# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _publ_contact_author_name 'Francisca Sanz Gonzalez' _publ_contact_author_address ; Servicio de Difracci\'on de Rayos X, Universidad de Salamanca, Plaza de los Caidos 1-5, 37008-Salamanca. Spain ; _publ_contact_author_email sdrayosx@usal.es _publ_contact_author_fax '+34 923294500' _publ_contact_author_phone '+34 923294474' _publ_contact_letter ; ; _publ_requested_category EO #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ;\ Bis-carbazolylamido urea receptor for short-chain dicarboxylate anions. ; _publ_section_title_footnote . # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address M.C.Caballero ; Departamento de Quimica Organica, Universidad de Salamanca, Plaza de los Caidos 1-5, 37008-Salamanca. Spain ; M.B.Jimenez ; Departamento de Ingenieria Quimica Industrial y del Medio Ambiente, Universidad Politecnica de Madrid, Jose Guti\'errez Abascal 2, 28006-Madrid, Spain ; V.Alcazar ; Departamento de Quimica Farmaceutica, Universidad de Salamanca, Facultad de Farmacia, Campus Miguel de Unamuno, 37007 Salamanca, Spain ; R.Pelaez ; Servicio General de Rayos X, Universidad de Salamanca, Plaza de los Caidos, 37008-Salamanca. Spain ; F.Sanz ; Departamento de Quimica Organica, Universidad de Salamanca, Plaza de los Caidos 1-5, 37008-Salamanca. Spain ; 'A.L. Fuentes' ; Departamento de Quimica Organica, Universidad de Salamanca, Plaza de los Caidos 1-5, 37008-Salamanca. Spain ; # TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ;\ ; _publ_section_exptl_refinement ; ; _publ_section_acknowledgements ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; data_fin _database_code_depnum_ccdc_archive 'CCDC 837724' #TrackingRef 'BASE1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H36 Cl4 N6 O3, 2(C16 H36 N), C3 H2 O4' _chemical_formula_sum 'C72 H110 Cl4 N8 O7' _chemical_formula_weight 1341.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.8187(3) _cell_length_b 16.0647(3) _cell_length_c 26.4451(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.0620(10) _cell_angle_gamma 90.00 _cell_volume 7983.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6410 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 55.50 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details 'SADABS (Bruker, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17057 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 48.05 _reflns_number_total 6410 _reflns_number_gt 4879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker 2006)' _computing_cell_refinement 'SAINT (Bruker 2006)' _computing_data_reduction 'SAINT (Bruker 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 2.3 (Macrae et al, 2008)' _computing_publication_material 'Bruker SHELXTL' _chemical_absolute_configuration rm _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^)+(0.1643P)^2^+4.1252P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6410 _refine_ls_number_parameters 854 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.2400 _refine_ls_wR_factor_gt 0.2180 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 2.144 _refine_ls_shift/su_mean 0.026 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 Cl1 Cl 1.07618(10) 0.14282(16) 0.36924(5) 0.1364(8) Uani 1 1 d . . . Cl2 Cl 0.76658(8) 0.34426(13) 0.16162(6) 0.1176(7) Uani 1 1 d . . . Cl3 Cl 0.76752(9) 0.24753(14) -0.15456(7) 0.1299(8) Uani 1 1 d . . . Cl4 Cl 1.11895(12) 0.31541(14) -0.33657(6) 0.1378(8) Uani 1 1 d . . . N1 N 1.1920(3) 0.1504(3) 0.1973(2) 0.0836(16) Uani 1 1 d . . . N2 N 1.0536(3) 0.2140(3) 0.15277(18) 0.0665(14) Uani 1 1 d . . . N3 N 0.9784(3) 0.2623(3) 0.05647(17) 0.0719(15) Uani 1 1 d . . . N4 N 0.9851(3) 0.2572(3) -0.03050(17) 0.0729(14) Uani 1 1 d . . . N5 N 1.0746(4) 0.2763(3) -0.1211(2) 0.0757(18) Uani 1 1 d . . . N6 N 1.2233(4) 0.2816(4) -0.1536(3) 0.094(2) Uani 1 1 d . . . N7 N 0.6943(3) 0.0273(3) -0.41572(19) 0.0968(15) Uani 1 1 d . . . N8 N 0.8534(3) -0.0016(3) 0.17338(16) 0.0822(13) Uani 1 1 d . . . O1 O 1.2656(3) 0.0802(4) 0.2519(2) 0.151(2) Uani 1 1 d . . . O2 O 0.8921(3) 0.3200(3) 0.00522(13) 0.1048(15) Uani 1 1 d . . . O3 O 1.3122(3) 0.3340(4) -0.19824(19) 0.145(2) Uani 1 1 d . . . O4 O 1.0935(4) 0.1572(4) 0.0460(2) 0.142(2) Uani 1 1 d . . . O5 O 1.1802(3) 0.2131(3) 0.0950(2) 0.138(2) Uani 1 1 d . . . O6 O 1.1550(3) 0.2589(3) -0.03282(15) 0.1228(17) Uani 1 1 d . . . O7 O 1.2180(2) 0.1659(3) -0.07072(16) 0.1177(15) Uani 1 1 d . . . C1 C 1.4558(14) -0.090(2) 0.0808(9) 0.54(3) Uani 1 1 d . . . H1A H 1.4675 -0.0387 0.0648 0.806 Uiso 1 1 calc R . . H1B H 1.4448 -0.1316 0.0553 0.806 Uiso 1 1 calc R . . H1C H 1.4956 -0.1086 0.1021 0.806 Uiso 1 1 calc R . . C2 C 1.3997(11) -0.0790(17) 0.1087(7) 0.404(16) Uani 1 1 d . . . H2A H 1.4086 -0.1065 0.1410 0.485 Uiso 1 1 calc R . . H2B H 1.3587 -0.1057 0.0918 0.485 Uiso 1 1 calc R . . C3 C 1.3818(7) 0.0114(12) 0.1181(5) 0.286(9) Uani 1 1 d . . . H3A H 1.4236 0.0393 0.1329 0.343 Uiso 1 1 calc R . . H3B H 1.3691 0.0381 0.0859 0.343 Uiso 1 1 calc R . . C4 C 1.3201(6) 0.0220(9) 0.1534(4) 0.201(5) Uani 1 1 d . . . H4A H 1.2771 0.0005 0.1363 0.241 Uiso 1 1 calc R . . H4B H 1.3300 -0.0118 0.1833 0.241 Uiso 1 1 calc R . . C5 C 1.3067(4) 0.1072(7) 0.1695(3) 0.143(3) Uani 1 1 d . . . H5A H 1.2882 0.1394 0.1406 0.171 Uiso 1 1 calc R . . H5B H 1.3511 0.1325 0.1818 0.171 Uiso 1 1 calc R . . C6 C 1.2540(4) 0.1102(5) 0.2109(3) 0.109(2) Uani 1 1 d . . . C7 C 1.1332(3) 0.1640(3) 0.2264(2) 0.0729(16) Uani 1 1 d . . . C8 C 1.1326(3) 0.1484(4) 0.2777(2) 0.0835(17) Uani 1 1 d . . . H8 H 1.1728 0.1264 0.2948 0.100 Uiso 1 1 calc R . . C9 C 1.0723(4) 0.1653(4) 0.3041(2) 0.0913(19) Uani 1 1 d . . . C10 C 1.0109(4) 0.1972(4) 0.2823(2) 0.0825(17) Uani 1 1 d . . . H10 H 0.9717 0.2084 0.3011 0.099 Uiso 1 1 calc R . . C11 C 1.0102(3) 0.2121(3) 0.23009(19) 0.0684(15) Uani 1 1 d . . . C12 C 1.0696(3) 0.1954(3) 0.20279(19) 0.0642(14) Uani 1 1 d . . . C13 C 0.9858(3) 0.2437(3) 0.14711(19) 0.0589(13) Uani 1 1 d . . . C14 C 0.9567(3) 0.2442(3) 0.19488(19) 0.0628(14) Uani 1 1 d . . . C15 C 0.8884(3) 0.2737(4) 0.1999(2) 0.0782(16) Uani 1 1 d . . . H15 H 0.8677 0.2734 0.2311 0.094 Uiso 1 1 calc R . . C16 C 0.8524(3) 0.3032(4) 0.1577(2) 0.0760(16) Uani 1 1 d . . . C17 C 0.8804(3) 0.3020(3) 0.1095(2) 0.0722(15) Uani 1 1 d . . . H17 H 0.8537 0.3225 0.0816 0.087 Uiso 1 1 calc R . . C18 C 0.9474(3) 0.2705(3) 0.10355(19) 0.0597(14) Uani 1 1 d . . . C19 C 0.9476(4) 0.2820(4) 0.0103(2) 0.0743(16) Uani 1 1 d . . . C20 C 0.9578(4) 0.2631(3) -0.0812(2) 0.0723(15) Uani 1 1 d . . . C21 C 0.8864(4) 0.2558(4) -0.0935(2) 0.0834(17) Uani 1 1 d . . . H21 H 0.8551 0.2470 -0.0680 0.100 Uiso 1 1 calc R . . C22 C 0.8600(3) 0.2611(4) -0.1434(3) 0.0867(17) Uani 1 1 d . . . C23 C 0.9023(5) 0.2757(4) -0.1820(2) 0.095(2) Uani 1 1 d . . . H23 H 0.8831 0.2826 -0.2149 0.114 Uiso 1 1 calc R . . C24 C 0.9756(4) 0.2800(4) -0.1712(2) 0.0780(16) Uani 1 1 d . . . C25 C 1.0022(4) 0.2726(3) -0.1215(2) 0.0694(15) Uani 1 1 d . . . C26 C 1.0954(4) 0.2848(3) -0.1695(2) 0.0745(16) Uani 1 1 d . . . C27 C 1.0345(4) 0.2879(4) -0.2022(2) 0.0799(17) Uani 1 1 d . . . C28 C 1.0417(4) 0.2972(4) -0.2549(2) 0.0971(19) Uani 1 1 d . . . H28 H 1.0020 0.2996 -0.2774 0.116 Uiso 1 1 calc R . . C29 C 1.1100(5) 0.3026(4) -0.2716(2) 0.099(2) Uani 1 1 d . . . C30 C 1.1696(4) 0.2980(4) -0.2400(2) 0.0933(19) Uani 1 1 d . . . H30 H 1.2143 0.3011 -0.2533 0.112 Uiso 1 1 calc R . . C31 C 1.1639(5) 0.2888(3) -0.1877(2) 0.0817(17) Uani 1 1 d . . . C32 C 1.2934(5) 0.3030(5) -0.1590(3) 0.112(2) Uani 1 1 d . . . C33 C 1.3441(4) 0.2861(6) -0.1146(3) 0.132(3) Uani 1 1 d . . . H33A H 1.3294 0.2356 -0.0980 0.158 Uiso 1 1 calc R . . H33B H 1.3911 0.2765 -0.1268 0.158 Uiso 1 1 calc R . . C34 C 1.3483(6) 0.3527(8) -0.0779(4) 0.191(4) Uani 1 1 d . . . H34A H 1.3022 0.3579 -0.0635 0.230 Uiso 1 1 calc R . . H34B H 1.3571 0.4041 -0.0957 0.230 Uiso 1 1 calc R . . C35 C 1.4043(8) 0.3445(13) -0.0345(5) 0.263(8) Uani 1 1 d . . . H35A H 1.4490 0.3285 -0.0483 0.316 Uiso 1 1 calc R . . H35B H 1.4111 0.3985 -0.0186 0.316 Uiso 1 1 calc R . . C36 C 1.3878(9) 0.2878(12) 0.0018(7) 0.283(8) Uani 1 1 d . . . H36A H 1.3839 0.2335 -0.0141 0.339 Uiso 1 1 calc R . . H36B H 1.3413 0.3019 0.0134 0.339 Uiso 1 1 calc R . . C37 C 1.4400(9) 0.2804(15) 0.0487(6) 0.350(12) Uani 1 1 d . . . H37A H 1.4723 0.2351 0.0440 0.525 Uiso 1 1 calc R . . H37B H 1.4138 0.2704 0.0782 0.525 Uiso 1 1 calc R . . H37C H 1.4665 0.3313 0.0530 0.525 Uiso 1 1 calc R . . C38 C 1.1585(5) 0.1778(5) 0.0573(3) 0.105(2) Uani 1 1 d . . . C39 C 1.2099(3) 0.1515(4) 0.0165(2) 0.104(2) Uani 1 1 d . . . H39A H 1.2583 0.1644 0.0283 0.125 Uiso 1 1 calc R . . H39B H 1.2066 0.0918 0.0115 0.125 Uiso 1 1 calc R . . C40 C 1.1933(4) 0.1949(5) -0.0332(2) 0.0875(18) Uani 1 1 d . . . C41 C 0.7481(4) 0.0859(4) -0.3907(3) 0.110(2) Uani 1 1 d . . . H41A H 0.7833 0.0990 -0.4150 0.132 Uiso 1 1 calc R . . H41B H 0.7239 0.1373 -0.3830 0.132 Uiso 1 1 calc R . . C42 C 0.7861(5) 0.0558(5) -0.3435(3) 0.136(3) Uani 1 1 d . . . H42A H 0.8139 0.0068 -0.3509 0.163 Uiso 1 1 calc R . . H42B H 0.7517 0.0402 -0.3191 0.163 Uiso 1 1 calc R . . C43 C 0.8354(6) 0.1240(7) -0.3208(4) 0.195(4) Uani 1 1 d . . . H43A H 0.8079 0.1737 -0.3148 0.234 Uiso 1 1 calc R . . H43B H 0.8711 0.1378 -0.3446 0.234 Uiso 1 1 calc R . . C44 C 0.8726(7) 0.0938(8) -0.2701(4) 0.241(6) Uani 1 1 d . . . H44A H 0.8373 0.0828 -0.2461 0.361 Uiso 1 1 calc R . . H44B H 0.9045 0.1363 -0.2571 0.361 Uiso 1 1 calc R . . H44C H 0.8989 0.0439 -0.2760 0.361 Uiso 1 1 calc R . . C45 C 0.6614(4) 0.0742(5) -0.4608(3) 0.118(2) Uani 1 1 d . . . H45A H 0.6989 0.0904 -0.4826 0.141 Uiso 1 1 calc R . . H45B H 0.6396 0.1247 -0.4488 0.141 Uiso 1 1 calc R . . C46 C 0.6059(5) 0.0251(7) -0.4918(4) 0.172(4) Uani 1 1 d . . . H46A H 0.5618 0.0337 -0.4752 0.206 Uiso 1 1 calc R . . H46B H 0.6184 -0.0329 -0.4864 0.206 Uiso 1 1 calc R . . C47 C 0.5826(7) 0.0338(9) -0.5588(10) 0.400(18) Uani 1 1 d . . . H47A H 0.5558 -0.0135 -0.5724 0.480 Uiso 1 1 calc R . . H47B H 0.5589 0.0856 -0.5680 0.480 Uiso 1 1 calc R . . C48 C 0.6419(6) 0.0326(6) -0.5679(5) 0.178(4) Uani 1 1 d . . . H48A H 0.6461 0.0167 -0.6026 0.266 Uiso 1 1 calc R . . H48B H 0.6668 -0.0069 -0.5462 0.266 Uiso 1 1 calc R . . H48C H 0.6622 0.0869 -0.5624 0.266 Uiso 1 1 calc R . . C49 C 0.7300(4) -0.0536(4) -0.4309(3) 0.108(2) Uani 1 1 d . . . H49A H 0.7485 -0.0809 -0.4002 0.129 Uiso 1 1 calc R . . H49B H 0.6937 -0.0897 -0.4464 0.129 Uiso 1 1 calc R . . C50 C 0.7891(4) -0.0470(6) -0.4662(3) 0.127(3) Uani 1 1 d . . . H50A H 0.8307 -0.0230 -0.4486 0.152 Uiso 1 1 calc R . . H50B H 0.7748 -0.0107 -0.4943 0.152 Uiso 1 1 calc R . . C51 C 0.8074(5) -0.1320(8) -0.4862(3) 0.179(4) Uani 1 1 d . . . H51A H 0.8229 -0.1671 -0.4579 0.215 Uiso 1 1 calc R . . H51B H 0.7646 -0.1566 -0.5020 0.215 Uiso 1 1 calc R . . C52 C 0.8615(7) -0.1317(10) -0.5221(5) 0.270(8) Uani 1 1 d . . . H52A H 0.8545 -0.0851 -0.5445 0.405 Uiso 1 1 calc R . . H52B H 0.8590 -0.1824 -0.5414 0.405 Uiso 1 1 calc R . . H52C H 0.9073 -0.1275 -0.5046 0.405 Uiso 1 1 calc R . . C53 C 0.6377(4) 0.0002(5) -0.3802(3) 0.120(2) Uani 1 1 d . . . H53A H 0.6608 -0.0266 -0.3508 0.144 Uiso 1 1 calc R . . H53B H 0.6070 -0.0405 -0.3973 0.144 Uiso 1 1 calc R . . C54 C 0.5923(5) 0.0721(6) -0.3625(4) 0.177(4) Uani 1 1 d . . . H54A H 0.5674 0.0984 -0.3913 0.212 Uiso 1 1 calc R . . H54B H 0.6222 0.1135 -0.3452 0.212 Uiso 1 1 calc R . . C55 C 0.5369(9) 0.0364(9) -0.3252(6) 0.255(8) Uani 1 1 d . . . H55A H 0.4985 0.0759 -0.3216 0.306 Uiso 1 1 calc R . . H55B H 0.5167 -0.0152 -0.3385 0.306 Uiso 1 1 calc R . . C56 C 0.5698(8) 0.0234(13) -0.2819(5) 0.292(10) Uani 1 1 d . . . H56A H 0.5944 -0.0289 -0.2826 0.437 Uiso 1 1 calc R . . H56B H 0.5361 0.0222 -0.2560 0.437 Uiso 1 1 calc R . . H56C H 0.6035 0.0674 -0.2749 0.437 Uiso 1 1 calc R . . C57 C 0.8771(4) 0.0286(4) 0.2265(2) 0.100(2) Uani 1 1 d . . . H57A H 0.9173 0.0659 0.2239 0.120 Uiso 1 1 calc R . . H57B H 0.8386 0.0601 0.2402 0.120 Uiso 1 1 calc R . . C58 C 0.8983(4) -0.0413(5) 0.2634(2) 0.117(2) Uani 1 1 d . . . H58A H 0.8572 -0.0765 0.2680 0.141 Uiso 1 1 calc R . . H58B H 0.9347 -0.0752 0.2489 0.141 Uiso 1 1 calc R . . C59 C 0.9255(5) -0.0094(6) 0.3132(3) 0.164(3) Uani 1 1 d . . . H59A H 0.8897 0.0265 0.3267 0.197 Uiso 1 1 calc R . . H59B H 0.9673 0.0243 0.3083 0.197 Uiso 1 1 calc R . . C60 C 0.9443(5) -0.0749(6) 0.3509(3) 0.166(3) Uani 1 1 d . . . H60A H 0.9527 -0.0500 0.3837 0.249 Uiso 1 1 calc R . . H60B H 0.9865 -0.1033 0.3415 0.249 Uiso 1 1 calc R . . H60C H 0.9058 -0.1140 0.3521 0.249 Uiso 1 1 calc R . . C61 C 0.9125(3) -0.0500(4) 0.1500(2) 0.0941(18) Uani 1 1 d . . . H61A H 0.9226 -0.0994 0.1703 0.113 Uiso 1 1 calc R . . H61B H 0.8960 -0.0682 0.1164 0.113 Uiso 1 1 calc R . . C62 C 0.9807(4) -0.0010(5) 0.1460(3) 0.118(2) Uani 1 1 d . . . H62A H 0.9728 0.0450 0.1226 0.141 Uiso 1 1 calc R . . H62B H 0.9958 0.0216 0.1788 0.141 Uiso 1 1 calc R . . C63 C 1.0365(5) -0.0570(6) 0.1276(4) 0.161(3) Uani 1 1 d . . . H63A H 1.0383 -0.1062 0.1489 0.193 Uiso 1 1 calc R . . H63B H 1.0216 -0.0749 0.0937 0.193 Uiso 1 1 calc R . . C64 C 1.1085(6) -0.0238(6) 0.1262(4) 0.189(4) Uani 1 1 d . . . H64A H 1.1410 -0.0682 0.1202 0.284 Uiso 1 1 calc R . . H64B H 1.1216 0.0022 0.1581 0.284 Uiso 1 1 calc R . . H64C H 1.1102 0.0166 0.0996 0.284 Uiso 1 1 calc R . . C65 C 0.8329(3) 0.0748(4) 0.1420(2) 0.0959(19) Uani 1 1 d . . . H65A H 0.8745 0.1101 0.1401 0.115 Uiso 1 1 calc R . . H65B H 0.7974 0.1059 0.1593 0.115 Uiso 1 1 calc R . . C66 C 0.8038(5) 0.0561(5) 0.0883(3) 0.132(3) Uani 1 1 d . . . H66A H 0.8405 0.0279 0.0703 0.159 Uiso 1 1 calc R . . H66B H 0.7639 0.0182 0.0900 0.159 Uiso 1 1 calc R . . C67 C 0.7805(5) 0.1296(5) 0.0591(3) 0.159(3) Uani 1 1 d . . . H67A H 0.8205 0.1673 0.0572 0.191 Uiso 1 1 calc R . . H67B H 0.7442 0.1580 0.0773 0.191 Uiso 1 1 calc R . . C68 C 0.7517(7) 0.1122(7) 0.0070(3) 0.224(6) Uani 1 1 d . . . H68A H 0.7560 0.1610 -0.0135 0.335 Uiso 1 1 calc R . . H68B H 0.7024 0.0970 0.0078 0.335 Uiso 1 1 calc R . . H68C H 0.7778 0.0673 -0.0071 0.335 Uiso 1 1 calc R . . C69 C 0.7906(3) -0.0597(4) 0.1761(2) 0.0943(18) Uani 1 1 d . . . H69A H 0.8056 -0.1080 0.1958 0.113 Uiso 1 1 calc R . . H69B H 0.7774 -0.0788 0.1421 0.113 Uiso 1 1 calc R . . C70 C 0.7249(4) -0.0236(5) 0.1987(3) 0.117(2) Uani 1 1 d . . . H70A H 0.7126 0.0289 0.1824 0.141 Uiso 1 1 calc R . . H70B H 0.7347 -0.0131 0.2345 0.141 Uiso 1 1 calc R . . C71 C 0.6628(5) -0.0837(5) 0.1918(4) 0.148(3) Uani 1 1 d . . . H71A H 0.6523 -0.0924 0.1558 0.178 Uiso 1 1 calc R . . H71B H 0.6765 -0.1369 0.2066 0.178 Uiso 1 1 calc R . . C72 C 0.5989(5) -0.0543(7) 0.2146(5) 0.229(6) Uani 1 1 d . . . H72A H 0.5723 -0.1011 0.2260 0.344 Uiso 1 1 calc R . . H72B H 0.5703 -0.0234 0.1901 0.344 Uiso 1 1 calc R . . H72C H 0.6120 -0.0191 0.2429 0.344 Uiso 1 1 calc R . . H1N H 1.189(2) 0.163(3) 0.1691(18) 0.047(17) Uiso 1 1 d . . . H2N H 1.080(2) 0.212(2) 0.1320(15) 0.029(14) Uiso 1 1 d . . . H3N H 1.013(2) 0.235(3) 0.0561(14) 0.027(15) Uiso 1 1 d . . . H4N H 1.027(3) 0.240(3) -0.0259(18) 0.07(2) Uiso 1 1 d . . . H5N H 1.098(2) 0.274(2) -0.1008(15) 0.016(16) Uiso 1 1 d . . . H6N H 1.222(3) 0.253(3) -0.1313(19) 0.058(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.1269(15) 0.223(2) 0.0593(9) 0.0110(10) 0.0039(9) 0.0186(14) Cl2 0.0837(12) 0.1591(18) 0.1122(12) 0.0078(11) 0.0268(9) 0.0368(11) Cl3 0.0942(15) 0.160(2) 0.1318(15) 0.0027(12) -0.0254(11) 0.0048(12) Cl4 0.206(2) 0.1449(18) 0.0652(10) 0.0084(10) 0.0277(11) -0.0080(14) N1 0.083(5) 0.099(4) 0.069(4) 0.006(3) 0.010(3) 0.009(3) N2 0.074(4) 0.073(4) 0.055(3) 0.000(2) 0.023(3) 0.002(3) N3 0.069(4) 0.080(4) 0.068(4) 0.008(2) 0.011(3) 0.020(3) N4 0.068(4) 0.085(4) 0.066(4) 0.002(2) 0.008(3) 0.010(3) N5 0.090(6) 0.081(4) 0.055(4) 0.002(3) -0.001(4) -0.007(3) N6 0.106(6) 0.105(5) 0.074(4) 0.016(3) 0.030(4) -0.015(4) N7 0.103(4) 0.081(4) 0.107(4) 0.004(3) 0.011(3) 0.002(3) N8 0.104(4) 0.062(3) 0.082(3) -0.010(3) 0.012(3) -0.005(3) O1 0.131(4) 0.225(7) 0.098(3) 0.029(4) 0.010(3) 0.080(4) O2 0.100(3) 0.140(4) 0.076(3) 0.015(2) 0.012(2) 0.047(3) O3 0.144(4) 0.189(6) 0.105(3) 0.019(3) 0.043(3) -0.057(4) O4 0.131(5) 0.133(5) 0.169(5) 0.007(3) 0.066(4) 0.039(4) O5 0.215(6) 0.120(4) 0.080(3) 0.007(3) 0.037(4) 0.020(4) O6 0.177(5) 0.100(4) 0.089(3) -0.006(3) -0.016(3) 0.035(4) O7 0.142(4) 0.136(4) 0.079(3) -0.014(3) 0.032(3) 0.004(3) C1 0.44(3) 0.78(7) 0.40(3) -0.16(4) 0.16(3) 0.25(4) C2 0.32(2) 0.56(4) 0.34(2) -0.21(3) 0.119(19) 0.10(2) C3 0.252(15) 0.41(3) 0.204(12) -0.083(14) 0.075(11) 0.125(15) C4 0.189(10) 0.270(16) 0.148(8) -0.029(9) 0.051(7) 0.024(10) C5 0.107(6) 0.186(10) 0.137(6) -0.005(6) 0.021(5) 0.046(6) C6 0.092(6) 0.143(7) 0.093(5) 0.011(4) 0.016(4) 0.038(5) C7 0.075(5) 0.080(4) 0.064(4) -0.007(3) 0.010(4) -0.006(3) C8 0.085(5) 0.097(5) 0.067(4) -0.004(3) -0.004(3) 0.001(3) C9 0.089(5) 0.125(6) 0.061(3) 0.000(3) 0.008(4) -0.002(4) C10 0.081(5) 0.101(5) 0.067(4) -0.004(3) 0.015(3) 0.000(4) C11 0.078(4) 0.068(4) 0.060(4) -0.008(3) 0.009(3) -0.004(3) C12 0.067(4) 0.069(4) 0.057(4) -0.004(3) 0.009(3) -0.005(3) C13 0.058(4) 0.053(4) 0.066(4) -0.001(3) 0.010(3) 0.005(3) C14 0.058(4) 0.061(4) 0.070(4) -0.007(3) 0.013(3) 0.001(3) C15 0.084(5) 0.080(4) 0.072(4) 0.001(3) 0.023(3) 0.000(3) C16 0.064(4) 0.076(4) 0.089(4) -0.006(3) 0.017(3) 0.007(3) C17 0.070(4) 0.072(4) 0.075(4) 0.003(3) 0.011(3) 0.007(3) C18 0.065(4) 0.052(4) 0.063(4) -0.001(3) 0.014(3) -0.001(3) C19 0.072(5) 0.073(4) 0.079(5) 0.011(3) 0.010(4) 0.009(3) C20 0.084(5) 0.062(4) 0.070(4) 0.000(3) -0.004(4) -0.002(3) C21 0.085(5) 0.082(5) 0.083(4) 0.003(3) 0.002(4) 0.002(3) C22 0.082(5) 0.088(5) 0.088(5) 0.003(3) -0.015(4) 0.004(3) C23 0.127(7) 0.087(5) 0.069(4) 0.002(3) -0.007(4) 0.001(4) C24 0.090(6) 0.072(5) 0.071(4) 0.000(3) 0.000(4) -0.005(3) C25 0.079(6) 0.068(4) 0.061(4) 0.000(3) 0.003(4) -0.001(3) C26 0.097(6) 0.069(4) 0.060(4) 0.000(3) 0.020(5) -0.008(3) C27 0.112(6) 0.067(4) 0.060(4) 0.003(3) 0.002(5) -0.006(3) C28 0.138(7) 0.083(5) 0.069(4) -0.001(3) -0.005(4) -0.004(4) C29 0.147(7) 0.091(5) 0.061(4) 0.004(3) 0.023(5) -0.002(4) C30 0.126(6) 0.088(5) 0.069(4) 0.004(3) 0.025(4) -0.008(4) C31 0.116(6) 0.065(4) 0.065(5) 0.001(3) 0.010(5) -0.006(4) C32 0.121(7) 0.120(6) 0.097(6) -0.002(4) 0.044(5) -0.027(5) C33 0.101(6) 0.191(9) 0.106(6) -0.004(6) 0.032(5) -0.021(5) C34 0.222(11) 0.228(13) 0.124(7) -0.027(8) 0.002(7) -0.031(9) C35 0.214(13) 0.41(3) 0.161(12) -0.012(13) -0.001(10) -0.073(15) C36 0.242(17) 0.35(2) 0.251(19) 0.054(16) -0.064(15) -0.035(15) C37 0.30(2) 0.55(4) 0.192(14) -0.013(17) -0.054(14) -0.07(2) C38 0.121(7) 0.099(6) 0.100(6) 0.028(5) 0.032(5) 0.039(5) C39 0.109(5) 0.133(6) 0.074(4) 0.016(4) 0.034(3) 0.044(4) C40 0.100(5) 0.096(6) 0.068(4) -0.008(4) 0.021(3) 0.001(4) C41 0.131(6) 0.083(5) 0.116(5) -0.005(4) 0.000(4) -0.017(4) C42 0.172(7) 0.128(7) 0.104(5) 0.001(5) -0.022(5) -0.002(6) C43 0.196(10) 0.198(11) 0.181(9) -0.027(8) -0.079(8) -0.005(9) C44 0.272(14) 0.235(15) 0.209(11) -0.088(10) -0.052(11) 0.000(11) C45 0.118(6) 0.108(6) 0.126(5) 0.020(5) -0.008(5) 0.010(5) C46 0.121(7) 0.173(10) 0.215(10) -0.025(8) -0.048(7) 0.044(7) C47 0.137(11) 0.210(16) 0.85(5) 0.31(2) 0.00(2) 0.035(11) C48 0.143(9) 0.118(8) 0.269(13) -0.001(7) -0.016(9) 0.025(7) C49 0.107(5) 0.088(6) 0.127(5) -0.013(4) -0.005(4) 0.009(4) C50 0.108(6) 0.165(8) 0.107(5) 0.012(5) 0.008(4) 0.025(5) C51 0.141(8) 0.255(13) 0.141(7) -0.056(8) 0.006(6) 0.066(8) C52 0.253(14) 0.35(2) 0.213(12) -0.026(12) 0.088(11) 0.106(14) C53 0.124(6) 0.085(6) 0.155(6) 0.013(4) 0.040(5) 0.015(4) C54 0.201(9) 0.124(8) 0.215(10) 0.024(7) 0.104(8) 0.046(7) C55 0.311(18) 0.219(14) 0.249(14) 0.080(12) 0.136(15) 0.151(13) C56 0.258(16) 0.42(3) 0.206(13) 0.105(16) 0.058(12) 0.140(16) C57 0.127(5) 0.091(5) 0.082(4) -0.013(4) 0.000(4) -0.003(4) C58 0.150(6) 0.115(6) 0.086(4) 0.001(4) -0.003(4) -0.009(5) C59 0.217(10) 0.159(9) 0.113(6) -0.001(6) -0.030(6) 0.013(7) C60 0.210(9) 0.171(9) 0.114(6) 0.036(6) -0.022(6) -0.009(7) C61 0.114(5) 0.080(5) 0.089(4) -0.010(3) 0.016(4) -0.005(4) C62 0.113(6) 0.102(6) 0.142(6) -0.022(4) 0.034(4) 0.003(5) C63 0.132(7) 0.123(8) 0.230(10) -0.036(7) 0.040(7) -0.027(6) C64 0.175(10) 0.131(9) 0.266(13) -0.020(8) 0.048(8) -0.018(7) C65 0.119(5) 0.075(5) 0.094(4) 0.002(4) 0.012(4) -0.002(4) C66 0.199(8) 0.092(6) 0.103(5) 0.013(4) -0.022(5) -0.010(5) C67 0.248(10) 0.101(7) 0.124(6) 0.012(5) -0.037(6) -0.017(6) C68 0.361(17) 0.159(10) 0.141(8) 0.032(7) -0.085(9) -0.026(10) C69 0.117(5) 0.077(5) 0.090(4) -0.001(3) 0.010(4) -0.011(4) C70 0.119(6) 0.121(7) 0.114(5) 0.002(4) 0.028(4) -0.001(5) C71 0.135(7) 0.120(7) 0.196(8) 0.027(6) 0.063(6) -0.013(6) C72 0.142(8) 0.188(11) 0.366(17) 0.066(11) 0.091(10) 0.018(8) _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 Cl1 C9 1.758(6) . ? Cl2 C16 1.753(6) . ? Cl3 C22 1.763(6) . ? Cl4 C29 1.747(6) . ? N1 C6 1.364(8) . ? N1 C7 1.398(7) . ? N1 H1N 0.77(4) . ? N2 C13 1.363(7) . ? N2 C12 1.374(7) . ? N2 H2N 0.76(4) . ? N3 C19 1.360(7) . ? N3 C18 1.410(6) . ? N3 H3N 0.78(4) . ? N4 C19 1.379(7) . ? N4 C20 1.412(7) . ? N4 H4N 0.84(5) . ? N5 C25 1.364(8) . ? N5 C26 1.366(7) . ? N5 H5N 0.68(4) . ? N6 C32 1.378(9) . ? N6 C31 1.403(8) . ? N6 H6N 0.75(5) . ? N7 C41 1.510(8) . ? N7 C45 1.514(8) . ? N7 C53 1.520(8) . ? N7 C49 1.527(8) . ? N8 C69 1.510(7) . ? N8 C61 1.515(7) . ? N8 C65 1.520(7) . ? N8 C57 1.530(7) . ? O1 C6 1.196(7) . ? O2 C19 1.212(6) . ? O3 C32 1.220(8) . ? O4 C38 1.288(9) . ? O5 C38 1.198(9) . ? O6 C40 1.255(7) . ? O7 C40 1.211(7) . ? C1 C2 1.33(2) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 C3 1.51(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.537(14) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.460(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.516(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C8 1.382(7) . ? C7 C12 1.413(7) . ? C8 C9 1.391(8) . ? C8 H8 0.9300 . ? C9 C10 1.362(8) . ? C10 C11 1.401(7) . ? C10 H10 0.9300 . ? C11 C12 1.389(7) . ? C11 C14 1.431(7) . ? C13 C18 1.395(7) . ? C13 C14 1.404(6) . ? C14 C15 1.383(7) . ? C15 C16 1.361(7) . ? C15 H15 0.9300 . ? C16 C17 1.404(7) . ? C17 C18 1.374(7) . ? C17 H17 0.9300 . ? C20 C21 1.371(8) . ? C20 C25 1.399(8) . ? C21 C22 1.387(8) . ? C21 H21 0.9300 . ? C22 C23 1.349(8) . ? C23 C24 1.396(8) . ? C23 H23 0.9300 . ? C24 C25 1.385(7) . ? C24 C27 1.419(8) . ? C26 C27 1.398(8) . ? C26 C31 1.401(8) . ? C27 C28 1.417(8) . ? C28 C29 1.384(9) . ? C28 H28 0.9300 . ? C29 C30 1.364(9) . ? C30 C31 1.402(8) . ? C30 H30 0.9300 . ? C32 C33 1.498(10) . ? C33 C34 1.443(12) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.522(16) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.370(18) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.545(18) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.545(9) . ? C39 C40 1.507(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C41 C42 1.486(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.536(12) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.556(14) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.514(11) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.81(2) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.155(14) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.495(9) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.510(12) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.429(13) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.526(10) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.580(14) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.289(17) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.525(9) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.480(9) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.481(11) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C62 1.515(8) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.484(10) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.458(11) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.525(8) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.466(10) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.479(11) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 C70 1.518(8) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.519(10) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.452(11) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? 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 C6 N1 C7 128.3(6) . . ? C6 N1 H1N 113(4) . . ? C7 N1 H1N 118(4) . . ? C13 N2 C12 109.8(5) . . ? C13 N2 H2N 126(3) . . ? C12 N2 H2N 124(3) . . ? C19 N3 C18 126.4(6) . . ? C19 N3 H3N 116(3) . . ? C18 N3 H3N 117(3) . . ? C19 N4 C20 123.3(6) . . ? C19 N4 H4N 120(3) . . ? C20 N4 H4N 117(3) . . ? C25 N5 C26 109.5(7) . . ? C25 N5 H5N 128(4) . . ? C26 N5 H5N 122(4) . . ? C32 N6 C31 130.2(7) . . ? C32 N6 H6N 108(4) . . ? C31 N6 H6N 120(4) . . ? C41 N7 C45 105.7(5) . . ? C41 N7 C53 112.5(5) . . ? C45 N7 C53 111.0(5) . . ? C41 N7 C49 110.6(5) . . ? C45 N7 C49 112.6(5) . . ? C53 N7 C49 104.6(5) . . ? C69 N8 C61 107.2(4) . . ? C69 N8 C65 110.5(5) . . ? C61 N8 C65 111.2(4) . . ? C69 N8 C57 110.0(4) . . ? C61 N8 C57 110.6(4) . . ? C65 N8 C57 107.4(4) . . ? C2 C1 H1A 110.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 109.0 . . ? C2 C1 H1C 109.0 . . ? H1A C1 H1C 110.0 . . ? H1B C1 H1C 109.0 . . ? C1 C2 C3 114(2) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2B 108.8 . . ? C3 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 112.8(16) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 115.4(12) . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? C4 C5 C6 111.7(8) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? O1 C6 N1 122.8(6) . . ? O1 C6 C5 123.2(7) . . ? N1 C6 C5 114.1(6) . . ? C8 C7 N1 124.2(6) . . ? C8 C7 C12 116.5(5) . . ? N1 C7 C12 119.3(5) . . ? C7 C8 C9 120.5(6) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 123.9(5) . . ? C10 C9 Cl1 118.8(5) . . ? C8 C9 Cl1 117.3(5) . . ? C9 C10 C11 116.5(5) . . ? C9 C10 H10 121.8 . . ? C11 C10 H10 121.8 . . ? C12 C11 C10 120.9(6) . . ? C12 C11 C14 106.8(4) . . ? C10 C11 C14 132.3(6) . . ? N2 C12 C11 108.5(5) . . ? N2 C12 C7 129.8(5) . . ? C11 C12 C7 121.7(5) . . ? N2 C13 C18 129.8(5) . . ? N2 C13 C14 108.1(5) . . ? C18 C13 C14 122.1(5) . . ? C15 C14 C13 119.9(5) . . ? C15 C14 C11 133.3(5) . . ? C13 C14 C11 106.8(5) . . ? C16 C15 C14 117.6(5) . . ? C16 C15 H15 121.2 . . ? C14 C15 H15 121.2 . . ? C15 C16 C17 123.1(5) . . ? C15 C16 Cl2 120.0(4) . . ? C17 C16 Cl2 116.8(5) . . ? C18 C17 C16 120.0(5) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 117.2(5) . . ? C17 C18 N3 124.2(5) . . ? C13 C18 N3 118.6(5) . . ? O2 C19 N3 122.8(6) . . ? O2 C19 N4 122.1(6) . . ? N3 C19 N4 115.1(6) . . ? C21 C20 C25 116.4(5) . . ? C21 C20 N4 121.5(6) . . ? C25 C20 N4 122.0(6) . . ? C20 C21 C22 121.3(6) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 122.3(6) . . ? C23 C22 Cl3 120.8(5) . . ? C21 C22 Cl3 116.9(5) . . ? C22 C23 C24 118.0(6) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C25 C24 C23 119.6(6) . . ? C25 C24 C27 107.5(6) . . ? C23 C24 C27 132.9(6) . . ? N5 C25 C24 108.3(6) . . ? N5 C25 C20 129.5(5) . . ? C24 C25 C20 122.2(7) . . ? N5 C26 C27 108.4(6) . . ? N5 C26 C31 129.9(7) . . ? C27 C26 C31 121.7(5) . . ? C26 C27 C28 119.6(6) . . ? C26 C27 C24 106.3(5) . . ? C28 C27 C24 134.1(7) . . ? C29 C28 C27 117.3(6) . . ? C29 C28 H28 121.3 . . ? C27 C28 H28 121.3 . . ? C30 C29 C28 123.3(6) . . ? C30 C29 Cl4 119.3(6) . . ? C28 C29 Cl4 117.5(7) . . ? C29 C30 C31 120.5(6) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C26 C31 N6 119.4(5) . . ? C26 C31 C30 117.6(7) . . ? N6 C31 C30 123.0(7) . . ? O3 C32 N6 120.9(8) . . ? O3 C32 C33 122.6(8) . . ? N6 C32 C33 116.5(6) . . ? C34 C33 C32 113.8(9) . . ? C34 C33 H33A 108.8 . . ? C32 C33 H33A 108.8 . . ? C34 C33 H33B 108.8 . . ? C32 C33 H33B 108.8 . . ? H33A C33 H33B 107.7 . . ? C33 C34 C35 117.0(12) . . ? C33 C34 H34A 108.0 . . ? C35 C34 H34A 108.1 . . ? C33 C34 H34B 108.1 . . ? C35 C34 H34B 108.0 . . ? H34A C34 H34B 107.3 . . ? C36 C35 C34 114.4(14) . . ? C36 C35 H35A 108.6 . . ? C34 C35 H35A 108.6 . . ? C36 C35 H35B 108.7 . . ? C34 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C35 C36 C37 117.1(16) . . ? C35 C36 H36A 108.0 . . ? C37 C36 H36A 107.9 . . ? C35 C36 H36B 108.0 . . ? C37 C36 H36B 108.0 . . ? H36A C36 H36B 107.3 . . ? C36 C37 H37A 109.6 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.4 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O5 C38 O4 126.2(8) . . ? O5 C38 C39 120.8(9) . . ? O4 C38 C39 113.0(8) . . ? C40 C39 C38 112.0(5) . . ? C40 C39 H39A 109.2 . . ? C38 C39 H39A 109.2 . . ? C40 C39 H39B 109.2 . . ? C38 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? O7 C40 O6 124.6(6) . . ? O7 C40 C39 117.8(7) . . ? O6 C40 C39 117.7(5) . . ? C42 C41 N7 116.5(6) . . ? C42 C41 H41A 108.1 . . ? N7 C41 H41A 108.2 . . ? C42 C41 H41B 108.2 . . ? N7 C41 H41B 108.2 . . ? H41A C41 H41B 107.3 . . ? C41 C42 C43 110.4(7) . . ? C41 C42 H42A 109.6 . . ? C43 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C43 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C42 C43 C44 110.4(9) . . ? C42 C43 H43A 109.5 . . ? C44 C43 H43A 109.5 . . ? C42 C43 H43B 109.6 . . ? C44 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.4 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N7 C45 C46 114.1(7) . . ? N7 C45 H45A 108.7 . . ? C46 C45 H45A 108.7 . . ? N7 C45 H45B 108.7 . . ? C46 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C45 C46 C47 128.0(10) . . ? C45 C46 H46A 105.3 . . ? C47 C46 H46A 105.3 . . ? C45 C46 H46B 105.3 . . ? C47 C46 H46B 105.3 . . ? H46A C46 H46B 106.0 . . ? C48 C47 C46 90.9(14) . . ? C48 C47 H47A 113.5 . . ? C46 C47 H47A 113.5 . . ? C48 C47 H47B 113.5 . . ? C46 C47 H47B 113.5 . . ? H47A C47 H47B 110.8 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 N7 117.2(6) . . ? C50 C49 H49A 108.0 . . ? N7 C49 H49A 108.0 . . ? C50 C49 H49B 108.0 . . ? N7 C49 H49B 108.0 . . ? H49A C49 H49B 107.2 . . ? C49 C50 C51 110.2(7) . . ? C49 C50 H50A 109.6 . . ? C51 C50 H50A 109.6 . . ? C49 C50 H50B 109.6 . . ? C51 C50 H50B 109.6 . . ? H50A C50 H50B 108.1 . . ? C52 C51 C50 114.4(11) . . ? C52 C51 H51A 108.7 . . ? C50 C51 H51A 108.6 . . ? C52 C51 H51B 108.7 . . ? C50 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.4 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N7 C53 C54 113.3(6) . . ? N7 C53 H53A 108.9 . . ? C54 C53 H53A 108.9 . . ? N7 C53 H53B 108.9 . . ? C54 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C53 C54 C55 108.4(8) . . ? C53 C54 H54A 110.0 . . ? C55 C54 H54A 110.1 . . ? C53 C54 H54B 110.0 . . ? C55 C54 H54B 109.9 . . ? H54A C54 H54B 108.4 . . ? C56 C55 C54 108.1(16) . . ? C56 C55 H55A 110.1 . . ? C54 C55 H55A 110.1 . . ? C56 C55 H55B 110.1 . . ? C54 C55 H55B 110.1 . . ? H55A C55 H55B 108.4 . . ? C55 C56 H56A 109.4 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.4 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N8 114.0(5) . . ? C58 C57 H57A 108.8 . . ? N8 C57 H57A 108.7 . . ? C58 C57 H57B 108.7 . . ? N8 C57 H57B 108.7 . . ? H57A C57 H57B 107.6 . . ? C59 C58 C57 112.3(6) . . ? C59 C58 H58A 109.1 . . ? C57 C58 H58A 109.2 . . ? C59 C58 H58B 109.1 . . ? C57 C58 H58B 109.1 . . ? H58A C58 H58B 107.9 . . ? C58 C59 C60 114.4(8) . . ? C58 C59 H59A 108.6 . . ? C60 C59 H59A 108.7 . . ? C58 C59 H59B 108.7 . . ? C60 C59 H59B 108.7 . . ? H59A C59 H59B 107.6 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 N8 113.9(5) . . ? C62 C61 H61A 108.8 . . ? N8 C61 H61A 108.8 . . ? C62 C61 H61B 108.8 . . ? N8 C61 H61B 108.8 . . ? H61A C61 H61B 107.7 . . ? C63 C62 C61 109.0(6) . . ? C63 C62 H62A 109.9 . . ? C61 C62 H62A 109.9 . . ? C63 C62 H62B 109.9 . . ? C61 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? C64 C63 C62 117.4(8) . . ? C64 C63 H63A 107.9 . . ? C62 C63 H63A 107.9 . . ? C64 C63 H63B 108.0 . . ? C62 C63 H63B 107.9 . . ? H63A C63 H63B 107.2 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.4 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N8 C65 C66 114.7(5) . . ? N8 C65 H65A 108.6 . . ? C66 C65 H65A 108.6 . . ? N8 C65 H65B 108.6 . . ? C66 C65 H65B 108.6 . . ? H65A C65 H65B 107.6 . . ? C67 C66 C65 114.4(6) . . ? C67 C66 H66A 108.6 . . ? C65 C66 H66A 108.6 . . ? C67 C66 H66B 108.7 . . ? C65 C66 H66B 108.7 . . ? H66A C66 H66B 107.6 . . ? C66 C67 C68 115.0(7) . . ? C66 C67 H67A 108.5 . . ? C68 C67 H67A 108.5 . . ? C66 C67 H67B 108.5 . . ? C68 C67 H67B 108.6 . . ? H67A C67 H67B 107.5 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.4 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N8 C69 C70 116.0(5) . . ? N8 C69 H69A 108.3 . . ? C70 C69 H69A 108.2 . . ? N8 C69 H69B 108.3 . . ? C70 C69 H69B 108.3 . . ? H69A C69 H69B 107.4 . . ? C69 C70 C71 110.3(6) . . ? C69 C70 H70A 109.6 . . ? C71 C70 H70A 109.6 . . ? C69 C70 H70B 109.6 . . ? C71 C70 H70B 109.6 . . ? H70A C70 H70B 108.1 . . ? C72 C71 C70 113.0(8) . . ? C72 C71 H71A 109.0 . . ? C70 C71 H71A 109.0 . . ? C72 C71 H71B 109.0 . . ? C70 C71 H71B 109.0 . . ? H71A C71 H71B 107.8 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 48.05 _diffrn_measured_fraction_theta_full 0.854 _refine_diff_density_max 1.049 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.053 _publ_section_title_footnote . # TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_exptl_prep ;\ ; _publ_section_exptl_refinement ; ; _publ_section_acknowledgements ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_table_legends ; ; data_twin _database_code_depnum_ccdc_archive 'CCDC 837725' #TrackingRef 'BASE2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H36 Cl4 N6 O3, 2(C16 H36 N), C2 O4' _chemical_formula_sum 'C71 H108 Cl4 N8 O7' _chemical_formula_weight 1327.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 27.892(3) _cell_length_b 17.1340(18) _cell_length_c 30.726(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.856(5) _cell_angle_gamma 90.00 _cell_volume 14631(3) _cell_formula_units_Z 8 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used 26060 _cell_measurement_theta_min 0.73 _cell_measurement_theta_max 22.12 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.93 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5712 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'BRUKER TWINABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 373(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26060 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1491 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.73 _diffrn_reflns_theta_max 22.12 _reflns_number_total 18233 _reflns_number_gt 15610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker 2005)' _computing_cell_refinement 'SAINT (Bruker 2005)' _computing_data_reduction 'SAINT (Bruker 2005)' _computing_structure_solution 'SIR2004 (Giacovazzo et al, 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1710P)^2^+233.2809P] 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 18233 _refine_ls_number_parameters 831 _refine_ls_number_restraints 402 _refine_ls_R_factor_all 0.2073 _refine_ls_R_factor_gt 0.1454 _refine_ls_wR_factor_ref 0.4070 _refine_ls_wR_factor_gt 0.3771 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.008 _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 -0.0555(5) 0.7065(8) 0.4879(4) 0.020(3) Uiso 1 1 d . . . O2 O -0.0902(4) 0.6923(5) 0.4626(3) 0.033(3) Uiso 1 1 d . . . N3 N -0.0142(4) 0.7440(6) 0.4771(3) 0.025(3) Uiso 1 1 d . . . H3 H 0.0068 0.7558 0.4983 0.030 Uiso 1 1 calc R . . C31 C -0.0033(5) 0.7645(8) 0.4351(4) 0.025(4) Uiso 1 1 d . . . C32 C -0.0311(5) 0.7416(8) 0.3961(4) 0.024(4) Uiso 1 1 d . . . H32 H -0.0605 0.7166 0.3975 0.029 Uiso 1 1 calc R . . C33 C -0.0134(5) 0.7575(8) 0.3557(4) 0.029(4) Uiso 1 1 d . . . C34 C 0.0291(5) 0.7936(7) 0.3505(4) 0.018(3) Uiso 1 1 d . . . H34 H 0.0395 0.8020 0.3229 0.021 Uiso 1 1 calc R . . C35 C 0.0566(5) 0.8177(8) 0.3880(4) 0.023(4) Uiso 1 1 d . . . C36 C 0.1011(5) 0.8589(8) 0.3953(4) 0.020(3) Uiso 1 1 d . . . C37 C 0.1333(5) 0.8887(8) 0.3678(4) 0.025(4) Uiso 1 1 d . . . H37 H 0.1287 0.8823 0.3377 0.030 Uiso 1 1 calc R . . C38 C 0.1714(5) 0.9271(8) 0.3865(4) 0.030(4) Uiso 1 1 d . . . C39 C 0.1817(5) 0.9385(7) 0.4320(4) 0.021(3) Uiso 1 1 d . . . H39 H 0.2094 0.9644 0.4431 0.025 Uiso 1 1 calc R . . C40 C 0.1495(5) 0.9102(8) 0.4589(4) 0.025(4) Uiso 1 1 d . . . C41 C 0.1094(5) 0.8664(8) 0.4426(4) 0.020(3) Uiso 1 1 d . . . N42 N 0.0724(4) 0.8325(6) 0.4610(3) 0.022(3) Uiso 1 1 d . . . H42 H 0.0698 0.8292 0.4886 0.027 Uiso 1 1 calc R . . C43 C 0.0402(5) 0.8046(8) 0.4298(4) 0.021(3) Uiso 1 1 d . . . N44 N 0.1564(4) 0.9157(6) 0.5061(3) 0.021(3) Uiso 1 1 d . . . H44 H 0.1380 0.8872 0.5206 0.026 Uiso 1 1 calc R . . C45 C 0.1887(6) 0.9607(9) 0.5295(5) 0.034(4) Uiso 1 1 d . . . O46 O 0.2177(4) 1.0033(6) 0.5132(3) 0.050(3) Uiso 1 1 d . . . C47 C 0.1823(6) 0.9613(10) 0.5778(5) 0.050(5) Uiso 1 1 d D . . H47A H 0.1623 1.0053 0.5845 0.060 Uiso 1 1 calc R . . H47B H 0.1659 0.9140 0.5855 0.060 Uiso 1 1 calc R . . C48 C 0.2295(6) 0.9667(10) 0.6049(5) 0.053(5) Uiso 1 1 d D . . H48A H 0.2471 1.0115 0.5953 0.064 Uiso 1 1 calc R . . H48B H 0.2483 0.9204 0.5999 0.064 Uiso 1 1 calc R . . C49 C 0.2240(6) 0.9746(9) 0.6546(5) 0.047(5) Uiso 1 1 d D . . H49A H 0.2558 0.9787 0.6698 0.057 Uiso 1 1 calc R . . H49B H 0.2070 1.0228 0.6596 0.057 Uiso 1 1 calc R . . C50 C 0.1978(6) 0.9085(9) 0.6741(5) 0.052(5) Uiso 1 1 d D . . H50A H 0.2111 0.8595 0.6649 0.062 Uiso 1 1 calc R . . H50B H 0.1642 0.9102 0.6631 0.062 Uiso 1 1 calc R . . C51 C 0.2013(6) 0.9112(10) 0.7240(4) 0.050(5) Uiso 1 1 d D . . H51A H 0.2331 0.8963 0.7354 0.075 Uiso 1 1 calc R . . H51B H 0.1782 0.8759 0.7346 0.075 Uiso 1 1 calc R . . H51C H 0.1946 0.9633 0.7335 0.075 Uiso 1 1 calc R . . N3B N -0.0511(4) 0.6843(6) 0.5315(3) 0.024(3) Uiso 1 1 d . . . H3B H -0.0228 0.6850 0.5450 0.028 Uiso 1 1 calc R . . C31B C -0.0896(5) 0.6609(8) 0.5549(4) 0.026(4) Uiso 1 1 d . . . C32B C -0.1362(5) 0.6546(7) 0.5382(4) 0.021(3) Uiso 1 1 d . . . H32B H -0.1432 0.6626 0.5084 0.026 Uiso 1 1 calc R . . C33B C -0.1740(5) 0.6369(8) 0.5634(4) 0.029(4) Uiso 1 1 d . . . C34B C -0.1647(5) 0.6217(7) 0.6085(4) 0.019(3) Uiso 1 1 d . . . H34B H -0.1897 0.6093 0.6255 0.023 Uiso 1 1 calc R . . C35B C -0.1181(5) 0.6256(8) 0.6269(4) 0.020(3) Uiso 1 1 d . . . C36B C -0.0952(5) 0.6159(8) 0.6694(4) 0.023(4) Uiso 1 1 d . . . C37B C -0.1123(6) 0.5972(8) 0.7094(4) 0.034(4) Uiso 1 1 d . . . H37B H -0.1449 0.5883 0.7120 0.040 Uiso 1 1 calc R . . C38B C -0.0792(5) 0.5925(8) 0.7448(4) 0.018(3) Uiso 1 1 d . . . C39B C -0.0314(5) 0.6064(8) 0.7443(4) 0.023(4) Uiso 1 1 d . . . H39B H -0.0114 0.6038 0.7700 0.028 Uiso 1 1 calc R . . C40B C -0.0120(5) 0.6248(8) 0.7045(4) 0.022(3) Uiso 1 1 d . . . C41B C -0.0465(5) 0.6296(8) 0.6677(4) 0.020(3) Uiso 1 1 d . . . N42B N -0.0367(4) 0.6468(6) 0.6247(3) 0.025(3) Uiso 1 1 d . . . H42B H -0.0090 0.6566 0.6156 0.030 Uiso 1 1 calc R . . C43B C -0.0805(5) 0.6447(8) 0.5998(4) 0.022(3) Uiso 1 1 d . . . N44B N 0.0355(4) 0.6418(6) 0.7002(3) 0.026(3) Uiso 1 1 d . . . H44B H 0.0410 0.6650 0.6763 0.031 Uiso 1 1 calc R . . C45B C 0.0742(6) 0.6277(9) 0.7275(5) 0.043(5) Uiso 1 1 d . . . O46B O 0.0717(4) 0.5982(6) 0.7647(3) 0.046(3) Uiso 1 1 d . . . C47B C 0.1222(6) 0.6490(12) 0.7105(6) 0.072(6) Uiso 1 1 d D B . H47C H 0.1279 0.6143 0.6866 0.086 Uiso 1 1 calc R . . H47D H 0.1200 0.7016 0.6990 0.086 Uiso 1 1 calc R . . C48B C 0.1644(6) 0.6447(12) 0.7436(6) 0.081(7) Uiso 1 1 d DU . . H48C H 0.1708 0.5908 0.7518 0.097 Uiso 1 1 calc R A 1 H48D H 0.1577 0.6735 0.7696 0.097 Uiso 1 1 calc R A 1 C49B C 0.2095(9) 0.6806(18) 0.7235(10) 0.081(10) Uiso 0.65(2) 1 d PDU B 1 H49C H 0.2009 0.7293 0.7089 0.097 Uiso 0.65(2) 1 calc PR B 1 H49D H 0.2348 0.6909 0.7464 0.097 Uiso 0.65(2) 1 calc PR B 1 C50B C 0.2268(11) 0.6225(19) 0.6914(11) 0.094(11) Uiso 0.65(2) 1 d PDU B 1 H50C H 0.2049 0.6219 0.6651 0.112 Uiso 0.65(2) 1 calc PR B 1 H50D H 0.2276 0.5706 0.7040 0.112 Uiso 0.65(2) 1 calc PR B 1 C51B C 0.2769(11) 0.646(2) 0.6802(12) 0.098(12) Uiso 0.65(2) 1 d PDU B 1 H51D H 0.2770 0.7003 0.6726 0.147 Uiso 0.65(2) 1 calc PR B 1 H51E H 0.2858 0.6154 0.6560 0.147 Uiso 0.65(2) 1 calc PR B 1 H51F H 0.2995 0.6371 0.7051 0.147 Uiso 0.65(2) 1 calc PR B 1 C1C C 0.5393(5) 0.2075(7) 0.4859(4) 0.017(3) Uiso 1 1 d . . . O2C O 0.5743(3) 0.1902(5) 0.4660(3) 0.030(3) Uiso 1 1 d . . . N3C N 0.5381(4) 0.1883(6) 0.5301(3) 0.019(3) Uiso 1 1 d . . . H3C H 0.5104 0.1883 0.5405 0.023 Uiso 1 1 calc R . . C31C C 0.5773(5) 0.1693(7) 0.5585(4) 0.019(3) Uiso 1 1 d . . . C32C C 0.6240(5) 0.1661(7) 0.5484(4) 0.016(3) Uiso 1 1 d . . . H32C H 0.6311 0.1735 0.5196 0.019 Uiso 1 1 calc R . . C33C C 0.6617(5) 0.1516(8) 0.5809(4) 0.022(4) Uiso 1 1 d . . . C34C C 0.6545(5) 0.1412(8) 0.6236(4) 0.025(4) Uiso 1 1 d . . . H34C H 0.6800 0.1342 0.6448 0.030 Uiso 1 1 calc R . . C35C C 0.6065(5) 0.1416(7) 0.6341(4) 0.017(3) Uiso 1 1 d . . . C36C C 0.5845(5) 0.1336(7) 0.6764(4) 0.014(3) Uiso 1 1 d . . . C37C C 0.6039(5) 0.1179(7) 0.7186(4) 0.019(3) Uiso 1 1 d . . . H37C H 0.6368 0.1117 0.7256 0.023 Uiso 1 1 calc R . . C38C C 0.5706(5) 0.1124(8) 0.7494(4) 0.025(4) Uiso 1 1 d . . . C39C C 0.5212(5) 0.1219(7) 0.7404(4) 0.023(4) Uiso 1 1 d . . . H39C H 0.5009 0.1171 0.7627 0.028 Uiso 1 1 calc R . . C40C C 0.5020(5) 0.1387(7) 0.6975(4) 0.017(3) Uiso 1 1 d . . . C41C C 0.5355(5) 0.1419(8) 0.6667(4) 0.021(3) Uiso 1 1 d . . . N42C N 0.5249(4) 0.1556(6) 0.6213(3) 0.020(3) Uiso 1 1 d . . . H42C H 0.4969 0.1627 0.6078 0.024 Uiso 1 1 calc R . . C43C C 0.5690(5) 0.1552(7) 0.6031(4) 0.018(3) Uiso 1 1 d . . . N44C N 0.4529(4) 0.1500(6) 0.6854(3) 0.018(3) Uiso 1 1 d . . . H44C H 0.4467 0.1706 0.6601 0.021 Uiso 1 1 calc R . . C45C C 0.4139(5) 0.1339(8) 0.7068(4) 0.020(3) Uiso 1 1 d . . . O46C O 0.4176(3) 0.1003(5) 0.7429(3) 0.027(2) Uiso 1 1 d . . . C47C C 0.3666(5) 0.1523(8) 0.6830(4) 0.022(3) Uiso 1 1 d . . . H47E H 0.3595 0.1125 0.6610 0.027 Uiso 1 1 calc R . . H47F H 0.3693 0.2017 0.6680 0.027 Uiso 1 1 calc R . . C48C C 0.3252(5) 0.1572(8) 0.7106(4) 0.026(4) Uiso 1 1 d . . . H48E H 0.3211 0.1069 0.7242 0.032 Uiso 1 1 calc R . . H48F H 0.3330 0.1948 0.7338 0.032 Uiso 1 1 calc R . . C49C C 0.2790(5) 0.1800(8) 0.6867(4) 0.027(4) Uiso 1 1 d . . . H49E H 0.2716 0.1422 0.6636 0.032 Uiso 1 1 calc R . . H49F H 0.2835 0.2301 0.6729 0.032 Uiso 1 1 calc R . . C50C C 0.2358(6) 0.1864(9) 0.7134(5) 0.042(4) Uiso 1 1 d . . . H50E H 0.2434 0.2226 0.7373 0.051 Uiso 1 1 calc R . . H50F H 0.2299 0.1357 0.7261 0.051 Uiso 1 1 calc R . . C51C C 0.1898(6) 0.2136(10) 0.6874(5) 0.053(5) Uiso 1 1 d . . . H51G H 0.1933 0.2670 0.6788 0.079 Uiso 1 1 calc R . . H51H H 0.1632 0.2093 0.7053 0.079 Uiso 1 1 calc R . . H51I H 0.1838 0.1816 0.6619 0.079 Uiso 1 1 calc R . . N3D N 0.5008(4) 0.2446(6) 0.4697(3) 0.023(3) Uiso 1 1 d . . . H3D H 0.4815 0.2607 0.4882 0.027 Uiso 1 1 calc R . . C31D C 0.4866(5) 0.2620(8) 0.4236(4) 0.024(4) Uiso 1 1 d . . . C32D C 0.5148(5) 0.2362(8) 0.3914(4) 0.023(4) Uiso 1 1 d . . . H32D H 0.5438 0.2104 0.3980 0.027 Uiso 1 1 calc R . . C33D C 0.4970(5) 0.2512(8) 0.3486(4) 0.024(4) Uiso 1 1 d . . . C34D C 0.4566(5) 0.2911(7) 0.3354(4) 0.016(3) Uiso 1 1 d . . . H34D H 0.4471 0.2997 0.3061 0.019 Uiso 1 1 calc R . . C35D C 0.4294(5) 0.3190(8) 0.3693(4) 0.021(3) Uiso 1 1 d . . . C36D C 0.3860(5) 0.3653(7) 0.3702(4) 0.019(3) Uiso 1 1 d . . . C37D C 0.3542(5) 0.3958(7) 0.3386(4) 0.017(3) Uiso 1 1 d . . . H37D H 0.3573 0.3866 0.3092 0.021 Uiso 1 1 calc R . . C38D C 0.3175(5) 0.4405(8) 0.3517(4) 0.021(3) Uiso 1 1 d . . . C39D C 0.3102(5) 0.4553(8) 0.3956(4) 0.022(4) Uiso 1 1 d . . . H39D H 0.2847 0.4863 0.4029 0.027 Uiso 1 1 calc R . . C40D C 0.3416(5) 0.4231(8) 0.4276(4) 0.019(3) Uiso 1 1 d . . . C41D C 0.3795(5) 0.3768(8) 0.4155(4) 0.021(3) Uiso 1 1 d . . . N42D N 0.4145(4) 0.3384(6) 0.4401(3) 0.021(3) Uiso 1 1 d . . . H42D H 0.4169 0.3350 0.4681 0.026 Uiso 1 1 calc R . . C43D C 0.4459(5) 0.3055(7) 0.4126(4) 0.017(3) Uiso 1 1 d . . . N44D N 0.3399(4) 0.4358(7) 0.4733(3) 0.027(3) Uiso 1 1 d . . . H44D H 0.3533 0.4009 0.4904 0.033 Uiso 1 1 calc R . . C45D C 0.3191(5) 0.4977(8) 0.4932(4) 0.022(3) Uiso 1 1 d . . . O46D O 0.2936(3) 0.5470(5) 0.4723(3) 0.029(2) Uiso 1 1 d . . . C47D C 0.3320(6) 0.5017(9) 0.5422(4) 0.039(4) Uiso 1 1 d . . . H47G H 0.3617 0.4733 0.5491 0.047 Uiso 1 1 calc R . . H47H H 0.3378 0.5558 0.5504 0.047 Uiso 1 1 calc R . . C48D C 0.2938(5) 0.4689(9) 0.5693(4) 0.031(4) Uiso 1 1 d . . . H48G H 0.2669 0.5051 0.5685 0.038 Uiso 1 1 calc R . . H48H H 0.2820 0.4201 0.5565 0.038 Uiso 1 1 calc R . . C49D C 0.3119(6) 0.4550(9) 0.6155(4) 0.038(4) Uiso 1 1 d . . . H49G H 0.3261 0.5030 0.6275 0.046 Uiso 1 1 calc R . . H49H H 0.3372 0.4160 0.6163 0.046 Uiso 1 1 calc R . . C50D C 0.2738(6) 0.4280(10) 0.6443(5) 0.044(4) Uiso 1 1 d . . . H50G H 0.2593 0.3803 0.6324 0.053 Uiso 1 1 calc R . . H50H H 0.2487 0.4673 0.6442 0.053 Uiso 1 1 calc R . . C51D C 0.2947(6) 0.4131(10) 0.6925(5) 0.058(5) Uiso 1 1 d . . . H51J H 0.3188 0.3730 0.6929 0.086 Uiso 1 1 calc R . . H51K H 0.2693 0.3967 0.7097 0.086 Uiso 1 1 calc R . . H51L H 0.3088 0.4603 0.7045 0.086 Uiso 1 1 calc R . . N9 N 0.5365(4) 0.4105(6) 0.6728(3) 0.024(3) Uiso 1 1 d . . . C91 C 0.5135(4) 0.4843(7) 0.6523(4) 0.024(4) Uiso 1 1 d D . . H91A H 0.5063 0.5194 0.6757 0.029 Uiso 1 1 calc R . . H91B H 0.5371 0.5100 0.6358 0.029 Uiso 1 1 calc R . . C92 C 0.4677(4) 0.4734(7) 0.6223(4) 0.027(4) Uiso 1 1 d D . . H92A H 0.4408 0.4644 0.6398 0.033 Uiso 1 1 calc R . . H92B H 0.4711 0.4279 0.6040 0.033 Uiso 1 1 calc R . . C93 C 0.4575(5) 0.5451(7) 0.5935(4) 0.033(4) Uiso 1 1 d D . . H93A H 0.4233 0.5484 0.5848 0.039 Uiso 1 1 calc R . . H93B H 0.4669 0.5919 0.6099 0.039 Uiso 1 1 calc R . . C94 C 0.4851(5) 0.5397(9) 0.5535(4) 0.043(4) Uiso 1 1 d D . . H94A H 0.5187 0.5329 0.5623 0.064 Uiso 1 1 calc R . . H94B H 0.4806 0.5867 0.5367 0.064 Uiso 1 1 calc R . . H94C H 0.4737 0.4959 0.5361 0.064 Uiso 1 1 calc R . . C91B C 0.5745(5) 0.4343(8) 0.7088(4) 0.021(3) Uiso 1 1 d . . . H91C H 0.5961 0.4713 0.6966 0.026 Uiso 1 1 calc R . . H91D H 0.5586 0.4612 0.7313 0.026 Uiso 1 1 calc R . . C92B C 0.6031(5) 0.3717(8) 0.7290(4) 0.028(4) Uiso 1 1 d . . . H92C H 0.6219 0.3478 0.7075 0.034 Uiso 1 1 calc R . . H92D H 0.5819 0.3321 0.7393 0.034 Uiso 1 1 calc R . . C93B C 0.6375(6) 0.4011(10) 0.7680(5) 0.054(5) Uiso 1 1 d . . . H93C H 0.6593 0.4397 0.7577 0.064 Uiso 1 1 calc R . . H93D H 0.6188 0.4259 0.7894 0.064 Uiso 1 1 calc R . . C94B C 0.6669(6) 0.3324(10) 0.7898(5) 0.059(5) Uiso 1 1 d . . . H94D H 0.6459 0.2993 0.8048 0.089 Uiso 1 1 calc R . . H94E H 0.6916 0.3527 0.8104 0.089 Uiso 1 1 calc R . . H94F H 0.6813 0.3029 0.7678 0.089 Uiso 1 1 calc R . . C91C C 0.4983(5) 0.3591(8) 0.6901(4) 0.026(4) Uiso 1 1 d . . . H91E H 0.4760 0.3430 0.6658 0.031 Uiso 1 1 calc R . . H91F H 0.5135 0.3125 0.7026 0.031 Uiso 1 1 calc R . . C92C C 0.4703(5) 0.3971(8) 0.7240(4) 0.032(4) Uiso 1 1 d . . . H92E H 0.4574 0.4467 0.7131 0.039 Uiso 1 1 calc R . . H92F H 0.4913 0.4070 0.7502 0.039 Uiso 1 1 calc R . . C93C C 0.4287(5) 0.3432(8) 0.7348(4) 0.031(4) Uiso 1 1 d . . . H93E H 0.4418 0.2921 0.7427 0.038 Uiso 1 1 calc R . . H93F H 0.4068 0.3370 0.7089 0.038 Uiso 1 1 calc R . . C94C C 0.4003(6) 0.3735(9) 0.7724(5) 0.045(5) Uiso 1 1 d . . . H94G H 0.4214 0.3776 0.7986 0.068 Uiso 1 1 calc R . . H94H H 0.3747 0.3378 0.7771 0.068 Uiso 1 1 calc R . . H94I H 0.3870 0.4239 0.7649 0.068 Uiso 1 1 calc R . . C91D C 0.5599(5) 0.3653(8) 0.6373(4) 0.025(4) Uiso 1 1 d . . . H91G H 0.5682 0.3135 0.6484 0.030 Uiso 1 1 calc R . . H91H H 0.5364 0.3591 0.6124 0.030 Uiso 1 1 calc R . . C92D C 0.6047(5) 0.4026(8) 0.6218(4) 0.026(4) Uiso 1 1 d . . . H92G H 0.6299 0.4024 0.6456 0.032 Uiso 1 1 calc R . . H92H H 0.5977 0.4566 0.6141 0.032 Uiso 1 1 calc R . . C93D C 0.6230(6) 0.3608(9) 0.5823(4) 0.040(4) Uiso 1 1 d . . . H93G H 0.6255 0.3053 0.5884 0.048 Uiso 1 1 calc R . . H93H H 0.6549 0.3799 0.5776 0.048 Uiso 1 1 calc R . . C94D C 0.5889(6) 0.3740(9) 0.5403(4) 0.038(4) Uiso 1 1 d . . . H94J H 0.5569 0.3580 0.5455 0.057 Uiso 1 1 calc R . . H94K H 0.6000 0.3437 0.5168 0.057 Uiso 1 1 calc R . . H94L H 0.5888 0.4283 0.5327 0.057 Uiso 1 1 calc R . . N6 N 0.3378(5) 0.1048(7) 0.4736(4) 0.037(3) Uiso 1 1 d . C . C61 C 0.3281(5) 0.1748(8) 0.5029(4) 0.040(4) Uiso 1 1 d D . . H61A H 0.3502 0.1727 0.5290 0.048 Uiso 1 1 calc R . . H61B H 0.3345 0.2225 0.4875 0.048 Uiso 1 1 calc R . . C62 C 0.2768(5) 0.1778(8) 0.5164(4) 0.040(4) Uiso 1 1 d D . . H62A H 0.2556 0.1969 0.4921 0.047 Uiso 1 1 calc R . . H62B H 0.2666 0.1254 0.5232 0.047 Uiso 1 1 calc R . . C63 C 0.2722(5) 0.2296(9) 0.5556(5) 0.052(5) Uiso 1 1 d D . . H63A H 0.2836 0.2815 0.5493 0.062 Uiso 1 1 calc R . . H63B H 0.2922 0.2092 0.5803 0.062 Uiso 1 1 calc R . . C64 C 0.2208(5) 0.2347(10) 0.5672(5) 0.055(5) Uiso 1 1 d D . . H64A H 0.2052 0.2784 0.5525 0.083 Uiso 1 1 calc R . . H64B H 0.2204 0.2412 0.5982 0.083 Uiso 1 1 calc R . . H64C H 0.2041 0.1876 0.5584 0.083 Uiso 1 1 calc R . . C61B C 0.3900(7) 0.1125(10) 0.4602(5) 0.064(6) Uiso 1 1 d D . . H61C H 0.4125 0.1024 0.4849 0.076 Uiso 0.617(18) 1 d P C 1 H61D H 0.3948 0.1662 0.4505 0.076 Uiso 0.617(18) 1 d P C 1 H61Y H 0.3887 0.1467 0.4345 0.076 Uiso 0.383(18) 1 d P C 2 H61Z H 0.4088 0.1395 0.4834 0.076 Uiso 0.383(18) 1 d P C 2 C62B C 0.3987(8) 0.0550(15) 0.4222(8) 0.059(8) Uiso 0.617(18) 1 d PDU C 1 H62C H 0.3925 0.0019 0.4311 0.071 Uiso 0.617(18) 1 calc PR C 1 H62D H 0.3767 0.0671 0.3969 0.071 Uiso 0.617(18) 1 calc PR C 1 C63B C 0.4499(8) 0.062(2) 0.4102(8) 0.076(9) Uiso 0.617(18) 1 d PDU C 1 H63C H 0.4569 0.1157 0.4033 0.092 Uiso 0.617(18) 1 calc PR C 1 H63D H 0.4541 0.0304 0.3845 0.092 Uiso 0.617(18) 1 calc PR C 1 C64B C 0.4845(9) 0.034(2) 0.4478(9) 0.078(9) Uiso 0.617(18) 1 d PDU C 1 H64D H 0.4822 0.0681 0.4724 0.118 Uiso 0.617(18) 1 calc PR C 1 H64E H 0.5168 0.0355 0.4391 0.118 Uiso 0.617(18) 1 calc PR C 1 H64F H 0.4765 -0.0181 0.4556 0.118 Uiso 0.617(18) 1 calc PR C 1 C61C C 0.3015(6) 0.1028(9) 0.4356(5) 0.052(5) Uiso 1 1 d D . . H61E H 0.2698 0.0993 0.4464 0.062 Uiso 1 1 calc R C . H61F H 0.3064 0.0556 0.4191 0.062 Uiso 1 1 calc R . . C62C C 0.3018(6) 0.1734(10) 0.4041(5) 0.054(5) Uiso 1 1 d D C . H62E H 0.3042 0.2215 0.4209 0.065 Uiso 1 1 calc R . . H62F H 0.3295 0.1701 0.3872 0.065 Uiso 1 1 calc R . . C63C C 0.2556(8) 0.1743(12) 0.3732(6) 0.094(8) Uiso 1 1 d D . . H63E H 0.2523 0.1257 0.3571 0.113 Uiso 1 1 calc R C . H63F H 0.2277 0.1804 0.3898 0.113 Uiso 1 1 calc R . . C64C C 0.2589(7) 0.2427(11) 0.3418(6) 0.087(7) Uiso 1 1 d D C . H64G H 0.2587 0.2909 0.3578 0.131 Uiso 1 1 calc R . . H64H H 0.2319 0.2415 0.3202 0.131 Uiso 1 1 calc R . . H64I H 0.2882 0.2389 0.3277 0.131 Uiso 1 1 calc R . . C61D C 0.3334(5) 0.0298(8) 0.4990(4) 0.037(4) Uiso 1 1 d DU . . H61G H 0.3423 -0.0132 0.4808 0.044 Uiso 1 1 calc R C . H61H H 0.2999 0.0228 0.5042 0.044 Uiso 1 1 calc R . . C62D C 0.3637(7) 0.0241(9) 0.5430(5) 0.085(6) Uiso 1 1 d DU C . H62G H 0.3974 0.0282 0.5380 0.102 Uiso 1 1 calc R . . H62H H 0.3559 0.0681 0.5611 0.102 Uiso 1 1 calc R . . C63D C 0.3561(7) -0.0495(9) 0.5674(5) 0.068(6) Uiso 1 1 d DU . . H63G H 0.3222 -0.0546 0.5718 0.082 Uiso 1 1 calc R C . H63H H 0.3651 -0.0935 0.5500 0.082 Uiso 1 1 calc R . . C64D C 0.3845(7) -0.0516(12) 0.6106(5) 0.090(7) Uiso 1 1 d DU C . H64J H 0.4145 -0.0249 0.6086 0.134 Uiso 1 1 calc R . . H64K H 0.3907 -0.1049 0.6190 0.134 Uiso 1 1 calc R . . H64L H 0.3667 -0.0265 0.6320 0.134 Uiso 1 1 calc R . . N7 N 0.0501(5) 0.1022(7) 0.3371(4) 0.042(4) Uiso 1 1 d . D . C71 C 0.0137(5) 0.1513(9) 0.3098(4) 0.040(4) Uiso 1 1 d D . . H71A H 0.0301 0.1970 0.2998 0.048 Uiso 1 1 calc R . . H71B H -0.0102 0.1695 0.3286 0.048 Uiso 1 1 calc R . . C72 C -0.0129(5) 0.1120(9) 0.2697(4) 0.044(5) Uiso 1 1 d D . . H72A H 0.0093 0.1031 0.2476 0.053 Uiso 1 1 calc R . . H72B H -0.0255 0.0619 0.2781 0.053 Uiso 1 1 calc R . . C73 C -0.0540(6) 0.1638(10) 0.2514(5) 0.070(6) Uiso 1 1 d D . . H73A H -0.0774 0.1691 0.2728 0.084 Uiso 1 1 calc R . . H73B H -0.0417 0.2154 0.2456 0.084 Uiso 1 1 calc R . . C74 C -0.0780(7) 0.1300(11) 0.2098(5) 0.074(6) Uiso 1 1 d D . . H74A H -0.0539 0.1165 0.1905 0.111 Uiso 1 1 calc R . . H74B H -0.0996 0.1678 0.1960 0.111 Uiso 1 1 calc R . . H74C H -0.0957 0.0841 0.2165 0.111 Uiso 1 1 calc R . . C71B C 0.0723(6) 0.1516(11) 0.3749(5) 0.065(6) Uiso 1 1 d D . . H71C H 0.0478 0.1633 0.3947 0.078 Uiso 0.635(17) 1 d P D 1 H71D H 0.0835 0.2007 0.3637 0.078 Uiso 0.635(17) 1 d P D 1 H71Y H 0.0778 0.2016 0.3613 0.078 Uiso 0.365(17) 1 d P D 2 H71Z H 0.0454 0.1606 0.3925 0.078 Uiso 0.365(17) 1 d P D 2 C72B C 0.1152(7) 0.1069(13) 0.3991(6) 0.057(8) Uiso 0.635(17) 1 d PDU D 1 H72C H 0.1049 0.0538 0.4040 0.068 Uiso 0.635(17) 1 calc PR D 1 H72D H 0.1410 0.1043 0.3798 0.068 Uiso 0.635(17) 1 calc PR D 1 C73B C 0.1352(8) 0.1402(16) 0.4419(6) 0.056(7) Uiso 0.635(17) 1 d PDU D 1 H73C H 0.1394 0.1960 0.4385 0.067 Uiso 0.635(17) 1 calc PR D 1 H73D H 0.1666 0.1176 0.4496 0.067 Uiso 0.635(17) 1 calc PR D 1 C74B C 0.1040(10) 0.1262(16) 0.4786(7) 0.049(7) Uiso 0.635(17) 1 d PDU D 1 H74D H 0.0708 0.1316 0.4680 0.073 Uiso 0.635(17) 1 calc PR D 1 H74E H 0.1117 0.1635 0.5014 0.073 Uiso 0.635(17) 1 calc PR D 1 H74F H 0.1096 0.0744 0.4899 0.073 Uiso 0.635(17) 1 calc PR D 1 C71C C 0.0237(5) 0.0303(10) 0.3529(5) 0.062(6) Uiso 1 1 d D . . H71E H 0.0141 -0.0021 0.3278 0.074 Uiso 1 1 calc R D . H71F H 0.0463 0.0003 0.3720 0.074 Uiso 1 1 calc R . . C72C C -0.0204(6) 0.0466(9) 0.3771(5) 0.052(5) Uiso 1 1 d D D . H72E H -0.0131 0.0905 0.3965 0.062 Uiso 1 1 calc R E 1 H72F H -0.0462 0.0627 0.3559 0.062 Uiso 1 1 calc R E 1 C73C C -0.0391(9) -0.0190(16) 0.4038(6) 0.065(8) Uiso 0.587(19) 1 d PD D 1 H73E H -0.0730 -0.0114 0.4072 0.078 Uiso 0.587(19) 1 calc PR D 1 H73F H -0.0352 -0.0686 0.3893 0.078 Uiso 0.587(19) 1 calc PR D 1 C74C C -0.0109(11) -0.0190(16) 0.4479(3) 0.063(8) Uiso 0.587(19) 1 d PD D 1 H74G H -0.0141 0.0309 0.4616 0.094 Uiso 0.587(19) 1 calc PR D 1 H74H H 0.0224 -0.0289 0.4443 0.094 Uiso 0.587(19) 1 calc PR D 1 H74I H -0.0231 -0.0590 0.4658 0.094 Uiso 0.587(19) 1 calc PR D 1 C73Z C -0.0189(14) -0.0314(17) 0.4014(12) 0.065(8) Uiso 0.413(19) 1 d PD D 2 H73Y H -0.0164 -0.0752 0.3817 0.078 Uiso 0.413(19) 1 calc PR D 2 H73Z H 0.0073 -0.0334 0.4243 0.078 Uiso 0.413(19) 1 calc PR D 2 C74Z C -0.0676(12) -0.029(3) 0.4201(13) 0.063(8) Uiso 0.413(19) 1 d PD D 2 H74J H -0.0666 -0.0602 0.4462 0.094 Uiso 0.413(19) 1 calc PR D 2 H74K H -0.0918 -0.0493 0.3990 0.094 Uiso 0.413(19) 1 calc PR D 2 H74L H -0.0754 0.0239 0.4271 0.094 Uiso 0.413(19) 1 calc PR D 2 C71D C 0.0900(7) 0.0755(11) 0.3079(6) 0.066(6) Uiso 1 1 d D . . H71G H 0.1114 0.0399 0.3247 0.079 Uiso 1 1 calc R D . H71H H 0.0749 0.0465 0.2833 0.079 Uiso 1 1 calc R . . C72D C 0.1200(8) 0.1404(12) 0.2905(6) 0.085(7) Uiso 1 1 d D D . H72G H 0.1318 0.1729 0.3149 0.102 Uiso 1 1 calc R . . H72H H 0.0990 0.1725 0.2711 0.102 Uiso 1 1 calc R . . C73D C 0.1627(8) 0.1161(14) 0.2661(7) 0.110(9) Uiso 1 1 d D . . H73G H 0.1812 0.1619 0.2594 0.132 Uiso 1 1 calc R D . H73H H 0.1835 0.0818 0.2843 0.132 Uiso 1 1 calc R . . C74D C 0.1461(8) 0.0755(14) 0.2251(7) 0.113(9) Uiso 1 1 d D D . H74M H 0.1264 0.0318 0.2316 0.170 Uiso 1 1 calc R . . H74N H 0.1734 0.0574 0.2110 0.170 Uiso 1 1 calc R . . H74O H 0.1277 0.1109 0.2061 0.170 Uiso 1 1 calc R . . N8 N 0.1635(5) 0.6237(8) 0.4719(4) 0.053(4) Uiso 1 1 d . G . C81 C 0.1817(5) 0.6948(10) 0.4993(6) 0.064(6) Uiso 1 1 d D . . H81A H 0.1769 0.7412 0.4814 0.077 Uiso 1 1 calc R . . H81B H 0.1621 0.7002 0.5237 0.077 Uiso 1 1 calc R . . C82 C 0.2345(5) 0.6917(9) 0.5171(5) 0.045(5) Uiso 1 1 d D . . H82A H 0.2405 0.6429 0.5326 0.054 Uiso 1 1 calc R . . H82B H 0.2546 0.6925 0.4928 0.054 Uiso 1 1 calc R . . C83 C 0.2487(5) 0.7580(9) 0.5471(5) 0.055(5) Uiso 1 1 d D . . H83A H 0.2266 0.7602 0.5699 0.067 Uiso 1 1 calc R . . H83B H 0.2455 0.8065 0.5308 0.067 Uiso 1 1 calc R . . C84 C 0.2990(6) 0.7517(11) 0.5680(6) 0.073(6) Uiso 1 1 d D . . H84A H 0.3027 0.7031 0.5835 0.109 Uiso 1 1 calc R . . H84B H 0.3052 0.7941 0.5881 0.109 Uiso 1 1 calc R . . H84C H 0.3213 0.7538 0.5459 0.109 Uiso 1 1 calc R . . C81B C 0.1095(7) 0.6372(12) 0.4572(7) 0.088(7) Uiso 1 1 d D . . H81C H 0.0910 0.6353 0.4825 0.105 Uiso 1 1 calc R F 1 H81D H 0.1055 0.6885 0.4442 0.105 Uiso 1 1 calc R F 1 C82B C 0.0906(9) 0.5752(16) 0.4240(8) 0.106(12) Uiso 0.62(2) 1 d PDU G 1 H82C H 0.1055 0.5838 0.3970 0.128 Uiso 0.62(2) 1 calc PR G 1 H82D H 0.1009 0.5243 0.4351 0.128 Uiso 0.62(2) 1 calc PR G 1 C83B C 0.0372(9) 0.5732(19) 0.4137(9) 0.094(11) Uiso 0.62(2) 1 d PDU G 1 H83C H 0.0298 0.5474 0.3858 0.113 Uiso 0.62(2) 1 calc PR G 1 H83D H 0.0251 0.6263 0.4110 0.113 Uiso 0.62(2) 1 calc PR G 1 C84B C 0.0121(9) 0.5313(19) 0.4482(9) 0.156(19) Uiso 0.62(2) 1 d PRDU G 1 H84M H 0.0106 0.4766 0.4417 0.233 Uiso 0.62(2) 1 calc PR G 1 H84N H -0.0199 0.5515 0.4490 0.233 Uiso 0.62(2) 1 calc PR G 1 H84O H 0.0296 0.5391 0.4762 0.233 Uiso 0.62(2) 1 calc PR G 1 C81C C 0.1926(6) 0.6110(9) 0.4352(5) 0.052(5) Uiso 1 1 d D . . H81E H 0.1822 0.5628 0.4208 0.062 Uiso 1 1 calc R G . H81F H 0.2258 0.6038 0.4467 0.062 Uiso 1 1 calc R . . C82C C 0.1910(7) 0.6772(10) 0.4003(5) 0.061(5) Uiso 1 1 d D G . H82E H 0.1586 0.6820 0.3863 0.074 Uiso 1 1 calc R . . H82F H 0.1998 0.7265 0.4143 0.074 Uiso 1 1 calc R . . C83C C 0.2257(8) 0.6580(12) 0.3664(6) 0.094(8) Uiso 1 1 d D . . H83E H 0.2577 0.6514 0.3809 0.113 Uiso 1 1 calc R G . H83F H 0.2163 0.6089 0.3524 0.113 Uiso 1 1 calc R . . C84C C 0.2270(7) 0.7196(11) 0.3325(6) 0.083(7) Uiso 1 1 d D G . H84G H 0.1960 0.7235 0.3165 0.124 Uiso 1 1 calc R . . H84H H 0.2507 0.7063 0.3128 0.124 Uiso 1 1 calc R . . H84I H 0.2352 0.7686 0.3462 0.124 Uiso 1 1 calc R . . C81D C 0.1693(6) 0.5515(10) 0.5019(4) 0.053(5) Uiso 1 1 d D . . H81G H 0.1547 0.5074 0.4860 0.064 Uiso 1 1 calc R G . H81H H 0.2035 0.5404 0.5069 0.064 Uiso 1 1 calc R . . C82D C 0.1486(7) 0.5552(9) 0.5463(5) 0.069(6) Uiso 1 1 d D G . H82G H 0.1690 0.5878 0.5659 0.083 Uiso 1 1 calc R . . H82H H 0.1168 0.5787 0.5429 0.083 Uiso 1 1 calc R . . C83D C 0.1450(7) 0.4753(9) 0.5659(5) 0.073(6) Uiso 1 1 d D . . H83G H 0.1241 0.4430 0.5465 0.087 Uiso 1 1 calc R G . H83H H 0.1766 0.4513 0.5686 0.087 Uiso 1 1 calc R . . C84D C 0.1259(7) 0.4786(12) 0.6096(5) 0.088(7) Uiso 1 1 d D G . H84J H 0.1507 0.4963 0.6309 0.131 Uiso 1 1 calc R . . H84K H 0.1154 0.4275 0.6175 0.131 Uiso 1 1 calc R . . H84L H 0.0992 0.5141 0.6087 0.131 Uiso 1 1 calc R . . O52 O 0.0432(4) 0.8261(6) 0.5421(3) 0.035(3) Uiso 1 1 d . . . C53 C 0.0764(6) 0.7924(8) 0.5637(4) 0.030(4) Uiso 1 1 d . . . O54 O 0.1196(4) 0.8001(6) 0.5615(3) 0.037(3) Uiso 1 1 d . . . C55 C 0.0599(6) 0.7297(9) 0.5947(5) 0.042(4) Uiso 1 1 d . . . O56 O 0.0411(4) 0.6695(6) 0.5777(3) 0.033(3) Uiso 1 1 d . . . O57 O 0.0637(4) 0.7459(6) 0.6353(3) 0.052(3) Uiso 1 1 d . . . O52B O 0.3740(3) 0.3299(5) 0.5385(3) 0.025(2) Uiso 1 1 d . . . C53B C 0.4162(5) 0.3133(7) 0.5451(4) 0.019(3) Uiso 1 1 d . . . O54B O 0.4518(3) 0.3380(5) 0.5267(3) 0.020(2) Uiso 1 1 d . . . C55B C 0.4299(5) 0.2488(8) 0.5792(4) 0.020(3) Uiso 1 1 d . . . O56B O 0.4269(3) 0.2638(5) 0.6196(3) 0.027(2) Uiso 1 1 d . . . O57B O 0.4458(3) 0.1845(5) 0.5652(3) 0.024(2) Uiso 1 1 d . . . Cl3 Cl -0.05100(15) 0.7261(2) 0.31016(11) 0.0382(11) Uani 1 1 d . . . Cl3B Cl -0.23171(14) 0.6329(2) 0.53941(12) 0.0367(10) Uani 1 1 d . . . Cl3C Cl 0.71985(14) 0.1522(2) 0.56432(12) 0.0360(10) Uani 1 1 d . . . Cl3D Cl 0.53232(14) 0.2139(2) 0.30813(11) 0.0321(10) Uani 1 1 d . . . Cl8 Cl 0.21459(15) 0.9663(2) 0.35313(12) 0.0394(11) Uani 1 1 d . . . Cl8B Cl -0.09910(16) 0.5659(2) 0.79634(12) 0.0446(12) Uani 1 1 d . . . Cl8C Cl 0.59218(15) 0.0953(2) 0.80376(11) 0.0373(10) Uani 1 1 d . . . Cl8D Cl 0.27503(15) 0.4811(2) 0.31231(12) 0.0373(11) Uani 1 1 d . . . C49X C 0.2153(13) 0.632(4) 0.7280(16) 0.081(10) Uiso 0.35(2) 1 d PD B 2 H49I H 0.2400 0.6478 0.7505 0.097 Uiso 0.35(2) 1 calc PR B 2 H49J H 0.2203 0.5781 0.7206 0.097 Uiso 0.35(2) 1 calc PR B 2 C50X C 0.2163(12) 0.684(3) 0.6883(19) 0.094(11) Uiso 0.35(2) 1 d PD B 2 H50I H 0.2127 0.7379 0.6968 0.112 Uiso 0.35(2) 1 calc PR B 2 H50J H 0.1894 0.6707 0.6675 0.112 Uiso 0.35(2) 1 calc PR B 2 C51X C 0.263(2) 0.674(4) 0.6669(19) 0.098(12) Uiso 0.35(2) 1 d PD B 2 H51M H 0.2893 0.6688 0.6891 0.147 Uiso 0.35(2) 1 calc PR B 2 H51N H 0.2684 0.7191 0.6493 0.147 Uiso 0.35(2) 1 calc PR B 2 H51O H 0.2613 0.6283 0.6488 0.147 Uiso 0.35(2) 1 calc PR B 2 C82X C 0.0741(13) 0.5744(19) 0.4405(16) 0.106(12) Uiso 0.38(2) 1 d PDU G 2 H82I H 0.0723 0.5830 0.4092 0.128 Uiso 0.38(2) 1 calc PR G 2 H82J H 0.0932 0.5273 0.4451 0.128 Uiso 0.38(2) 1 calc PR G 2 C83X C 0.0243(18) 0.545(4) 0.4466(14) 0.094(11) Uiso 0.38(2) 1 d PDU G 2 H83I H 0.0053 0.5863 0.4583 0.113 Uiso 0.38(2) 1 calc PR G 2 H83J H 0.0260 0.5017 0.4670 0.113 Uiso 0.38(2) 1 calc PR G 2 C84X C 0.0015(18) 0.519(4) 0.4028(18) 0.156(19) Uiso 0.38(2) 1 d PDU G 2 H84D H -0.0244 0.4837 0.4070 0.233 Uiso 0.38(2) 1 calc PR G 2 H84E H 0.0251 0.4932 0.3870 0.233 Uiso 0.38(2) 1 calc PR G 2 H84F H -0.0107 0.5637 0.3866 0.233 Uiso 0.38(2) 1 calc PR G 2 C62Z C 0.4164(15) 0.0372(18) 0.4495(9) 0.059(8) Uiso 0.383(18) 1 d PDU C 2 H62I H 0.4200 0.0058 0.4758 0.071 Uiso 0.383(18) 1 calc PR C 2 H62J H 0.3957 0.0085 0.4281 0.071 Uiso 0.383(18) 1 calc PR C 2 C63Z C 0.4651(13) 0.044(4) 0.4322(12) 0.076(9) Uiso 0.383(18) 1 d PDU C 2 H63I H 0.4844 -0.0016 0.4412 0.092 Uiso 0.383(18) 1 calc PR C 2 H63J H 0.4815 0.0898 0.4442 0.092 Uiso 0.383(18) 1 calc PR C 2 C64Z C 0.4596(17) 0.049(3) 0.3831(11) 0.078(9) Uiso 0.383(18) 1 d PDU C 2 H64M H 0.4467 0.0006 0.3712 0.118 Uiso 0.383(18) 1 calc PR C 2 H64N H 0.4904 0.0584 0.3724 0.118 Uiso 0.383(18) 1 calc PR C 2 H64O H 0.4381 0.0908 0.3743 0.118 Uiso 0.383(18) 1 calc PR C 2 C72Y C 0.1123(11) 0.139(3) 0.4101(8) 0.057(8) Uiso 0.365(17) 1 d PDU D 2 H72I H 0.1290 0.1878 0.4165 0.068 Uiso 0.365(17) 1 calc PR D 2 H72J H 0.1353 0.1020 0.4000 0.068 Uiso 0.365(17) 1 calc PR D 2 C73Y C 0.0927(12) 0.108(3) 0.4511(7) 0.056(7) Uiso 0.365(17) 1 d PDU D 2 H73I H 0.0643 0.1372 0.4574 0.067 Uiso 0.365(17) 1 calc PR D 2 H73J H 0.0839 0.0535 0.4474 0.067 Uiso 0.365(17) 1 calc PR D 2 C74Y C 0.1316(13) 0.117(3) 0.4880(8) 0.049(7) Uiso 0.365(17) 1 d PDU D 2 H74P H 0.1583 0.0842 0.4827 0.073 Uiso 0.365(17) 1 calc PR D 2 H74Q H 0.1192 0.1025 0.5150 0.073 Uiso 0.365(17) 1 calc PR D 2 H74R H 0.1420 0.1705 0.4896 0.073 Uiso 0.365(17) 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl3 0.047(3) 0.041(3) 0.026(2) -0.0068(19) -0.0029(19) -0.014(2) Cl3B 0.039(3) 0.036(2) 0.035(2) 0.0057(19) 0.0031(19) -0.007(2) Cl3C 0.036(3) 0.040(2) 0.033(2) 0.0027(19) 0.0092(19) 0.003(2) Cl3D 0.046(3) 0.031(2) 0.021(2) -0.0033(17) 0.0100(18) 0.013(2) Cl8 0.043(3) 0.033(2) 0.044(2) 0.009(2) 0.014(2) -0.008(2) Cl8B 0.056(3) 0.049(3) 0.030(2) 0.009(2) 0.014(2) -0.001(2) Cl8C 0.045(3) 0.045(3) 0.022(2) 0.0071(18) -0.0006(18) -0.007(2) Cl8D 0.052(3) 0.029(2) 0.029(2) 0.0012(18) -0.0013(19) 0.010(2) _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 O2 1.213(15) . ? C1 N3 1.383(16) . ? C1 N3B 1.389(15) . ? N3 C31 1.397(16) . ? N3 H3 0.8600 . ? C31 C43 1.414(18) . ? C31 C32 1.425(18) . ? C32 C33 1.402(18) . ? C32 H32 0.9300 . ? C33 C34 1.358(18) . ? C33 Cl3 1.760(14) . ? C34 C35 1.391(17) . ? C34 H34 0.9300 . ? C35 C43 1.416(17) . ? C35 C36 1.430(18) . ? C36 C37 1.381(18) . ? C36 C41 1.457(17) . ? C37 C38 1.338(18) . ? C37 H37 0.9300 . ? C38 C39 1.416(18) . ? C38 Cl8 1.779(15) . ? C39 C40 1.361(18) . ? C39 H39 0.9300 . ? C40 C41 1.405(18) . ? C40 N44 1.448(16) . ? C41 N42 1.348(16) . ? N42 C43 1.345(16) . ? N42 H42 0.8600 . ? N44 C45 1.347(17) . ? N44 H44 0.8600 . ? C45 O46 1.228(16) . ? C45 C47 1.511(19) . ? C47 C48 1.497(18) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.555(18) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.500(18) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.529(16) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? N3B C31B 1.402(16) . ? N3B H3B 0.8600 . ? C31B C32B 1.362(18) . ? C31B C43B 1.409(17) . ? C32B C33B 1.393(18) . ? C32B H32B 0.9300 . ? C33B C34B 1.412(17) . ? C33B Cl3B 1.713(15) . ? C34B C35B 1.376(18) . ? C34B H34B 0.9300 . ? C35B C36B 1.415(17) . ? C35B C43B 1.431(18) . ? C36B C41B 1.383(18) . ? C36B C37B 1.394(18) . ? C37B C38B 1.366(18) . ? C37B H37B 0.9300 . ? C38B C39B 1.356(17) . ? C38B Cl8B 1.782(13) . ? C39B C40B 1.412(17) . ? C39B H39B 0.9300 . ? C40B N44B 1.374(16) . ? C40B C41B 1.424(18) . ? C41B N42B 1.403(15) . ? N42B C43B 1.384(16) . ? N42B H42B 0.8600 . ? N44B C45B 1.332(18) . ? N44B H44B 0.8600 . ? C45B O46B 1.257(16) . ? C45B C47B 1.52(2) . ? C47B C48B 1.490(19) . ? C47B H47C 0.9700 . ? C47B H47D 0.9700 . ? C48B C49X 1.550(19) . ? C48B C49B 1.57(2) . ? C48B H48C 0.9700 . ? C48B H48D 0.9700 . ? C49B C50B 1.51(2) . ? C49B H49C 0.9700 . ? C49B H49D 0.9700 . ? C50B C51B 1.522(19) . ? C50B H50C 0.9700 . ? C50B H50D 0.9700 . ? C51B H51D 0.9600 . ? C51B H51E 0.9600 . ? C51B H51F 0.9600 . ? C1C O2C 1.233(14) . ? C1C N3D 1.310(15) . ? C1C N3C 1.401(15) . ? N3C C31C 1.379(15) . ? N3C H3C 0.8600 . ? C31C C32C 1.368(17) . ? C31C C43C 1.430(17) . ? C32C C33C 1.410(17) . ? C32C H32C 0.9300 . ? C33C C34C 1.356(17) . ? C33C Cl3C 1.740(14) . ? C34C C35C 1.403(18) . ? C34C H34C 0.9300 . ? C35C C43C 1.375(17) . ? C35C C36C 1.489(16) . ? C36C C41C 1.379(17) . ? C36C C37C 1.390(16) . ? C37C C38C 1.384(18) . ? C37C H37C 0.9300 . ? C38C C39C 1.392(18) . ? C38C Cl8C 1.751(13) . ? C39C C40C 1.408(17) . ? C39C H39C 0.9300 . ? C40C C41C 1.388(18) . ? C40C N44C 1.401(16) . ? C41C N42C 1.421(15) . ? N42C C43C 1.392(16) . ? N42C H42C 0.8600 . ? N44C C45C 1.345(16) . ? N44C H44C 0.8600 . ? C45C O46C 1.248(14) . ? C45C C47C 1.486(18) . ? C47C C48C 1.491(18) . ? C47C H47E 0.9700 . ? C47C H47F 0.9700 . ? C48C C49C 1.481(18) . ? C48C H48E 0.9700 . ? C48C H48F 0.9700 . ? C49C C50C 1.520(19) . ? C49C H49E 0.9700 . ? C49C H49F 0.9700 . ? C50C C51C 1.53(2) . ? C50C H50E 0.9700 . ? C50C H50F 0.9700 . ? C51C H51G 0.9600 . ? C51C H51H 0.9600 . ? C51C H51I 0.9600 . ? N3D C31D 1.468(16) . ? N3D H3D 0.8600 . ? C31D C43D 1.377(18) . ? C31D C32D 1.387(18) . ? C32D C33D 1.388(17) . ? C32D H32D 0.9300 . ? C33D C34D 1.351(18) . ? C33D Cl3D 1.770(13) . ? C34D C35D 1.421(17) . ? C34D H34D 0.9300 . ? C35D C43D 1.392(17) . ? C35D C36D 1.448(18) . ? C36D C37D 1.364(17) . ? C36D C41D 1.432(17) . ? C37D C38D 1.366(17) . ? C37D H37D 0.9300 . ? C38D C39D 1.403(17) . ? C38D Cl8D 1.763(13) . ? C39D C40D 1.376(17) . ? C39D H39D 0.9300 . ? C40D C41D 1.396(18) . ? C40D N44D 1.426(15) . ? C41D N42D 1.353(16) . ? N42D C43D 1.386(15) . ? N42D H42D 0.8600 . ? N44D C45D 1.376(16) . ? N44D H44D 0.8600 . ? C45D O46D 1.246(14) . ? C45D C47D 1.519(18) . ? C47D C48D 1.517(19) . ? C47D H47G 0.9700 . ? C47D H47H 0.9700 . ? C48D C49D 1.486(18) . ? C48D H48G 0.9700 . ? C48D H48H 0.9700 . ? C49D C50D 1.51(2) . ? C49D H49G 0.9700 . ? C49D H49H 0.9700 . ? C50D C51D 1.57(2) . ? C50D H50G 0.9700 . ? C50D H50H 0.9700 . ? C51D H51J 0.9600 . ? C51D H51K 0.9600 . ? C51D H51L 0.9600 . ? N9 C91C 1.513(17) . ? N9 C91B 1.520(16) . ? N9 C91D 1.530(16) . ? N9 C91 1.531(15) . ? C91 C92 1.521(12) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 C93 1.527(12) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 C94 1.508(12) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C91B C92B 1.446(18) . ? C91B H91C 0.9700 . ? C91B H91D 0.9700 . ? C92B C93B 1.55(2) . ? C92B H92C 0.9700 . ? C92B H92D 0.9700 . ? C93B C94B 1.55(2) . ? C93B H93C 0.9700 . ? C93B H93D 0.9700 . ? C94B H94D 0.9600 . ? C94B H94E 0.9600 . ? C94B H94F 0.9600 . ? C91C C92C 1.501(18) . ? C91C H91E 0.9700 . ? C91C H91F 0.9700 . ? C92C C93C 1.540(19) . ? C92C H92E 0.9700 . ? C92C H92F 0.9700 . ? C93C C94C 1.546(19) . ? C93C H93E 0.9700 . ? C93C H93F 0.9700 . ? C94C H94G 0.9600 . ? C94C H94H 0.9600 . ? C94C H94I 0.9600 . ? C91D C92D 1.517(18) . ? C91D H91G 0.9700 . ? C91D H91H 0.9700 . ? C92D C93D 1.532(18) . ? C92D H92G 0.9700 . ? C92D H92H 0.9700 . ? C93D C94D 1.553(19) . ? C93D H93G 0.9700 . ? C93D H93H 0.9700 . ? C94D H94J 0.9600 . ? C94D H94K 0.9600 . ? C94D H94L 0.9600 . ? N6 C61C 1.481(18) . ? N6 C61D 1.512(17) . ? N6 C61 1.538(17) . ? N6 C61B 1.55(2) . ? C61 C62 1.522(13) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.509(12) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.509(13) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C61B C62Z 1.536(18) . ? C61B C62B 1.564(15) . ? C61B H61C 0.957(18) . ? C61B H61D 0.980(18) . ? C61B H61Y 0.982(18) . ? C61B H61Z 0.965(18) . ? C62B C63B 1.510(15) . ? C62B H62C 0.9700 . ? C62B H62D 0.9700 . ? C63B C64B 1.515(15) . ? C63B H63C 0.9700 . ? C63B H63D 0.9700 . ? C64B H64D 0.9600 . ? C64B H64E 0.9600 . ? C64B H64F 0.9600 . ? C61C C62C 1.551(19) . ? C61C H61E 0.9700 . ? C61C H61F 0.9700 . ? C62C C63C 1.54(2) . ? C62C H62E 0.9700 . ? C62C H62F 0.9700 . ? C63C C64C 1.53(2) . ? C63C H63E 0.9700 . ? C63C H63F 0.9700 . ? C64C H64G 0.9600 . ? C64C H64H 0.9600 . ? C64C H64I 0.9600 . ? C61D C62D 1.536(13) . ? C61D H61G 0.9700 . ? C61D H61H 0.9700 . ? C62D C63D 1.491(13) . ? C62D H62G 0.9700 . ? C62D H62H 0.9700 . ? C63D C64D 1.487(13) . ? C63D H63G 0.9700 . ? C63D H63H 0.9700 . ? C64D H64J 0.9600 . ? C64D H64K 0.9600 . ? C64D H64L 0.9600 . ? N7 C71 1.516(18) . ? N7 C71B 1.53(2) . ? N7 C71C 1.535(19) . ? N7 C71D 1.56(2) . ? C71 C72 1.537(13) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C73 1.519(13) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.507(13) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C71B C72Y 1.502(18) . ? C71B C72B 1.554(15) . ? C71B H71C 0.973(18) . ? C71B H71D 0.970(19) . ? C71B H71Y 0.971(18) . ? C71B H71Z 0.974(18) . ? C72B C73B 1.498(14) . ? C72B H72C 0.9700 . ? C72B H72D 0.9700 . ? C73B C74B 1.501(14) . ? C73B H73C 0.9700 . ? C73B H73D 0.9700 . ? C74B H74D 0.9600 . ? C74B H74E 0.9600 . ? C74B H74F 0.9600 . ? C71C C72C 1.516(13) . ? C71C H71E 0.9700 . ? C71C H71F 0.9700 . ? C72C C73C 1.510(15) . ? C72C C73Z 1.529(18) . ? C72C H72E 0.9700 . ? C72C H72F 0.9700 . ? C73C C74C 1.506(15) . ? C73C H73E 0.9700 . ? C73C H73F 0.9700 . ? C74C H74G 0.9600 . ? C74C H74H 0.9600 . ? C74C H74I 0.9600 . ? C73Z C74Z 1.521(19) . ? C73Z H73Y 0.9700 . ? C73Z H73Z 0.9700 . ? C74Z H74J 0.9600 . ? C74Z H74K 0.9600 . ? C74Z H74L 0.9600 . ? C71D C72D 1.52(2) . ? C71D H71G 0.9700 . ? C71D H71H 0.9700 . ? C72D C73D 1.52(2) . ? C72D H72G 0.9700 . ? C72D H72H 0.9700 . ? C73D C74D 1.478(15) . ? C73D H73G 0.9700 . ? C73D H73H 0.9700 . ? C74D H74M 0.9600 . ? C74D H74N 0.9600 . ? C74D H74O 0.9600 . ? N8 C81C 1.462(19) . ? N8 C81D 1.541(18) . ? N8 C81 1.54(2) . ? N8 C81B 1.55(2) . ? C81 C82 1.528(13) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 C83 1.496(13) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C84 1.498(13) . ? C83 H83A 0.9700 . ? C83 H83B 0.9700 . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C81B C82X 1.520(19) . ? C81B C82B 1.534(15) . ? C81B H81C 0.9700 . ? C81B H81D 0.9700 . ? C82B C83B 1.498(14) . ? C82B H82C 0.9700 . ? C82B H82D 0.9700 . ? C83B C84B 1.5033 . ? C83B H83C 0.9700 . ? C83B H83D 0.9700 . ? C84B H84M 0.9600 . ? C84B H84N 0.9600 . ? C84B H84O 0.9600 . ? C81C C82C 1.559(19) . ? C81C H81E 0.9700 . ? C81C H81F 0.9700 . ? C82C C83C 1.52(2) . ? C82C H82E 0.9700 . ? C82C H82F 0.9700 . ? C83C C84C 1.49(2) . ? C83C H83E 0.9700 . ? C83C H83F 0.9700 . ? C84C H84G 0.9600 . ? C84C H84H 0.9600 . ? C84C H84I 0.9600 . ? C81D C82D 1.529(13) . ? C81D H81G 0.9700 . ? C81D H81H 0.9700 . ? C82D C83D 1.502(13) . ? C82D H82G 0.9700 . ? C82D H82H 0.9700 . ? C83D C84D 1.489(13) . ? C83D H83G 0.9700 . ? C83D H83H 0.9700 . ? C84D H84J 0.9600 . ? C84D H84K 0.9600 . ? C84D H84L 0.9600 . ? O52 C53 1.236(16) . ? C53 O54 1.218(16) . ? C53 C55 1.53(2) . ? C55 O56 1.250(17) . ? C55 O57 1.275(17) . ? O52B C53B 1.210(14) . ? C53B O54B 1.257(14) . ? C53B C55B 1.549(17) . ? C55B O56B 1.276(14) . ? C55B O57B 1.276(14) . ? C49X C50X 1.51(2) . ? C49X H49I 0.9700 . ? C49X H49J 0.9700 . ? C50X C51X 1.522(15) . ? C50X H50I 0.9700 . ? C50X H50J 0.9700 . ? C51X H51M 0.9600 . ? C51X H51N 0.9600 . ? C51X H51O 0.9600 . ? C82X C83X 1.502(14) . ? C82X H82I 0.9700 . ? C82X H82J 0.9700 . ? C83X C84X 1.506(12) . ? C83X H83I 0.9700 . ? C83X H83J 0.9700 . ? C84X H84D 0.9600 . ? C84X H84E 0.9600 . ? C84X H84F 0.9600 . ? C62Z C63Z 1.503(16) . ? C62Z H61C 1.57(3) . ? C62Z H62I 0.9700 . ? C62Z H62J 0.9700 . ? C63Z C64Z 1.508(12) . ? C63Z H63I 0.9700 . ? C63Z H63J 0.9700 . ? C64Z H64M 0.9600 . ? C64Z H64N 0.9600 . ? C64Z H64O 0.9600 . ? C72Y C73Y 1.511(16) . ? C72Y H72I 0.9700 . ? C72Y H72J 0.9700 . ? C73Y C74Y 1.510(12) . ? C73Y H73I 0.9700 . ? C73Y H73J 0.9700 . ? C74Y H74P 0.9600 . ? C74Y H74Q 0.9600 . ? C74Y H74R 0.9600 . ? 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 O2 C1 N3 125.3(12) . . ? O2 C1 N3B 124.1(13) . . ? N3 C1 N3B 110.5(12) . . ? C1 N3 C31 126.0(12) . . ? C1 N3 H3 117.0 . . ? C31 N3 H3 117.0 . . ? N3 C31 C43 119.0(12) . . ? N3 C31 C32 124.2(13) . . ? C43 C31 C32 116.6(12) . . ? C33 C32 C31 118.9(13) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C34 C33 C32 124.6(13) . . ? C34 C33 Cl3 120.9(10) . . ? C32 C33 Cl3 114.4(11) . . ? C33 C34 C35 117.6(12) . . ? C33 C34 H34 121.2 . . ? C35 C34 H34 121.2 . . ? C34 C35 C43 120.4(13) . . ? C34 C35 C36 133.3(12) . . ? C43 C35 C36 106.2(11) . . ? C37 C36 C35 133.5(12) . . ? C37 C36 C41 121.4(13) . . ? C35 C36 C41 105.1(11) . . ? C38 C37 C36 116.9(13) . . ? C38 C37 H37 121.5 . . ? C36 C37 H37 121.5 . . ? C37 C38 C39 125.4(14) . . ? C37 C38 Cl8 119.3(11) . . ? C39 C38 Cl8 115.2(11) . . ? C40 C39 C38 117.5(13) . . ? C40 C39 H39 121.3 . . ? C38 C39 H39 121.3 . . ? C39 C40 C41 121.3(12) . . ? C39 C40 N44 123.1(13) . . ? C41 C40 N44 115.3(12) . . ? N42 C41 C40 134.0(12) . . ? N42 C41 C36 108.6(12) . . ? C40 C41 C36 117.2(12) . . ? C43 N42 C41 110.1(11) . . ? C43 N42 H42 125.0 . . ? C41 N42 H42 125.0 . . ? N42 C43 C31 128.2(12) . . ? N42 C43 C35 110.0(12) . . ? C31 C43 C35 121.8(12) . . ? C45 N44 C40 126.7(12) . . ? C45 N44 H44 116.6 . . ? C40 N44 H44 116.6 . . ? O46 C45 N44 123.8(14) . . ? O46 C45 C47 122.2(14) . . ? N44 C45 C47 113.6(14) . . ? C48 C47 C45 112.0(14) . . ? C48 C47 H47A 109.2 . . ? C45 C47 H47A 109.2 . . ? C48 C47 H47B 109.2 . . ? C45 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? C47 C48 C49 113.3(13) . . ? C47 C48 H48A 108.9 . . ? C49 C48 H48A 108.9 . . ? C47 C48 H48B 108.9 . . ? C49 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? C50 C49 C48 114.8(13) . . ? C50 C49 H49A 108.6 . . ? C48 C49 H49A 108.6 . . ? C50 C49 H49B 108.6 . . ? C48 C49 H49B 108.6 . . ? H49A C49 H49B 107.5 . . ? C49 C50 C51 112.8(13) . . ? C49 C50 H50A 109.0 . . ? C51 C50 H50A 109.0 . . ? C49 C50 H50B 109.0 . . ? C51 C50 H50B 109.0 . . ? H50A C50 H50B 107.8 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C1 N3B C31B 124.5(12) . . ? C1 N3B H3B 117.8 . . ? C31B N3B H3B 117.8 . . ? C32B C31B N3B 125.3(12) . . ? C32B C31B C43B 116.2(13) . . ? N3B C31B C43B 118.5(13) . . ? C31B C32B C33B 123.5(13) . . ? C31B C32B H32B 118.3 . . ? C33B C32B H32B 118.3 . . ? C32B C33B C34B 120.0(14) . . ? C32B C33B Cl3B 119.7(11) . . ? C34B C33B Cl3B 120.2(11) . . ? C35B C34B C33B 118.9(13) . . ? C35B C34B H34B 120.5 . . ? C33B C34B H34B 120.5 . . ? C34B C35B C36B 135.3(13) . . ? C34B C35B C43B 119.1(12) . . ? C36B C35B C43B 105.6(12) . . ? C41B C36B C37B 119.0(12) . . ? C41B C36B C35B 108.2(11) . . ? C37B C36B C35B 132.8(14) . . ? C38B C37B C36B 117.0(14) . . ? C38B C37B H37B 121.5 . . ? C36B C37B H37B 121.5 . . ? C39B C38B C37B 125.5(13) . . ? C39B C38B Cl8B 115.8(10) . . ? C37B C38B Cl8B 118.7(11) . . ? C38B C39B C40B 119.8(13) . . ? C38B C39B H39B 120.1 . . ? C40B C39B H39B 120.1 . . ? N44B C40B C39B 125.0(12) . . ? N44B C40B C41B 120.2(12) . . ? C39B C40B C41B 114.7(13) . . ? C36B C41B N42B 110.0(11) . . ? C36B C41B C40B 123.9(12) . . ? N42B C41B C40B 126.0(12) . . ? C43B N42B C41B 106.3(11) . . ? C43B N42B H42B 126.8 . . ? C41B N42B H42B 126.8 . . ? N42B C43B C31B 127.8(13) . . ? N42B C43B C35B 109.9(11) . . ? C31B C43B C35B 122.3(13) . . ? C45B N44B C40B 129.6(13) . . ? C45B N44B H44B 115.2 . . ? C40B N44B H44B 115.2 . . ? O46B C45B N44B 122.9(16) . . ? O46B C45B C47B 121.6(15) . . ? N44B C45B C47B 115.5(14) . . ? C48B C47B C45B 115.0(15) . . ? C48B C47B H47C 108.5 . . ? C45B C47B H47C 108.5 . . ? C48B C47B H47D 108.5 . . ? C45B C47B H47D 108.5 . . ? H47C C47B H47D 107.5 . . ? C47B C48B C49X 119(3) . . ? C47B C48B C49B 109.0(18) . . ? C49X C48B C49B 32(2) . . ? C47B C48B H48C 109.9 . . ? C49X C48B H48C 78.4 . . ? C49B C48B H48C 109.9 . . ? C47B C48B H48D 109.9 . . ? C49X C48B H48D 124.6 . . ? C49B C48B H48D 109.9 . . ? H48C C48B H48D 108.3 . . ? C50B C49B C48B 108(2) . . ? C50B C49B H49C 110.1 . . ? C48B C49B H49C 110.1 . . ? C50B C49B H49D 110.1 . . ? C48B C49B H49D 110.1 . . ? H49C C49B H49D 108.4 . . ? C49B C50B C51B 109(2) . . ? C49B C50B H50C 109.9 . . ? C51B C50B H50C 109.9 . . ? C49B C50B H50D 109.9 . . ? C51B C50B H50D 109.9 . . ? H50C C50B H50D 108.3 . . ? O2C C1C N3D 125.9(12) . . ? O2C C1C N3C 120.7(12) . . ? N3D C1C N3C 113.4(11) . . ? C31C N3C C1C 125.9(12) . . ? C31C N3C H3C 117.0 . . ? C1C N3C H3C 117.0 . . ? C32C C31C N3C 125.8(12) . . ? C32C C31C C43C 116.6(12) . . ? N3C C31C C43C 117.6(12) . . ? C31C C32C C33C 120.9(12) . . ? C31C C32C H32C 119.5 . . ? C33C C32C H32C 119.5 . . ? C34C C33C C32C 123.1(13) . . ? C34C C33C Cl3C 120.2(11) . . ? C32C C33C Cl3C 116.6(10) . . ? C33C C34C C35C 116.4(13) . . ? C33C C34C H34C 121.8 . . ? C35C C34C H34C 121.8 . . ? C43C C35C C34C 121.8(12) . . ? C43C C35C C36C 105.8(11) . . ? C34C C35C C36C 132.3(12) . . ? C41C C36C C37C 121.4(11) . . ? C41C C36C C35C 106.1(10) . . ? C37C C36C C35C 132.4(12) . . ? C38C C37C C36C 114.8(13) . . ? C38C C37C H37C 122.6 . . ? C36C C37C H37C 122.6 . . ? C37C C38C C39C 124.5(13) . . ? C37C C38C Cl8C 117.9(11) . . ? C39C C38C Cl8C 117.6(10) . . ? C38C C39C C40C 120.2(12) . . ? C38C C39C H39C 119.9 . . ? C40C C39C H39C 119.9 . . ? C41C C40C N44C 120.9(11) . . ? C41C C40C C39C 114.8(12) . . ? N44C C40C C39C 124.3(11) . . ? C36C C41C C40C 124.2(12) . . ? C36C C41C N42C 110.4(11) . . ? C40C C41C N42C 125.4(13) . . ? C43C N42C C41C 106.0(11) . . ? C43C N42C H42C 127.0 . . ? C41C N42C H42C 127.0 . . ? C35C C43C N42C 111.7(11) . . ? C35C C43C C31C 121.1(13) . . ? N42C C43C C31C 127.2(12) . . ? C45C N44C C40C 130.9(11) . . ? C45C N44C H44C 114.6 . . ? C40C N44C H44C 114.6 . . ? O46C C45C N44C 121.3(13) . . ? O46C C45C C47C 122.5(13) . . ? N44C C45C C47C 116.0(11) . . ? C45C C47C C48C 115.5(11) . . ? C45C C47C H47E 108.4 . . ? C48C C47C H47E 108.4 . . ? C45C C47C H47F 108.4 . . ? C48C C47C H47F 108.4 . . ? H47E C47C H47F 107.5 . . ? C49C C48C C47C 114.5(11) . . ? C49C C48C H48E 108.6 . . ? C47C C48C H48E 108.6 . . ? C49C C48C H48F 108.6 . . ? C47C C48C H48F 108.6 . . ? H48E C48C H48F 107.6 . . ? C48C C49C C50C 116.6(12) . . ? C48C C49C H49E 108.1 . . ? C50C C49C H49E 108.1 . . ? C48C C49C H49F 108.1 . . ? C50C C49C H49F 108.1 . . ? H49E C49C H49F 107.3 . . ? C49C C50C C51C 114.2(13) . . ? C49C C50C H50E 108.7 . . ? C51C C50C H50E 108.7 . . ? C49C C50C H50F 108.7 . . ? C51C C50C H50F 108.7 . . ? H50E C50C H50F 107.6 . . ? C50C C51C H51G 109.5 . . ? C50C C51C H51H 109.5 . . ? H51G C51C H51H 109.5 . . ? C50C C51C H51I 109.5 . . ? H51G C51C H51I 109.5 . . ? H51H C51C H51I 109.5 . . ? C1C N3D C31D 127.6(11) . . ? C1C N3D H3D 116.2 . . ? C31D N3D H3D 116.2 . . ? C43D C31D C32D 120.3(12) . . ? C43D C31D N3D 119.6(12) . . ? C32D C31D N3D 120.1(12) . . ? C31D C32D C33D 115.9(13) . . ? C31D C32D H32D 122.0 . . ? C33D C32D H32D 122.0 . . ? C34D C33D C32D 126.8(13) . . ? C34D C33D Cl3D 118.2(10) . . ? C32D C33D Cl3D 115.0(10) . . ? C33D C34D C35D 115.8(12) . . ? C33D C34D H34D 122.1 . . ? C35D C34D H34D 122.1 . . ? C43D C35D C34D 119.3(12) . . ? C43D C35D C36D 106.3(11) . . ? C34D C35D C36D 134.3(12) . . ? C37D C36D C41D 120.7(13) . . ? C37D C36D C35D 133.6(12) . . ? C41D C36D C35D 105.7(11) . . ? C36D C37D C38D 117.6(12) . . ? C36D C37D H37D 121.2 . . ? C38D C37D H37D 121.2 . . ? C37D C38D C39D 123.9(13) . . ? C37D C38D Cl8D 119.6(10) . . ? C39D C38D Cl8D 116.5(10) . . ? C40D C39D C38D 118.6(13) . . ? C40D C39D H39D 120.7 . . ? C38D C39D H39D 120.7 . . ? C39D C40D C41D 119.2(12) . . ? C39D C40D N44D 124.8(12) . . ? C41D C40D N44D 116.0(11) . . ? N42D C41D C40D 130.8(12) . . ? N42D C41D C36D 109.2(12) . . ? C40D C41D C36D 119.9(12) . . ? C41D N42D C43D 108.8(11) . . ? C41D N42D H42D 125.6 . . ? C43D N42D H42D 125.6 . . ? C31D C43D N42D 128.5(12) . . ? C31D C43D C35D 121.6(12) . . ? N42D C43D C35D 109.8(12) . . ? C45D N44D C40D 127.3(11) . . ? C45D N44D H44D 116.3 . . ? C40D N44D H44D 116.3 . . ? O46D C45D N44D 122.4(12) . . ? O46D C45D C47D 123.9(12) . . ? N44D C45D C47D 113.7(12) . . ? C48D C47D C45D 114.1(12) . . ? C48D C47D H47G 108.7 . . ? C45D C47D H47G 108.7 . . ? C48D C47D H47H 108.7 . . ? C45D C47D H47H 108.7 . . ? H47G C47D H47H 107.6 . . ? C49D C48D C47D 112.7(12) . . ? C49D C48D H48G 109.1 . . ? C47D C48D H48G 109.1 . . ? C49D C48D H48H 109.1 . . ? C47D C48D H48H 109.1 . . ? H48G C48D H48H 107.8 . . ? C48D C49D C50D 114.0(13) . . ? C48D C49D H49G 108.7 . . ? C50D C49D H49G 108.7 . . ? C48D C49D H49H 108.7 . . ? C50D C49D H49H 108.7 . . ? H49G C49D H49H 107.6 . . ? C49D C50D C51D 112.2(13) . . ? C49D C50D H50G 109.2 . . ? C51D C50D H50G 109.2 . . ? C49D C50D H50H 109.2 . . ? C51D C50D H50H 109.2 . . ? H50G C50D H50H 107.9 . . ? C50D C51D H51J 109.5 . . ? C50D C51D H51K 109.5 . . ? H51J C51D H51K 109.5 . . ? C50D C51D H51L 109.5 . . ? H51J C51D H51L 109.5 . . ? H51K C51D H51L 109.5 . . ? C91C N9 C91B 111.8(10) . . ? C91C N9 C91D 108.2(10) . . ? C91B N9 C91D 109.8(10) . . ? C91C N9 C91 110.0(10) . . ? C91B N9 C91 108.6(9) . . ? C91D N9 C91 108.3(9) . . ? C92 C91 N9 116.6(10) . . ? C92 C91 H91A 108.1 . . ? N9 C91 H91A 108.1 . . ? C92 C91 H91B 108.1 . . ? N9 C91 H91B 108.1 . . ? H91A C91 H91B 107.3 . . ? C91 C92 C93 110.9(10) . . ? C91 C92 H92A 109.5 . . ? C93 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? C93 C92 H92B 109.5 . . ? H92A C92 H92B 108.0 . . ? C94 C93 C92 109.8(10) . . ? C94 C93 H93A 109.7 . . ? C92 C93 H93A 109.7 . . ? C94 C93 H93B 109.7 . . ? C92 C93 H93B 109.7 . . ? H93A C93 H93B 108.2 . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C92B C91B N9 116.1(11) . . ? C92B C91B H91C 108.3 . . ? N9 C91B H91C 108.3 . . ? C92B C91B H91D 108.3 . . ? N9 C91B H91D 108.3 . . ? H91C C91B H91D 107.4 . . ? C91B C92B C93B 111.9(12) . . ? C91B C92B H92C 109.2 . . ? C93B C92B H92C 109.2 . . ? C91B C92B H92D 109.2 . . ? C93B C92B H92D 109.2 . . ? H92C C92B H92D 107.9 . . ? C94B C93B C92B 110.8(13) . . ? C94B C93B H93C 109.5 . . ? C92B C93B H93C 109.5 . . ? C94B C93B H93D 109.5 . . ? C92B C93B H93D 109.5 . . ? H93C C93B H93D 108.1 . . ? C93B C94B H94D 109.5 . . ? C93B C94B H94E 109.5 . . ? H94D C94B H94E 109.5 . . ? C93B C94B H94F 109.5 . . ? H94D C94B H94F 109.5 . . ? H94E C94B H94F 109.5 . . ? C92C C91C N9 114.5(11) . . ? C92C C91C H91E 108.6 . . ? N9 C91C H91E 108.6 . . ? C92C C91C H91F 108.6 . . ? N9 C91C H91F 108.6 . . ? H91E C91C H91F 107.6 . . ? C91C C92C C93C 109.6(11) . . ? C91C C92C H92E 109.8 . . ? C93C C92C H92E 109.8 . . ? C91C C92C H92F 109.8 . . ? C93C C92C H92F 109.8 . . ? H92E C92C H92F 108.2 . . ? C92C C93C C94C 113.8(12) . . ? C92C C93C H93E 108.8 . . ? C94C C93C H93E 108.8 . . ? C92C C93C H93F 108.8 . . ? C94C C93C H93F 108.8 . . ? H93E C93C H93F 107.7 . . ? C93C C94C H94G 109.5 . . ? C93C C94C H94H 109.5 . . ? H94G C94C H94H 109.5 . . ? C93C C94C H94I 109.5 . . ? H94G C94C H94I 109.5 . . ? H94H C94C H94I 109.5 . . ? C92D C91D N9 115.1(10) . . ? C92D C91D H91G 108.5 . . ? N9 C91D H91G 108.5 . . ? C92D C91D H91H 108.5 . . ? N9 C91D H91H 108.5 . . ? H91G C91D H91H 107.5 . . ? C91D C92D C93D 112.9(12) . . ? C91D C92D H92G 109.0 . . ? C93D C92D H92G 109.0 . . ? C91D C92D H92H 109.0 . . ? C93D C92D H92H 109.0 . . ? H92G C92D H92H 107.8 . . ? C92D C93D C94D 111.6(12) . . ? C92D C93D H93G 109.3 . . ? C94D C93D H93G 109.3 . . ? C92D C93D H93H 109.3 . . ? C94D C93D H93H 109.3 . . ? H93G C93D H93H 108.0 . . ? C93D C94D H94J 109.5 . . ? C93D C94D H94K 109.5 . . ? H94J C94D H94K 109.5 . . ? C93D C94D H94L 109.5 . . ? H94J C94D H94L 109.5 . . ? H94K C94D H94L 109.5 . . ? C61C N6 C61D 107.8(11) . . ? C61C N6 C61 109.6(12) . . ? C61D N6 C61 109.6(10) . . ? C61C N6 C61B 112.8(12) . . ? C61D N6 C61B 109.2(12) . . ? C61 N6 C61B 107.8(11) . . ? C62 C61 N6 113.7(11) . . ? C62 C61 H61A 108.8 . . ? N6 C61 H61A 108.8 . . ? C62 C61 H61B 108.8 . . ? N6 C61 H61B 108.8 . . ? H61A C61 H61B 107.7 . . ? C63 C62 C61 112.5(11) . . ? C63 C62 H62A 109.1 . . ? C61 C62 H62A 109.1 . . ? C63 C62 H62B 109.1 . . ? C61 C62 H62B 109.1 . . ? H62A C62 H62B 107.8 . . ? C62 C63 C64 111.7(12) . . ? C62 C63 H63A 109.3 . . ? C64 C63 H63A 109.3 . . ? C62 C63 H63B 109.3 . . ? C64 C63 H63B 109.3 . . ? H63A C63 H63B 107.9 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62Z C61B N6 118(2) . . ? C62Z C61B C62B 37.1(15) . . ? N6 C61B C62B 110.7(14) . . ? C62Z C61B H61C 74.0(17) . . ? N6 C61B H61C 109.9(15) . . ? C62B C61B H61C 110.2(16) . . ? C62Z C61B H61D 130(2) . . ? N6 C61B H61D 108.5(14) . . ? C62B C61B H61D 109.3(17) . . ? H61C C61B H61D 108.3(17) . . ? C62Z C61B H61Y 108.4(17) . . ? N6 C61B H61Y 106.9(15) . . ? C62B C61B H61Y 76.9(15) . . ? H61C C61B H61Y 136(2) . . ? H61D C61B H61Y 36.0(7) . . ? C62Z C61B H61Z 109(2) . . ? N6 C61B H61Z 107.9(13) . . ? C62B C61B H61Z 138.2(17) . . ? H61C C61B H61Z 39.2(7) . . ? H61D C61B H61Z 72.2(12) . . ? H61Y C61B H61Z 106.8(17) . . ? C63B C62B C61B 110.0(16) . . ? C63B C62B H62C 109.7 . . ? C61B C62B H62C 109.7 . . ? C63B C62B H62D 109.7 . . ? C61B C62B H62D 109.7 . . ? H62C C62B H62D 108.2 . . ? C62B C63B C64B 110.2(18) . . ? C62B C63B H63C 109.6 . . ? C64B C63B H63C 109.6 . . ? C62B C63B H63D 109.6 . . ? C64B C63B H63D 109.6 . . ? H63C C63B H63D 108.1 . . ? N6 C61C C62C 115.7(13) . . ? N6 C61C H61E 108.3 . . ? C62C C61C H61E 108.3 . . ? N6 C61C H61F 108.3 . . ? C62C C61C H61F 108.3 . . ? H61E C61C H61F 107.4 . . ? C63C C62C C61C 110.2(14) . . ? C63C C62C H62E 109.6 . . ? C61C C62C H62E 109.6 . . ? C63C C62C H62F 109.6 . . ? C61C C62C H62F 109.6 . . ? H62E C62C H62F 108.1 . . ? C64C C63C C62C 107.8(16) . . ? C64C C63C H63E 110.1 . . ? C62C C63C H63E 110.1 . . ? C64C C63C H63F 110.1 . . ? C62C C63C H63F 110.1 . . ? H63E C63C H63F 108.5 . . ? C63C C64C H64G 109.5 . . ? C63C C64C H64H 109.5 . . ? H64G C64C H64H 109.5 . . ? C63C C64C H64I 109.5 . . ? H64G C64C H64I 109.5 . . ? H64H C64C H64I 109.5 . . ? N6 C61D C62D 116.4(11) . . ? N6 C61D H61G 108.2 . . ? C62D C61D H61G 108.2 . . ? N6 C61D H61H 108.2 . . ? C62D C61D H61H 108.2 . . ? H61G C61D H61H 107.3 . . ? C63D C62D C61D 113.9(12) . . ? C63D C62D H62G 108.8 . . ? C61D C62D H62G 108.8 . . ? C63D C62D H62H 108.8 . . ? C61D C62D H62H 108.8 . . ? H62G C62D H62H 107.7 . . ? C64D C63D C62D 112.4(13) . . ? C64D C63D H63G 109.1 . . ? C62D C63D H63G 109.1 . . ? C64D C63D H63H 109.1 . . ? C62D C63D H63H 109.1 . . ? H63G C63D H63H 107.9 . . ? C63D C64D H64J 109.5 . . ? C63D C64D H64K 109.5 . . ? H64J C64D H64K 109.5 . . ? C63D C64D H64L 109.5 . . ? H64J C64D H64L 109.5 . . ? H64K C64D H64L 109.5 . . ? C71 N7 C71B 108.9(11) . . ? C71 N7 C71C 107.8(12) . . ? C71B N7 C71C 112.2(12) . . ? C71 N7 C71D 108.9(12) . . ? C71B N7 C71D 109.7(13) . . ? C71C N7 C71D 109.4(12) . . ? N7 C71 C72 117.0(12) . . ? N7 C71 H71A 108.0 . . ? C72 C71 H71A 108.0 . . ? N7 C71 H71B 108.0 . . ? C72 C71 H71B 108.0 . . ? H71A C71 H71B 107.3 . . ? C73 C72 C71 109.8(11) . . ? C73 C72 H72A 109.7 . . ? C71 C72 H72A 109.7 . . ? C73 C72 H72B 109.7 . . ? C71 C72 H72B 109.7 . . ? H72A C72 H72B 108.2 . . ? C74 C73 C72 110.9(12) . . ? C74 C73 H73A 109.5 . . ? C72 C73 H73A 109.5 . . ? C74 C73 H73B 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 108.1 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C72Y C71B N7 134(3) . . ? C72Y C71B C72B 25(2) . . ? N7 C71B C72B 109.6(13) . . ? C72Y C71B H71C 96(2) . . ? N7 C71B H71C 109.1(15) . . ? C72B C71B H71C 110.8(15) . . ? C72Y C71B H71D 98(2) . . ? N7 C71B H71D 109.3(14) . . ? C72B C71B H71D 109.9(17) . . ? H71C C71B H71D 108.0(18) . . ? C72Y C71B H71Y 108(2) . . ? N7 C71B H71Y 103.2(13) . . ? C72B C71B H71Y 119.9(18) . . ? H71C C71B H71Y 103.5(17) . . ? H71D C71B H71Y 10.07(19) . . ? C72Y C71B H71Z 101(2) . . ? N7 C71B H71Z 103.1(14) . . ? C72B C71B H71Z 114.3(16) . . ? H71C C71B H71Z 6.08(11) . . ? H71D C71B H71Z 110.3(18) . . ? H71Y C71B H71Z 104.9(17) . . ? C73B C72B C71B 116.4(16) . . ? C73B C72B H72C 108.2 . . ? C71B C72B H72C 108.2 . . ? C73B C72B H72D 108.2 . . ? C71B C72B H72D 108.2 . . ? H72C C72B H72D 107.3 . . ? C72B C73B C74B 113.7(17) . . ? C72B C73B H73C 108.8 . . ? C74B C73B H73C 108.8 . . ? C72B C73B H73D 108.8 . . ? C74B C73B H73D 108.8 . . ? H73C C73B H73D 107.7 . . ? C72C C71C N7 116.0(13) . . ? C72C C71C H71E 108.3 . . ? N7 C71C H71E 108.3 . . ? C72C C71C H71F 108.3 . . ? N7 C71C H71F 108.3 . . ? H71E C71C H71F 107.4 . . ? C73C C72C C71C 117.5(16) . . ? C73C C72C C73Z 23.2(15) . . ? C71C C72C C73Z 95.1(11) . . ? C73C C72C H72E 107.9 . . ? C71C C72C H72E 107.9 . . ? C73Z C72C H72E 112.5 . . ? C73C C72C H72F 107.9 . . ? C71C C72C H72F 107.9 . . ? C73Z C72C H72F 124.5 . . ? H72E C72C H72F 107.2 . . ? C74C C73C C72C 108.1(16) . . ? C74C C73C H73E 110.1 . . ? C72C C73C H73E 110.1 . . ? C74C C73C H73F 110.1 . . ? C72C C73C H73F 110.1 . . ? H73E C73C H73F 108.4 . . ? C74Z C73Z C72C 100(2) . . ? C74Z C73Z H73Y 111.8 . . ? C72C C73Z H73Y 111.8 . . ? C74Z C73Z H73Z 111.8 . . ? C72C C73Z H73Z 111.8 . . ? H73Y C73Z H73Z 109.5 . . ? C73Z C74Z H74J 109.5 . . ? C73Z C74Z H74K 109.5 . . ? H74J C74Z H74K 109.5 . . ? C73Z C74Z H74L 109.5 . . ? H74J C74Z H74L 109.5 . . ? H74K C74Z H74L 109.5 . . ? C72D C71D N7 115.5(15) . . ? C72D C71D H71G 108.4 . . ? N7 C71D H71G 108.4 . . ? C72D C71D H71H 108.4 . . ? N7 C71D H71H 108.4 . . ? H71G C71D H71H 107.5 . . ? C71D C72D C73D 116.9(17) . . ? C71D C72D H72G 108.1 . . ? C73D C72D H72G 108.1 . . ? C71D C72D H72H 108.1 . . ? C73D C72D H72H 108.1 . . ? H72G C72D H72H 107.3 . . ? C74D C73D C72D 110.3(18) . . ? C74D C73D H73G 109.6 . . ? C72D C73D H73G 109.6 . . ? C74D C73D H73H 109.6 . . ? C72D C73D H73H 109.6 . . ? H73G C73D H73H 108.1 . . ? C73D C74D H74M 109.5 . . ? C73D C74D H74N 109.5 . . ? H74M C74D H74N 109.5 . . ? C73D C74D H74O 109.5 . . ? H74M C74D H74O 109.5 . . ? H74N C74D H74O 109.5 . . ? C81C N8 C81D 107.7(12) . . ? C81C N8 C81 111.0(13) . . ? C81D N8 C81 107.3(12) . . ? C81C N8 C81B 112.7(14) . . ? C81D N8 C81B 110.1(14) . . ? C81 N8 C81B 107.9(12) . . ? C82 C81 N8 115.5(13) . . ? C82 C81 H81A 108.4 . . ? N8 C81 H81A 108.4 . . ? C82 C81 H81B 108.4 . . ? N8 C81 H81B 108.4 . . ? H81A C81 H81B 107.5 . . ? C83 C82 C81 112.9(12) . . ? C83 C82 H82A 109.0 . . ? C81 C82 H82A 109.0 . . ? C83 C82 H82B 109.0 . . ? C81 C82 H82B 109.0 . . ? H82A C82 H82B 107.8 . . ? C82 C83 C84 113.5(13) . . ? C82 C83 H83A 108.9 . . ? C84 C83 H83A 108.9 . . ? C82 C83 H83B 108.9 . . ? C84 C83 H83B 108.9 . . ? H83A C83 H83B 107.7 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C82X C81B C82B 27(3) . . ? C82X C81B N8 125(2) . . ? C82B C81B N8 111.2(15) . . ? C82X C81B H81C 82.6 . . ? C82B C81B H81C 109.4 . . ? N8 C81B H81C 109.4 . . ? C82X C81B H81D 116.9 . . ? C82B C81B H81D 109.4 . . ? N8 C81B H81D 109.4 . . ? H81C C81B H81D 108.0 . . ? C83B C82B C81B 115.9(18) . . ? C83B C82B H82C 108.3 . . ? C81B C82B H82C 108.3 . . ? C83B C82B H82D 108.3 . . ? C81B C82B H82D 108.3 . . ? H82C C82B H82D 107.4 . . ? C82B C83B C84B 112.0(14) . . ? C82B C83B H83C 109.2 . . ? C84B C83B H83C 109.2 . . ? C82B C83B H83D 109.2 . . ? C84B C83B H83D 109.2 . . ? H83C C83B H83D 107.9 . . ? N8 C81C C82C 115.9(14) . . ? N8 C81C H81E 108.3 . . ? C82C C81C H81E 108.3 . . ? N8 C81C H81F 108.3 . . ? C82C C81C H81F 108.3 . . ? H81E C81C H81F 107.4 . . ? C83C C82C C81C 109.3(14) . . ? C83C C82C H82E 109.8 . . ? C81C C82C H82E 109.8 . . ? C83C C82C H82F 109.8 . . ? C81C C82C H82F 109.8 . . ? H82E C82C H82F 108.3 . . ? C84C C83C C82C 112.5(17) . . ? C84C C83C H83E 109.1 . . ? C82C C83C H83E 109.1 . . ? C84C C83C H83F 109.1 . . ? C82C C83C H83F 109.1 . . ? H83E C83C H83F 107.8 . . ? C83C C84C H84G 109.5 . . ? C83C C84C H84H 109.5 . . ? H84G C84C H84H 109.5 . . ? C83C C84C H84I 109.5 . . ? H84G C84C H84I 109.5 . . ? H84H C84C H84I 109.5 . . ? C82D C81D N8 118.1(13) . . ? C82D C81D H81G 107.8 . . ? N8 C81D H81G 107.8 . . ? C82D C81D H81H 107.8 . . ? N8 C81D H81H 107.8 . . ? H81G C81D H81H 107.1 . . ? C83D C82D C81D 111.3(12) . . ? C83D C82D H82G 109.4 . . ? C81D C82D H82G 109.4 . . ? C83D C82D H82H 109.4 . . ? C81D C82D H82H 109.4 . . ? H82G C82D H82H 108.0 . . ? C84D C83D C82D 111.6(13) . . ? C84D C83D H83G 109.3 . . ? C82D C83D H83G 109.3 . . ? C84D C83D H83H 109.3 . . ? C82D C83D H83H 109.3 . . ? H83G C83D H83H 108.0 . . ? C83D C84D H84J 109.5 . . ? C83D C84D H84K 109.5 . . ? H84J C84D H84K 109.5 . . ? C83D C84D H84L 109.5 . . ? H84J C84D H84L 109.5 . . ? H84K C84D H84L 109.5 . . ? O54 C53 O52 128.4(14) . . ? O54 C53 C55 117.4(14) . . ? O52 C53 C55 114.1(14) . . ? O56 C55 O57 125.8(15) . . ? O56 C55 C53 117.2(13) . . ? O57 C55 C53 116.9(14) . . ? O52B C53B O54B 129.7(12) . . ? O52B C53B C55B 117.5(12) . . ? O54B C53B C55B 112.8(12) . . ? O56B C55B O57B 123.7(12) . . ? O56B C55B C53B 118.8(11) . . ? O57B C55B C53B 117.4(11) . . ? C50X C49X C48B 104(3) . . ? C50X C49X H49I 110.9 . . ? C48B C49X H49I 110.9 . . ? C50X C49X H49J 110.9 . . ? C48B C49X H49J 110.9 . . ? H49I C49X H49J 108.9 . . ? C49X C50X C51X 111(3) . . ? C49X C50X H50I 109.4 . . ? C51X C50X H50I 109.4 . . ? C49X C50X H50J 109.4 . . ? C51X C50X H50J 109.4 . . ? H50I C50X H50J 108.0 . . ? C50X C51X H51M 109.5 . . ? C50X C51X H51N 109.5 . . ? H51M C51X H51N 109.5 . . ? C50X C51X H51O 109.5 . . ? H51M C51X H51O 109.5 . . ? H51N C51X H51O 109.5 . . ? C83X C82X C81B 141(4) . . ? C83X C82X H82I 101.8 . . ? C81B C82X H82I 101.8 . . ? C83X C82X H82J 101.8 . . ? C81B C82X H82J 101.8 . . ? H82I C82X H82J 104.7 . . ? C82X C83X C84X 108.1(19) . . ? C82X C83X H83I 110.1 . . ? C84X C83X H83I 110.1 . . ? C82X C83X H83J 110.1 . . ? C84X C83X H83J 110.1 . . ? H83I C83X H83J 108.4 . . ? C83X C84X H84D 109.5 . . ? C83X C84X H84E 109.5 . . ? H84D C84X H84E 109.5 . . ? C83X C84X H84F 109.5 . . ? H84D C84X H84F 109.5 . . ? H84E C84X H84F 109.5 . . ? C63Z C62Z C61B 119(4) . . ? C63Z C62Z H61C 108(3) . . ? C61B C62Z H61C 35.9(9) . . ? C63Z C62Z H62I 107.7 . . ? C61B C62Z H62I 107.7 . . ? H61C C62Z H62I 79.9 . . ? C63Z C62Z H62J 107.7 . . ? C61B C62Z H62J 107.7 . . ? H61C C62Z H62J 139.2 . . ? H62I C62Z H62J 107.1 . . ? C62Z C63Z C64Z 110(2) . . ? C62Z C63Z H63I 109.7 . . ? C64Z C63Z H63I 109.7 . . ? C62Z C63Z H63J 109.7 . . ? C64Z C63Z H63J 109.7 . . ? H63I C63Z H63J 108.2 . . ? C63Z C64Z H64M 109.5 . . ? C63Z C64Z H64N 109.5 . . ? H64M C64Z H64N 109.5 . . ? C63Z C64Z H64O 109.5 . . ? H64M C64Z H64O 109.5 . . ? H64N C64Z H64O 109.5 . . ? C71B C72Y C73Y 111(2) . . ? C71B C72Y H72I 109.5 . . ? C73Y C72Y H72I 109.5 . . ? C71B C72Y H72J 109.5 . . ? C73Y C72Y H72J 109.5 . . ? H72I C72Y H72J 108.1 . . ? C74Y C73Y C72Y 107.5(18) . . ? C74Y C73Y H73I 110.2 . . ? C72Y C73Y H73I 110.2 . . ? C74Y C73Y H73J 110.2 . . ? C72Y C73Y H73J 110.2 . . ? H73I C73Y H73J 108.5 . . ? C73Y C74Y H74P 109.5 . . ? C73Y C74Y H74Q 109.5 . . ? H74P C74Y H74Q 109.5 . . ? C73Y C74Y H74R 109.5 . . ? H74P C74Y H74R 109.5 . . ? H74Q C74Y H74R 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 O2 C1 N3 C31 -7(2) . . . . ? N3B C1 N3 C31 170.6(12) . . . . ? C1 N3 C31 C43 178.4(12) . . . . ? C1 N3 C31 C32 -8(2) . . . . ? N3 C31 C32 C33 -172.1(13) . . . . ? C43 C31 C32 C33 2.1(19) . . . . ? C31 C32 C33 C34 0(2) . . . . ? C31 C32 C33 Cl3 179.9(10) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? Cl3 C33 C34 C35 179.1(10) . . . . ? C33 C34 C35 C43 -0.1(19) . . . . ? C33 C34 C35 C36 -177.5(15) . . . . ? C34 C35 C36 C37 -1(3) . . . . ? C43 C35 C36 C37 -178.7(15) . . . . ? C34 C35 C36 C41 178.9(14) . . . . ? C43 C35 C36 C41 1.3(15) . . . . ? C35 C36 C37 C38 177.6(15) . . . . ? C41 C36 C37 C38 -2(2) . . . . ? C36 C37 C38 C39 1(2) . . . . ? C36 C37 C38 Cl8 179.4(10) . . . . ? C37 C38 C39 C40 -2(2) . . . . ? Cl8 C38 C39 C40 179.5(10) . . . . ? C38 C39 C40 C41 4(2) . . . . ? C38 C39 C40 N44 178.0(12) . . . . ? C39 C40 C41 N42 -179.3(14) . . . . ? N44 C40 C41 N42 7(2) . . . . ? C39 C40 C41 C36 -6(2) . . . . ? N44 C40 C41 C36 -179.7(11) . . . . ? C37 C36 C41 N42 179.8(12) . . . . ? C35 C36 C41 N42 -0.2(15) . . . . ? C37 C36 C41 C40 5(2) . . . . ? C35 C36 C41 C40 -175.4(12) . . . . ? C40 C41 N42 C43 173.0(15) . . . . ? C36 C41 N42 C43 -1.1(15) . . . . ? C41 N42 C43 C31 179.4(14) . . . . ? C41 N42 C43 C35 2.0(15) . . . . ? N3 C31 C43 N42 -6(2) . . . . ? C32 C31 C43 N42 179.6(13) . . . . ? N3 C31 C43 C35 171.2(12) . . . . ? C32 C31 C43 C35 -3(2) . . . . ? C34 C35 C43 N42 180.0(12) . . . . ? C36 C35 C43 N42 -2.1(15) . . . . ? C34 C35 C43 C31 2(2) . . . . ? C36 C35 C43 C31 -179.6(13) . . . . ? C39 C40 N44 C45 14(2) . . . . ? C41 C40 N44 C45 -172.2(13) . . . . ? C40 N44 C45 O46 -1(2) . . . . ? C40 N44 C45 C47 172.3(13) . . . . ? O46 C45 C47 C48 -41(2) . . . . ? N44 C45 C47 C48 145.2(14) . . . . ? C45 C47 C48 C49 175.1(13) . . . . ? C47 C48 C49 C50 59(2) . . . . ? C48 C49 C50 C51 169.6(14) . . . . ? O2 C1 N3B C31B -17(2) . . . . ? N3 C1 N3B C31B 165.4(11) . . . . ? C1 N3B C31B C32B 2(2) . . . . ? C1 N3B C31B C43B -175.9(12) . . . . ? N3B C31B C32B C33B -174.9(13) . . . . ? C43B C31B C32B C33B 3(2) . . . . ? C31B C32B C33B C34B -2(2) . . . . ? C31B C32B C33B Cl3B 178.2(11) . . . . ? C32B C33B C34B C35B 1(2) . . . . ? Cl3B C33B C34B C35B -179.7(10) . . . . ? C33B C34B C35B C36B 178.8(15) . . . . ? C33B C34B C35B C43B -0.1(19) . . . . ? C34B C35B C36B C41B -178.2(15) . . . . ? C43B C35B C36B C41B 0.7(15) . . . . ? C34B C35B C36B C37B 1(3) . . . . ? C43B C35B C36B C37B 180.0(15) . . . . ? C41B C36B C37B C38B -1(2) . . . . ? C35B C36B C37B C38B 179.9(14) . . . . ? C36B C37B C38B C39B 2(2) . . . . ? C36B C37B C38B Cl8B -178.1(10) . . . . ? C37B C38B C39B C40B -2(2) . . . . ? Cl8B C38B C39B C40B 177.5(10) . . . . ? C38B C39B C40B N44B 178.3(13) . . . . ? C38B C39B C40B C41B 2.0(19) . . . . ? C37B C36B C41B N42B 179.6(12) . . . . ? C35B C36B C41B N42B -1.1(16) . . . . ? C37B C36B C41B C40B 1(2) . . . . ? C35B C36B C41B C40B -179.7(12) . . . . ? N44B C40B C41B C36B -177.9(12) . . . . ? C39B C40B C41B C36B -1(2) . . . . ? N44B C40B C41B N42B 4(2) . . . . ? C39B C40B C41B N42B -179.9(12) . . . . ? C36B C41B N42B C43B 1.0(15) . . . . ? C40B C41B N42B C43B 179.6(13) . . . . ? C41B N42B C43B C31B 177.5(13) . . . . ? C41B N42B C43B C35B -0.5(15) . . . . ? C32B C31B C43B N42B -180.0(13) . . . . ? N3B C31B C43B N42B -2(2) . . . . ? C32B C31B C43B C35B -2(2) . . . . ? N3B C31B C43B C35B 175.7(12) . . . . ? C34B C35B C43B N42B 179.0(12) . . . . ? C36B C35B C43B N42B -0.1(15) . . . . ? C34B C35B C43B C31B 1(2) . . . . ? C36B C35B C43B C31B -178.2(12) . . . . ? C39B C40B N44B C45B 18(2) . . . . ? C41B C40B N44B C45B -166.3(14) . . . . ? C40B N44B C45B O46B -4(3) . . . . ? C40B N44B C45B C47B 175.3(14) . . . . ? O46B C45B C47B C48B -10(3) . . . . ? N44B C45B C47B C48B 170.9(16) . . . . ? C45B C47B C48B C49X 156(3) . . . . ? C45B C47B C48B C49B -171.2(17) . . . . ? C47B C48B C49B C50B -75(3) . . . . ? C49X C48B C49B C50B 40(4) . . . . ? C48B C49B C50B C51B -166(3) . . . . ? O2C C1C N3C C31C 18.4(19) . . . . ? N3D C1C N3C C31C -161.0(12) . . . . ? C1C N3C C31C C32C 0(2) . . . . ? C1C N3C C31C C43C 177.0(11) . . . . ? N3C C31C C32C C33C 175.3(12) . . . . ? C43C C31C C32C C33C -1.7(19) . . . . ? C31C C32C C33C C34C -1(2) . . . . ? C31C C32C C33C Cl3C -177.8(10) . . . . ? C32C C33C C34C C35C 3(2) . . . . ? Cl3C C33C C34C C35C 179.9(10) . . . . ? C33C C34C C35C C43C -3(2) . . . . ? C33C C34C C35C C36C -178.8(13) . . . . ? C43C C35C C36C C41C 0.9(14) . . . . ? C34C C35C C36C C41C 177.4(14) . . . . ? C43C C35C C36C C37C 178.4(13) . . . . ? C34C C35C C36C C37C -5(2) . . . . ? C41C C36C C37C C38C -0.6(19) . . . . ? C35C C36C C37C C38C -177.8(13) . . . . ? C36C C37C C38C C39C 0(2) . . . . ? C36C C37C C38C Cl8C -178.4(9) . . . . ? C37C C38C C39C C40C 0(2) . . . . ? Cl8C C38C C39C C40C 177.7(10) . . . . ? C38C C39C C40C C41C 2.0(19) . . . . ? C38C C39C C40C N44C -179.3(12) . . . . ? C37C C36C C41C C40C 3(2) . . . . ? C35C C36C C41C C40C -179.5(12) . . . . ? C37C C36C C41C N42C -178.6(11) . . . . ? C35C C36C C41C N42C -0.7(14) . . . . ? N44C C40C C41C C36C 178.1(12) . . . . ? C39C C40C C41C C36C -3(2) . . . . ? N44C C40C C41C N42C -1(2) . . . . ? C39C C40C C41C N42C 178.1(12) . . . . ? C36C C41C N42C C43C 0.2(14) . . . . ? C40C C41C N42C C43C 179.0(13) . . . . ? C34C C35C C43C N42C -177.8(12) . . . . ? C36C C35C C43C N42C -0.8(15) . . . . ? C34C C35C C43C C31C 0(2) . . . . ? C36C C35C C43C C31C 177.2(11) . . . . ? C41C N42C C43C C35C 0.4(14) . . . . ? C41C N42C C43C C31C -177.5(12) . . . . ? C32C C31C C43C C35C 2.0(19) . . . . ? N3C C31C C43C C35C -175.2(12) . . . . ? C32C C31C C43C N42C 179.7(12) . . . . ? N3C C31C C43C N42C 2(2) . . . . ? C41C C40C N44C C45C 164.3(13) . . . . ? C39C C40C N44C C45C -14(2) . . . . ? C40C N44C C45C O46C -4(2) . . . . ? C40C N44C C45C C47C -178.5(12) . . . . ? O46C C45C C47C C48C 22.8(19) . . . . ? N44C C45C C47C C48C -162.4(12) . . . . ? C45C C47C C48C C49C 176.6(12) . . . . ? C47C C48C C49C C50C -179.7(12) . . . . ? C48C C49C C50C C51C 177.4(13) . . . . ? O2C C1C N3D C31D 11(2) . . . . ? N3C C1C N3D C31D -169.2(11) . . . . ? C1C N3D C31D C43D -176.6(13) . . . . ? C1C N3D C31D C32D 2(2) . . . . ? C43D C31D C32D C33D -5(2) . . . . ? N3D C31D C32D C33D 176.2(12) . . . . ? C31D C32D C33D C34D 3(2) . . . . ? C31D C32D C33D Cl3D -177.3(10) . . . . ? C32D C33D C34D C35D -1(2) . . . . ? Cl3D C33D C34D C35D 179.4(9) . . . . ? C33D C34D C35D C43D 1.2(19) . . . . ? C33D C34D C35D C36D 177.4(14) . . . . ? C43D C35D C36D C37D -179.6(15) . . . . ? C34D C35D C36D C37D 4(3) . . . . ? C43D C35D C36D C41D 0.0(14) . . . . ? C34D C35D C36D C41D -176.5(14) . . . . ? C41D C36D C37D C38D 3(2) . . . . ? C35D C36D C37D C38D -177.3(14) . . . . ? C36D C37D C38D C39D -1(2) . . . . ? C36D C37D C38D Cl8D -179.7(10) . . . . ? C37D C38D C39D C40D 0(2) . . . . ? Cl8D C38D C39D C40D 178.2(10) . . . . ? C38D C39D C40D C41D -0.1(19) . . . . ? C38D C39D C40D N44D 177.2(12) . . . . ? C39D C40D C41D N42D -179.4(13) . . . . ? N44D C40D C41D N42D 3(2) . . . . ? C39D C40D C41D C36D 2(2) . . . . ? N44D C40D C41D C36D -175.6(12) . . . . ? C37D C36D C41D N42D 177.5(12) . . . . ? C35D C36D C41D N42D -2.1(15) . . . . ? C37D C36D C41D C40D -4(2) . . . . ? C35D C36D C41D C40D 176.8(12) . . . . ? C40D C41D N42D C43D -175.3(14) . . . . ? C36D C41D N42D C43D 3.5(15) . . . . ? C32D C31D C43D N42D -177.6(13) . . . . ? N3D C31D C43D N42D 1(2) . . . . ? C32D C31D C43D C35D 6(2) . . . . ? N3D C31D C43D C35D -175.7(12) . . . . ? C41D N42D C43D C31D 179.6(14) . . . . ? C41D N42D C43D C35D -3.5(15) . . . . ? C34D C35D C43D C31D -4(2) . . . . ? C36D C35D C43D C31D 179.2(12) . . . . ? C34D C35D C43D N42D 179.2(11) . . . . ? C36D C35D C43D N42D 2.1(15) . . . . ? C39D C40D N44D C45D -23(2) . . . . ? C41D C40D N44D C45D 154.8(13) . . . . ? C40D N44D C45D O46D 9(2) . . . . ? C40D N44D C45D C47D -168.6(12) . . . . ? O46D C45D C47D C48D 83.2(18) . . . . ? N44D C45D C47D C48D -99.4(15) . . . . ? C45D C47D C48D C49D 165.4(13) . . . . ? C47D C48D C49D C50D 175.7(13) . . . . ? C48D C49D C50D C51D 179.2(13) . . . . ? C91C N9 C91 C92 -45.1(14) . . . . ? C91B N9 C91 C92 -167.7(11) . . . . ? C91D N9 C91 C92 73.0(13) . . . . ? N9 C91 C92 C93 -162.3(10) . . . . ? C91 C92 C93 C94 84.8(14) . . . . ? C91C N9 C91B C92B 64.0(15) . . . . ? C91D N9 C91B C92B -56.1(15) . . . . ? C91 N9 C91B C92B -174.5(11) . . . . ? N9 C91B C92B C93B -174.7(12) . . . . ? C91B C92B C93B C94B 178.7(13) . . . . ? C91B N9 C91C C92C 61.7(15) . . . . ? C91D N9 C91C C92C -177.2(11) . . . . ? C91 N9 C91C C92C -59.1(14) . . . . ? N9 C91C C92C C93C 173.1(11) . . . . ? C91C C92C C93C C94C 174.8(12) . . . . ? C91C N9 C91D C92D -170.1(11) . . . . ? C91B N9 C91D C92D -47.8(14) . . . . ? C91 N9 C91D C92D 70.7(14) . . . . ? N9 C91D C92D C93D -172.6(11) . . . . ? C91D C92D C93D C94D 70.7(16) . . . . ? C61C N6 C61 C62 53.2(15) . . . . ? C61D N6 C61 C62 -64.9(15) . . . . ? C61B N6 C61 C62 176.4(12) . . . . ? N6 C61 C62 C63 161.7(12) . . . . ? C61 C62 C63 C64 177.5(13) . . . . ? C61C N6 C61B C62Z -86(2) . . . . ? C61D N6 C61B C62Z 34(2) . . . . ? C61 N6 C61B C62Z 153.0(18) . . . . ? C61C N6 C61B C62B -46(2) . . . . ? C61D N6 C61B C62B 74.2(18) . . . . ? C61 N6 C61B C62B -166.9(15) . . . . ? C62Z C61B C62B C63B -70(3) . . . . ? N6 C61B C62B C63B -178.6(17) . . . . ? C61B C62B C63B C64B 66(3) . . . . ? C61D N6 C61C C62C -177.3(13) . . . . ? C61 N6 C61C C62C 63.5(17) . . . . ? C61B N6 C61C C62C -56.7(18) . . . . ? N6 C61C C62C C63C -166.2(15) . . . . ? C61C C62C C63C C64C -177.6(15) . . . . ? C61C N6 C61D C62D -172.6(14) . . . . ? C61 N6 C61D C62D -53.3(17) . . . . ? C61B N6 C61D C62D 64.5(16) . . . . ? N6 C61D C62D C63D 177.3(14) . . . . ? C61D C62D C63D C64D -177.9(15) . . . . ? C71B N7 C71 C72 179.9(13) . . . . ? C71C N7 C71 C72 -58.1(17) . . . . ? C71D N7 C71 C72 60.4(17) . . . . ? N7 C71 C72 C73 169.6(14) . . . . ? C71 C72 C73 C74 175.1(15) . . . . ? C71 N7 C71B C72Y -174(2) . . . . ? C71C N7 C71B C72Y 67(3) . . . . ? C71D N7 C71B C72Y -55(3) . . . . ? C71 N7 C71B C72B -171.3(15) . . . . ? C71C N7 C71B C72B 69.5(18) . . . . ? C71D N7 C71B C72B -52.3(19) . . . . ? C72Y C71B C72B C73B 6(3) . . . . ? N7 C71B C72B C73B -168.9(16) . . . . ? C71B C72B C73B C74B 75(3) . . . . ? C71 N7 C71C C72C -54.4(17) . . . . ? C71B N7 C71C C72C 65.4(18) . . . . ? C71D N7 C71C C72C -172.7(14) . . . . ? N7 C71C C72C C73C -163.4(14) . . . . ? N7 C71C C72C C73Z -157(2) . . . . ? C71C C72C C73C C74C 84(3) . . . . ? C73Z C72C C73C C74C 67(5) . . . . ? C73C C72C C73Z C74Z -4(4) . . . . ? C71C C72C C73Z C74Z -169(3) . . . . ? C71 N7 C71D C72D 63.8(19) . . . . ? C71B N7 C71D C72D -55(2) . . . . ? C71C N7 C71D C72D -178.7(15) . . . . ? N7 C71D C72D C73D 173.5(16) . . . . ? C71D C72D C73D C74D 66(3) . . . . ? C81C N8 C81 C82 -56.5(19) . . . . ? C81D N8 C81 C82 60.9(18) . . . . ? C81B N8 C81 C82 179.6(15) . . . . ? N8 C81 C82 C83 -173.9(14) . . . . ? C81 C82 C83 C84 174.7(15) . . . . ? C81C N8 C81B C82X 74(3) . . . . ? C81D N8 C81B C82X -46(3) . . . . ? C81 N8 C81B C82X -163(3) . . . . ? C81C N8 C81B C82B 48(2) . . . . ? C81D N8 C81B C82B -72(2) . . . . ? C81 N8 C81B C82B 171.2(18) . . . . ? C82X C81B C82B C83B 42(3) . . . . ? N8 C81B C82B C83B 169.2(19) . . . . ? C81B C82B C83B C84B -80(2) . . . . ? C81D N8 C81C C82C 178.9(14) . . . . ? C81 N8 C81C C82C -64.0(19) . . . . ? C81B N8 C81C C82C 57(2) . . . . ? N8 C81C C82C C83C 175.9(16) . . . . ? C81C C82C C83C C84C -178.6(17) . . . . ? C81C N8 C81D C82D 170.9(15) . . . . ? C81 N8 C81D C82D 51.3(18) . . . . ? C81B N8 C81D C82D -65.9(19) . . . . ? N8 C81D C82D C83D 164.5(15) . . . . ? C81D C82D C83D C84D 178.7(16) . . . . ? O54 C53 C55 O56 -107.5(16) . . . . ? O52 C53 C55 O56 68.8(19) . . . . ? O54 C53 C55 O57 76.9(19) . . . . ? O52 C53 C55 O57 -106.7(16) . . . . ? O52B C53B C55B O56B -71.3(17) . . . . ? O54B C53B C55B O56B 111.9(13) . . . . ? O52B C53B C55B O57B 112.0(14) . . . . ? O54B C53B C55B O57B -64.7(16) . . . . ? C47B C48B C49X C50X 41(6) . . . . ? C49B C48B C49X C50X -37(3) . . . . ? C48B C49X C50X C51X -176(5) . . . . ? C82B C81B C82X C83X -162(7) . . . . ? N8 C81B C82X C83X 132(5) . . . . ? C81B C82X C83X C84X 144(5) . . . . ? N6 C61B C62Z C63Z 174(2) . . . . ? C62B C61B C62Z C63Z 86(3) . . . . ? C61B C62Z C63Z C64Z -90(5) . . . . ? N7 C71B C72Y C73Y -94(4) . . . . ? C72B C71B C72Y C73Y -100(6) . . . . ? C71B C72Y C73Y C74Y -165(4) . . . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 22.12 _diffrn_measured_fraction_theta_full 0.886 _refine_diff_density_max 0.608 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.128