0.0512(18) 0.0234(12) 0.085(2) -0.0010(12) 0.0390(16) -0.0005(11) N41 0.0277(16) 0.0216(13) 0.0530(18) 0.0009(12) 0.0185(13) -0.0004(11) N42 0.0353(18) 0.0237(13) 0.064(2) 0.0055(13) 0.0269(15) 0.0017(12) C11 0.0241(18) 0.0266(16) 0.0400(18) 0.0015(13) 0.0072(14) -0.0019(13) C12 0.030(2) 0.0224(15) 0.0423(19) 0.0005(13) 0.0074(15) -0.0031(13) C13 0.0290(19) 0.0227(15) 0.0390(18) 0.0021(13) 0.0050(15) 0.0010(13) C14 0.0244(19) 0.0269(16) 0.0442(19) 0.0012(14) 0.0062(15) -0.0002(13) C15 0.0270(19) 0.0208(15) 0.0380(18) 0.0004(12) 0.0079(14) -0.0005(13) C16 0.0287(19) 0.0192(15) 0.0402(18) 0.0007(13) 0.0094(14) 0.0041(13) O16 0.0248(13) 0.0192(11) 0.0554(15) -0.0001(10) 0.0071(11) 0.0017(9) C17 0.032(2) 0.0214(15) 0.050(2) 0.0045(14) 0.0072(16) 0.0023(14) C171 0.042(2) 0.0318(18) 0.053(2) 0.0086(16) 0.0010(18) 0.0041(16) C172 0.042(2) 0.0214(17) 0.081(3) 0.0086(17) 0.005(2) 0.0013(15) C173 0.048(3) 0.0309(18) 0.065(3) 0.0015(17) 0.017(2) 0.0130(17) C18 0.0283(19) 0.0210(15) 0.046(2) 0.0012(13) 0.0101(15) -0.0012(13) C181 0.034(2) 0.0244(16) 0.049(2) -0.0015(14) 0.0016(16) -0.0010(14) C182 0.038(2) 0.0298(17) 0.059(2) -0.0009(16) 0.0228(18) -0.0038(15) C21 0.035(2) 0.0256(16) 0.046(2) 0.0014(14) 0.0116(16) 0.0038(14) C22 0.044(2) 0.0191(16) 0.056(2) 0.0024(15) 0.0102(18) 0.0032(15) C23 0.048(3) 0.0232(17) 0.055(2) 0.0021(15) 0.0094(19) 0.0007(16) C24 0.034(2) 0.0216(16) 0.052(2) 0.0038(14) 0.0085(16) -0.0036(14) C25 0.033(2) 0.0218(15) 0.0423(19) 0.0028(13) 0.0112(15) 0.0015(13) C26 0.032(2) 0.0202(15) 0.0432(19) -0.0012(13) 0.0107(15) -0.0001(13) C27 0.067(3) 0.0212(18) 0.081(3) 0.0077(18) -0.004(2) -0.0076(18) C31 0.034(2) 0.0359(18) 0.046(2) 0.0046(15) 0.0106(16) 0.0135(15) C32 0.043(2) 0.0363(19) 0.051(2) 0.0042(16) 0.0153(18) 0.0149(17) C33 0.048(3) 0.041(2) 0.052(2) 0.0090(17) 0.0187(19) 0.0232(18) C34 0.040(2) 0.049(2) 0.047(2) 0.0110(18) 0.0110(18) 0.0229(18) C35 0.035(2) 0.049(2) 0.043(2) 0.0066(17) 0.0132(17) 0.0129(17) C36 0.034(2) 0.0337(18) 0.045(2) 0.0057(15) 0.0147(16) 0.0131(15) O36 0.0303(14) 0.0325(12) 0.0464(14) 0.0037(10) 0.0076(11) 0.0108(10) C37 0.062(3) 0.042(2) 0.075(3) 0.010(2) 0.020(2) 0.026(2) C371 0.093(5) 0.054(3) 0.119(5) 0.016(3) 0.001(4) 0.042(3) C372 0.181(9) 0.059(4) 0.316(14) 0.086(6) 0.173(10) 0.054(5) C373 0.127(6) 0.060(3) 0.103(5) -0.020(3) -0.002(4) 0.051(4) C38 0.033(2) 0.050(2) 0.054(2) 0.0016(18) 0.0115(18) 0.0120(17) C381 0.039(3) 0.070(3) 0.071(3) -0.001(2) 0.001(2) 0.020(2) C382 0.037(3) 0.060(3) 0.082(3) 0.001(2) 0.028(2) 0.008(2) C41 0.029(2) 0.0345(18) 0.052(2) 0.0023(16) 0.0098(17) 0.0040(15) C42 0.039(2) 0.040(2) 0.058(2) -0.0030(18) 0.0141(19) 0.0043(17) C43 0.045(3) 0.053(2) 0.050(2) -0.0046(18) 0.0090(19) 0.0047(19) C44 0.036(2) 0.060(3) 0.049(2) -0.0001(19) 0.0026(18) 0.0080(19) C45 0.033(2) 0.043(2) 0.051(2) 0.0032(17) 0.0123(17) 0.0079(16) C46 0.033(2) 0.0362(18) 0.046(2) 0.0007(15) 0.0110(16) 0.0025(15) C47 0.067(3) 0.068(3) 0.055(3) -0.013(2) 0.010(2) 0.008(2) C471 0.172(8) 0.103(5) 0.057(3) 0.013(3) 0.038(4) 0.062(5) C472 0.093(5) 0.190(8) 0.080(4) -0.065(5) 0.013(4) -0.039(5) C473 0.095(4) 0.083(4) 0.062(3) -0.018(3) 0.016(3) 0.026(3) C51 0.0265(19) 0.0253(16) 0.0424(19) 0.0045(13) 0.0127(15) 0.0025(13) C52 0.033(2) 0.0259(16) 0.052(2) 0.0051(15) 0.0144(17) 0.0047(14) C53 0.039(2) 0.0220(16) 0.045(2) 0.0028(14) 0.0135(16) -0.0014(14) C54 0.034(2) 0.0270(16) 0.050(2) 0.0022(14) 0.0191(17) -0.0039(14) C55 0.0308(19) 0.0250(16) 0.0375(18) 0.0021(13) 0.0121(15) -0.0012(13) C56 0.0297(19) 0.0205(15) 0.0393(18) 0.0024(13) 0.0128(14) -0.0004(13) O56 0.0261(13) 0.0193(10) 0.0477(13) 0.0030(9) 0.0159(10) 0.0027(9) C57 0.047(2) 0.0233(17) 0.064(2) 0.0105(16) 0.025(2) 0.0012(15) C571 0.258(11) 0.047(3) 0.085(4) 0.022(3) 0.080(6) -0.015(4) C572 0.065(4) 0.042(3) 0.350(14) 0.070(5) -0.005(6) -0.025(3) C573 0.164(7) 0.024(2) 0.160(6) -0.006(3) 0.125(6) -0.010(3) C58 0.031(2) 0.0248(16) 0.051(2) 0.0017(14) 0.0191(16) -0.0018(14) C581 0.064(3) 0.0301(18) 0.064(3) 0.0004(17) 0.042(2) -0.0009(18) C582 0.028(2) 0.0292(17) 0.076(3) -0.0026(17) 0.0137(19) -0.0030(15) C61 0.0227(18) 0.0239(15) 0.0394(18) 0.0007(13) 0.0107(14) -0.0011(12) C62 0.0299(19) 0.0214(15) 0.046(2) -0.0003(13) 0.0138(15) 0.0011(13) C63 0.0276(19) 0.0269(16) 0.0404(19) -0.0011(13) 0.0109(15) 0.0018(13) C64 0.0285(19) 0.0273(16) 0.046(2) -0.0025(14) 0.0152(15) -0.0001(14) C65 0.0289(19) 0.0237(15) 0.0387(18) 0.0008(13) 0.0135(15) 0.0010(13) C66 0.0236(18) 0.0212(15) 0.0413(18) -0.0009(13) 0.0081(14) 0.0026(12) C67 0.036(2) 0.0238(16) 0.051(2) 0.0018(14) 0.0197(17) 0.0056(14) C671 0.058(3) 0.062(3) 0.056(3) 0.009(2) 0.018(2) 0.032(2) C672 0.059(3) 0.0350(19) 0.062(3) 0.0023(17) 0.035(2) 0.0135(18) C673 0.056(3) 0.030(2) 0.100(4) -0.010(2) 0.037(3) 0.0002(18) C71 0.032(2) 0.0309(17) 0.048(2) 0.0046(15) 0.0137(16) -0.0048(14) C72 0.030(2) 0.0336(18) 0.048(2) 0.0022(15) 0.0119(16) -0.0052(15) C73 0.047(3) 0.050(2) 0.054(2) 0.0023(18) 0.021(2) -0.0074(19) C74 0.057(3) 0.052(2) 0.061(3) 0.008(2) 0.030(2) -0.013(2) C75 0.056(3) 0.035(2) 0.068(3) 0.0130(18) 0.016(2) -0.0115(18) C76 0.046(2) 0.0310(18) 0.065(3) 0.0062(17) 0.021(2) -0.0047(16) O72 0.0280(14) 0.0363(13) 0.0474(14) 0.0001(11) 0.0117(11) -0.0004(10) C81 0.027(2) 0.0355(18) 0.048(2) -0.0029(15) 0.0137(16) -0.0022(15) C82 0.0241(19) 0.044(2) 0.043(2) -0.0022(15) 0.0119(15) -0.0031(15) C83 0.040(2) 0.043(2) 0.062(3) 0.0008(18) 0.011(2) -0.0149(18) C84 0.038(3) 0.058(3) 0.077(3) 0.004(2) -0.003(2) -0.018(2) C85 0.035(2) 0.063(3) 0.071(3) 0.011(2) -0.001(2) -0.004(2) C86 0.034(2) 0.046(2) 0.059(2) 0.0066(18) 0.0105(18) 0.0010(17) O1A 0.243(8) 0.104(4) 0.192(6) -0.081(4) 0.141(6) -0.094(5) C2A 0.228(13) 0.191(10) 0.178(10) -0.087(8) 0.132(10) -0.119(10) C3A 0.222(15) 0.56(3) 0.097(7) -0.117(13) 0.088(9) -0.151(18) O1B 0.106(4) 0.171(5) 0.098(4) -0.055(4) 0.035(3) 0.037(4) C2B 0.199(11) 0.101(6) 0.127(7) 0.047(5) 0.082(8) 0.041(6) C3B 0.220(11) 0.141(7) 0.078(5) -0.036(5) 0.067(6) -0.069(7) O1C 0.128(4) 0.093(3) 0.106(3) -0.017(3) 0.043(3) 0.014(3) C2C 0.126(6) 0.100(5) 0.072(4) -0.007(3) 0.022(4) 0.016(4) C3C 0.180(9) 0.114(6) 0.098(6) 0.004(5) 0.011(6) 0.008(6) O1D 0.302(10) 0.083(3) 0.116(4) 0.016(3) 0.026(6) 0.008(5) C2D 0.128(7) 0.094(5) 0.219(11) 0.077(6) 0.056(7) 0.020(5) C3D 0.167(9) 0.112(6) 0.135(8) 0.028(6) -0.001(7) -0.022(6) O1E 0.078(3) 0.0518(19) 0.110(3) -0.0046(19) 0.028(2) 0.0094(18) C2E 0.119(6) 0.085(4) 0.088(4) 0.002(3) 0.039(4) -0.015(4) C3E 0.127(7) 0.114(6) 0.100(5) 0.017(4) 0.020(5) -0.029(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 O1 1.251(4) . ? C1 N12 1.352(4) . ? C1 N11 1.355(4) . ? N11 C81 1.426(5) . ? N11 H11 0.8800 . ? N12 C11 1.416(4) . ? N12 H12 0.8800 . ? C2 O2 1.192(5) . ? C2 N21 1.358(5) . ? C2 N22 1.370(5) . ? N21 C21 1.400(5) . ? N21 H21 0.8800 . ? N22 C31 1.408(5) . ? N22 H22 0.8800 . ? C3 O3 1.236(4) . ? C3 N31 1.361(5) . ? C3 N32 1.375(5) . ? N31 C41 1.430(5) . ? N31 H31 0.8800 . ? N32 C51 1.416(4) . ? N32 H32 0.8800 . ? C4 O4 1.230(4) . ? C4 N41 1.373(4) . ? C4 N42 1.376(4) . ? N41 C61 1.411(4) . ? N41 H41 0.8800 . ? N42 C71 1.407(4) . ? N42 H42 0.8800 . ? C11 C12 1.386(5) . ? C11 C16 1.394(4) . ? C12 C13 1.398(5) . ? C12 H12A 0.9500 . ? C13 C14 1.395(5) . ? C13 C17 1.540(4) . ? C14 C15 1.402(4) . ? C14 H14 0.9500 . ? C15 C16 1.384(5) . ? C15 C18 1.536(4) . ? C16 O16 1.387(4) . ? O16 C26 1.381(4) . ? C17 C171 1.528(5) . ? C17 C172 1.538(5) . ? C17 C173 1.539(6) . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? C173 H17G 0.9800 . ? C173 H17H 0.9800 . ? C173 H17I 0.9800 . ? C18 C25 1.533(4) . ? C18 C182 1.540(5) . ? C18 C181 1.540(5) . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C182 H18D 0.9800 . ? C182 H18E 0.9800 . ? C182 H18F 0.9800 . ? C21 C22 1.395(5) . ? C21 C26 1.406(5) . ? C22 C23 1.391(6) . ? C22 H22A 0.9500 . ? C23 C24 1.392(5) . ? C23 C27 1.543(5) . ? C24 C25 1.404(5) . ? C24 H24 0.9500 . ? C25 C26 1.378(5) . ? C27 C274 1.487(5) . ? C27 C276 1.489(5) . ? C27 C271 1.490(5) . ? C27 C272 1.491(5) . ? C27 C275 1.532(5) . ? C27 C273 1.551(5) . ? C271 H27A 0.9800 . ? C271 H27B 0.9800 . ? C271 H27C 0.9800 . ? C272 H27D 0.9800 . ? C272 H27E 0.9800 . ? C272 H27F 0.9800 . ? C273 H27G 0.9800 . ? C273 H27H 0.9800 . ? C273 H27I 0.9800 . ? C274 H27J 0.9800 . ? C274 H27K 0.9800 . ? C274 H27L 0.9800 . ? C275 H27M 0.9800 . ? C275 H27N 0.9800 . ? C275 H27O 0.9800 . ? C276 H27P 0.9800 . ? C276 H27Q 0.9800 . ? C276 H27R 0.9800 . ? C31 C32 1.387(5) . ? C31 C36 1.405(5) . ? C32 C33 1.399(6) . ? C32 H32A 0.9500 . ? C33 C34 1.386(6) . ? C33 C37 1.536(5) . ? C34 C35 1.393(5) . ? C34 H34 0.9500 . ? C35 C36 1.385(5) . ? C35 C38 1.535(6) . ? C36 O36 1.402(4) . ? O36 C46 1.394(4) . ? C37 C372 1.508(9) . ? C37 C371 1.512(7) . ? C37 C373 1.521(8) . ? C371 H37A 0.9800 . ? C371 H37B 0.9800 . ? C371 H37C 0.9800 . ? C372 H37D 0.9800 . ? C372 H37E 0.9800 . ? C372 H37F 0.9800 . ? C373 H37G 0.9800 . ? C373 H37H 0.9800 . ? C373 H37I 0.9800 . ? C38 C381 1.528(6) . ? C38 C45 1.535(5) . ? C38 C382 1.540(6) . ? C381 H38A 0.9800 . ? C381 H38B 0.9800 . ? C381 H38C 0.9800 . ? C382 H38D 0.9800 . ? C382 H38E 0.9800 . ? C382 H38F 0.9800 . ? C41 C46 1.386(5) . ? C41 C42 1.400(6) . ? C42 C43 1.399(6) . ? C42 H42A 0.9500 . ? C43 C44 1.406(6) . ? C43 C47 1.545(6) . ? C44 C45 1.396(6) . ? C44 H44 0.9500 . ? C45 C46 1.397(5) . ? C47 C472 1.518(9) . ? C47 C473 1.519(7) . ? C47 C471 1.534(8) . ? C471 H47A 0.9800 . ? C471 H47B 0.9800 . ? C471 H47C 0.9800 . ? C472 H47D 0.9800 . ? C472 H47E 0.9800 . ? C472 H47F 0.9800 . ? C473 H47G 0.9800 . ? C473 H47H 0.9800 . ? C473 H47I 0.9800 . ? C51 C52 1.393(5) . ? C51 C56 1.402(5) . ? C52 C53 1.401(5) . ? C52 H52 0.9500 . ? C53 C54 1.389(5) . ? C53 C57 1.549(4) . ? C54 C55 1.407(4) . ? C54 H54 0.9500 . ? C55 C56 1.380(5) . ? C55 C58 1.525(5) . ? C56 O56 1.398(4) . ? O56 C66 1.391(4) . ? C57 C572 1.481(8) . ? C57 C573 1.505(6) . ? C57 C571 1.519(7) . ? C571 H57A 0.9800 . ? C571 H57B 0.9800 . ? C571 H57C 0.9800 . ? C572 H57D 0.9800 . ? C572 H57E 0.9800 . ? C572 H57F 0.9800 . ? C573 H57G 0.9800 . ? C573 H57H 0.9800 . ? C573 H57I 0.9800 . ? C58 C581 1.529(5) . ? C58 C65 1.532(4) . ? C58 C582 1.541(5) . ? C581 H58A 0.9800 . ? C581 H58B 0.9800 . ? C581 H58C 0.9800 . ? C582 H58D 0.9800 . ? C582 H58E 0.9800 . ? C582 H58F 0.9800 . ? C61 C62 1.390(4) . ? C61 C66 1.422(4) . ? C62 C63 1.393(5) . ? C62 H62 0.9500 . ? C63 C64 1.393(5) . ? C63 C67 1.537(4) . ? C64 C65 1.397(4) . ? C64 H64 0.9500 . ? C65 C66 1.375(5) . ? C67 C671 1.520(6) . ? C67 C673 1.529(5) . ? C67 C672 1.538(5) . ? C671 H67A 0.9800 . ? C671 H67B 0.9800 . ? C671 H67C 0.9800 . ? C672 H67D 0.9800 . ? C672 H67E 0.9800 . ? C672 H67F 0.9800 . ? C673 H67G 0.9800 . ? C673 H67H 0.9800 . ? C673 H67I 0.9800 . ? C71 C72 1.399(5) . ? C71 C76 1.401(5) . ? C72 C73 1.381(5) . ? C72 O72 1.409(4) . ? C73 C74 1.388(6) . ? C73 H73 0.9500 . ? C74 C75 1.370(6) . ? C74 H74 0.9500 . ? C75 C76 1.395(6) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? O72 C82 1.377(4) . ? C81 C86 1.372(5) . ? C81 C82 1.408(5) . ? C82 C83 1.379(5) . ? C83 C84 1.392(6) . ? C83 H83 0.9500 . ? C84 C85 1.389(6) . ? C84 H84 0.9500 . ? C85 C86 1.379(6) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? O1A C2A 1.438(11) . ? O1A H1A 0.8400 . ? C2A C3A 1.405(14) . ? C2A H2A1 0.9900 . ? C2A H2A2 0.9900 . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? O1B C2B 1.337(10) . ? O1B H1B 0.8400 . ? C2B C3B 1.481(13) . ? C2B H2B1 0.9900 . ? C2B H2B2 0.9900 . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? O1C C2C 1.455(9) . ? O1C H1C 0.8400 . ? C2C C3C 1.509(10) . ? C2C H2C1 0.9900 . ? C2C H2C2 0.9900 . ? C3C H3C1 0.9800 . ? C3C H3C2 0.9800 . ? C3C H3C3 0.9800 . ? O1D C2D 1.378(9) . ? O1D H1D 0.8400 . ? C2D C3D 1.446(13) . ? C2D H2D1 0.9900 . ? C2D H2D2 0.9900 . ? C3D H3D1 0.9800 . ? C3D H3D2 0.9800 . ? C3D H3D3 0.9800 . ? O1E C2E 1.391(7) . ? O1E H1E 0.8400 . ? C2E C3E 1.467(10) . ? C2E H2E1 0.9900 . ? C2E H2E2 0.9900 . ? C3E H3E1 0.9800 . ? C3E H3E2 0.9800 . ? C3E H3E3 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 O1 C1 N12 122.5(3) . . ? O1 C1 N11 122.3(3) . . ? N12 C1 N11 115.3(3) . . ? C1 N11 C81 123.0(3) . . ? C1 N11 H11 118.5 . . ? C81 N11 H11 118.5 . . ? C1 N12 C11 125.4(3) . . ? C1 N12 H12 117.3 . . ? C11 N12 H12 117.3 . . ? O2 C2 N21 122.8(4) . . ? O2 C2 N22 124.5(4) . . ? N21 C2 N22 112.7(3) . . ? C2 N21 C21 129.8(3) . . ? C2 N21 H21 115.1 . . ? C21 N21 H21 115.1 . . ? C2 N22 C31 127.5(3) . . ? C2 N22 H22 116.3 . . ? C31 N22 H22 116.3 . . ? O3 C3 N31 122.5(3) . . ? O3 C3 N32 123.0(3) . . ? N31 C3 N32 114.5(3) . . ? C3 N31 C41 120.5(3) . . ? C3 N31 H31 119.8 . . ? C41 N31 H31 119.8 . . ? C3 N32 C51 122.3(3) . . ? C3 N32 H32 118.8 . . ? C51 N32 H32 118.8 . . ? O4 C4 N41 124.4(3) . . ? O4 C4 N42 123.4(3) . . ? N41 C4 N42 112.2(3) . . ? C4 N41 C61 126.8(3) . . ? C4 N41 H41 116.6 . . ? C61 N41 H41 116.6 . . ? C4 N42 C71 127.6(3) . . ? C4 N42 H42 116.2 . . ? C71 N42 H42 116.2 . . ? C12 C11 C16 119.3(3) . . ? C12 C11 N12 122.3(3) . . ? C16 C11 N12 118.0(3) . . ? C11 C12 C13 120.8(3) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C14 C13 C12 117.8(3) . . ? C14 C13 C17 119.7(3) . . ? C12 C13 C17 122.4(3) . . ? C13 C14 C15 123.1(3) . . ? C13 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C16 C15 C14 116.6(3) . . ? C16 C15 C18 122.0(3) . . ? C14 C15 C18 121.3(3) . . ? C15 C16 O16 123.4(3) . . ? C15 C16 C11 122.3(3) . . ? O16 C16 C11 114.3(3) . . ? C26 O16 C16 118.1(3) . . ? C171 C17 C172 107.9(3) . . ? C171 C17 C173 110.0(3) . . ? C172 C17 C173 107.8(3) . . ? C171 C17 C13 108.8(3) . . ? C172 C17 C13 112.4(3) . . ? C173 C17 C13 109.9(3) . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C17 C172 H17D 109.5 . . ? C17 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? C17 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? C17 C173 H17G 109.5 . . ? C17 C173 H17H 109.5 . . ? H17G C173 H17H 109.5 . . ? C17 C173 H17I 109.5 . . ? H17G C173 H17I 109.5 . . ? H17H C173 H17I 109.5 . . ? C25 C18 C15 110.1(3) . . ? C25 C18 C182 109.1(3) . . ? C15 C18 C182 109.8(3) . . ? C25 C18 C181 109.4(3) . . ? C15 C18 C181 109.1(3) . . ? C182 C18 C181 109.4(3) . . ? C18 C181 H18A 109.5 . . ? C18 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C18 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C18 C182 H18D 109.5 . . ? C18 C182 H18E 109.5 . . ? H18D C182 H18E 109.5 . . ? C18 C182 H18F 109.5 . . ? H18D C182 H18F 109.5 . . ? H18E C182 H18F 109.5 . . ? C22 C21 N21 126.1(3) . . ? C22 C21 C26 118.5(3) . . ? N21 C21 C26 115.4(3) . . ? C23 C22 C21 120.4(3) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 118.9(3) . . ? C22 C23 C27 119.5(3) . . ? C24 C23 C27 121.6(3) . . ? C23 C24 C25 122.6(3) . . ? C23 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C26 C25 C24 116.6(3) . . ? C26 C25 C18 121.8(3) . . ? C24 C25 C18 121.6(3) . . ? C25 C26 O16 124.1(3) . . ? C25 C26 C21 122.9(3) . . ? O16 C26 C21 113.0(3) . . ? C274 C27 C276 122.1(7) . . ? C274 C27 C271 128.0(6) . . ? C276 C27 C271 38.8(5) . . ? C274 C27 C272 28.9(4) . . ? C276 C27 C272 134.5(6) . . ? C271 C27 C272 117.2(6) . . ? C274 C27 C275 98.2(7) . . ? C276 C27 C275 96.1(8) . . ? C271 C27 C275 57.7(7) . . ? C272 C27 C275 71.5(7) . . ? C274 C27 C23 115.1(5) . . ? C276 C27 C23 115.3(5) . . ? C271 C27 C23 115.2(4) . . ? C272 C27 C23 110.1(4) . . ? C275 C27 C23 103.5(6) . . ? C274 C27 C273 75.4(6) . . ? C276 C27 C273 64.9(6) . . ? C271 C27 C273 102.4(5) . . ? C272 C27 C273 104.1(6) . . ? C275 C27 C273 149.5(7) . . ? C23 C27 C273 106.1(4) . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C27 C272 H27D 109.5 . . ? C27 C272 H27E 109.5 . . ? H27D C272 H27E 109.5 . . ? C27 C272 H27F 109.5 . . ? H27D C272 H27F 109.5 . . ? H27E C272 H27F 109.5 . . ? C27 C273 H27G 109.5 . . ? C27 C273 H27H 109.5 . . ? H27G C273 H27H 109.5 . . ? C27 C273 H27I 109.5 . . ? H27G C273 H27I 109.5 . . ? H27H C273 H27I 109.5 . . ? C27 C274 H27J 109.5 . . ? C27 C274 H27K 109.5 . . ? H27J C274 H27K 109.5 . . ? C27 C274 H27L 109.5 . . ? H27J C274 H27L 109.5 . . ? H27K C274 H27L 109.5 . . ? C27 C275 H27M 109.5 . . ? C27 C275 H27N 109.5 . . ? H27M C275 H27N 109.5 . . ? C27 C275 H27O 109.5 . . ? H27M C275 H27O 109.5 . . ? H27N C275 H27O 109.5 . . ? C27 C276 H27P 109.5 . . ? C27 C276 H27Q 109.5 . . ? H27P C276 H27Q 109.5 . . ? C27 C276 H27R 109.5 . . ? H27P C276 H27R 109.5 . . ? H27Q C276 H27R 109.5 . . ? C32 C31 C36 118.0(3) . . ? C32 C31 N22 124.9(4) . . ? C36 C31 N22 117.1(3) . . ? C31 C32 C33 121.3(4) . . ? C31 C32 H32A 119.3 . . ? C33 C32 H32A 119.3 . . ? C34 C33 C32 118.7(3) . . ? C34 C33 C37 121.9(4) . . ? C32 C33 C37 119.4(4) . . ? C33 C34 C35 121.9(4) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C36 C35 C34 117.9(4) . . ? C36 C35 C38 117.1(3) . . ? C34 C35 C38 125.0(4) . . ? C35 C36 O36 120.6(3) . . ? C35 C36 C31 122.2(3) . . ? O36 C36 C31 117.3(3) . . ? C46 O36 C36 113.7(3) . . ? C372 C37 C371 107.9(6) . . ? C372 C37 C373 112.2(6) . . ? C371 C37 C373 106.1(5) . . ? C372 C37 C33 108.1(4) . . ? C371 C37 C33 112.8(4) . . ? C373 C37 C33 109.7(4) . . ? C37 C371 H37A 109.5 . . ? C37 C371 H37B 109.5 . . ? H37A C371 H37B 109.5 . . ? C37 C371 H37C 109.5 . . ? H37A C371 H37C 109.5 . . ? H37B C371 H37C 109.5 . . ? C37 C372 H37D 109.5 . . ? C37 C372 H37E 109.5 . . ? H37D C372 H37E 109.5 . . ? C37 C372 H37F 109.5 . . ? H37D C372 H37F 109.5 . . ? H37E C372 H37F 109.5 . . ? C37 C373 H37G 109.5 . . ? C37 C373 H37H 109.5 . . ? H37G C373 H37H 109.5 . . ? C37 C373 H37I 109.5 . . ? H37G C373 H37I 109.5 . . ? H37H C373 H37I 109.5 . . ? C381 C38 C45 112.4(4) . . ? C381 C38 C35 112.2(3) . . ? C45 C38 C35 106.6(3) . . ? C381 C38 C382 108.9(4) . . ? C45 C38 C382 108.0(3) . . ? C35 C38 C382 108.7(3) . . ? C38 C381 H38A 109.5 . . ? C38 C381 H38B 109.5 . . ? H38A C381 H38B 109.5 . . ? C38 C381 H38C 109.5 . . ? H38A C381 H38C 109.5 . . ? H38B C381 H38C 109.5 . . ? C38 C382 H38D 109.5 . . ? C38 C382 H38E 109.5 . . ? H38D C382 H38E 109.5 . . ? C38 C382 H38F 109.5 . . ? H38D C382 H38F 109.5 . . ? H38E C382 H38F 109.5 . . ? C46 C41 C42 119.4(3) . . ? C46 C41 N31 122.5(3) . . ? C42 C41 N31 118.1(3) . . ? C43 C42 C41 121.6(4) . . ? C43 C42 H42A 119.2 . . ? C41 C42 H42A 119.2 . . ? C42 C43 C44 117.2(4) . . ? C42 C43 C47 121.3(4) . . ? C44 C43 C47 121.5(4) . . ? C45 C44 C43 122.3(4) . . ? C45 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? C44 C45 C46 118.4(3) . . ? C44 C45 C38 124.8(4) . . ? C46 C45 C38 116.8(3) . . ? C41 C46 O36 118.7(3) . . ? C41 C46 C45 120.9(3) . . ? O36 C46 C45 120.4(3) . . ? C472 C47 C473 111.0(5) . . ? C472 C47 C471 109.1(6) . . ? C473 C47 C471 105.4(5) . . ? C472 C47 C43 109.0(5) . . ? C473 C47 C43 112.8(4) . . ? C471 C47 C43 109.4(4) . . ? C47 C471 H47A 109.5 . . ? C47 C471 H47B 109.5 . . ? H47A C471 H47B 109.5 . . ? C47 C471 H47C 109.5 . . ? H47A C471 H47C 109.5 . . ? H47B C471 H47C 109.5 . . ? C47 C472 H47D 109.5 . . ? C47 C472 H47E 109.5 . . ? H47D C472 H47E 109.5 . . ? C47 C472 H47F 109.5 . . ? H47D C472 H47F 109.5 . . ? H47E C472 H47F 109.5 . . ? C47 C473 H47G 109.5 . . ? C47 C473 H47H 109.5 . . ? H47G C473 H47H 109.5 . . ? C47 C473 H47I 109.5 . . ? H47G C473 H47I 109.5 . . ? H47H C473 H47I 109.5 . . ? C52 C51 C56 119.0(3) . . ? C52 C51 N32 123.5(3) . . ? C56 C51 N32 117.3(3) . . ? C51 C52 C53 121.1(3) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C54 C53 C52 117.7(3) . . ? C54 C53 C57 121.0(3) . . ? C52 C53 C57 121.2(3) . . ? C53 C54 C55 122.7(3) . . ? C53 C54 H54 118.6 . . ? C55 C54 H54 118.6 . . ? C56 C55 C54 117.6(3) . . ? C56 C55 C58 122.1(3) . . ? C54 C55 C58 120.2(3) . . ? C55 C56 O56 123.7(3) . . ? C55 C56 C51 121.6(3) . . ? O56 C56 C51 114.7(3) . . ? C66 O56 C56 117.5(2) . . ? C572 C57 C573 109.3(6) . . ? C572 C57 C571 109.3(6) . . ? C573 C57 C571 106.4(5) . . ? C572 C57 C53 111.5(3) . . ? C573 C57 C53 112.1(3) . . ? C571 C57 C53 108.1(4) . . ? C57 C571 H57A 109.5 . . ? C57 C571 H57B 109.5 . . ? H57A C571 H57B 109.5 . . ? C57 C571 H57C 109.5 . . ? H57A C571 H57C 109.5 . . ? H57B C571 H57C 109.5 . . ? C57 C572 H57D 109.5 . . ? C57 C572 H57E 109.5 . . ? H57D C572 H57E 109.5 . . ? C57 C572 H57F 109.5 . . ? H57D C572 H57F 109.5 . . ? H57E C572 H57F 109.5 . . ? C57 C573 H57G 109.5 . . ? C57 C573 H57H 109.5 . . ? H57G C573 H57H 109.5 . . ? C57 C573 H57I 109.5 . . ? H57G C573 H57I 109.5 . . ? H57H C573 H57I 109.5 . . ? C55 C58 C581 109.7(3) . . ? C55 C58 C65 110.1(3) . . ? C581 C58 C65 109.9(3) . . ? C55 C58 C582 109.0(3) . . ? C581 C58 C582 110.0(3) . . ? C65 C58 C582 108.0(3) . . ? C58 C581 H58A 109.5 . . ? C58 C581 H58B 109.5 . . ? H58A C581 H58B 109.5 . . ? C58 C581 H58C 109.5 . . ? H58A C581 H58C 109.5 . . ? H58B C581 H58C 109.5 . . ? C58 C582 H58D 109.5 . . ? C58 C582 H58E 109.5 . . ? H58D C582 H58E 109.5 . . ? C58 C582 H58F 109.5 . . ? H58D C582 H58F 109.5 . . ? H58E C582 H58F 109.5 . . ? C62 C61 N41 124.5(3) . . ? C62 C61 C66 118.1(3) . . ? N41 C61 C66 117.4(3) . . ? C61 C62 C63 121.7(3) . . ? C61 C62 H62 119.2 . . ? C63 C62 H62 119.2 . . ? C64 C63 C62 118.1(3) . . ? C64 C63 C67 120.4(3) . . ? C62 C63 C67 121.4(3) . . ? C63 C64 C65 122.4(3) . . ? C63 C64 H64 118.8 . . ? C65 C64 H64 118.8 . . ? C66 C65 C64 118.1(3) . . ? C66 C65 C58 122.3(3) . . ? C64 C65 C58 119.5(3) . . ? C65 C66 O56 123.7(3) . . ? C65 C66 C61 121.6(3) . . ? O56 C66 C61 114.7(3) . . ? C671 C67 C673 109.7(3) . . ? C671 C67 C63 108.2(3) . . ? C673 C67 C63 111.5(3) . . ? C671 C67 C672 109.0(3) . . ? C673 C67 C672 107.4(3) . . ? C63 C67 C672 111.0(3) . . ? C67 C671 H67A 109.5 . . ? C67 C671 H67B 109.5 . . ? H67A C671 H67B 109.5 . . ? C67 C671 H67C 109.5 . . ? H67A C671 H67C 109.5 . . ? H67B C671 H67C 109.5 . . ? C67 C672 H67D 109.5 . . ? C67 C672 H67E 109.5 . . ? H67D C672 H67E 109.5 . . ? C67 C672 H67F 109.5 . . ? H67D C672 H67F 109.5 . . ? H67E C672 H67F 109.5 . . ? C67 C673 H67G 109.5 . . ? C67 C673 H67H 109.5 . . ? H67G C673 H67H 109.5 . . ? C67 C673 H67I 109.5 . . ? H67G C673 H67I 109.5 . . ? H67H C673 H67I 109.5 . . ? C72 C71 C76 117.7(3) . . ? C72 C71 N42 116.3(3) . . ? C76 C71 N42 125.9(3) . . ? C73 C72 C71 122.3(3) . . ? C73 C72 O72 120.1(3) . . ? C71 C72 O72 117.4(3) . . ? C72 C73 C74 119.2(4) . . ? C72 C73 H73 120.4 . . ? C74 C73 H73 120.4 . . ? C75 C74 C73 119.5(4) . . ? C75 C74 H74 120.2 . . ? C73 C74 H74 120.2 . . ? C74 C75 C76 121.9(4) . . ? C74 C75 H75 119.1 . . ? C76 C75 H75 119.1 . . ? C75 C76 C71 119.4(4) . . ? C75 C76 H76 120.3 . . ? C71 C76 H76 120.3 . . ? C82 O72 C72 117.8(3) . . ? C86 C81 C82 120.1(3) . . ? C86 C81 N11 120.0(3) . . ? C82 C81 N11 119.9(3) . . ? O72 C82 C83 124.0(3) . . ? O72 C82 C81 116.5(3) . . ? C83 C82 C81 119.4(4) . . ? C82 C83 C84 119.9(4) . . ? C82 C83 H83 120.1 . . ? C84 C83 H83 120.1 . . ? C85 C84 C83 120.4(4) . . ? C85 C84 H84 119.8 . . ? C83 C84 H84 119.8 . . ? C86 C85 C84 119.6(4) . . ? C86 C85 H85 120.2 . . ? C84 C85 H85 120.2 . . ? C81 C86 C85 120.6(4) . . ? C81 C86 H86 119.7 . . ? C85 C86 H86 119.7 . . ? C2A O1A H1A 109.5 . . ? C3A C2A O1A 125.6(10) . . ? C3A C2A H2A1 105.9 . . ? O1A C2A H2A1 105.9 . . ? C3A C2A H2A2 105.9 . . ? O1A C2A H2A2 105.9 . . ? H2A1 C2A H2A2 106.2 . . ? C2A C3A H3A1 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2B O1B H1B 109.5 . . ? O1B C2B C3B 111.3(8) . . ? O1B C2B H2B1 109.4 . . ? C3B C2B H2B1 109.4 . . ? O1B C2B H2B2 109.4 . . ? C3B C2B H2B2 109.4 . . ? H2B1 C2B H2B2 108.0 . . ? C2B C3B H3B1 109.5 . . ? C2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2C O1C H1C 109.5 . . ? O1C C2C C3C 107.5(7) . . ? O1C C2C H2C1 110.2 . . ? C3C C2C H2C1 110.2 . . ? O1C C2C H2C2 110.2 . . ? C3C C2C H2C2 110.2 . . ? H2C1 C2C H2C2 108.5 . . ? C2C C3C H3C1 109.5 . . ? C2C C3C H3C2 109.5 . . ? H3C1 C3C H3C2 109.5 . . ? C2C C3C H3C3 109.5 . . ? H3C1 C3C H3C3 109.5 . . ? H3C2 C3C H3C3 109.5 . . ? C2D O1D H1D 109.5 . . ? O1D C2D C3D 109.0(9) . . ? O1D C2D H2D1 109.9 . . ? C3D C2D H2D1 109.9 . . ? O1D C2D H2D2 109.9 . . ? C3D C2D H2D2 109.9 . . ? H2D1 C2D H2D2 108.3 . . ? C2D C3D H3D1 109.5 . . ? C2D C3D H3D2 109.5 . . ? H3D1 C3D H3D2 109.5 . . ? C2D C3D H3D3 109.5 . . ? H3D1 C3D H3D3 109.5 . . ? H3D2 C3D H3D3 109.5 . . ? C2E O1E H1E 109.5 . . ? O1E C2E C3E 117.0(6) . . ? O1E C2E H2E1 108.0 . . ? C3E C2E H2E1 108.0 . . ? O1E C2E H2E2 108.0 . . ? C3E C2E H2E2 108.0 . . ? H2E1 C2E H2E2 107.3 . . ? C2E C3E H3E1 109.5 . . ? C2E C3E H3E2 109.5 . . ? H3E1 C3E H3E2 109.5 . . ? C2E C3E H3E3 109.5 . . ? H3E1 C3E H3E3 109.5 . . ? H3E2 C3E H3E3 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 O1 C1 N11 C81 6.8(5) . . . . ? N12 C1 N11 C81 -174.8(3) . . . . ? O1 C1 N12 C11 -7.0(5) . . . . ? N11 C1 N12 C11 174.5(3) . . . . ? O2 C2 N21 C21 -10.9(8) . . . . ? N22 C2 N21 C21 171.6(4) . . . . ? O2 C2 N22 C31 7.8(7) . . . . ? N21 C2 N22 C31 -174.8(4) . . . . ? O3 C3 N31 C41 12.0(5) . . . . ? N32 C3 N31 C41 -170.0(3) . . . . ? O3 C3 N32 C51 -36.4(5) . . . . ? N31 C3 N32 C51 145.5(3) . . . . ? O4 C4 N41 C61 -8.8(6) . . . . ? N42 C4 N41 C61 171.6(3) . . . . ? O4 C4 N42 C71 8.7(6) . . . . ? N41 C4 N42 C71 -171.7(3) . . . . ? C1 N12 C11 C12 -53.0(5) . . . . ? C1 N12 C11 C16 133.3(3) . . . . ? C16 C11 C12 C13 0.4(5) . . . . ? N12 C11 C12 C13 -173.2(3) . . . . ? C11 C12 C13 C14 2.1(5) . . . . ? C11 C12 C13 C17 177.7(3) . . . . ? C12 C13 C14 C15 -1.6(5) . . . . ? C17 C13 C14 C15 -177.2(3) . . . . ? C13 C14 C15 C16 -1.5(5) . . . . ? C13 C14 C15 C18 174.6(3) . . . . ? C14 C15 C16 O16 -176.6(3) . . . . ? C18 C15 C16 O16 7.4(5) . . . . ? C14 C15 C16 C11 4.2(5) . . . . ? C18 C15 C16 C11 -171.8(3) . . . . ? C12 C11 C16 C15 -3.8(5) . . . . ? N12 C11 C16 C15 170.1(3) . . . . ? C12 C11 C16 O16 176.9(3) . . . . ? N12 C11 C16 O16 -9.2(4) . . . . ? C15 C16 O16 C26 -5.1(5) . . . . ? C11 C16 O16 C26 174.2(3) . . . . ? C14 C13 C17 C171 59.6(4) . . . . ? C12 C13 C17 C171 -115.8(4) . . . . ? C14 C13 C17 C172 179.1(3) . . . . ? C12 C13 C17 C172 3.6(5) . . . . ? C14 C13 C17 C173 -60.9(4) . . . . ? C12 C13 C17 C173 123.7(4) . . . . ? C16 C15 C18 C25 -2.5(4) . . . . ? C14 C15 C18 C25 -178.3(3) . . . . ? C16 C15 C18 C182 -122.6(4) . . . . ? C14 C15 C18 C182 61.6(4) . . . . ? C16 C15 C18 C181 117.6(4) . . . . ? C14 C15 C18 C181 -58.3(4) . . . . ? C2 N21 C21 C22 6.5(7) . . . . ? C2 N21 C21 C26 -171.7(4) . . . . ? N21 C21 C22 C23 -176.0(4) . . . . ? C26 C21 C22 C23 2.1(6) . . . . ? C21 C22 C23 C24 0.3(6) . . . . ? C21 C22 C23 C27 -178.6(4) . . . . ? C22 C23 C24 C25 -0.6(6) . . . . ? C27 C23 C24 C25 178.2(4) . . . . ? C23 C24 C25 C26 -1.5(6) . . . . ? C23 C24 C25 C18 176.3(4) . . . . ? C15 C18 C25 C26 -4.3(5) . . . . ? C182 C18 C25 C26 116.2(4) . . . . ? C181 C18 C25 C26 -124.2(4) . . . . ? C15 C18 C25 C24 178.0(3) . . . . ? C182 C18 C25 C24 -61.4(4) . . . . ? C181 C18 C25 C24 58.2(4) . . . . ? C24 C25 C26 O16 -175.3(3) . . . . ? C18 C25 C26 O16 7.0(5) . . . . ? C24 C25 C26 C21 4.0(5) . . . . ? C18 C25 C26 C21 -173.7(3) . . . . ? C16 O16 C26 C25 -2.2(5) . . . . ? C16 O16 C26 C21 178.4(3) . . . . ? C22 C21 C26 C25 -4.4(6) . . . . ? N21 C21 C26 C25 173.9(3) . . . . ? C22 C21 C26 O16 175.0(3) . . . . ? N21 C21 C26 O16 -6.7(5) . . . . ? C22 C23 C27 C274 -23.3(7) . . . . ? C24 C23 C27 C274 157.9(6) . . . . ? C22 C23 C27 C276 127.3(7) . . . . ? C24 C23 C27 C276 -51.5(8) . . . . ? C22 C23 C27 C271 170.4(5) . . . . ? C24 C23 C27 C271 -8.4(7) . . . . ? C22 C23 C27 C272 -54.2(7) . . . . ? C24 C23 C27 C272 126.9(6) . . . . ? C22 C23 C27 C275 -129.2(7) . . . . ? C24 C23 C27 C275 52.0(7) . . . . ? C22 C23 C27 C273 57.9(6) . . . . ? C24 C23 C27 C273 -121.0(5) . . . . ? C2 N22 C31 C32 -15.3(6) . . . . ? C2 N22 C31 C36 163.3(4) . . . . ? C36 C31 C32 C33 -1.3(6) . . . . ? N22 C31 C32 C33 177.2(4) . . . . ? C31 C32 C33 C34 2.2(6) . . . . ? C31 C32 C33 C37 -175.5(4) . . . . ? C32 C33 C34 C35 -1.2(6) . . . . ? C37 C33 C34 C35 176.4(4) . . . . ? C33 C34 C35 C36 -0.6(6) . . . . ? C33 C34 C35 C38 179.8(4) . . . . ? C34 C35 C36 O36 -177.2(3) . . . . ? C38 C35 C36 O36 2.5(5) . . . . ? C34 C35 C36 C31 1.5(6) . . . . ? C38 C35 C36 C31 -178.8(3) . . . . ? C32 C31 C36 C35 -0.6(6) . . . . ? N22 C31 C36 C35 -179.2(4) . . . . ? C32 C31 C36 O36 178.2(3) . . . . ? N22 C31 C36 O36 -0.5(5) . . . . ? C35 C36 O36 C46 36.8(5) . . . . ? C31 C36 O36 C46 -142.0(3) . . . . ? C34 C33 C37 C372 -108.6(7) . . . . ? C32 C33 C37 C372 69.0(7) . . . . ? C34 C33 C37 C371 10.7(7) . . . . ? C32 C33 C37 C371 -171.7(5) . . . . ? C34 C33 C37 C373 128.8(5) . . . . ? C32 C33 C37 C373 -53.6(6) . . . . ? C36 C35 C38 C381 -162.9(4) . . . . ? C34 C35 C38 C381 16.7(6) . . . . ? C36 C35 C38 C45 -39.6(5) . . . . ? C34 C35 C38 C45 140.1(4) . . . . ? C36 C35 C38 C382 76.5(4) . . . . ? C34 C35 C38 C382 -103.8(4) . . . . ? C3 N31 C41 C46 -69.1(5) . . . . ? C3 N31 C41 C42 110.0(4) . . . . ? C46 C41 C42 C43 0.9(6) . . . . ? N31 C41 C42 C43 -178.2(4) . . . . ? C41 C42 C43 C44 -3.6(6) . . . . ? C41 C42 C43 C47 174.5(4) . . . . ? C42 C43 C44 C45 2.4(7) . . . . ? C47 C43 C44 C45 -175.7(4) . . . . ? C43 C44 C45 C46 1.3(6) . . . . ? C43 C44 C45 C38 -176.6(4) . . . . ? C381 C38 C45 C44 -17.6(6) . . . . ? C35 C38 C45 C44 -140.8(4) . . . . ? C382 C38 C45 C44 102.5(5) . . . . ? C381 C38 C45 C46 164.4(4) . . . . ? C35 C38 C45 C46 41.2(5) . . . . ? C382 C38 C45 C46 -75.5(5) . . . . ? C42 C41 C46 O36 -177.2(3) . . . . ? N31 C41 C46 O36 1.9(5) . . . . ? C42 C41 C46 C45 3.0(6) . . . . ? N31 C41 C46 C45 -177.8(3) . . . . ? C36 O36 C46 C41 145.4(3) . . . . ? C36 O36 C46 C45 -34.9(5) . . . . ? C44 C45 C46 C41 -4.1(6) . . . . ? C38 C45 C46 C41 174.0(4) . . . . ? C44 C45 C46 O36 176.1(4) . . . . ? C38 C45 C46 O36 -5.8(5) . . . . ? C42 C43 C47 C472 119.5(6) . . . . ? C44 C43 C47 C472 -62.5(7) . . . . ? C42 C43 C47 C473 -4.3(7) . . . . ? C44 C43 C47 C473 173.7(5) . . . . ? C42 C43 C47 C471 -121.2(6) . . . . ? C44 C43 C47 C471 56.8(7) . . . . ? C3 N32 C51 C52 40.2(5) . . . . ? C3 N32 C51 C56 -135.9(3) . . . . ? C56 C51 C52 C53 4.0(5) . . . . ? N32 C51 C52 C53 -172.0(3) . . . . ? C51 C52 C53 C54 -1.1(5) . . . . ? C51 C52 C53 C57 175.4(3) . . . . ? C52 C53 C54 C55 -1.4(6) . . . . ? C57 C53 C54 C55 -177.8(3) . . . . ? C53 C54 C55 C56 0.7(5) . . . . ? C53 C54 C55 C58 179.0(3) . . . . ? C54 C55 C56 O56 -179.5(3) . . . . ? C58 C55 C56 O56 2.2(5) . . . . ? C54 C55 C56 C51 2.4(5) . . . . ? C58 C55 C56 C51 -175.8(3) . . . . ? C52 C51 C56 C55 -4.8(5) . . . . ? N32 C51 C56 C55 171.5(3) . . . . ? C52 C51 C56 O56 177.0(3) . . . . ? N32 C51 C56 O56 -6.7(4) . . . . ? C55 C56 O56 C66 -6.0(5) . . . . ? C51 C56 O56 C66 172.2(3) . . . . ? C54 C53 C57 C572 -38.1(7) . . . . ? C52 C53 C57 C572 145.6(6) . . . . ? C54 C53 C57 C573 -161.0(5) . . . . ? C52 C53 C57 C573 22.6(6) . . . . ? C54 C53 C57 C571 82.0(6) . . . . ? C52 C53 C57 C571 -94.3(5) . . . . ? C56 C55 C58 C581 125.6(4) . . . . ? C54 C55 C58 C581 -52.6(4) . . . . ? C56 C55 C58 C65 4.5(5) . . . . ? C54 C55 C58 C65 -173.7(3) . . . . ? C56 C55 C58 C582 -113.9(4) . . . . ? C54 C55 C58 C582 67.9(4) . . . . ? C4 N41 C61 C62 -0.6(6) . . . . ? C4 N41 C61 C66 -178.5(3) . . . . ? N41 C61 C62 C63 -177.3(3) . . . . ? C66 C61 C62 C63 0.6(5) . . . . ? C61 C62 C63 C64 2.2(5) . . . . ? C61 C62 C63 C67 177.4(3) . . . . ? C62 C63 C64 C65 -2.5(5) . . . . ? C67 C63 C64 C65 -177.7(3) . . . . ? C63 C64 C65 C66 -0.2(5) . . . . ? C63 C64 C65 C58 176.5(3) . . . . ? C55 C58 C65 C66 -8.1(5) . . . . ? C581 C58 C65 C66 -129.2(4) . . . . ? C582 C58 C65 C66 110.9(4) . . . . ? C55 C58 C65 C64 175.3(3) . . . . ? C581 C58 C65 C64 54.3(4) . . . . ? C582 C58 C65 C64 -65.7(4) . . . . ? C64 C65 C66 O56 -178.1(3) . . . . ? C58 C65 C66 O56 5.3(5) . . . . ? C64 C65 C66 C61 3.1(5) . . . . ? C58 C65 C66 C61 -173.5(3) . . . . ? C56 O56 C66 C65 2.1(5) . . . . ? C56 O56 C66 C61 -179.0(3) . . . . ? C62 C61 C66 C65 -3.3(5) . . . . ? N41 C61 C66 C65 174.7(3) . . . . ? C62 C61 C66 O56 177.8(3) . . . . ? N41 C61 C66 O56 -4.2(4) . . . . ? C64 C63 C67 C671 84.5(4) . . . . ? C62 C63 C67 C671 -90.6(4) . . . . ? C64 C63 C67 C673 -154.8(4) . . . . ? C62 C63 C67 C673 30.1(5) . . . . ? C64 C63 C67 C672 -35.1(5) . . . . ? C62 C63 C67 C672 149.8(4) . . . . ? C4 N42 C71 C72 174.8(4) . . . . ? C4 N42 C71 C76 -3.9(6) . . . . ? C76 C71 C72 C73 2.5(6) . . . . ? N42 C71 C72 C73 -176.3(4) . . . . ? C76 C71 C72 O72 178.9(3) . . . . ? N42 C71 C72 O72 0.0(5) . . . . ? C71 C72 C73 C74 -1.8(6) . . . . ? O72 C72 C73 C74 -178.0(4) . . . . ? C72 C73 C74 C75 0.0(7) . . . . ? C73 C74 C75 C76 1.0(7) . . . . ? C74 C75 C76 C71 -0.2(7) . . . . ? C72 C71 C76 C75 -1.5(6) . . . . ? N42 C71 C76 C75 177.2(4) . . . . ? C73 C72 O72 C82 -84.3(4) . . . . ? C71 C72 O72 C82 99.3(4) . . . . ? C1 N11 C81 C86 -120.5(4) . . . . ? C1 N11 C81 C82 62.4(5) . . . . ? C72 O72 C82 C83 14.2(5) . . . . ? C72 O72 C82 C81 -167.2(3) . . . . ? C86 C81 C82 O72 -177.4(3) . . . . ? N11 C81 C82 O72 -0.3(5) . . . . ? C86 C81 C82 C83 1.2(6) . . . . ? N11 C81 C82 C83 178.4(3) . . . . ? O72 C82 C83 C84 177.3(4) . . . . ? C81 C82 C83 C84 -1.3(6) . . . . ? C82 C83 C84 C85 1.1(7) . . . . ? C83 C84 C85 C86 -0.8(8) . . . . ? C82 C81 C86 C85 -1.0(6) . . . . ? N11 C81 C86 C85 -178.1(4) . . . . ? C84 C85 C86 C81 0.7(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 N11 H11 O1B 0.88 2.14 2.929(6) 148.9 . N12 H12 O1B 0.88 1.99 2.821(5) 157.1 . N21 H21 O16 0.88 2.11 2.550(4) 110.4 . N31 H31 O1E 0.88 2.30 2.904(4) 125.4 . N32 H32 O1 0.88 2.14 2.987(4) 162.1 . N41 H41 O1 0.88 2.10 2.904(4) 152.1 . N42 H42 O1 0.88 1.95 2.788(3) 159.3 . O1A H1A O3 0.84 2.41 2.754(6) 105.4 4_576 O1B H1B O1A 0.84 2.18 2.802(10) 130.5 . O1C H1C O1D 0.84 1.88 2.699(8) 163.4 4_565 O1D H1D O4 0.84 1.95 2.766(7) 164.0 4_566 O1E H1E O1C 0.84 1.91 2.740(6) 169.5 . _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.276 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.084