# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr Guoqiang Yang' _publ_contact_author_email gqyang@iccas.ac.cn loop_ _publ_author_name 'Guoqiang Yang' 'Dehui Hu' data_60909a _database_code_depnum_ccdc_archive 'CCDC 798936' #TrackingRef '- 1-0.5H2O revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H30 N6 O4, 0.5(H2 O)' _chemical_formula_sum 'C21 H31 N6 O4.50' _chemical_formula_weight 439.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/3' '-y, x-y, z+2/3' '-x, -y, z' '-x+y, -x, z+1/3' 'y, -x+y, z+2/3' _cell_length_a 16.533(4) _cell_length_b 16.533(4) _cell_length_c 14.654(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3468.9(17) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2654 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 19.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1410 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9750 _exptl_absorpt_correction_T_max 0.9821 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 18887 _diffrn_reflns_av_R_equivalents 0.0550 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4093 _reflns_number_gt 2626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Six restraints were added to deal with the disorder of ethyl group as follow: SADI 0.02 C7 C8 C7 C8' SADI 0.02 C8 C9 C8' C9' SIMU 0.02 C8 C8' SIMU 0.02 C9 C9' ISOR 0.01 C8 C8' C9 C9' ; _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^)+(0.0321P)^2^+0.6008P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0047(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1.3(14) _refine_ls_number_reflns 4093 _refine_ls_number_parameters 308 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.26421(15) 0.14462(15) -0.11937(14) 0.0665(6) Uani 1 1 d . . . O2 O 0.05369(16) 0.15764(16) -0.10276(17) 0.0817(8) Uani 1 1 d . . . O3 O 0.65029(14) 0.67789(14) 0.07279(14) 0.0602(6) Uani 1 1 d . . . O4 O 0.61342(15) 0.50774(15) -0.13943(14) 0.0618(6) Uani 1 1 d . . . N1 N 0.15602(18) 0.10221(18) -0.00963(18) 0.0604(7) Uani 1 1 d . . . H1 H 0.1172 0.0583 0.0257 0.073 Uiso 1 1 calc R . . N2 N 0.16776(18) 0.18996(17) -0.00135(17) 0.0572(7) Uani 1 1 d . . . H2 H 0.2098 0.2300 0.0347 0.069 Uiso 1 1 calc R . . N3 N 0.18342(15) 0.36099(17) 0.03642(17) 0.0525(6) Uani 1 1 d . . . H3 H 0.2113 0.3447 0.0756 0.063 Uiso 1 1 calc R . . N4 N 0.39873(15) 0.56182(15) 0.05742(15) 0.0449(6) Uani 1 1 d . A . H4 H 0.3852 0.5507 0.0005 0.054 Uiso 1 1 calc R . . N5 N 0.55861(16) 0.61586(15) -0.05114(16) 0.0515(6) Uani 1 1 d . . . H5 H 0.5029 0.5833 -0.0723 0.062 Uiso 1 1 calc R . . N6 N 0.63408(16) 0.65021(17) -0.11023(15) 0.0505(6) Uani 1 1 d . . . H6 H 0.6680 0.7095 -0.1185 0.061 Uiso 1 1 calc R . . C1 C 0.1784(2) -0.0164(2) -0.0778(2) 0.0707(10) Uani 1 1 d . . . H1A H 0.1819 -0.0324 -0.1400 0.106 Uiso 1 1 d R . . H1B H 0.1159 -0.0552 -0.0555 0.106 Uiso 1 1 d R . . H1C H 0.2210 -0.0260 -0.0412 0.106 Uiso 1 1 d R . . C2 C 0.2039(2) 0.0835(2) -0.0717(2) 0.0535(8) Uani 1 1 d . . . C3 C 0.1132(2) 0.2134(2) -0.0499(2) 0.0573(8) Uani 1 1 d . . . C4 C 0.1279(2) 0.3055(2) -0.0330(2) 0.0514(8) Uani 1 1 d . . . C5 C 0.0969(2) 0.3571(2) -0.0800(2) 0.0611(9) Uani 1 1 d . A . C6 C 0.0338(3) 0.3241(3) -0.1622(3) 0.0995(14) Uani 1 1 d . . . H6A H 0.0275 0.2663 -0.1836 0.149 Uiso 1 1 calc R . . H6B H 0.0603 0.3702 -0.2096 0.149 Uiso 1 1 calc R . . H6C H -0.0265 0.3147 -0.1458 0.149 Uiso 1 1 calc R . . C7 C 0.1356(2) 0.4442(2) -0.0375(2) 0.0619(9) Uani 1 1 d D . . C8 C 0.1335(7) 0.5297(5) -0.0739(10) 0.086(3) Uani 0.69(3) 1 d PDU A 1 H8A H 0.0817 0.5093 -0.1162 0.103 Uiso 0.69(3) 1 calc PR A 1 H8B H 0.1226 0.5610 -0.0235 0.103 Uiso 0.69(3) 1 calc PR A 1 C9 C 0.2223(12) 0.5979(6) -0.1215(8) 0.151(5) Uani 0.69(3) 1 d PDU A 1 H9A H 0.2146 0.6462 -0.1492 0.227 Uiso 0.69(3) 1 calc PR A 1 H9B H 0.2369 0.5660 -0.1677 0.227 Uiso 0.69(3) 1 calc PR A 1 H9C H 0.2724 0.6252 -0.0779 0.227 Uiso 0.69(3) 1 calc PR A 1 C8' C 0.101(2) 0.5150(17) -0.0439(18) 0.096(6) Uani 0.31(3) 1 d PDU A 2 H8'1 H 0.0378 0.4859 -0.0684 0.115 Uiso 0.31(3) 1 calc PR A 2 H8'2 H 0.1015 0.5414 0.0154 0.115 Uiso 0.31(3) 1 calc PR A 2 C9' C 0.170(3) 0.589(2) -0.108(2) 0.154(10) Uani 0.31(3) 1 d PDU A 2 H9'1 H 0.1537 0.6369 -0.1161 0.232 Uiso 0.31(3) 1 calc PR A 2 H9'2 H 0.1679 0.5612 -0.1662 0.232 Uiso 0.31(3) 1 calc PR A 2 H9'3 H 0.2315 0.6159 -0.0830 0.232 Uiso 0.31(3) 1 calc PR A 2 C10 C 0.18796(19) 0.4442(2) 0.0346(2) 0.0486(7) Uani 1 1 d . A . C11 C 0.23598(19) 0.5136(2) 0.1081(2) 0.0575(8) Uani 1 1 d . . . H11A H 0.2021 0.4875 0.1645 0.069 Uiso 1 1 calc R A . H11B H 0.2313 0.5685 0.0941 0.069 Uiso 1 1 calc R . . C12 C 0.33605(19) 0.54461(18) 0.1248(2) 0.0463(7) Uani 1 1 d . A . C13 C 0.3831(2) 0.5696(2) 0.2060(2) 0.0559(8) Uani 1 1 d . . . C14 C 0.3393(2) 0.5605(3) 0.2985(2) 0.0786(11) Uani 1 1 d . A . H14A H 0.2884 0.5735 0.2923 0.094 Uiso 1 1 calc R . . H14B H 0.3854 0.6075 0.3388 0.094 Uiso 1 1 calc R . . C15 C 0.3021(3) 0.4658(3) 0.3422(3) 0.1047(14) Uani 1 1 d . . . H15A H 0.2584 0.4184 0.3017 0.157 Uiso 1 1 calc R A . H15B H 0.2714 0.4638 0.3984 0.157 Uiso 1 1 calc R . . H15C H 0.3529 0.4548 0.3543 0.157 Uiso 1 1 calc R . . C16 C 0.4786(2) 0.6053(2) 0.1872(2) 0.0565(8) Uani 1 1 d . A . C17 C 0.5555(2) 0.6433(3) 0.2567(2) 0.1000(15) Uani 1 1 d . . . H17A H 0.6043 0.6320 0.2369 0.150 Uiso 1 1 calc R A . H17B H 0.5313 0.6130 0.3142 0.150 Uiso 1 1 calc R . . H17C H 0.5800 0.7093 0.2633 0.150 Uiso 1 1 calc R . . C18 C 0.48715(18) 0.59973(18) 0.0933(2) 0.0440(7) Uani 1 1 d . . . C19 C 0.5718(2) 0.63316(19) 0.0401(2) 0.0479(7) Uani 1 1 d . A . C20 C 0.6545(2) 0.5929(2) -0.1540(2) 0.0515(8) Uani 1 1 d . . . C21 C 0.7269(2) 0.6367(2) -0.2275(2) 0.0695(9) Uani 1 1 d . . . H21A H 0.7640 0.6069 -0.2292 0.104 Uiso 1 1 d R . . H21B H 0.7663 0.7020 -0.2149 0.104 Uiso 1 1 d R . . H21C H 0.6968 0.6291 -0.2855 0.104 Uiso 1 1 d R . . O5 O 0.0000 1.0000 0.1202(2) 0.0627(8) Uani 1 2 d S . . H5A H 0.0293 0.9800 0.1522 0.094 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0642(14) 0.0552(13) 0.0656(15) 0.0043(12) 0.0166(12) 0.0190(12) O2 0.0662(15) 0.0660(15) 0.0992(19) -0.0277(14) -0.0326(14) 0.0227(14) O3 0.0402(13) 0.0711(14) 0.0592(13) -0.0041(11) -0.0016(10) 0.0202(11) O4 0.0629(14) 0.0521(14) 0.0634(14) 0.0023(12) 0.0119(11) 0.0234(12) N1 0.0594(17) 0.0447(16) 0.0693(18) 0.0064(13) 0.0153(14) 0.0201(14) N2 0.0572(17) 0.0473(16) 0.0600(17) -0.0075(13) -0.0009(13) 0.0208(14) N3 0.0478(14) 0.0578(16) 0.0529(15) -0.0040(14) -0.0107(13) 0.0270(13) N4 0.0445(14) 0.0466(14) 0.0455(14) -0.0002(12) -0.0019(12) 0.0241(12) N5 0.0382(14) 0.0526(15) 0.0528(17) -0.0010(13) 0.0039(12) 0.0146(12) N6 0.0438(14) 0.0470(15) 0.0521(16) 0.0027(13) 0.0084(13) 0.0164(12) C1 0.070(2) 0.061(2) 0.088(3) 0.0036(19) 0.0033(19) 0.0386(19) C2 0.0456(19) 0.049(2) 0.063(2) -0.0031(17) -0.0060(17) 0.0212(17) C3 0.0426(18) 0.057(2) 0.062(2) -0.0007(18) 0.0015(17) 0.0169(17) C4 0.0440(18) 0.0533(19) 0.0506(18) -0.0086(16) -0.0083(15) 0.0195(16) C5 0.0472(19) 0.071(2) 0.060(2) 0.0041(18) -0.0073(16) 0.0256(18) C6 0.100(3) 0.105(3) 0.096(3) -0.014(2) -0.053(3) 0.053(3) C7 0.053(2) 0.066(2) 0.069(2) 0.0039(19) -0.0104(18) 0.0321(18) C8 0.070(6) 0.075(4) 0.107(7) 0.016(4) -0.019(5) 0.032(4) C9 0.152(9) 0.107(5) 0.176(7) 0.080(5) 0.001(6) 0.051(5) C8' 0.095(10) 0.094(9) 0.093(9) 0.008(7) -0.006(7) 0.043(7) C9' 0.161(14) 0.150(12) 0.170(13) 0.032(8) 0.004(9) 0.091(9) C10 0.0378(16) 0.0506(19) 0.058(2) -0.0035(16) 0.0030(16) 0.0228(15) C11 0.0468(18) 0.0610(19) 0.070(2) -0.0110(18) -0.0002(17) 0.0309(16) C12 0.0394(16) 0.0428(17) 0.0570(19) -0.0047(15) 0.0022(16) 0.0209(14) C13 0.0444(18) 0.067(2) 0.053(2) -0.0089(17) 0.0026(16) 0.0255(16) C14 0.058(2) 0.106(3) 0.063(2) -0.021(2) 0.000(2) 0.034(2) C15 0.101(3) 0.133(4) 0.077(3) 0.023(3) 0.036(2) 0.056(3) C16 0.0471(19) 0.070(2) 0.051(2) -0.0081(17) -0.0038(16) 0.0278(17) C17 0.056(2) 0.163(4) 0.059(2) -0.022(3) -0.0173(19) 0.038(3) C18 0.0350(17) 0.0432(17) 0.0498(19) -0.0041(14) -0.0019(14) 0.0165(14) C19 0.046(2) 0.0392(17) 0.055(2) 0.0014(15) 0.0001(17) 0.0194(15) C20 0.0414(18) 0.059(2) 0.0465(19) -0.0007(17) 0.0003(14) 0.0195(17) C21 0.059(2) 0.079(2) 0.0527(19) 0.0043(18) 0.0129(17) 0.0206(19) O5 0.0617(19) 0.0666(19) 0.0602(18) 0.000 0.000 0.0324(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.223(3) . ? O2 C3 1.230(4) . ? O3 C19 1.225(3) . ? O4 C20 1.238(3) . ? N1 C2 1.340(4) . ? N1 N2 1.369(3) . ? N1 H1 0.8600 . ? N2 C3 1.349(4) . ? N2 H2 0.8600 . ? N3 C10 1.341(3) . ? N3 C4 1.370(4) . ? N3 H3 0.8600 . ? N4 C12 1.355(3) . ? N4 C18 1.375(3) . ? N4 H4 0.8600 . ? N5 C19 1.361(4) . ? N5 N6 1.386(3) . ? N5 H5 0.8600 . ? N6 C20 1.320(4) . ? N6 H6 0.8600 . ? C1 C2 1.489(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C3 C4 1.437(4) . ? C4 C5 1.379(4) . ? C5 C7 1.396(4) . ? C5 C6 1.505(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C10 1.366(4) . ? C7 C8 1.527(7) . ? C7 C8' 1.546(15) . ? C8 C9 1.504(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C8' C9' 1.514(18) . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C9' H9'1 0.9600 . ? C9' H9'2 0.9600 . ? C9' H9'3 0.9600 . ? C10 C11 1.482(4) . ? C11 C12 1.488(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.367(4) . ? C13 C16 1.409(4) . ? C13 C14 1.509(4) . ? C14 C15 1.510(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C18 1.390(4) . ? C16 C17 1.499(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.449(4) . ? C20 C21 1.501(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? O5 H5A 0.8502 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 N2 121.2(2) . . ? C2 N1 H1 119.4 . . ? N2 N1 H1 119.4 . . ? C3 N2 N1 119.8(3) . . ? C3 N2 H2 120.1 . . ? N1 N2 H2 120.1 . . ? C10 N3 C4 110.3(3) . . ? C10 N3 H3 124.8 . . ? C4 N3 H3 124.8 . . ? C12 N4 C18 110.1(2) . . ? C12 N4 H4 125.0 . . ? C18 N4 H4 125.0 . . ? C19 N5 N6 120.7(2) . . ? C19 N5 H5 119.6 . . ? N6 N5 H5 119.6 . . ? C20 N6 N5 120.7(2) . . ? C20 N6 H6 119.7 . . ? N5 N6 H6 119.7 . . ? C2 C1 H1A 109.8 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.0 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 N1 122.0(3) . . ? O1 C2 C1 123.0(3) . . ? N1 C2 C1 115.1(3) . . ? O2 C3 N2 121.0(3) . . ? O2 C3 C4 123.4(3) . . ? N2 C3 C4 115.5(3) . . ? N3 C4 C5 106.7(3) . . ? N3 C4 C3 122.6(3) . . ? C5 C4 C3 130.6(3) . . ? C4 C5 C7 107.2(3) . . ? C4 C5 C6 125.4(3) . . ? C7 C5 C6 127.4(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C10 C7 C5 108.0(3) . . ? C10 C7 C8 125.3(4) . . ? C5 C7 C8 126.1(5) . . ? C10 C7 C8' 121.6(9) . . ? C5 C7 C8' 127.0(10) . . ? C8 C7 C8' 24.2(8) . . ? C9 C8 C7 113.0(6) . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C9' C8' C7 103.5(16) . . ? C9' C8' H8'1 111.1 . . ? C7 C8' H8'1 111.1 . . ? C9' C8' H8'2 111.1 . . ? C7 C8' H8'2 111.1 . . ? H8'1 C8' H8'2 109.0 . . ? C8' C9' H9'1 109.5 . . ? C8' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C8' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? N3 C10 C7 107.8(3) . . ? N3 C10 C11 120.9(3) . . ? C7 C10 C11 131.1(3) . . ? C10 C11 C12 117.4(2) . . ? C10 C11 H11A 108.0 . . ? C12 C11 H11A 108.0 . . ? C10 C11 H11B 108.0 . . ? C12 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? N4 C12 C13 108.1(2) . . ? N4 C12 C11 123.6(3) . . ? C13 C12 C11 127.9(3) . . ? C12 C13 C16 107.8(3) . . ? C12 C13 C14 125.4(3) . . ? C16 C13 C14 126.8(3) . . ? C13 C14 C15 114.2(3) . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? C15 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C13 107.2(3) . . ? C18 C16 C17 127.4(3) . . ? C13 C16 C17 125.5(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C16 106.8(2) . . ? N4 C18 C19 124.8(3) . . ? C16 C18 C19 128.2(3) . . ? O3 C19 N5 121.4(3) . . ? O3 C19 C18 123.3(3) . . ? N5 C19 C18 115.2(3) . . ? O4 C20 N6 122.8(3) . . ? O4 C20 C21 121.6(3) . . ? N6 C20 C21 115.5(3) . . ? C20 C21 H21A 109.3 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.6 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 C2 N1 N2 C3 90.6(3) . . . . ? C19 N5 N6 C20 113.5(3) . . . . ? N2 N1 C2 O1 4.9(4) . . . . ? N2 N1 C2 C1 -175.4(3) . . . . ? N1 N2 C3 O2 -1.1(4) . . . . ? N1 N2 C3 C4 177.1(3) . . . . ? C10 N3 C4 C5 0.1(3) . . . . ? C10 N3 C4 C3 177.6(3) . . . . ? O2 C3 C4 N3 169.1(3) . . . . ? N2 C3 C4 N3 -9.1(4) . . . . ? O2 C3 C4 C5 -14.1(5) . . . . ? N2 C3 C4 C5 167.8(3) . . . . ? N3 C4 C5 C7 0.5(3) . . . . ? C3 C4 C5 C7 -176.8(3) . . . . ? N3 C4 C5 C6 179.9(3) . . . . ? C3 C4 C5 C6 2.6(6) . . . . ? C4 C5 C7 C10 -0.8(4) . . . . ? C6 C5 C7 C10 179.8(3) . . . . ? C4 C5 C7 C8 169.9(7) . . . . ? C6 C5 C7 C8 -9.5(9) . . . . ? C4 C5 C7 C8' -159.9(15) . . . . ? C6 C5 C7 C8' 20.7(16) . . . . ? C10 C7 C8 C9 70.7(11) . . . . ? C5 C7 C8 C9 -98.5(8) . . . . ? C8' C7 C8 C9 160(3) . . . . ? C10 C7 C8' C9' 99(2) . . . . ? C5 C7 C8' C9' -104.0(17) . . . . ? C8 C7 C8' C9' -7(2) . . . . ? C4 N3 C10 C7 -0.6(3) . . . . ? C4 N3 C10 C11 173.9(2) . . . . ? C5 C7 C10 N3 0.9(4) . . . . ? C8 C7 C10 N3 -169.9(8) . . . . ? C8' C7 C10 N3 161.3(14) . . . . ? C5 C7 C10 C11 -172.8(3) . . . . ? C8 C7 C10 C11 16.4(9) . . . . ? C8' C7 C10 C11 -12.3(15) . . . . ? N3 C10 C11 C12 58.0(4) . . . . ? C7 C10 C11 C12 -129.0(3) . . . . ? C18 N4 C12 C13 -1.2(3) . . . . ? C18 N4 C12 C11 172.9(2) . . . . ? C10 C11 C12 N4 40.2(4) . . . . ? C10 C11 C12 C13 -146.9(3) . . . . ? N4 C12 C13 C16 1.3(3) . . . . ? C11 C12 C13 C16 -172.4(3) . . . . ? N4 C12 C13 C14 -179.2(3) . . . . ? C11 C12 C13 C14 7.1(5) . . . . ? C12 C13 C14 C15 85.7(4) . . . . ? C16 C13 C14 C15 -94.9(4) . . . . ? C12 C13 C16 C18 -1.0(3) . . . . ? C14 C13 C16 C18 179.5(3) . . . . ? C12 C13 C16 C17 178.2(3) . . . . ? C14 C13 C16 C17 -1.3(6) . . . . ? C12 N4 C18 C16 0.6(3) . . . . ? C12 N4 C18 C19 -175.1(3) . . . . ? C13 C16 C18 N4 0.2(3) . . . . ? C17 C16 C18 N4 -178.9(3) . . . . ? C13 C16 C18 C19 175.7(3) . . . . ? C17 C16 C18 C19 -3.4(6) . . . . ? N6 N5 C19 O3 -1.3(4) . . . . ? N6 N5 C19 C18 175.3(2) . . . . ? N4 C18 C19 O3 169.8(3) . . . . ? C16 C18 C19 O3 -4.9(5) . . . . ? N4 C18 C19 N5 -6.8(4) . . . . ? C16 C18 C19 N5 178.5(3) . . . . ? N5 N6 C20 O4 -6.1(4) . . . . ? N5 N6 C20 C21 169.9(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.123 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.030 # Attachment '- 2-H2O.cif' data_60909b _database_code_depnum_ccdc_archive 'CCDC 798937' #TrackingRef '- 2-H2O.cif' _audit_update_record ; 2011-06-29 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H34 N6 O4, 0.25(O)' _chemical_formula_sum 'C23 H34 N6 O4.25' _chemical_formula_weight 462.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.094(4) _cell_length_b 12.534(4) _cell_length_c 18.268(6) _cell_angle_alpha 75.307(4) _cell_angle_beta 71.083(5) _cell_angle_gamma 78.421(5) _cell_volume 2512.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1865 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 19.94 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.795793 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 293(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 13721 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8760 _reflns_number_gt 4682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+2.4884P] 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 8760 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1360 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.2306 _refine_ls_wR_factor_gt 0.1998 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.4534(4) 0.7841(4) 0.0604(2) 0.0992(14) Uani 1 1 d . . . O2 O 0.3911(3) 0.4844(3) 0.10632(17) 0.0644(9) Uani 1 1 d . . . O3 O 0.8637(3) 0.7696(2) 0.34128(17) 0.0541(8) Uani 1 1 d . . . O4 O 0.7040(3) 1.0091(2) 0.20701(18) 0.0662(9) Uani 1 1 d . . . O5 O 0.4491(3) 0.8110(3) 0.32014(19) 0.0713(10) Uani 1 1 d . . . O6 O 0.6737(3) 0.6377(3) 0.17484(17) 0.0586(8) Uani 1 1 d . . . O7 O 0.9839(3) 1.0851(3) 0.39663(17) 0.0621(9) Uani 1 1 d . . . O8 O 0.7059(3) 0.9784(3) 0.4800(2) 0.0802(11) Uani 1 1 d . . . N1 N 0.5464(4) 0.6254(4) 0.0224(2) 0.0633(11) Uani 1 1 d . . . H1 H 0.5833 0.5927 -0.0164 0.076 Uiso 1 1 calc R . . N2 N 0.5399(4) 0.5699(3) 0.0994(2) 0.0653(12) Uani 1 1 d . . . H2 H 0.5920 0.5748 0.1207 0.078 Uiso 1 1 calc R . . N3 N 0.4938(3) 0.5020(3) 0.26779(18) 0.0438(9) Uani 1 1 d . . . H3 H 0.5517 0.5407 0.2480 0.053 Uiso 1 1 calc R . . N4 N 0.6127(3) 0.6317(3) 0.37355(18) 0.0436(8) Uani 1 1 d . . . H4 H 0.5535 0.6832 0.3768 0.052 Uiso 1 1 calc R . . N5 N 0.6796(3) 0.8454(3) 0.3382(2) 0.0531(10) Uani 1 1 d . . . H5 H 0.6121 0.8355 0.3367 0.064 Uiso 1 1 calc R . . N6 N 0.7013(3) 0.9511(3) 0.3339(2) 0.0538(10) Uani 1 1 d . . . H6 H 0.7099 0.9671 0.3747 0.065 Uiso 1 1 calc R . . N7 N 0.5102(3) 0.8155(3) 0.1902(2) 0.0616(11) Uani 1 1 d . . . H7 H 0.4904 0.8169 0.1487 0.074 Uiso 1 1 calc R . . N8 N 0.6269(3) 0.8180(3) 0.1823(2) 0.0586(10) Uani 1 1 d . . . H8 H 0.6494 0.8781 0.1838 0.070 Uiso 1 1 calc R . . N9 N 0.8743(3) 0.8319(3) 0.14625(19) 0.0520(9) Uani 1 1 d . . . H9 H 0.8331 0.8949 0.1532 0.062 Uiso 1 1 calc R . . N10 N 1.0103(3) 0.9373(3) 0.24382(19) 0.0507(9) Uani 1 1 d . . . H10 H 0.9894 0.8726 0.2670 0.061 Uiso 1 1 calc R . . N11 N 0.9354(3) 0.9156(3) 0.41334(19) 0.0535(10) Uani 1 1 d . . . H11 H 0.9401 0.8587 0.3938 0.064 Uiso 1 1 calc R . . N12 N 0.8858(3) 0.9126(3) 0.49361(19) 0.0511(9) Uani 1 1 d . . . H12 H 0.9279 0.8853 0.5256 0.061 Uiso 1 1 calc R . . C1 C 0.4849(11) 0.9007(6) -0.0965(5) 0.177(5) Uani 1 1 d . . . H1A H 0.4147 0.9299 -0.0605 0.266 Uiso 1 1 calc R . . H1B H 0.4789 0.9254 -0.1494 0.266 Uiso 1 1 calc R . . H1C H 0.5521 0.9266 -0.0929 0.266 Uiso 1 1 calc R . . C2 C 0.4984(6) 0.7787(5) -0.0760(3) 0.0907(19) Uani 1 1 d . . . H2A H 0.5731 0.7503 -0.1096 0.109 Uiso 1 1 calc R . . H2B H 0.4363 0.7532 -0.0874 0.109 Uiso 1 1 calc R . . C3 C 0.4946(5) 0.7300(5) 0.0093(3) 0.0706(15) Uani 1 1 d . . . C4 C 0.4523(4) 0.5088(3) 0.1405(2) 0.0454(10) Uani 1 1 d . . . C5 C 0.4326(4) 0.4731(3) 0.2250(2) 0.0431(10) Uani 1 1 d . . . C6 C 0.3473(4) 0.4114(4) 0.2783(2) 0.0493(11) Uani 1 1 d . . . C7 C 0.2565(5) 0.3635(5) 0.2611(3) 0.0759(16) Uani 1 1 d . . . H7A H 0.2085 0.4223 0.2359 0.114 Uiso 1 1 d R . . H7B H 0.2077 0.3254 0.3097 0.114 Uiso 1 1 d R . . H7C H 0.2951 0.3121 0.2268 0.114 Uiso 1 1 d R . . C8 C 0.3571(4) 0.4029(3) 0.3544(2) 0.0473(11) Uani 1 1 d . . . C9 C 0.2791(4) 0.3487(4) 0.4317(3) 0.0620(13) Uani 1 1 d . . . H9A H 0.3212 0.3307 0.4712 0.074 Uiso 1 1 calc R . . H9B H 0.2620 0.2795 0.4258 0.074 Uiso 1 1 calc R . . C10 C 0.1643(5) 0.4204(6) 0.4607(3) 0.097(2) Uani 1 1 d . . . H10A H 0.1802 0.4857 0.4719 0.145 Uiso 1 1 calc R . . H10B H 0.1159 0.3793 0.5079 0.145 Uiso 1 1 calc R . . H10C H 0.1240 0.4419 0.4208 0.145 Uiso 1 1 calc R . . C11 C 0.4486(4) 0.4599(3) 0.3453(2) 0.0425(10) Uani 1 1 d . . . C12 C 0.4905(4) 0.4789(4) 0.4091(2) 0.0557(12) Uani 1 1 d . . . H12A H 0.4311 0.5309 0.4368 0.067 Uiso 1 1 calc R . . H12B H 0.4948 0.4090 0.4467 0.067 Uiso 1 1 calc R . . C13 C 0.6064(4) 0.5217(3) 0.3850(2) 0.0452(11) Uani 1 1 d . . . C14 C 0.7185(4) 0.4663(3) 0.3746(2) 0.0487(11) Uani 1 1 d . . . C15 C 0.7503(5) 0.3421(4) 0.3855(3) 0.0732(15) Uani 1 1 d . . . H15A H 0.6882 0.3104 0.3788 0.088 Uiso 1 1 calc R . . H15B H 0.8222 0.3252 0.3448 0.088 Uiso 1 1 calc R . . C16 C 0.7678(7) 0.2884(5) 0.4651(4) 0.111(2) Uani 1 1 d . . . H16A H 0.8310 0.3174 0.4715 0.167 Uiso 1 1 calc R . . H16B H 0.7870 0.2094 0.4689 0.167 Uiso 1 1 calc R . . H16C H 0.6966 0.3039 0.5057 0.167 Uiso 1 1 calc R . . C17 C 0.7968(4) 0.5453(4) 0.3562(2) 0.0467(11) Uani 1 1 d . . . C18 C 0.9273(4) 0.5231(4) 0.3386(3) 0.0682(14) Uani 1 1 d . . . H18A H 0.9558 0.4571 0.3170 0.102 Uiso 1 1 calc R . . H18B H 0.9486 0.5128 0.3865 0.102 Uiso 1 1 calc R . . H18C H 0.9618 0.5851 0.3011 0.102 Uiso 1 1 calc R . . C19 C 0.7282(4) 0.6486(3) 0.3560(2) 0.0408(10) Uani 1 1 d . . . C20 C 0.7638(4) 0.7572(3) 0.3446(2) 0.0439(10) Uani 1 1 d . . . C21 C 0.7093(4) 1.0287(4) 0.2684(3) 0.0512(11) Uani 1 1 d . . . C22 C 0.7226(5) 1.1414(4) 0.2755(3) 0.0749(16) Uani 1 1 d . . . H22A H 0.6795 1.1507 0.3289 0.090 Uiso 1 1 calc R . . H22B H 0.8052 1.1427 0.2689 0.090 Uiso 1 1 calc R . . C23 C 0.6854(9) 1.2333(5) 0.2234(5) 0.152(4) Uani 1 1 d . . . H23A H 0.7343 1.2312 0.1705 0.228 Uiso 1 1 calc R . . H23B H 0.6913 1.3004 0.2373 0.228 Uiso 1 1 calc R . . H23C H 0.6050 1.2314 0.2266 0.228 Uiso 1 1 calc R . . C24 C 0.2406(6) 0.7267(6) 0.3153(5) 0.118(3) Uani 1 1 d . . . H24A H 0.2824 0.6543 0.3094 0.176 Uiso 1 1 calc R . . H24B H 0.1636 0.7323 0.3092 0.176 Uiso 1 1 calc R . . H24C H 0.2332 0.7379 0.3668 0.176 Uiso 1 1 calc R . . C25 C 0.3058(4) 0.8118(5) 0.2548(3) 0.0729(15) Uani 1 1 d . . . H25A H 0.2618 0.8844 0.2606 0.088 Uiso 1 1 calc R . . H25B H 0.3106 0.8010 0.2031 0.088 Uiso 1 1 calc R . . C26 C 0.4280(4) 0.8109(4) 0.2584(3) 0.0568(12) Uani 1 1 d . . . C27 C 0.7058(4) 0.7265(4) 0.1724(2) 0.0479(11) Uani 1 1 d . . . C28 C 0.8291(4) 0.7352(4) 0.1545(2) 0.0475(11) Uani 1 1 d . . . C29 C 0.9243(4) 0.6537(4) 0.1378(3) 0.0565(12) Uani 1 1 d . . . C30 C 0.9190(6) 0.5356(4) 0.1369(4) 0.0881(18) Uani 1 1 d . . . H30A H 0.8968 0.5335 0.0915 0.132 Uiso 1 1 calc R . . H30B H 0.8619 0.5046 0.1841 0.132 Uiso 1 1 calc R . . H30C H 0.9950 0.4930 0.1348 0.132 Uiso 1 1 calc R . . C31 C 1.0268(4) 0.7032(5) 0.1201(3) 0.0644(13) Uani 1 1 d . . . C32 C 1.1522(5) 0.6463(6) 0.0947(4) 0.0933(19) Uani 1 1 d . . . H32A H 1.2041 0.6837 0.1077 0.112 Uiso 1 1 calc R . . H32B H 1.1563 0.5700 0.1238 0.112 Uiso 1 1 calc R . . C33 C 1.1941(6) 0.6472(7) 0.0073(4) 0.129(3) Uani 1 1 d . . . H33A H 1.1472 0.6047 -0.0050 0.194 Uiso 1 1 calc R . . H33B H 1.2752 0.6150 -0.0069 0.194 Uiso 1 1 calc R . . H33C H 1.1866 0.7224 -0.0217 0.194 Uiso 1 1 calc R . . C34 C 0.9938(4) 0.8120(5) 0.1255(2) 0.0571(12) Uani 1 1 d . . . C35 C 1.0686(5) 0.9022(5) 0.1062(3) 0.0820(18) Uani 1 1 d . . . H35A H 1.0611 0.9501 0.0568 0.098 Uiso 1 1 calc R . . H35B H 1.1500 0.8679 0.0967 0.098 Uiso 1 1 calc R . . C36 C 1.0466(4) 0.9750(4) 0.1645(2) 0.0573(13) Uani 1 1 d . . . C37 C 1.0705(5) 1.0813(5) 0.1499(3) 0.0717(16) Uani 1 1 d . . . C38 C 1.1068(7) 1.1593(7) 0.0694(3) 0.126(3) Uani 1 1 d . . . H38A H 1.0812 1.1355 0.0316 0.151 Uiso 1 1 calc R . . H38B H 1.0679 1.2340 0.0736 0.151 Uiso 1 1 calc R . . C39 C 1.2314(10) 1.1606(13) 0.0413(5) 0.235(7) Uani 1 1 d . . . H39A H 1.2592 1.1689 0.0828 0.353 Uiso 1 1 calc R . . H39B H 1.2496 1.2216 -0.0027 0.353 Uiso 1 1 calc R . . H39C H 1.2691 1.0920 0.0248 0.353 Uiso 1 1 calc R . . C40 C 1.0493(4) 1.1100(4) 0.2234(3) 0.0592(13) Uani 1 1 d . . . C41 C 1.0618(7) 1.2218(5) 0.2344(3) 0.102(2) Uani 1 1 d . . . H41A H 1.0104 1.2344 0.2847 0.153 Uiso 1 1 d R . . H41B H 1.0410 1.2790 0.1931 0.153 Uiso 1 1 d R . . H41C H 1.1418 1.2232 0.2323 0.153 Uiso 1 1 d R . . C42 C 1.0122(4) 1.0197(4) 0.2816(2) 0.0451(10) Uani 1 1 d . . . C43 C 0.9762(4) 1.0106(4) 0.3664(2) 0.0428(10) Uani 1 1 d . . . C44 C 0.7716(5) 0.9526(4) 0.5213(3) 0.0577(12) Uani 1 1 d . . . C45 C 0.7312(5) 0.9617(5) 0.6065(3) 0.0666(14) Uani 1 1 d . . . H45A H 0.7319 1.0377 0.6096 0.080 Uiso 1 1 calc R . . H45B H 0.7864 0.9141 0.6330 0.080 Uiso 1 1 calc R . . C46 C 0.6100(5) 0.9299(5) 0.6487(3) 0.0911(18) Uani 1 1 d . . . H46A H 0.5541 0.9794 0.6246 0.137 Uiso 1 1 calc R . . H46B H 0.5898 0.9348 0.7032 0.137 Uiso 1 1 calc R . . H46C H 0.6084 0.8550 0.6454 0.137 Uiso 1 1 calc R . . O9 O 0.5083(8) 0.1616(8) 0.4947(6) 0.115(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.123(4) 0.119(3) 0.075(3) -0.045(2) -0.052(3) 0.015(3) O2 0.072(2) 0.090(2) 0.0489(18) -0.0229(17) -0.0258(17) -0.0262(19) O3 0.055(2) 0.0560(19) 0.0613(19) -0.0119(15) -0.0232(16) -0.0186(16) O4 0.097(3) 0.056(2) 0.058(2) -0.0189(16) -0.0333(19) -0.0116(18) O5 0.067(2) 0.098(3) 0.058(2) -0.0296(18) -0.0334(18) 0.0133(19) O6 0.072(2) 0.063(2) 0.0532(18) -0.0128(15) -0.0227(16) -0.0265(17) O7 0.079(2) 0.069(2) 0.0516(18) -0.0220(16) -0.0201(17) -0.0250(18) O8 0.068(2) 0.118(3) 0.066(2) -0.031(2) -0.033(2) 0.002(2) N1 0.089(3) 0.074(3) 0.035(2) -0.0119(19) -0.020(2) -0.026(3) N2 0.079(3) 0.094(3) 0.035(2) -0.002(2) -0.024(2) -0.039(3) N3 0.053(2) 0.050(2) 0.0349(19) -0.0056(15) -0.0154(16) -0.0208(18) N4 0.052(2) 0.044(2) 0.0427(19) -0.0084(15) -0.0226(17) -0.0088(17) N5 0.060(2) 0.040(2) 0.073(3) -0.0135(18) -0.036(2) -0.0067(19) N6 0.078(3) 0.043(2) 0.057(2) -0.0171(18) -0.034(2) -0.0080(19) N7 0.053(3) 0.095(3) 0.051(2) -0.027(2) -0.023(2) -0.012(2) N8 0.054(3) 0.065(3) 0.068(3) -0.027(2) -0.021(2) -0.011(2) N9 0.060(3) 0.057(2) 0.047(2) -0.0218(17) -0.0120(19) -0.019(2) N10 0.056(2) 0.061(2) 0.042(2) -0.0138(17) -0.0105(18) -0.0255(19) N11 0.067(3) 0.060(2) 0.038(2) -0.0163(17) -0.0101(18) -0.021(2) N12 0.056(3) 0.065(2) 0.038(2) -0.0124(17) -0.0170(18) -0.012(2) C1 0.337(15) 0.092(6) 0.135(7) -0.013(5) -0.154(9) 0.029(7) C2 0.131(6) 0.095(5) 0.057(3) -0.008(3) -0.044(4) -0.021(4) C3 0.083(4) 0.094(4) 0.052(3) -0.020(3) -0.034(3) -0.018(3) C4 0.049(3) 0.052(3) 0.042(2) -0.019(2) -0.015(2) -0.006(2) C5 0.050(3) 0.048(2) 0.039(2) -0.0134(19) -0.017(2) -0.010(2) C6 0.055(3) 0.055(3) 0.045(2) -0.013(2) -0.016(2) -0.015(2) C7 0.078(4) 0.104(4) 0.065(3) -0.016(3) -0.029(3) -0.042(3) C8 0.053(3) 0.048(3) 0.044(2) -0.007(2) -0.015(2) -0.014(2) C9 0.070(3) 0.071(3) 0.049(3) -0.005(2) -0.017(3) -0.027(3) C10 0.076(4) 0.142(6) 0.060(4) -0.021(4) -0.006(3) -0.007(4) C11 0.054(3) 0.046(2) 0.033(2) -0.0040(18) -0.017(2) -0.016(2) C12 0.071(3) 0.071(3) 0.034(2) -0.004(2) -0.019(2) -0.030(3) C13 0.065(3) 0.047(3) 0.036(2) -0.0076(19) -0.025(2) -0.018(2) C14 0.069(3) 0.043(2) 0.041(2) -0.0132(19) -0.019(2) -0.010(2) C15 0.102(4) 0.048(3) 0.069(3) -0.017(3) -0.019(3) -0.011(3) C16 0.170(7) 0.049(3) 0.101(5) -0.008(3) -0.044(5) 0.018(4) C17 0.053(3) 0.051(3) 0.040(2) -0.0099(19) -0.018(2) -0.006(2) C18 0.064(3) 0.071(3) 0.072(3) -0.024(3) -0.020(3) 0.001(3) C19 0.045(3) 0.045(2) 0.041(2) -0.0116(19) -0.0207(19) -0.009(2) C20 0.053(3) 0.048(3) 0.036(2) -0.0095(19) -0.016(2) -0.013(2) C21 0.059(3) 0.047(3) 0.058(3) -0.018(2) -0.028(2) -0.004(2) C22 0.114(5) 0.046(3) 0.088(4) -0.014(3) -0.056(4) -0.017(3) C23 0.313(13) 0.050(4) 0.155(7) 0.000(4) -0.165(8) -0.026(5) C24 0.075(5) 0.111(5) 0.157(7) 0.012(5) -0.047(5) -0.019(4) C25 0.052(3) 0.099(4) 0.072(3) -0.019(3) -0.029(3) 0.002(3) C26 0.056(3) 0.067(3) 0.056(3) -0.025(2) -0.028(3) 0.008(2) C27 0.065(3) 0.054(3) 0.034(2) -0.010(2) -0.019(2) -0.019(3) C28 0.056(3) 0.053(3) 0.042(2) -0.016(2) -0.016(2) -0.015(2) C29 0.067(3) 0.057(3) 0.050(3) -0.016(2) -0.019(2) -0.007(3) C30 0.105(5) 0.062(3) 0.095(4) -0.027(3) -0.020(4) -0.006(3) C31 0.056(3) 0.086(4) 0.055(3) -0.029(3) -0.016(2) 0.000(3) C32 0.066(4) 0.121(5) 0.094(5) -0.039(4) -0.020(3) 0.004(4) C33 0.085(5) 0.188(8) 0.102(5) -0.067(5) 0.000(4) 0.015(5) C34 0.048(3) 0.088(4) 0.042(3) -0.024(2) -0.006(2) -0.020(3) C35 0.076(4) 0.128(5) 0.058(3) -0.038(3) 0.000(3) -0.057(4) C36 0.055(3) 0.085(4) 0.041(3) -0.020(2) -0.008(2) -0.030(3) C37 0.085(4) 0.093(4) 0.046(3) -0.007(3) -0.012(3) -0.051(3) C38 0.164(7) 0.186(8) 0.045(3) -0.011(4) 0.001(4) -0.128(6) C39 0.206(11) 0.43(2) 0.087(6) 0.017(8) -0.027(7) -0.194(13) C40 0.065(3) 0.071(3) 0.049(3) -0.013(2) -0.012(2) -0.032(3) C41 0.156(6) 0.085(4) 0.073(4) -0.007(3) -0.017(4) -0.073(4) C42 0.043(2) 0.059(3) 0.042(2) -0.014(2) -0.014(2) -0.018(2) C43 0.043(2) 0.053(3) 0.041(2) -0.015(2) -0.017(2) -0.012(2) C44 0.063(3) 0.065(3) 0.049(3) -0.016(2) -0.015(3) -0.015(3) C45 0.072(4) 0.082(4) 0.049(3) -0.024(3) -0.011(3) -0.014(3) C46 0.074(4) 0.103(5) 0.080(4) -0.029(3) 0.005(3) -0.008(4) O9 0.096(7) 0.112(7) 0.128(8) -0.015(6) -0.032(6) -0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C3 1.210(6) . ? O2 C4 1.233(4) . ? O3 C20 1.229(5) . ? O4 C21 1.231(5) . ? O5 C26 1.235(5) . ? O6 C27 1.236(5) . ? O7 C43 1.231(4) . ? O8 C44 1.211(5) . ? N1 C3 1.334(7) . ? N1 N2 1.387(5) . ? N1 H1 0.8600 . ? N2 C4 1.339(5) . ? N2 H2 0.8600 . ? N3 C11 1.347(5) . ? N3 C5 1.385(5) . ? N3 H3 0.8600 . ? N4 C13 1.356(5) . ? N4 C19 1.376(5) . ? N4 H4 0.8600 . ? N5 C20 1.354(5) . ? N5 N6 1.380(4) . ? N5 H5 0.8600 . ? N6 C21 1.326(5) . ? N6 H6 0.8600 . ? N7 C26 1.315(6) . ? N7 N8 1.378(5) . ? N7 H7 0.8600 . ? N8 C27 1.347(6) . ? N8 H8 0.8600 . ? N9 C34 1.358(6) . ? N9 C28 1.382(5) . ? N9 H9 0.8600 . ? N10 C36 1.355(5) . ? N10 C42 1.388(5) . ? N10 H10 0.8600 . ? N11 C43 1.357(5) . ? N11 N12 1.386(4) . ? N11 H11 0.8600 . ? N12 C44 1.347(6) . ? N12 H12 0.8600 . ? C1 C2 1.468(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.511(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C5 1.446(5) . ? C5 C6 1.378(6) . ? C6 C8 1.408(5) . ? C6 C7 1.500(6) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C11 1.378(5) . ? C8 C9 1.501(6) . ? C9 C10 1.509(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.499(5) . ? C12 C13 1.492(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.370(6) . ? C14 C17 1.411(6) . ? C14 C15 1.504(6) . ? C15 C16 1.502(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C19 1.391(6) . ? C17 C18 1.487(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.454(5) . ? C21 C22 1.496(6) . ? C22 C23 1.396(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.467(8) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.498(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C27 C28 1.439(6) . ? C28 C29 1.386(6) . ? C29 C31 1.404(7) . ? C29 C30 1.500(7) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C34 1.362(7) . ? C31 C32 1.516(7) . ? C32 C33 1.507(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.491(6) . ? C35 C36 1.500(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.362(6) . ? C37 C40 1.408(6) . ? C37 C38 1.528(7) . ? C38 C39 1.428(12) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C42 1.378(6) . ? C40 C41 1.508(7) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.448(5) . ? C44 C45 1.498(6) . ? C45 C46 1.500(7) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 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 C3 N1 N2 119.2(4) . . ? C3 N1 H1 120.4 . . ? N2 N1 H1 120.4 . . ? C4 N2 N1 119.9(4) . . ? C4 N2 H2 120.1 . . ? N1 N2 H2 120.1 . . ? C11 N3 C5 109.4(3) . . ? C11 N3 H3 125.3 . . ? C5 N3 H3 125.3 . . ? C13 N4 C19 109.8(4) . . ? C13 N4 H4 125.1 . . ? C19 N4 H4 125.1 . . ? C20 N5 N6 120.5(4) . . ? C20 N5 H5 119.7 . . ? N6 N5 H5 119.7 . . ? C21 N6 N5 121.6(3) . . ? C21 N6 H6 119.2 . . ? N5 N6 H6 119.2 . . ? C26 N7 N8 122.7(4) . . ? C26 N7 H7 118.7 . . ? N8 N7 H7 118.7 . . ? C27 N8 N7 120.1(4) . . ? C27 N8 H8 120.0 . . ? N7 N8 H8 120.0 . . ? C34 N9 C28 109.5(4) . . ? C34 N9 H9 125.3 . . ? C28 N9 H9 125.3 . . ? C36 N10 C42 109.1(4) . . ? C36 N10 H10 125.4 . . ? C42 N10 H10 125.4 . . ? C43 N11 N12 118.3(3) . . ? C43 N11 H11 120.8 . . ? N12 N11 H11 120.8 . . ? C44 N12 N11 119.8(4) . . ? C44 N12 H12 120.1 . . ? N11 N12 H12 120.1 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 114.4(5) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? O1 C3 N1 123.0(5) . . ? O1 C3 C2 122.3(6) . . ? N1 C3 C2 114.5(5) . . ? O2 C4 N2 120.0(4) . . ? O2 C4 C5 121.8(4) . . ? N2 C4 C5 118.1(4) . . ? C6 C5 N3 107.2(3) . . ? C6 C5 C4 127.8(4) . . ? N3 C5 C4 124.9(4) . . ? C5 C6 C8 107.7(4) . . ? C5 C6 C7 127.5(4) . . ? C8 C6 C7 124.8(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C8 C6 106.9(4) . . ? C11 C8 C9 125.8(4) . . ? C6 C8 C9 127.2(4) . . ? C8 C9 C10 113.3(4) . . ? C8 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 C8 108.8(3) . . ? N3 C11 C12 123.8(3) . . ? C8 C11 C12 127.4(4) . . ? C13 C12 C11 117.5(3) . . ? C13 C12 H12A 107.9 . . ? C11 C12 H12A 107.9 . . ? C13 C12 H12B 107.9 . . ? C11 C12 H12B 107.9 . . ? H12A C12 H12B 107.2 . . ? N4 C13 C14 108.0(4) . . ? N4 C13 C12 121.2(4) . . ? C14 C13 C12 130.7(4) . . ? C13 C14 C17 108.2(4) . . ? C13 C14 C15 125.3(4) . . ? C17 C14 C15 126.4(5) . . ? C16 C15 C14 113.2(4) . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C14 106.5(4) . . ? C19 C17 C18 126.6(4) . . ? C14 C17 C18 126.9(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 C17 107.5(3) . . ? N4 C19 C20 123.2(4) . . ? C17 C19 C20 129.2(4) . . ? O3 C20 N5 121.2(4) . . ? O3 C20 C19 122.8(4) . . ? N5 C20 C19 116.0(4) . . ? O4 C21 N6 122.1(4) . . ? O4 C21 C22 122.9(4) . . ? N6 C21 C22 115.0(4) . . ? C23 C22 C21 117.6(4) . . ? C23 C22 H22A 107.9 . . ? C21 C22 H22A 107.9 . . ? C23 C22 H22B 107.9 . . ? C21 C22 H22B 107.9 . . ? H22A C22 H22B 107.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C24 C25 C26 114.3(5) . . ? C24 C25 H25A 108.7 . . ? C26 C25 H25A 108.7 . . ? C24 C25 H25B 108.7 . . ? C26 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? O5 C26 N7 122.5(4) . . ? O5 C26 C25 122.5(5) . . ? N7 C26 C25 115.0(4) . . ? O6 C27 N8 120.6(4) . . ? O6 C27 C28 120.4(4) . . ? N8 C27 C28 118.8(4) . . ? N9 C28 C29 106.9(4) . . ? N9 C28 C27 124.8(4) . . ? C29 C28 C27 128.1(4) . . ? C28 C29 C31 107.2(4) . . ? C28 C29 C30 126.4(5) . . ? C31 C29 C30 126.4(5) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C34 C31 C29 108.1(4) . . ? C34 C31 C32 126.3(5) . . ? C29 C31 C32 125.5(5) . . ? C33 C32 C31 112.1(5) . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N9 C34 C31 108.3(4) . . ? N9 C34 C35 122.3(5) . . ? C31 C34 C35 129.2(5) . . ? C34 C35 C36 119.1(4) . . ? C34 C35 H35A 107.5 . . ? C36 C35 H35A 107.5 . . ? C34 C35 H35B 107.5 . . ? C36 C35 H35B 107.5 . . ? H35A C35 H35B 107.0 . . ? N10 C36 C37 108.8(4) . . ? N10 C36 C35 122.9(4) . . ? C37 C36 C35 128.0(4) . . ? C36 C37 C40 107.5(4) . . ? C36 C37 C38 127.2(5) . . ? C40 C37 C38 125.3(5) . . ? C39 C38 C37 111.6(7) . . ? C39 C38 H38A 109.3 . . ? C37 C38 H38A 109.3 . . ? C39 C38 H38B 109.3 . . ? C37 C38 H38B 109.3 . . ? H38A C38 H38B 108.0 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C37 107.7(4) . . ? C42 C40 C41 127.2(4) . . ? C37 C40 C41 125.0(4) . . ? C40 C41 H41A 109.4 . . ? C40 C41 H41B 109.4 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 N10 106.9(4) . . ? C40 C42 C43 128.1(4) . . ? N10 C42 C43 124.9(4) . . ? O7 C43 N11 119.7(4) . . ? O7 C43 C42 122.0(4) . . ? N11 C43 C42 118.3(3) . . ? O8 C44 N12 121.9(4) . . ? O8 C44 C45 122.5(5) . . ? N12 C44 C45 115.7(4) . . ? C44 C45 C46 113.1(4) . . ? C44 C45 H45A 109.0 . . ? C46 C45 H45A 109.0 . . ? C44 C45 H45B 109.0 . . ? C46 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 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 C3 N1 N2 C4 91.9(5) . . . . ? C20 N5 N6 C21 111.8(5) . . . . ? C26 N7 N8 C27 104.8(5) . . . . ? C43 N11 N12 C44 84.3(5) . . . . ? N2 N1 C3 O1 8.8(8) . . . . ? N2 N1 C3 C2 -175.1(4) . . . . ? C1 C2 C3 O1 18.7(10) . . . . ? C1 C2 C3 N1 -157.5(7) . . . . ? N1 N2 C4 O2 13.7(7) . . . . ? N1 N2 C4 C5 -166.3(4) . . . . ? C11 N3 C5 C6 0.0(5) . . . . ? C11 N3 C5 C4 176.4(4) . . . . ? O2 C4 C5 C6 -0.9(7) . . . . ? N2 C4 C5 C6 179.1(4) . . . . ? O2 C4 C5 N3 -176.6(4) . . . . ? N2 C4 C5 N3 3.4(6) . . . . ? N3 C5 C6 C8 0.0(5) . . . . ? C4 C5 C6 C8 -176.3(4) . . . . ? N3 C5 C6 C7 178.3(5) . . . . ? C4 C5 C6 C7 2.0(8) . . . . ? C5 C6 C8 C11 0.0(5) . . . . ? C7 C6 C8 C11 -178.3(5) . . . . ? C5 C6 C8 C9 176.5(4) . . . . ? C7 C6 C8 C9 -1.8(8) . . . . ? C11 C8 C9 C10 96.5(6) . . . . ? C6 C8 C9 C10 -79.5(6) . . . . ? C5 N3 C11 C8 0.0(5) . . . . ? C5 N3 C11 C12 -177.5(4) . . . . ? C6 C8 C11 N3 0.0(5) . . . . ? C9 C8 C11 N3 -176.6(4) . . . . ? C6 C8 C11 C12 177.4(4) . . . . ? C9 C8 C11 C12 0.8(7) . . . . ? N3 C11 C12 C13 -15.8(7) . . . . ? C8 C11 C12 C13 167.2(4) . . . . ? C19 N4 C13 C14 -0.2(4) . . . . ? C19 N4 C13 C12 176.7(3) . . . . ? C11 C12 C13 N4 96.4(5) . . . . ? C11 C12 C13 C14 -87.5(6) . . . . ? N4 C13 C14 C17 0.1(4) . . . . ? C12 C13 C14 C17 -176.4(4) . . . . ? N4 C13 C14 C15 177.0(4) . . . . ? C12 C13 C14 C15 0.5(7) . . . . ? C13 C14 C15 C16 -97.4(6) . . . . ? C17 C14 C15 C16 78.9(7) . . . . ? C13 C14 C17 C19 0.0(4) . . . . ? C15 C14 C17 C19 -176.8(4) . . . . ? C13 C14 C17 C18 -178.8(4) . . . . ? C15 C14 C17 C18 4.4(7) . . . . ? C13 N4 C19 C17 0.2(4) . . . . ? C13 N4 C19 C20 -176.6(3) . . . . ? C14 C17 C19 N4 -0.1(4) . . . . ? C18 C17 C19 N4 178.7(4) . . . . ? C14 C17 C19 C20 176.5(4) . . . . ? C18 C17 C19 C20 -4.7(7) . . . . ? N6 N5 C20 O3 -5.1(6) . . . . ? N6 N5 C20 C19 174.6(3) . . . . ? N4 C19 C20 O3 168.3(4) . . . . ? C17 C19 C20 O3 -7.9(6) . . . . ? N4 C19 C20 N5 -11.4(5) . . . . ? C17 C19 C20 N5 172.5(4) . . . . ? N5 N6 C21 O4 -4.0(7) . . . . ? N5 N6 C21 C22 174.9(4) . . . . ? O4 C21 C22 C23 23.8(9) . . . . ? N6 C21 C22 C23 -155.1(7) . . . . ? N8 N7 C26 O5 1.7(7) . . . . ? N8 N7 C26 C25 178.4(4) . . . . ? C24 C25 C26 O5 -50.6(8) . . . . ? C24 C25 C26 N7 132.7(6) . . . . ? N7 N8 C27 O6 -4.4(6) . . . . ? N7 N8 C27 C28 172.3(4) . . . . ? C34 N9 C28 C29 -0.4(5) . . . . ? C34 N9 C28 C27 -176.9(4) . . . . ? O6 C27 C28 N9 176.4(4) . . . . ? N8 C27 C28 N9 -0.3(6) . . . . ? O6 C27 C28 C29 0.6(7) . . . . ? N8 C27 C28 C29 -176.1(4) . . . . ? N9 C28 C29 C31 0.5(5) . . . . ? C27 C28 C29 C31 176.8(4) . . . . ? N9 C28 C29 C30 -178.2(4) . . . . ? C27 C28 C29 C30 -1.9(7) . . . . ? C28 C29 C31 C34 -0.4(5) . . . . ? C30 C29 C31 C34 178.3(5) . . . . ? C28 C29 C31 C32 -177.1(5) . . . . ? C30 C29 C31 C32 1.6(8) . . . . ? C34 C31 C32 C33 -93.0(7) . . . . ? C29 C31 C32 C33 83.1(7) . . . . ? C28 N9 C34 C31 0.1(5) . . . . ? C28 N9 C34 C35 175.3(4) . . . . ? C29 C31 C34 N9 0.2(5) . . . . ? C32 C31 C34 N9 176.9(5) . . . . ? C29 C31 C34 C35 -174.5(4) . . . . ? C32 C31 C34 C35 2.1(8) . . . . ? N9 C34 C35 C36 53.8(7) . . . . ? C31 C34 C35 C36 -132.1(6) . . . . ? C42 N10 C36 C37 -0.9(5) . . . . ? C42 N10 C36 C35 172.6(4) . . . . ? C34 C35 C36 N10 34.1(8) . . . . ? C34 C35 C36 C37 -153.8(6) . . . . ? N10 C36 C37 C40 0.7(6) . . . . ? C35 C36 C37 C40 -172.3(5) . . . . ? N10 C36 C37 C38 -176.0(6) . . . . ? C35 C36 C37 C38 10.9(10) . . . . ? C36 C37 C38 C39 -98.4(9) . . . . ? C40 C37 C38 C39 85.4(10) . . . . ? C36 C37 C40 C42 -0.3(6) . . . . ? C38 C37 C40 C42 176.6(6) . . . . ? C36 C37 C40 C41 -178.3(5) . . . . ? C38 C37 C40 C41 -1.5(9) . . . . ? C37 C40 C42 N10 -0.3(5) . . . . ? C41 C40 C42 N10 177.7(5) . . . . ? C37 C40 C42 C43 -177.8(4) . . . . ? C41 C40 C42 C43 0.2(8) . . . . ? C36 N10 C42 C40 0.7(5) . . . . ? C36 N10 C42 C43 178.4(4) . . . . ? N12 N11 C43 O7 10.2(6) . . . . ? N12 N11 C43 C42 -171.2(4) . . . . ? C40 C42 C43 O7 -5.6(7) . . . . ? N10 C42 C43 O7 177.3(4) . . . . ? C40 C42 C43 N11 175.8(4) . . . . ? N10 C42 C43 N11 -1.3(6) . . . . ? N11 N12 C44 O8 9.7(7) . . . . ? N11 N12 C44 C45 -171.0(4) . . . . ? O8 C44 C45 C46 38.5(7) . . . . ? N12 C44 C45 C46 -140.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.271 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.052 # Attachment '- 1-2THF.cif' data_r80111e _database_code_depnum_ccdc_archive 'CCDC 798938' #TrackingRef '- 1-2THF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H30 N6 O4, 2(C4 H8 O)' _chemical_formula_sum 'C29 H46 N6 O6' _chemical_formula_weight 574.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.579(2) _cell_length_b 19.247(4) _cell_length_c 30.125(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.26(3) _cell_angle_gamma 90.00 _cell_volume 6117(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9220 _cell_measurement_theta_min 1.720 _cell_measurement_theta_max 27.912 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9826 _exptl_absorpt_correction_T_max 0.9912 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36831 _diffrn_reflns_av_R_equivalents 0.2518 _diffrn_reflns_av_sigmaI/netI 0.2304 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.02 _reflns_number_total 10687 _reflns_number_gt 5156 _reflns_threshold_expression >2sigma(I) _computing_data_collection crystalclear _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10687 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2043 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.1999 _refine_ls_wR_factor_gt 0.1681 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.4029(3) 1.11981(15) 0.27624(13) 0.0357(9) Uani 1 1 d . . . O2 O 0.5414(2) 0.95041(14) 0.33244(13) 0.0318(9) Uani 1 1 d . . . O3 O 0.6649(3) 1.04580(15) 0.02831(13) 0.0356(9) Uani 1 1 d . . . O4 O 0.4409(3) 1.11624(15) 0.09087(13) 0.0362(9) Uani 1 1 d . . . O5 O 0.7250(3) 0.10630(15) 0.22571(13) 0.0346(9) Uani 1 1 d . . . O6 O 0.5211(2) -0.05141(14) 0.16534(12) 0.0317(9) Uani 1 1 d . . . O7 O 0.3964(2) 0.06301(15) 0.46866(13) 0.0316(8) Uani 1 1 d . . . O8 O 0.6932(3) 0.09980(15) 0.41188(13) 0.0380(9) Uani 1 1 d . . . N1 N 0.5592(3) 1.09149(17) 0.32929(15) 0.0319(11) Uani 1 1 d . . . H1 H 0.5898 1.0968 0.3563 0.038 Uiso 1 1 calc R . . N2 N 0.6186(3) 1.04705(17) 0.30030(15) 0.0314(10) Uani 1 1 d . . . H2 H 0.6616 1.0643 0.2798 0.038 Uiso 1 1 calc R . . N3 N 0.7707(3) 0.96345(17) 0.24865(15) 0.0309(10) Uani 1 1 d . . . H3 H 0.7897 1.0068 0.2470 0.037 Uiso 1 1 calc R . . N4 N 0.7731(3) 0.96512(17) 0.13339(15) 0.0287(10) Uani 1 1 d . . . H4 H 0.7081 0.9461 0.1440 0.034 Uiso 1 1 calc R . . N5 N 0.5459(3) 0.99070(17) 0.07722(15) 0.0288(10) Uani 1 1 d . . . H5 H 0.5432 0.9626 0.0993 0.035 Uiso 1 1 calc R . . N6 N 0.4354(3) 1.01393(17) 0.05334(15) 0.0296(10) Uani 1 1 d . . . H6 H 0.3953 0.9874 0.0341 0.035 Uiso 1 1 calc R . . N7 N 0.5649(3) 0.08793(17) 0.17263(15) 0.0328(11) Uani 1 1 d . . . H7 H 0.5367 0.0946 0.1454 0.039 Uiso 1 1 calc R . . N8 N 0.4903(3) 0.05109(17) 0.20121(16) 0.0353(11) Uani 1 1 d . . . H8 H 0.4592 0.0720 0.2232 0.042 Uiso 1 1 calc R . . N9 N 0.3048(3) -0.01575(18) 0.25016(15) 0.0299(10) Uani 1 1 d . . . H9 H 0.3124 0.0276 0.2568 0.036 Uiso 1 1 calc R . . N10 N 0.2846(3) -0.00639(17) 0.36092(15) 0.0284(10) Uani 1 1 d . . . H10 H 0.3449 -0.0315 0.3520 0.034 Uiso 1 1 calc R . . N11 N 0.5088(3) 0.00392(17) 0.42002(15) 0.0318(11) Uani 1 1 d . . . H11 H 0.5105 -0.0175 0.3950 0.038 Uiso 1 1 calc R . . N12 N 0.6174(3) 0.00817(17) 0.44943(15) 0.0324(11) Uani 1 1 d . . . H12 H 0.6302 -0.0217 0.4705 0.039 Uiso 1 1 calc R . . C1 C 0.4032(4) 1.1733(2) 0.3485(2) 0.0383(14) Uani 1 1 d . . . H1C H 0.4084 1.2207 0.3388 0.057 Uiso 1 1 calc R . . H1D H 0.4532 1.1676 0.3762 0.057 Uiso 1 1 calc R . . H1E H 0.3165 1.1619 0.3526 0.057 Uiso 1 1 calc R . . C2 C 0.4526(4) 1.1259(2) 0.3140(2) 0.0328(13) Uani 1 1 d . . . C3 C 0.6086(4) 0.9771(2) 0.3044(2) 0.0334(13) Uani 1 1 d . . . C4 C 0.6811(4) 0.9358(2) 0.27512(19) 0.0302(12) Uani 1 1 d . . . C5 C 0.6772(4) 0.8638(2) 0.26772(18) 0.0275(12) Uani 1 1 d . . . C6 C 0.7690(4) 0.8493(2) 0.23721(17) 0.0258(11) Uani 1 1 d . . . C7 C 0.8241(4) 0.9115(2) 0.22567(18) 0.0278(12) Uani 1 1 d . . . C8 C 0.5926(4) 0.8130(2) 0.28855(18) 0.0318(13) Uani 1 1 d . . . H8C H 0.6227 0.8055 0.3190 0.048 Uiso 1 1 calc R . . H8D H 0.5928 0.7698 0.2727 0.048 Uiso 1 1 calc R . . H8E H 0.5079 0.8311 0.2874 0.048 Uiso 1 1 calc R . . C9 C 0.8018(4) 0.7790(2) 0.2181(2) 0.0366(13) Uani 1 1 d . . . H9A H 0.8926 0.7719 0.2227 0.044 Uiso 1 1 calc R . . H9B H 0.7607 0.7429 0.2343 0.044 Uiso 1 1 calc R . . C10 C 0.7623(4) 0.7713(2) 0.1688(2) 0.0424(14) Uani 1 1 d . . . H10A H 0.6719 0.7753 0.1641 0.064 Uiso 1 1 calc R . . H10B H 0.7885 0.7267 0.1586 0.064 Uiso 1 1 calc R . . H10C H 0.8017 0.8072 0.1524 0.064 Uiso 1 1 calc R . . C11 C 0.9287(4) 0.9263(2) 0.19587(18) 0.0311(12) Uani 1 1 d . . . H11C H 0.9938 0.9527 0.2128 0.037 Uiso 1 1 calc R . . H11D H 0.9662 0.8824 0.1881 0.037 Uiso 1 1 calc R . . C12 C 0.8934(4) 0.9649(2) 0.15380(19) 0.0313(13) Uani 1 1 d . . . C13 C 0.9708(4) 0.9989(2) 0.12576(19) 0.0303(12) Uani 1 1 d . . . C14 C 0.8952(4) 1.0218(2) 0.08790(19) 0.0303(13) Uani 1 1 d . . . C15 C 0.7713(4) 1.0003(2) 0.09325(18) 0.0270(12) Uani 1 1 d . . . C16 C 1.1116(4) 1.0124(2) 0.1366(2) 0.0382(14) Uani 1 1 d . . . H16A H 1.1453 0.9769 0.1570 0.046 Uiso 1 1 calc R . . H16B H 1.1551 1.0086 0.1095 0.046 Uiso 1 1 calc R . . C17 C 1.1392(4) 1.0835(2) 0.1573(2) 0.0496(17) Uani 1 1 d . . . H17A H 1.1113 1.1191 0.1365 0.074 Uiso 1 1 calc R . . H17B H 1.2287 1.0881 0.1646 0.074 Uiso 1 1 calc R . . H17C H 1.0951 1.0881 0.1839 0.074 Uiso 1 1 calc R . . C18 C 0.9440(4) 1.0599(2) 0.0491(2) 0.0445(15) Uani 1 1 d . . . H18A H 0.8783 1.0626 0.0254 0.067 Uiso 1 1 calc R . . H18B H 1.0155 1.0355 0.0389 0.067 Uiso 1 1 calc R . . H18C H 0.9693 1.1060 0.0581 0.067 Uiso 1 1 calc R . . C19 C 0.6595(4) 1.0150(2) 0.06367(19) 0.0274(12) Uani 1 1 d . . . C20 C 0.3927(4) 1.0785(2) 0.06099(19) 0.0316(13) Uani 1 1 d . . . C21 C 0.2828(4) 1.1023(2) 0.03036(19) 0.0369(14) Uani 1 1 d . . . H21A H 0.2157 1.1181 0.0476 0.055 Uiso 1 1 calc R . . H21B H 0.2529 1.0643 0.0118 0.055 Uiso 1 1 calc R . . H21C H 0.3094 1.1397 0.0121 0.055 Uiso 1 1 calc R . . C22 C 0.7446(4) 0.1522(2) 0.1515(2) 0.0387(14) Uani 1 1 d . . . H22A H 0.7543 0.2001 0.1602 0.058 Uiso 1 1 calc R . . H22B H 0.6940 0.1493 0.1238 0.058 Uiso 1 1 calc R . . H22C H 0.8264 0.1322 0.1482 0.058 Uiso 1 1 calc R . . C23 C 0.6800(4) 0.1131(2) 0.1869(2) 0.0327(13) Uani 1 1 d . . . C24 C 0.4674(4) -0.0179(2) 0.19418(18) 0.0279(12) Uani 1 1 d . . . C25 C 0.3756(4) -0.0508(2) 0.22032(19) 0.0307(13) Uani 1 1 d . . . C26 C 0.3346(4) -0.1196(2) 0.21885(19) 0.0318(13) Uani 1 1 d . . . C27 C 0.2381(4) -0.1253(2) 0.24868(18) 0.0283(12) Uani 1 1 d . . . C28 C 0.2215(4) -0.0606(2) 0.26725(18) 0.0290(12) Uani 1 1 d . . . C29 C 0.3802(4) -0.1773(2) 0.1904(2) 0.0388(14) Uani 1 1 d . . . H29A H 0.3514 -0.1692 0.1599 0.058 Uiso 1 1 calc R . . H29B H 0.3471 -0.2208 0.2000 0.058 Uiso 1 1 calc R . . H29C H 0.4712 -0.1788 0.1932 0.058 Uiso 1 1 calc R . . C30 C 0.1649(4) -0.1907(2) 0.25839(19) 0.0362(14) Uani 1 1 d . . . H30A H 0.1486 -0.2167 0.2310 0.043 Uiso 1 1 calc R . . H30B H 0.0837 -0.1776 0.2688 0.043 Uiso 1 1 calc R . . C31 C 0.2343(5) -0.2378(2) 0.2931(2) 0.0507(16) Uani 1 1 d . . . H31A H 0.3100 -0.2556 0.2815 0.076 Uiso 1 1 calc R . . H31B H 0.1802 -0.2757 0.2999 0.076 Uiso 1 1 calc R . . H31C H 0.2564 -0.2116 0.3196 0.076 Uiso 1 1 calc R . . C32 C 0.1256(4) -0.0360(2) 0.29756(19) 0.0357(13) Uani 1 1 d . . . H32A H 0.0658 -0.0067 0.2803 0.043 Uiso 1 1 calc R . . H32B H 0.0789 -0.0764 0.3066 0.043 Uiso 1 1 calc R . . C33 C 0.1686(4) 0.0025(2) 0.33817(18) 0.0282(12) Uani 1 1 d . . . C34 C 0.0987(4) 0.0470(2) 0.36378(18) 0.0287(12) Uani 1 1 d . . . C35 C 0.1743(4) 0.0641(2) 0.40234(19) 0.0301(13) Uani 1 1 d . . . C36 C 0.2908(4) 0.0309(2) 0.40034(18) 0.0274(12) Uani 1 1 d . . . C37 C -0.0325(4) 0.0714(2) 0.34809(19) 0.0369(13) Uani 1 1 d . . . H37A H -0.0780 0.0837 0.3738 0.044 Uiso 1 1 calc R . . H37B H -0.0778 0.0336 0.3327 0.044 Uiso 1 1 calc R . . C38 C -0.0312(5) 0.1335(3) 0.3172(2) 0.0587(19) Uani 1 1 d . . . H38A H 0.0083 0.1721 0.3328 0.088 Uiso 1 1 calc R . . H38B H -0.1167 0.1455 0.3071 0.088 Uiso 1 1 calc R . . H38C H 0.0154 0.1221 0.2920 0.088 Uiso 1 1 calc R . . C39 C 0.1378(4) 0.1124(2) 0.43817(19) 0.0373(13) Uani 1 1 d . . . H39A H 0.0535 0.1294 0.4310 0.056 Uiso 1 1 calc R . . H39B H 0.1959 0.1508 0.4405 0.056 Uiso 1 1 calc R . . H39C H 0.1408 0.0880 0.4660 0.056 Uiso 1 1 calc R . . C40 C 0.3998(4) 0.0348(2) 0.43204(19) 0.0274(12) Uani 1 1 d . . . C41 C 0.7022(4) 0.0601(2) 0.4442(2) 0.0330(13) Uani 1 1 d . . . C42 C 0.8092(4) 0.0631(2) 0.4803(2) 0.0405(14) Uani 1 1 d . . . H42A H 0.8844 0.0437 0.4693 0.061 Uiso 1 1 calc R . . H42B H 0.7865 0.0370 0.5056 0.061 Uiso 1 1 calc R . . H42C H 0.8247 0.1106 0.4888 0.061 Uiso 1 1 calc R . . O9 O 0.5810(3) 0.73835(16) 0.01493(14) 0.0476(10) Uani 1 1 d . . . C43 C 0.6141(4) 0.7584(2) 0.0597(2) 0.0394(14) Uani 1 1 d . . . H43A H 0.6870 0.7891 0.0611 0.047 Uiso 1 1 calc R . . H43B H 0.6348 0.7179 0.0779 0.047 Uiso 1 1 calc R . . C44 C 0.4994(4) 0.7958(2) 0.0760(2) 0.0429(15) Uani 1 1 d . . . H44A H 0.5244 0.8321 0.0972 0.051 Uiso 1 1 calc R . . H44B H 0.4426 0.7637 0.0894 0.051 Uiso 1 1 calc R . . C45 C 0.4394(4) 0.8257(2) 0.0326(2) 0.0404(15) Uani 1 1 d . . . H45A H 0.4802 0.8687 0.0249 0.048 Uiso 1 1 calc R . . H45B H 0.3495 0.8339 0.0343 0.048 Uiso 1 1 calc R . . C46 C 0.4630(4) 0.7685(2) -0.0009(2) 0.0433(15) Uani 1 1 d . . . H46A H 0.3957 0.7342 -0.0018 0.052 Uiso 1 1 calc R . . H46B H 0.4681 0.7877 -0.0305 0.052 Uiso 1 1 calc R . . O10 O 0.1643(3) 0.77758(17) 0.07466(15) 0.0501(11) Uani 1 1 d . . . C47 C 0.1065(5) 0.8418(2) 0.0861(2) 0.0570(19) Uani 1 1 d . . . H47A H 0.1554 0.8805 0.0759 0.068 Uiso 1 1 calc R . . H47B H 0.1048 0.8453 0.1182 0.068 Uiso 1 1 calc R . . C48 C -0.0263(4) 0.8448(3) 0.0647(2) 0.0571(19) Uani 1 1 d . . . H48A H -0.0343 0.8804 0.0419 0.068 Uiso 1 1 calc R . . H48B H -0.0870 0.8540 0.0866 0.068 Uiso 1 1 calc R . . C49 C -0.0453(4) 0.7726(2) 0.0447(2) 0.0503(17) Uani 1 1 d . . . H49A H -0.0846 0.7416 0.0650 0.060 Uiso 1 1 calc R . . H49B H -0.0971 0.7744 0.0168 0.060 Uiso 1 1 calc R . . C50 C 0.0879(4) 0.7501(3) 0.0376(2) 0.0514(17) Uani 1 1 d . . . H50A H 0.0938 0.6998 0.0369 0.062 Uiso 1 1 calc R . . H50B H 0.1146 0.7686 0.0099 0.062 Uiso 1 1 calc R . . O11 O 0.0856(3) 0.21907(16) 0.06938(15) 0.0500(11) Uani 1 1 d . . . C51 C -0.0180(5) 0.2504(2) 0.0898(2) 0.059(2) Uani 1 1 d . . . H51A H -0.0095 0.2433 0.1218 0.071 Uiso 1 1 calc R . . H51B H -0.0978 0.2304 0.0781 0.071 Uiso 1 1 calc R . . C52 C -0.0135(5) 0.3277(2) 0.0789(3) 0.064(2) Uani 1 1 d . . . H52A H -0.0759 0.3395 0.0549 0.077 Uiso 1 1 calc R . . H52B H -0.0287 0.3556 0.1048 0.077 Uiso 1 1 calc R . . C53 C 0.1186(5) 0.3384(3) 0.0652(3) 0.088(3) Uani 1 1 d . . . H53A H 0.1164 0.3539 0.0345 0.105 Uiso 1 1 calc R . . H53B H 0.1624 0.3731 0.0839 0.105 Uiso 1 1 calc R . . C54 C 0.1846(5) 0.2699(2) 0.0704(2) 0.0525(17) Uani 1 1 d . . . H54A H 0.2387 0.2622 0.0462 0.063 Uiso 1 1 calc R . . H54B H 0.2359 0.2679 0.0984 0.063 Uiso 1 1 calc R . . O12 O 0.4492(4) 0.3510(2) 0.1282(2) 0.0856(16) Uani 1 1 d . . . C55 C 0.5521(6) 0.3067(3) 0.1352(3) 0.088(3) Uani 1 1 d . . . H55A H 0.5298 0.2609 0.1237 0.106 Uiso 1 1 calc R . . H55B H 0.5753 0.3025 0.1668 0.106 Uiso 1 1 calc R . . C56 C 0.6601(5) 0.3343(4) 0.1124(3) 0.085(3) Uani 1 1 d . . . H56A H 0.6953 0.2994 0.0937 0.102 Uiso 1 1 calc R . . H56B H 0.7263 0.3515 0.1336 0.102 Uiso 1 1 calc R . . C57 C 0.5979(5) 0.3941(3) 0.0843(3) 0.070(2) Uani 1 1 d . . . H57A H 0.6180 0.4390 0.0977 0.084 Uiso 1 1 calc R . . H57B H 0.6245 0.3936 0.0541 0.084 Uiso 1 1 calc R . . C58 C 0.4600(5) 0.3778(3) 0.0851(3) 0.0637(19) Uani 1 1 d . . . H58A H 0.4088 0.4193 0.0802 0.076 Uiso 1 1 calc R . . H58B H 0.4338 0.3437 0.0626 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0489(18) 0.0413(17) 0.016(3) -0.0013(17) -0.0040(17) 0.0040(15) O2 0.0365(16) 0.0364(16) 0.023(3) 0.0020(16) 0.0077(15) 0.0017(14) O3 0.0408(17) 0.0439(18) 0.022(3) 0.0067(17) -0.0005(16) -0.0033(14) O4 0.0511(18) 0.0421(17) 0.015(3) -0.0024(17) -0.0028(16) -0.0015(15) O5 0.0474(17) 0.0431(18) 0.013(3) -0.0003(16) 0.0007(16) -0.0028(14) O6 0.0345(16) 0.0417(17) 0.019(3) -0.0002(16) 0.0045(15) -0.0028(14) O7 0.0397(16) 0.0421(17) 0.013(3) -0.0001(16) 0.0010(15) 0.0000(14) O8 0.0502(18) 0.0405(17) 0.023(3) 0.0050(17) 0.0021(17) -0.0029(15) N1 0.042(2) 0.036(2) 0.016(3) -0.0026(18) 0.0005(19) 0.0057(17) N2 0.042(2) 0.037(2) 0.017(3) -0.0029(19) 0.0121(18) 0.0034(17) N3 0.0363(19) 0.0365(19) 0.021(3) 0.0012(19) 0.0079(18) -0.0048(17) N4 0.0299(18) 0.0367(19) 0.019(3) 0.0006(19) -0.0035(16) -0.0032(16) N5 0.0323(19) 0.0359(19) 0.017(3) 0.0067(18) -0.0035(17) 0.0008(16) N6 0.0299(18) 0.037(2) 0.021(3) 0.0011(18) -0.0045(17) -0.0012(16) N7 0.044(2) 0.044(2) 0.011(3) 0.0043(19) 0.0023(19) -0.0082(18) N8 0.046(2) 0.041(2) 0.019(4) -0.005(2) 0.0068(19) -0.0107(18) N9 0.038(2) 0.0377(19) 0.014(3) -0.0031(19) 0.0045(18) 0.0031(17) N10 0.0311(18) 0.0370(19) 0.018(3) 0.0007(19) 0.0043(17) 0.0073(16) N11 0.0333(19) 0.041(2) 0.021(4) -0.0009(19) -0.0021(18) 0.0007(17) N12 0.0307(18) 0.038(2) 0.028(4) 0.0068(19) -0.0023(18) 0.0026(17) C1 0.054(3) 0.041(3) 0.021(5) 0.002(2) 0.007(2) 0.007(2) C2 0.046(3) 0.031(2) 0.023(5) 0.002(2) 0.008(2) -0.002(2) C3 0.035(2) 0.042(3) 0.023(4) -0.003(2) -0.002(2) 0.001(2) C4 0.033(2) 0.037(2) 0.019(4) -0.004(2) -0.001(2) 0.008(2) C5 0.030(2) 0.035(2) 0.017(4) 0.002(2) 0.002(2) 0.0013(19) C6 0.034(2) 0.038(2) 0.005(4) 0.001(2) 0.0011(19) 0.003(2) C7 0.034(2) 0.041(2) 0.008(4) -0.003(2) 0.000(2) 0.007(2) C8 0.036(2) 0.040(2) 0.020(4) 0.004(2) 0.006(2) 0.003(2) C9 0.042(2) 0.042(3) 0.027(5) -0.006(2) 0.001(2) 0.004(2) C10 0.051(3) 0.045(3) 0.032(5) -0.004(3) 0.010(3) 0.005(2) C11 0.033(2) 0.038(2) 0.022(4) -0.001(2) 0.001(2) 0.003(2) C12 0.030(2) 0.033(2) 0.030(4) -0.002(2) -0.001(2) 0.0065(19) C13 0.033(2) 0.036(2) 0.023(4) -0.003(2) 0.004(2) 0.002(2) C14 0.034(2) 0.029(2) 0.029(4) 0.002(2) 0.009(2) 0.0005(19) C15 0.034(2) 0.029(2) 0.017(4) 0.005(2) 0.001(2) 0.0044(19) C16 0.033(2) 0.046(3) 0.036(5) 0.004(3) -0.002(2) -0.009(2) C17 0.040(3) 0.050(3) 0.056(6) 0.006(3) -0.014(3) -0.008(2) C18 0.041(3) 0.056(3) 0.036(5) 0.011(3) 0.005(2) -0.008(2) C19 0.034(2) 0.028(2) 0.021(4) -0.002(2) 0.007(2) 0.0027(19) C20 0.035(2) 0.039(3) 0.021(4) 0.005(2) 0.009(2) -0.004(2) C21 0.037(2) 0.047(3) 0.027(5) 0.005(3) 0.002(2) 0.003(2) C22 0.053(3) 0.036(2) 0.028(5) 0.002(2) 0.007(3) -0.011(2) C23 0.047(3) 0.027(2) 0.024(5) -0.004(2) 0.005(3) -0.007(2) C24 0.033(2) 0.042(2) 0.009(4) -0.001(2) 0.001(2) -0.004(2) C25 0.029(2) 0.039(2) 0.024(4) -0.002(2) 0.005(2) -0.001(2) C26 0.031(2) 0.046(3) 0.018(4) 0.001(2) -0.002(2) 0.003(2) C27 0.032(2) 0.041(2) 0.011(4) 0.003(2) -0.002(2) 0.003(2) C28 0.031(2) 0.039(2) 0.017(4) -0.006(2) 0.002(2) 0.004(2) C29 0.048(3) 0.038(2) 0.032(5) -0.001(2) 0.013(3) 0.004(2) C30 0.038(2) 0.042(3) 0.030(5) -0.010(2) 0.009(2) -0.003(2) C31 0.066(3) 0.048(3) 0.039(5) 0.015(3) 0.006(3) -0.014(3) C32 0.033(2) 0.052(3) 0.022(4) -0.006(3) 0.002(2) 0.002(2) C33 0.032(2) 0.035(2) 0.018(4) 0.005(2) 0.004(2) 0.0039(19) C34 0.030(2) 0.035(2) 0.020(4) 0.002(2) 0.001(2) 0.0007(19) C35 0.034(2) 0.027(2) 0.029(4) 0.000(2) 0.003(2) 0.0016(19) C36 0.031(2) 0.036(2) 0.016(4) 0.000(2) 0.005(2) -0.0014(19) C37 0.034(2) 0.051(3) 0.026(4) -0.007(3) 0.001(2) 0.005(2) C38 0.057(3) 0.060(3) 0.056(6) 0.007(3) -0.009(3) 0.016(3) C39 0.047(3) 0.043(3) 0.022(4) -0.007(2) 0.004(2) 0.005(2) C40 0.038(2) 0.030(2) 0.015(4) 0.002(2) 0.007(2) -0.003(2) C41 0.041(3) 0.032(2) 0.027(5) -0.005(2) 0.006(2) 0.003(2) C42 0.045(3) 0.046(3) 0.029(5) 0.006(3) -0.005(2) -0.006(2) O9 0.065(2) 0.0523(19) 0.026(3) 0.0008(19) 0.0067(19) 0.0139(17) C43 0.047(3) 0.050(3) 0.021(5) 0.004(3) 0.001(2) 0.004(2) C44 0.054(3) 0.041(3) 0.034(5) -0.002(3) 0.008(3) 0.005(2) C45 0.040(2) 0.041(3) 0.040(5) 0.011(3) 0.004(2) -0.002(2) C46 0.054(3) 0.043(3) 0.032(5) 0.001(3) -0.003(3) -0.005(2) O10 0.0489(19) 0.054(2) 0.048(4) 0.007(2) 0.0043(19) -0.0009(17) C47 0.065(3) 0.047(3) 0.058(6) -0.006(3) 0.003(3) -0.003(3) C48 0.053(3) 0.055(3) 0.064(6) -0.006(3) 0.015(3) 0.010(3) C49 0.052(3) 0.053(3) 0.045(6) -0.005(3) -0.004(3) 0.009(3) C50 0.059(3) 0.053(3) 0.043(6) -0.008(3) 0.009(3) 0.007(3) O11 0.056(2) 0.0447(18) 0.052(4) -0.0080(19) 0.023(2) -0.0030(17) C51 0.074(4) 0.047(3) 0.060(6) -0.007(3) 0.037(4) -0.002(3) C52 0.067(4) 0.047(3) 0.082(7) -0.004(3) 0.031(4) 0.002(3) C53 0.069(4) 0.043(3) 0.156(10) -0.007(4) 0.043(5) -0.003(3) C54 0.056(3) 0.058(3) 0.044(6) -0.012(3) 0.008(3) -0.005(3) O12 0.085(3) 0.108(3) 0.064(6) 0.002(3) 0.009(3) 0.006(3) C55 0.096(5) 0.090(4) 0.087(8) 0.056(5) 0.056(5) 0.065(4) C56 0.040(3) 0.151(6) 0.064(7) 0.013(5) -0.007(3) 0.017(4) C57 0.094(4) 0.059(3) 0.061(7) 0.004(4) 0.030(4) -0.007(3) C58 0.063(4) 0.101(5) 0.025(6) 0.009(4) -0.003(3) 0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.223(6) . ? O2 C3 1.253(6) . ? O3 C19 1.224(6) . ? O4 C20 1.236(6) . ? O5 C23 1.237(6) . ? O6 C24 1.252(6) . ? O7 C40 1.232(6) . ? O8 C41 1.237(6) . ? N1 C2 1.359(6) . ? N1 N2 1.404(5) . ? N1 H1 0.8600 . ? N2 C3 1.358(5) . ? N2 H2 0.8600 . ? N3 C7 1.361(5) . ? N3 C4 1.390(6) . ? N3 H3 0.8600 . ? N4 C12 1.372(5) . ? N4 C15 1.385(6) . ? N4 H4 0.8600 . ? N5 C19 1.380(5) . ? N5 N6 1.401(4) . ? N5 H5 0.8600 . ? N6 C20 1.348(5) . ? N6 H6 0.8600 . ? N7 C23 1.351(5) . ? N7 N8 1.402(5) . ? N7 H7 0.8600 . ? N8 C24 1.363(5) . ? N8 H8 0.8600 . ? N9 C28 1.361(5) . ? N9 C25 1.387(6) . ? N9 H9 0.8600 . ? N10 C33 1.371(5) . ? N10 C36 1.385(6) . ? N10 H10 0.8600 . ? N11 C40 1.370(5) . ? N11 N12 1.400(5) . ? N11 H11 0.8600 . ? N12 C41 1.360(5) . ? N12 H12 0.8600 . ? C1 C2 1.506(7) . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C3 C4 1.449(7) . ? C4 C5 1.404(6) . ? C5 C6 1.413(6) . ? C5 C8 1.494(6) . ? C6 C7 1.388(6) . ? C6 C9 1.521(6) . ? C7 C11 1.504(6) . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C8 H8E 0.9600 . ? C9 C10 1.521(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.492(7) . ? C11 H11C 0.9700 . ? C11 H11D 0.9700 . ? C12 C13 1.384(7) . ? C13 C14 1.414(7) . ? C13 C16 1.524(5) . ? C14 C15 1.394(5) . ? C14 C18 1.504(7) . ? C15 C19 1.455(6) . ? C16 C17 1.522(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C20 C21 1.501(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.508(7) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C24 C25 1.442(6) . ? C25 C26 1.392(6) . ? C26 C27 1.414(7) . ? C26 C29 1.504(6) . ? C27 C28 1.382(6) . ? C27 C30 1.518(6) . ? C28 C32 1.492(6) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.529(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.473(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.400(6) . ? C34 C35 1.400(7) . ? C34 C37 1.508(5) . ? C35 C36 1.393(5) . ? C35 C39 1.497(7) . ? C36 C40 1.444(6) . ? C37 C38 1.515(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C41 C42 1.510(7) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? O9 C43 1.420(6) . ? O9 C46 1.426(5) . ? C43 C44 1.523(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.524(7) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.526(7) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? O10 C50 1.430(7) . ? O10 C47 1.433(6) . ? C47 C48 1.502(7) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.522(7) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.505(6) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? O11 C51 1.430(5) . ? O11 C54 1.431(5) . ? C51 C52 1.524(7) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.501(7) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.495(7) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? O12 C55 1.386(6) . ? O12 C58 1.411(8) . ? C55 C56 1.475(8) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 C57 1.547(8) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.495(7) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 N2 119.0(5) . . ? C2 N1 H1 120.5 . . ? N2 N1 H1 120.5 . . ? C3 N2 N1 120.4(4) . . ? C3 N2 H2 119.8 . . ? N1 N2 H2 119.8 . . ? C7 N3 C4 109.6(3) . . ? C7 N3 H3 125.2 . . ? C4 N3 H3 125.2 . . ? C12 N4 C15 110.2(4) . . ? C12 N4 H4 124.9 . . ? C15 N4 H4 124.9 . . ? C19 N5 N6 116.9(4) . . ? C19 N5 H5 121.6 . . ? N6 N5 H5 121.6 . . ? C20 N6 N5 118.9(4) . . ? C20 N6 H6 120.5 . . ? N5 N6 H6 120.5 . . ? C23 N7 N8 121.4(5) . . ? C23 N7 H7 119.3 . . ? N8 N7 H7 119.3 . . ? C24 N8 N7 119.9(4) . . ? C24 N8 H8 120.1 . . ? N7 N8 H8 120.1 . . ? C28 N9 C25 109.4(3) . . ? C28 N9 H9 125.3 . . ? C25 N9 H9 125.3 . . ? C33 N10 C36 110.4(4) . . ? C33 N10 H10 124.8 . . ? C36 N10 H10 124.8 . . ? C40 N11 N12 118.3(4) . . ? C40 N11 H11 120.8 . . ? N12 N11 H11 120.8 . . ? C41 N12 N11 119.2(4) . . ? C41 N12 H12 120.4 . . ? N11 N12 H12 120.4 . . ? C2 C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C2 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? O1 C2 N1 123.8(5) . . ? O1 C2 C1 123.6(4) . . ? N1 C2 C1 112.5(5) . . ? O2 C3 N2 121.3(4) . . ? O2 C3 C4 122.5(4) . . ? N2 C3 C4 116.1(4) . . ? N3 C4 C5 107.5(4) . . ? N3 C4 C3 123.6(4) . . ? C5 C4 C3 128.9(4) . . ? C4 C5 C6 106.5(4) . . ? C4 C5 C8 126.2(4) . . ? C6 C5 C8 127.3(4) . . ? C7 C6 C5 108.3(4) . . ? C7 C6 C9 124.1(4) . . ? C5 C6 C9 127.5(4) . . ? N3 C7 C6 108.0(4) . . ? N3 C7 C11 121.0(4) . . ? C6 C7 C11 130.9(4) . . ? C5 C8 H8C 109.5 . . ? C5 C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? C5 C8 H8E 109.5 . . ? H8C C8 H8E 109.5 . . ? H8D C8 H8E 109.5 . . ? C10 C9 C6 113.7(4) . . ? C10 C9 H9A 108.8 . . ? C6 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C6 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C7 116.9(4) . . ? C12 C11 H11C 108.1 . . ? C7 C11 H11C 108.1 . . ? C12 C11 H11D 108.1 . . ? C7 C11 H11D 108.1 . . ? H11C C11 H11D 107.3 . . ? N4 C12 C13 107.2(5) . . ? N4 C12 C11 123.2(4) . . ? C13 C12 C11 129.1(4) . . ? C12 C13 C14 108.3(4) . . ? C12 C13 C16 124.3(5) . . ? C14 C13 C16 127.3(4) . . ? C15 C14 C13 107.1(4) . . ? C15 C14 C18 127.9(5) . . ? C13 C14 C18 124.9(4) . . ? N4 C15 C14 107.1(4) . . ? N4 C15 C19 126.0(4) . . ? C14 C15 C19 126.8(5) . . ? C17 C16 C13 113.4(4) . . ? C17 C16 H16A 108.9 . . ? C13 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C13 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C19 N5 121.3(4) . . ? O3 C19 C15 122.6(4) . . ? N5 C19 C15 116.0(4) . . ? O4 C20 N6 122.7(4) . . ? O4 C20 C21 121.8(4) . . ? N6 C20 C21 115.4(4) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 N7 122.5(5) . . ? O5 C23 C22 123.9(4) . . ? N7 C23 C22 113.6(5) . . ? O6 C24 N8 121.7(4) . . ? O6 C24 C25 120.7(4) . . ? N8 C24 C25 117.6(4) . . ? N9 C25 C26 107.5(4) . . ? N9 C25 C24 123.9(4) . . ? C26 C25 C24 128.4(5) . . ? C25 C26 C27 107.0(4) . . ? C25 C26 C29 127.5(4) . . ? C27 C26 C29 125.5(4) . . ? C28 C27 C26 107.8(4) . . ? C28 C27 C30 126.0(4) . . ? C26 C27 C30 126.2(4) . . ? N9 C28 C27 108.2(4) . . ? N9 C28 C32 121.3(4) . . ? C27 C28 C32 130.2(4) . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 C31 113.4(4) . . ? C27 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? C27 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C28 119.0(4) . . ? C33 C32 H32A 107.6 . . ? C28 C32 H32A 107.6 . . ? C33 C32 H32B 107.6 . . ? C28 C32 H32B 107.6 . . ? H32A C32 H32B 107.0 . . ? N10 C33 C34 106.9(4) . . ? N10 C33 C32 124.2(4) . . ? C34 C33 C32 128.5(4) . . ? C33 C34 C35 108.0(4) . . ? C33 C34 C37 122.0(5) . . ? C35 C34 C37 130.0(4) . . ? C36 C35 C34 108.0(4) . . ? C36 C35 C39 126.3(5) . . ? C34 C35 C39 125.7(4) . . ? N10 C36 C35 106.8(4) . . ? N10 C36 C40 125.4(4) . . ? C35 C36 C40 127.8(5) . . ? C34 C37 C38 112.9(4) . . ? C34 C37 H37A 109.0 . . ? C38 C37 H37A 109.0 . . ? C34 C37 H37B 109.0 . . ? C38 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 C40 N11 120.6(4) . . ? O7 C40 C36 122.7(4) . . ? N11 C40 C36 116.7(4) . . ? O8 C41 N12 122.1(5) . . ? O8 C41 C42 123.5(4) . . ? N12 C41 C42 114.3(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C43 O9 C46 110.8(4) . . ? O9 C43 C44 106.8(4) . . ? O9 C43 H43A 110.4 . . ? C44 C43 H43A 110.4 . . ? O9 C43 H43B 110.4 . . ? C44 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? C43 C44 C45 101.0(5) . . ? C43 C44 H44A 111.6 . . ? C45 C44 H44A 111.6 . . ? C43 C44 H44B 111.6 . . ? C45 C44 H44B 111.6 . . ? H44A C44 H44B 109.4 . . ? C44 C45 C46 102.5(4) . . ? C44 C45 H45A 111.3 . . ? C46 C45 H45A 111.3 . . ? C44 C45 H45B 111.3 . . ? C46 C45 H45B 111.3 . . ? H45A C45 H45B 109.2 . . ? O9 C46 C45 104.7(4) . . ? O9 C46 H46A 110.8 . . ? C45 C46 H46A 110.8 . . ? O9 C46 H46B 110.8 . . ? C45 C46 H46B 110.8 . . ? H46A C46 H46B 108.9 . . ? C50 O10 C47 106.2(4) . . ? O10 C47 C48 109.4(4) . . ? O10 C47 H47A 109.8 . . ? C48 C47 H47A 109.8 . . ? O10 C47 H47B 109.8 . . ? C48 C47 H47B 109.8 . . ? H47A C47 H47B 108.2 . . ? C47 C48 C49 103.1(4) . . ? C47 C48 H48A 111.1 . . ? C49 C48 H48A 111.1 . . ? C47 C48 H48B 111.1 . . ? C49 C48 H48B 111.1 . . ? H48A C48 H48B 109.1 . . ? C50 C49 C48 102.8(4) . . ? C50 C49 H49A 111.2 . . ? C48 C49 H49A 111.2 . . ? C50 C49 H49B 111.2 . . ? C48 C49 H49B 111.2 . . ? H49A C49 H49B 109.1 . . ? O10 C50 C49 105.3(4) . . ? O10 C50 H50A 110.7 . . ? C49 C50 H50A 110.7 . . ? O10 C50 H50B 110.7 . . ? C49 C50 H50B 110.7 . . ? H50A C50 H50B 108.8 . . ? C51 O11 C54 106.6(3) . . ? O11 C51 C52 106.4(4) . . ? O11 C51 H51A 110.5 . . ? C52 C51 H51A 110.5 . . ? O11 C51 H51B 110.5 . . ? C52 C51 H51B 110.5 . . ? H51A C51 H51B 108.6 . . ? C53 C52 C51 103.8(4) . . ? C53 C52 H52A 111.0 . . ? C51 C52 H52A 111.0 . . ? C53 C52 H52B 111.0 . . ? C51 C52 H52B 111.0 . . ? H52A C52 H52B 109.0 . . ? C54 C53 C52 106.7(4) . . ? C54 C53 H53A 110.4 . . ? C52 C53 H53A 110.4 . . ? C54 C53 H53B 110.4 . . ? C52 C53 H53B 110.4 . . ? H53A C53 H53B 108.6 . . ? O11 C54 C53 105.4(4) . . ? O11 C54 H54A 110.7 . . ? C53 C54 H54A 110.7 . . ? O11 C54 H54B 110.7 . . ? C53 C54 H54B 110.7 . . ? H54A C54 H54B 108.8 . . ? C55 O12 C58 104.3(5) . . ? O12 C55 C56 109.6(5) . . ? O12 C55 H55A 109.8 . . ? C56 C55 H55A 109.8 . . ? O12 C55 H55B 109.8 . . ? C56 C55 H55B 109.8 . . ? H55A C55 H55B 108.2 . . ? C55 C56 C57 102.2(4) . . ? C55 C56 H56A 111.3 . . ? C57 C56 H56A 111.3 . . ? C55 C56 H56B 111.3 . . ? C57 C56 H56B 111.3 . . ? H56A C56 H56B 109.2 . . ? C58 C57 C56 102.2(5) . . ? C58 C57 H57A 111.3 . . ? C56 C57 H57A 111.3 . . ? C58 C57 H57B 111.3 . . ? C56 C57 H57B 111.3 . . ? H57A C57 H57B 109.2 . . ? O12 C58 C57 103.7(5) . . ? O12 C58 H58A 111.0 . . ? C57 C58 H58A 111.0 . . ? O12 C58 H58B 111.0 . . ? C57 C58 H58B 111.0 . . ? H58A C58 H58B 109.0 . . ? 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 C2 N1 N2 C3 -105.5(5) . . . . ? C19 N5 N6 C20 -77.3(5) . . . . ? C23 N7 N8 C24 -112.7(5) . . . . ? C40 N11 N12 C41 -94.2(5) . . . . ? N2 N1 C2 O1 1.3(6) . . . . ? N2 N1 C2 C1 -177.9(3) . . . . ? N1 N2 C3 O2 3.7(7) . . . . ? N1 N2 C3 C4 -175.5(4) . . . . ? C7 N3 C4 C5 -1.0(5) . . . . ? C7 N3 C4 C3 178.8(5) . . . . ? O2 C3 C4 N3 -169.9(5) . . . . ? N2 C3 C4 N3 9.3(7) . . . . ? O2 C3 C4 C5 9.9(9) . . . . ? N2 C3 C4 C5 -171.0(5) . . . . ? N3 C4 C5 C6 1.5(5) . . . . ? C3 C4 C5 C6 -178.2(5) . . . . ? N3 C4 C5 C8 -178.8(4) . . . . ? C3 C4 C5 C8 1.4(8) . . . . ? C4 C5 C6 C7 -1.6(5) . . . . ? C8 C5 C6 C7 178.8(4) . . . . ? C4 C5 C6 C9 -179.6(5) . . . . ? C8 C5 C6 C9 0.8(8) . . . . ? C4 N3 C7 C6 0.0(5) . . . . ? C4 N3 C7 C11 -177.2(4) . . . . ? C5 C6 C7 N3 1.0(5) . . . . ? C9 C6 C7 N3 179.1(4) . . . . ? C5 C6 C7 C11 177.8(5) . . . . ? C9 C6 C7 C11 -4.1(8) . . . . ? C7 C6 C9 C10 -66.9(6) . . . . ? C5 C6 C9 C10 110.8(6) . . . . ? N3 C7 C11 C12 -70.6(6) . . . . ? C6 C7 C11 C12 112.9(5) . . . . ? C15 N4 C12 C13 -1.6(5) . . . . ? C15 N4 C12 C11 -175.0(4) . . . . ? C7 C11 C12 N4 -24.4(7) . . . . ? C7 C11 C12 C13 163.7(5) . . . . ? N4 C12 C13 C14 1.4(5) . . . . ? C11 C12 C13 C14 174.3(5) . . . . ? N4 C12 C13 C16 177.7(4) . . . . ? C11 C12 C13 C16 -9.4(8) . . . . ? C12 C13 C14 C15 -0.8(5) . . . . ? C16 C13 C14 C15 -176.9(4) . . . . ? C12 C13 C14 C18 -178.8(4) . . . . ? C16 C13 C14 C18 5.1(8) . . . . ? C12 N4 C15 C14 1.1(5) . . . . ? C12 N4 C15 C19 -175.9(4) . . . . ? C13 C14 C15 N4 -0.2(5) . . . . ? C18 C14 C15 N4 177.8(4) . . . . ? C13 C14 C15 C19 176.8(4) . . . . ? C18 C14 C15 C19 -5.2(8) . . . . ? C12 C13 C16 C17 -94.2(6) . . . . ? C14 C13 C16 C17 81.3(7) . . . . ? N6 N5 C19 O3 -11.8(6) . . . . ? N6 N5 C19 C15 169.7(4) . . . . ? N4 C15 C19 O3 -179.1(4) . . . . ? C14 C15 C19 O3 4.5(8) . . . . ? N4 C15 C19 N5 -0.7(7) . . . . ? C14 C15 C19 N5 -177.1(4) . . . . ? N5 N6 C20 O4 -6.3(7) . . . . ? N5 N6 C20 C21 173.2(4) . . . . ? N8 N7 C23 O5 -1.3(6) . . . . ? N8 N7 C23 C22 -179.0(4) . . . . ? N7 N8 C24 O6 7.1(7) . . . . ? N7 N8 C24 C25 -171.1(4) . . . . ? C28 N9 C25 C26 0.1(5) . . . . ? C28 N9 C25 C24 176.1(4) . . . . ? O6 C24 C25 N9 -174.4(5) . . . . ? N8 C24 C25 N9 3.8(7) . . . . ? O6 C24 C25 C26 0.7(8) . . . . ? N8 C24 C25 C26 178.9(5) . . . . ? N9 C25 C26 C27 -0.4(5) . . . . ? C24 C25 C26 C27 -176.2(5) . . . . ? N9 C25 C26 C29 178.2(5) . . . . ? C24 C25 C26 C29 2.4(8) . . . . ? C25 C26 C27 C28 0.5(5) . . . . ? C29 C26 C27 C28 -178.1(5) . . . . ? C25 C26 C27 C30 -179.9(4) . . . . ? C29 C26 C27 C30 1.5(8) . . . . ? C25 N9 C28 C27 0.2(5) . . . . ? C25 N9 C28 C32 -175.0(4) . . . . ? C26 C27 C28 N9 -0.5(5) . . . . ? C30 C27 C28 N9 180.0(4) . . . . ? C26 C27 C28 C32 174.2(5) . . . . ? C30 C27 C28 C32 -5.4(9) . . . . ? C28 C27 C30 C31 -97.2(6) . . . . ? C26 C27 C30 C31 83.3(7) . . . . ? N9 C28 C32 C33 -55.3(7) . . . . ? C27 C28 C32 C33 130.7(6) . . . . ? C36 N10 C33 C34 0.1(5) . . . . ? C36 N10 C33 C32 -172.8(4) . . . . ? C28 C32 C33 N10 -29.3(7) . . . . ? C28 C32 C33 C34 159.4(5) . . . . ? N10 C33 C34 C35 -0.4(5) . . . . ? C32 C33 C34 C35 172.1(5) . . . . ? N10 C33 C34 C37 177.0(4) . . . . ? C32 C33 C34 C37 -10.4(7) . . . . ? C33 C34 C35 C36 0.6(5) . . . . ? C37 C34 C35 C36 -176.6(4) . . . . ? C33 C34 C35 C39 177.8(4) . . . . ? C37 C34 C35 C39 0.7(8) . . . . ? C33 N10 C36 C35 0.2(5) . . . . ? C33 N10 C36 C40 -178.5(4) . . . . ? C34 C35 C36 N10 -0.5(5) . . . . ? C39 C35 C36 N10 -177.7(4) . . . . ? C34 C35 C36 C40 178.2(4) . . . . ? C39 C35 C36 C40 1.0(8) . . . . ? C33 C34 C37 C38 -83.2(6) . . . . ? C35 C34 C37 C38 93.6(7) . . . . ? N12 N11 C40 O7 -3.0(6) . . . . ? N12 N11 C40 C36 178.4(4) . . . . ? N10 C36 C40 O7 -172.5(4) . . . . ? C35 C36 C40 O7 9.0(7) . . . . ? N10 C36 C40 N11 6.0(6) . . . . ? C35 C36 C40 N11 -172.5(4) . . . . ? N11 N12 C41 O8 -7.1(7) . . . . ? N11 N12 C41 C42 174.8(4) . . . . ? C46 O9 C43 C44 8.8(5) . . . . ? O9 C43 C44 C45 -28.7(5) . . . . ? C43 C44 C45 C46 36.7(4) . . . . ? C43 O9 C46 C45 15.2(5) . . . . ? C44 C45 C46 O9 -32.7(5) . . . . ? C50 O10 C47 C48 16.1(6) . . . . ? O10 C47 C48 C49 6.8(7) . . . . ? C47 C48 C49 C50 -25.6(7) . . . . ? C47 O10 C50 C49 -32.9(6) . . . . ? C48 C49 C50 O10 36.5(6) . . . . ? C54 O11 C51 C52 32.3(6) . . . . ? O11 C51 C52 C53 -17.8(7) . . . . ? C51 C52 C53 C54 -2.3(8) . . . . ? C51 O11 C54 C53 -33.5(7) . . . . ? C52 C53 C54 O11 21.6(8) . . . . ? C58 O12 C55 C56 33.5(8) . . . . ? O12 C55 C56 C57 -9.8(8) . . . . ? C55 C56 C57 C58 -16.0(8) . . . . ? C55 O12 C58 C57 -43.4(7) . . . . ? C56 C57 C58 O12 36.1(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O8 0.86 1.93 2.775(6) 166.8 1_565 N2 H2 O5 0.86 1.98 2.827(5) 167.8 1_565 N3 H3 O5 0.86 2.12 2.867(5) 145.4 1_565 N4 H4 O6 0.86 2.13 2.918(5) 152.9 1_565 N5 H5 O6 0.86 2.04 2.806(6) 148.4 1_565 N6 H6 O3 0.86 2.04 2.848(6) 155.6 3_675 N7 H7 O4 0.86 1.91 2.758(6) 167.3 1_545 N8 H8 O1 0.86 1.97 2.832(6) 174.9 1_545 N9 H9 O1 0.86 2.08 2.895(5) 157.8 1_545 N11 H11 O2 0.86 2.03 2.877(6) 166.6 1_545 N10 H10 O2 0.86 2.23 3.026(4) 153.9 1_545 N12 H12 O7 0.86 2.04 2.836(6) 154.3 3_656 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.333 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.069 # Attachment '- 3-2THF revised.cif' data_r90427f _database_code_depnum_ccdc_archive 'CCDC 798939' #TrackingRef '- 3-2THF revised.cif' _audit_update_record ; 2011-06-21 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H38 N6 O4, 2(C4 H8 O)' _chemical_formula_sum 'C33 H54 N6 O6' _chemical_formula_weight 630.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.690(3) _cell_length_b 18.545(4) _cell_length_c 22.889(5) _cell_angle_alpha 71.70(3) _cell_angle_beta 82.55(3) _cell_angle_gamma 77.24(3) _cell_volume 6938(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14860 _cell_measurement_theta_min 1.557 _cell_measurement_theta_max 27.801 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9835 _exptl_absorpt_correction_T_max 0.9917 _exptl_absorpt_process_details crystalclear _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55260 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.02 _reflns_number_total 24237 _reflns_number_gt 19066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restraints were used to deal with the disorder of C17 and one of the THF molecules as follow: SADI 0.02 C16 C17 C16 C17' SIMU 0.02 C17 C17' ISOR 0.01 C17 C17' O20A C13A C14A C15A C16A O20B C13B C14B C15B C16B ; _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^)+(0.0919P)^2^+8.6058P] 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 24237 _refine_ls_number_parameters 1700 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.42811(10) 0.09911(11) 0.32002(8) 0.0310(4) Uani 1 1 d . . . O2 O 0.44668(10) -0.06854(10) 0.49233(8) 0.0261(4) Uani 1 1 d . . . O3 O -0.00362(10) 0.33322(9) 0.36447(8) 0.0223(4) Uani 1 1 d . B . O4 O 0.12560(10) 0.28159(10) 0.22598(8) 0.0242(4) Uani 1 1 d . . . O5 O 0.15664(10) 0.05818(10) 0.34459(8) 0.0237(4) Uani 1 1 d . . . O6 O 0.24864(10) 0.16367(10) 0.42459(8) 0.0232(4) Uani 1 1 d . . . O7 O -0.17896(10) 0.51788(10) 0.20635(8) 0.0260(4) Uani 1 1 d . . . O8 O -0.16194(10) 0.32117(11) 0.24896(9) 0.0311(4) Uani 1 1 d . . . O9 O 0.33737(10) 0.70754(10) 0.29058(8) 0.0241(4) Uani 1 1 d . . . O10 O 0.50036(10) 0.67173(10) 0.16856(8) 0.0231(4) Uani 1 1 d . . . O11 O 0.05338(10) 1.05598(10) 0.03164(8) 0.0260(4) Uani 1 1 d . . . O12 O 0.06130(11) 0.89094(12) 0.16290(9) 0.0344(5) Uani 1 1 d . . . O13 O 0.62459(10) 0.70577(11) 0.27874(9) 0.0311(4) Uani 1 1 d . . . O14 O 0.65440(10) 0.49691(10) 0.33768(8) 0.0235(4) Uani 1 1 d . . . O15 O 0.25185(10) 0.81543(10) 0.07871(8) 0.0239(4) Uani 1 1 d . . . O16 O 0.32447(10) 0.90159(10) 0.20765(8) 0.0242(4) Uani 1 1 d . . . N1 N 0.45273(12) 0.07474(12) 0.42004(10) 0.0242(5) Uani 1 1 d . . . H1 H 0.4838 0.0763 0.4454 0.029 Uiso 1 1 calc R . . N2 N 0.38296(12) 0.05036(12) 0.44207(10) 0.0239(5) Uani 1 1 d . . . H2 H 0.3395 0.0813 0.4321 0.029 Uiso 1 1 calc R . . N3 N 0.23796(11) 0.00363(11) 0.49010(9) 0.0181(4) Uani 1 1 d . . . H3 H 0.2310 0.0518 0.4692 0.022 Uiso 1 1 calc R . . N4 N 0.06331(11) 0.12683(11) 0.43002(9) 0.0195(4) Uani 1 1 d . . . H4 H 0.0744 0.1090 0.3988 0.023 Uiso 1 1 calc R . . N5 N 0.01757(12) 0.23567(12) 0.31995(9) 0.0228(5) Uani 1 1 d . B . H5 H 0.0303 0.1868 0.3243 0.027 Uiso 1 1 calc R . . N6 N -0.00069(12) 0.28777(12) 0.26266(9) 0.0233(5) Uani 1 1 d . . . H6 H -0.0485 0.3077 0.2552 0.028 Uiso 1 1 calc R . . N7 N 0.26430(12) 0.11180(11) 0.32491(10) 0.0226(5) Uani 1 1 d . . . H7 H 0.3138 0.1045 0.3168 0.027 Uiso 1 1 calc R . . N8 N 0.22424(12) 0.18587(11) 0.32441(10) 0.0222(5) Uani 1 1 d . . . H8 H 0.2002 0.2159 0.2927 0.027 Uiso 1 1 calc R . . N9 N 0.18734(11) 0.34550(11) 0.31001(9) 0.0188(4) Uani 1 1 d . . . H9 H 0.1946 0.3353 0.2753 0.023 Uiso 1 1 calc R . . N10 N 0.01358(11) 0.47484(11) 0.26291(9) 0.0187(4) Uani 1 1 d . . . H10 H 0.0142 0.4374 0.2966 0.022 Uiso 1 1 calc R . . N11 N -0.13610(12) 0.43088(12) 0.29584(9) 0.0223(5) Uani 1 1 d . . . H11 H -0.1012 0.4133 0.3223 0.027 Uiso 1 1 calc R . . N12 N -0.20547(12) 0.40322(12) 0.30721(10) 0.0228(5) Uani 1 1 d . . . H12 H -0.2416 0.4180 0.3323 0.027 Uiso 1 1 calc R . . N13 N 0.46294(12) 0.71911(12) 0.27116(9) 0.0212(4) Uani 1 1 d . . . H13 H 0.5090 0.7067 0.2840 0.025 Uiso 1 1 calc R . . N14 N 0.44891(12) 0.76872(12) 0.21203(9) 0.0210(4) Uani 1 1 d . . . H14 H 0.4274 0.8165 0.2068 0.025 Uiso 1 1 calc R . . N15 N 0.42997(11) 0.87526(11) 0.09401(9) 0.0183(4) Uani 1 1 d . . . H15 H 0.4171 0.8968 0.1230 0.022 Uiso 1 1 calc R . . N16 N 0.26302(11) 0.98963(11) 0.02387(9) 0.0189(4) Uani 1 1 d . . . H16 H 0.2712 0.9399 0.0339 0.023 Uiso 1 1 calc R . . N17 N 0.12054(12) 0.93343(12) 0.04434(10) 0.0245(5) Uani 1 1 d . . . H17 H 0.1640 0.9030 0.0404 0.029 Uiso 1 1 calc R . . N18 N 0.05182(12) 0.90509(12) 0.06202(10) 0.0250(5) Uani 1 1 d . . . H18 H 0.0273 0.8972 0.0352 0.030 Uiso 1 1 calc R . . N19 N 0.68285(12) 0.61085(12) 0.23573(10) 0.0231(5) Uani 1 1 d . . . H19 H 0.7238 0.5916 0.2169 0.028 Uiso 1 1 calc R . . N20 N 0.61611(12) 0.57946(12) 0.24506(10) 0.0228(5) Uani 1 1 d . . . H20 H 0.5832 0.5945 0.2171 0.027 Uiso 1 1 calc R . . N21 N 0.47391(11) 0.52273(11) 0.26618(9) 0.0182(4) Uani 1 1 d . . . H21 H 0.4764 0.5568 0.2308 0.022 Uiso 1 1 calc R . . N22 N 0.30431(11) 0.63729(11) 0.20082(9) 0.0186(4) Uani 1 1 d . . . H22 H 0.2920 0.6500 0.2344 0.022 Uiso 1 1 calc R . . N23 N 0.25900(12) 0.79582(11) 0.18131(10) 0.0218(5) Uani 1 1 d . . . H23 H 0.2756 0.7650 0.2158 0.026 Uiso 1 1 calc R . . N24 N 0.22171(12) 0.87167(11) 0.17702(10) 0.0219(5) Uani 1 1 d . . . H24 H 0.1756 0.8879 0.1642 0.026 Uiso 1 1 calc R . . C1 C 0.67524(18) 0.1072(2) 0.27348(17) 0.0466(8) Uani 1 1 d . . . H1A H 0.6706 0.1623 0.2574 0.070 Uiso 1 1 calc R . . H1B H 0.7018 0.0833 0.2430 0.070 Uiso 1 1 calc R . . H1C H 0.7041 0.0885 0.3097 0.070 Uiso 1 1 calc R . . C2 C 0.59448(17) 0.0873(2) 0.28995(15) 0.0391(7) Uani 1 1 d . . . H2A H 0.5646 0.1089 0.2537 0.047 Uiso 1 1 calc R . . H2B H 0.5993 0.0315 0.3021 0.047 Uiso 1 1 calc R . . C3 C 0.55111(15) 0.11748(16) 0.34163(12) 0.0264(6) Uani 1 1 d . . . H3A H 0.5817 0.0969 0.3775 0.032 Uiso 1 1 calc R . . H3B H 0.5450 0.1734 0.3290 0.032 Uiso 1 1 calc R . . C4 C 0.47184(14) 0.09587(14) 0.35910(12) 0.0232(5) Uani 1 1 d . . . C5 C 0.38408(14) -0.02277(14) 0.47952(11) 0.0194(5) Uani 1 1 d . . . C6 C 0.30969(14) -0.04531(13) 0.50193(11) 0.0183(5) Uani 1 1 d . . . C7 C 0.29554(14) -0.11823(14) 0.53634(11) 0.0189(5) Uani 1 1 d . . . C8 C 0.35463(15) -0.19169(14) 0.55750(13) 0.0260(6) Uani 1 1 d . . . H8C H 0.4054 -0.1823 0.5408 0.039 Uiso 1 1 calc R . . H8D H 0.3425 -0.2312 0.5435 0.039 Uiso 1 1 calc R . . H8E H 0.3536 -0.2083 0.6017 0.039 Uiso 1 1 calc R . . C9 C 0.21392(14) -0.11262(14) 0.54602(11) 0.0195(5) Uani 1 1 d . . . C10 C 0.17144(15) -0.17796(14) 0.57740(12) 0.0235(5) Uani 1 1 d . . . H10A H 0.1179 -0.1566 0.5872 0.028 Uiso 1 1 calc R . . H10B H 0.1947 -0.2081 0.6159 0.028 Uiso 1 1 calc R . . C11 C 0.17296(17) -0.23151(16) 0.53812(14) 0.0336(7) Uani 1 1 d . . . H11A H 0.1468 -0.2029 0.5012 0.050 Uiso 1 1 calc R . . H11B H 0.1471 -0.2732 0.5611 0.050 Uiso 1 1 calc R . . H11C H 0.2258 -0.2521 0.5275 0.050 Uiso 1 1 calc R . . C12 C 0.18029(14) -0.03666(14) 0.51677(11) 0.0188(5) Uani 1 1 d . . . C13 C 0.09563(14) -0.00278(14) 0.50781(12) 0.0221(5) Uani 1 1 d . . . H13A H 0.0803 -0.0204 0.4762 0.026 Uiso 1 1 calc R . . H13B H 0.0664 -0.0244 0.5458 0.026 Uiso 1 1 calc R . . C14 C 0.07087(14) 0.08381(14) 0.49017(11) 0.0191(5) Uani 1 1 d . . . C15 C 0.04648(15) 0.13237(15) 0.52664(11) 0.0239(6) Uani 1 1 d . B . C16 C 0.04095(19) 0.10770(16) 0.59605(12) 0.0364(7) Uani 1 1 d D . . H16A H 0.0856 0.0675 0.6103 0.044 Uiso 1 1 calc R A 1 H16B H 0.0443 0.1515 0.6095 0.044 Uiso 1 1 calc R A 1 C17 C -0.0271(3) 0.0798(3) 0.6251(2) 0.0347(12) Uani 0.668(6) 1 d PDU B 1 H17A H -0.0251 0.0657 0.6690 0.052 Uiso 0.668(6) 1 calc PR B 1 H17B H -0.0305 0.0353 0.6133 0.052 Uiso 0.668(6) 1 calc PR B 1 H17C H -0.0719 0.1196 0.6125 0.052 Uiso 0.668(6) 1 calc PR B 1 C17' C 0.0958(5) 0.1206(6) 0.6259(4) 0.041(3) Uani 0.332(6) 1 d PDU B 2 H17D H 0.0847 0.1017 0.6697 0.061 Uiso 0.332(6) 1 calc PR B 2 H17E H 0.0954 0.1751 0.6144 0.061 Uiso 0.332(6) 1 calc PR B 2 H17F H 0.1460 0.0941 0.6149 0.061 Uiso 0.332(6) 1 calc PR B 2 C18 C 0.02382(14) 0.20880(14) 0.48698(11) 0.0210(5) Uani 1 1 d . . . C19 C -0.00810(17) 0.28051(15) 0.50629(12) 0.0287(6) Uani 1 1 d . B . H19A H 0.0025 0.3250 0.4736 0.043 Uiso 1 1 calc R . . H19B H 0.0160 0.2773 0.5425 0.043 Uiso 1 1 calc R . . H19C H -0.0632 0.2850 0.5152 0.043 Uiso 1 1 calc R . . C20 C 0.03486(13) 0.20388(13) 0.42706(11) 0.0182(5) Uani 1 1 d . B . C21 C 0.01505(13) 0.26309(14) 0.36922(11) 0.0188(5) Uani 1 1 d . . . C22 C 0.05615(15) 0.30736(14) 0.21855(11) 0.0209(5) Uani 1 1 d . . . C23 C 0.02666(15) 0.36339(15) 0.15880(11) 0.0245(6) Uani 1 1 d . . . H23C H 0.0434 0.4120 0.1519 0.029 Uiso 1 1 calc R . . H23D H -0.0297 0.3735 0.1619 0.029 Uiso 1 1 calc R . . C24 C 0.05577(17) 0.33247(17) 0.10441(12) 0.0329(7) Uani 1 1 d . . . H24A H 0.0389 0.2840 0.1112 0.040 Uiso 1 1 calc R . . H24B H 0.1121 0.3223 0.1012 0.040 Uiso 1 1 calc R . . C25 C 0.0257(2) 0.3895(2) 0.04443(14) 0.0487(9) Uani 1 1 d . . . H25A H -0.0298 0.3958 0.0460 0.073 Uiso 1 1 calc R . . H25B H 0.0484 0.3703 0.0105 0.073 Uiso 1 1 calc R . . H25C H 0.0395 0.4386 0.0389 0.073 Uiso 1 1 calc R . . C26 C 0.30611(18) -0.16937(16) 0.38342(14) 0.0368(7) Uani 1 1 d . . . H26A H 0.3288 -0.1742 0.3441 0.055 Uiso 1 1 calc R . . H26B H 0.2813 -0.2126 0.4042 0.055 Uiso 1 1 calc R . . H26C H 0.3460 -0.1686 0.4078 0.055 Uiso 1 1 calc R . . C27 C 0.24622(16) -0.09459(14) 0.37413(12) 0.0259(6) Uani 1 1 d . . . H27A H 0.2052 -0.0961 0.3505 0.031 Uiso 1 1 calc R . . H27B H 0.2231 -0.0900 0.4139 0.031 Uiso 1 1 calc R . . C28 C 0.28261(14) -0.02469(14) 0.34068(11) 0.0211(5) Uani 1 1 d . . . H28A H 0.3281 -0.0274 0.3614 0.025 Uiso 1 1 calc R . . H28B H 0.2998 -0.0264 0.2990 0.025 Uiso 1 1 calc R . . C29 C 0.22794(14) 0.05141(14) 0.33767(11) 0.0190(5) Uani 1 1 d . . . C30 C 0.22408(14) 0.20954(14) 0.37504(11) 0.0207(5) Uani 1 1 d . . . C31 C 0.19728(14) 0.29126(13) 0.36734(11) 0.0190(5) Uani 1 1 d . . . C32 C 0.17965(14) 0.33057(14) 0.41171(11) 0.0208(5) Uani 1 1 d . . . C33 C 0.18674(16) 0.29548(16) 0.47986(12) 0.0292(6) Uani 1 1 d . . . H33A H 0.1641 0.2500 0.4939 0.044 Uiso 1 1 calc R . . H33B H 0.1601 0.3322 0.5008 0.044 Uiso 1 1 calc R . . H33C H 0.2406 0.2818 0.4885 0.044 Uiso 1 1 calc R . . C34 C 0.15766(14) 0.41039(14) 0.37976(11) 0.0208(5) Uani 1 1 d . . . C35 C 0.13291(16) 0.47613(15) 0.40746(13) 0.0285(6) Uani 1 1 d . . . H35A H 0.1569 0.5190 0.3825 0.034 Uiso 1 1 calc R . . H35B H 0.1522 0.4598 0.4483 0.034 Uiso 1 1 calc R . . C36 C 0.04594(19) 0.5043(2) 0.41259(17) 0.0498(9) Uani 1 1 d . . . H36A H 0.0263 0.5214 0.3723 0.075 Uiso 1 1 calc R . . H36B H 0.0347 0.5465 0.4301 0.075 Uiso 1 1 calc R . . H36C H 0.0217 0.4628 0.4386 0.075 Uiso 1 1 calc R . . C37 C 0.16423(13) 0.41739(14) 0.31723(11) 0.0191(5) Uani 1 1 d . . . C38 C 0.15309(14) 0.48730(14) 0.26238(12) 0.0223(5) Uani 1 1 d . . . H38A H 0.1923 0.4786 0.2302 0.027 Uiso 1 1 calc R . . H38B H 0.1622 0.5308 0.2737 0.027 Uiso 1 1 calc R . . C39 C 0.07487(14) 0.50940(14) 0.23606(11) 0.0194(5) Uani 1 1 d . . . C40 C 0.05169(14) 0.56719(14) 0.18290(11) 0.0211(5) Uani 1 1 d . . . C41 C 0.10413(15) 0.61571(15) 0.13770(12) 0.0271(6) Uani 1 1 d . . . H41A H 0.1457 0.6203 0.1593 0.033 Uiso 1 1 calc R . . H41B H 0.0747 0.6673 0.1201 0.033 Uiso 1 1 calc R . . C42 C 0.13867(18) 0.5806(2) 0.08631(14) 0.0434(8) Uani 1 1 d . . . H42A H 0.1677 0.5294 0.1036 0.065 Uiso 1 1 calc R . . H42B H 0.1725 0.6121 0.0589 0.065 Uiso 1 1 calc R . . H42C H 0.0977 0.5779 0.0638 0.065 Uiso 1 1 calc R . . C43 C -0.02705(14) 0.56741(14) 0.17705(11) 0.0216(5) Uani 1 1 d . . . C44 C -0.07474(16) 0.61972(17) 0.12513(12) 0.0339(7) Uani 1 1 d . . . H44A H -0.0897 0.5894 0.1030 0.051 Uiso 1 1 calc R . . H44B H -0.0447 0.6554 0.0977 0.051 Uiso 1 1 calc R . . H44C H -0.1204 0.6480 0.1414 0.051 Uiso 1 1 calc R . . C45 C -0.05005(14) 0.50935(14) 0.22755(11) 0.0190(5) Uani 1 1 d . . . C46 C -0.12505(14) 0.48672(14) 0.24152(11) 0.0194(5) Uani 1 1 d . . . C47 C -0.21505(15) 0.35259(15) 0.27812(12) 0.0242(6) Uani 1 1 d . . . C48 C -0.29611(15) 0.33558(16) 0.28541(12) 0.0262(6) Uani 1 1 d . . . H48A H -0.3272 0.3589 0.3153 0.031 Uiso 1 1 calc R . . H48B H -0.2934 0.2801 0.3011 0.031 Uiso 1 1 calc R . . C49 C -0.33541(16) 0.36658(17) 0.22461(13) 0.0332(6) Uani 1 1 d . . . H49A H -0.3023 0.3464 0.1938 0.040 Uiso 1 1 calc R . . H49B H -0.3416 0.4225 0.2106 0.040 Uiso 1 1 calc R . . C50 C -0.41481(17) 0.34440(19) 0.23039(15) 0.0396(7) Uani 1 1 d . . . H50A H -0.4088 0.2891 0.2431 0.059 Uiso 1 1 calc R . . H50B H -0.4375 0.3654 0.1912 0.059 Uiso 1 1 calc R . . H50C H -0.4480 0.3648 0.2604 0.059 Uiso 1 1 calc R . . C51 C 0.50202(18) 0.70530(17) 0.41480(13) 0.0352(7) Uani 1 1 d . . . H51A H 0.4979 0.7488 0.3783 0.053 Uiso 1 1 calc R . . H51B H 0.5507 0.6982 0.4321 0.053 Uiso 1 1 calc R . . H51C H 0.4602 0.7145 0.4443 0.053 Uiso 1 1 calc R . . C52 C 0.49776(15) 0.63280(15) 0.39832(12) 0.0257(6) Uani 1 1 d . . . H52A H 0.5046 0.5888 0.4351 0.031 Uiso 1 1 calc R . . H52B H 0.5404 0.6239 0.3686 0.031 Uiso 1 1 calc R . . C53 C 0.42177(15) 0.63688(15) 0.37159(11) 0.0237(5) Uani 1 1 d . . . H53A H 0.4201 0.5850 0.3713 0.028 Uiso 1 1 calc R . . H53B H 0.3797 0.6508 0.4001 0.028 Uiso 1 1 calc R . . C54 C 0.40404(14) 0.69079(14) 0.30797(11) 0.0193(5) Uani 1 1 d . . . C55 C 0.46963(13) 0.74067(14) 0.16265(11) 0.0187(5) Uani 1 1 d . . . C56 C 0.45707(13) 0.79692(14) 0.10241(11) 0.0182(5) Uani 1 1 d . . . C57 C 0.47085(13) 0.78536(14) 0.04432(11) 0.0185(5) Uani 1 1 d . . . C58 C 0.50539(16) 0.71055(15) 0.03055(12) 0.0260(6) Uani 1 1 d . . . H58A H 0.5609 0.7016 0.0307 0.039 Uiso 1 1 calc R . . H58B H 0.4912 0.7132 -0.0093 0.039 Uiso 1 1 calc R . . H58C H 0.4861 0.6689 0.0614 0.039 Uiso 1 1 calc R . . C59 C 0.45147(14) 0.85879(14) 0.00026(11) 0.0197(5) Uani 1 1 d . . . C60 C 0.45738(16) 0.87562(16) -0.06871(11) 0.0268(6) Uani 1 1 d . . . H60A H 0.4976 0.8365 -0.0799 0.032 Uiso 1 1 calc R . . H60B H 0.4731 0.9252 -0.0874 0.032 Uiso 1 1 calc R . . C61 C 0.3823(2) 0.8775(2) -0.09504(14) 0.0495(9) Uani 1 1 d . . . H61A H 0.3684 0.8274 -0.0793 0.074 Uiso 1 1 calc R . . H61B H 0.3893 0.8912 -0.1392 0.074 Uiso 1 1 calc R . . H61C H 0.3417 0.9151 -0.0832 0.074 Uiso 1 1 calc R . . C62 C 0.42690(13) 0.91310(14) 0.03224(11) 0.0185(5) Uani 1 1 d . . . C63 C 0.40459(14) 0.99957(13) 0.00957(11) 0.0204(5) Uani 1 1 d . . . H63A H 0.4281 1.0169 -0.0319 0.024 Uiso 1 1 calc R . . H63B H 0.4270 1.0209 0.0354 0.024 Uiso 1 1 calc R . . C64 C 0.31929(14) 1.03317(14) 0.00826(11) 0.0190(5) Uani 1 1 d . . . C65 C 0.28350(14) 1.11095(14) -0.00556(11) 0.0206(5) Uani 1 1 d . . . C66 C 0.32426(16) 1.17865(15) -0.02438(13) 0.0275(6) Uani 1 1 d . . . H66A H 0.3794 1.1594 -0.0198 0.033 Uiso 1 1 calc R . . H66B H 0.3058 1.2099 0.0034 0.033 Uiso 1 1 calc R . . C67 C 0.31240(17) 1.23001(16) -0.09039(13) 0.0324(6) Uani 1 1 d . . . H67A H 0.3290 1.1994 -0.1183 0.049 Uiso 1 1 calc R . . H67B H 0.3424 1.2700 -0.0999 0.049 Uiso 1 1 calc R . . H67C H 0.2584 1.2530 -0.0945 0.049 Uiso 1 1 calc R . . C68 C 0.20197(14) 1.11379(14) 0.00315(11) 0.0213(5) Uani 1 1 d . . . C69 C 0.14163(16) 1.18647(15) -0.00445(13) 0.0292(6) Uani 1 1 d . . . H69A H 0.1269 1.2059 -0.0463 0.044 Uiso 1 1 calc R . . H69B H 0.1625 1.2246 0.0053 0.044 Uiso 1 1 calc R . . H69C H 0.0969 1.1754 0.0228 0.044 Uiso 1 1 calc R . . C70 C 0.19022(14) 1.03788(14) 0.02107(11) 0.0198(5) Uani 1 1 d . . . C71 C 0.11714(14) 1.01078(14) 0.03340(11) 0.0208(5) Uani 1 1 d . . . C72 C 0.02389(15) 0.89002(15) 0.12140(12) 0.0248(6) Uani 1 1 d . . . C73 C -0.05717(15) 0.87275(16) 0.13351(13) 0.0304(6) Uani 1 1 d . . . H73A H -0.0586 0.8279 0.1693 0.036 Uiso 1 1 calc R . . H73B H -0.0709 0.8607 0.0984 0.036 Uiso 1 1 calc R . . C74 C -0.11557(17) 0.9409(2) 0.14449(17) 0.0445(8) Uani 1 1 d . . . H74A H -0.1136 0.9855 0.1085 0.053 Uiso 1 1 calc R . . H74B H -0.1010 0.9530 0.1792 0.053 Uiso 1 1 calc R . . C75 C -0.19870(18) 0.9269(2) 0.15730(17) 0.0494(9) Uani 1 1 d . . . H75A H -0.2141 0.9162 0.1227 0.074 Uiso 1 1 calc R . . H75B H -0.2328 0.9721 0.1639 0.074 Uiso 1 1 calc R . . H75C H -0.2015 0.8836 0.1934 0.074 Uiso 1 1 calc R . . C76 C 0.88174(18) 0.6809(2) 0.30408(17) 0.0496(9) Uani 1 1 d . . . H76A H 0.9140 0.6622 0.2728 0.074 Uiso 1 1 calc R . . H76B H 0.9053 0.6577 0.3428 0.074 Uiso 1 1 calc R . . H76C H 0.8761 0.7361 0.2931 0.074 Uiso 1 1 calc R . . C77 C 0.80226(16) 0.65981(19) 0.30972(14) 0.0360(7) Uani 1 1 d . . . H77A H 0.7701 0.6785 0.3416 0.043 Uiso 1 1 calc R . . H77B H 0.8081 0.6039 0.3222 0.043 Uiso 1 1 calc R . . C78 C 0.76176(15) 0.69388(16) 0.24962(12) 0.0274(6) Uani 1 1 d . . . H78A H 0.7552 0.7498 0.2373 0.033 Uiso 1 1 calc R . . H78B H 0.7939 0.6756 0.2175 0.033 Uiso 1 1 calc R . . C79 C 0.68333(15) 0.67147(15) 0.25633(12) 0.0247(6) Uani 1 1 d . . . C80 C 0.60362(14) 0.52447(14) 0.29925(11) 0.0189(5) Uani 1 1 d . . . C81 C 0.53067(14) 0.49769(13) 0.30888(11) 0.0190(5) Uani 1 1 d . . . C82 C 0.50440(14) 0.44284(14) 0.35984(11) 0.0199(5) Uani 1 1 d . . . C83 C 0.54379(15) 0.40130(15) 0.41888(12) 0.0262(6) Uani 1 1 d . . . H83A H 0.5876 0.3634 0.4116 0.039 Uiso 1 1 calc R . . H83B H 0.5078 0.3761 0.4494 0.039 Uiso 1 1 calc R . . H83C H 0.5610 0.4379 0.4333 0.039 Uiso 1 1 calc R . . C84 C 0.43055(14) 0.43446(14) 0.34729(11) 0.0203(5) Uani 1 1 d . . . C85 C 0.38108(15) 0.37927(14) 0.38842(12) 0.0245(6) Uani 1 1 d . . . H85A H 0.3280 0.3970 0.3763 0.029 Uiso 1 1 calc R . . H85B H 0.3812 0.3799 0.4306 0.029 Uiso 1 1 calc R . . C86 C 0.40909(18) 0.29614(16) 0.38570(14) 0.0368(7) Uani 1 1 d . . . H86A H 0.4113 0.2953 0.3438 0.055 Uiso 1 1 calc R . . H86B H 0.3737 0.2644 0.4105 0.055 Uiso 1 1 calc R . . H86C H 0.4599 0.2765 0.4012 0.055 Uiso 1 1 calc R . . C87 C 0.41384(14) 0.48483(13) 0.28937(11) 0.0190(5) Uani 1 1 d . . . C88 C 0.34280(14) 0.49674(14) 0.25506(12) 0.0218(5) Uani 1 1 d . . . H88A H 0.3439 0.4500 0.2442 0.026 Uiso 1 1 calc R . . H88B H 0.2973 0.5034 0.2829 0.026 Uiso 1 1 calc R . . C89 C 0.33325(14) 0.56395(14) 0.19745(11) 0.0188(5) Uani 1 1 d . . . C90 C 0.34604(14) 0.56684(14) 0.13585(11) 0.0200(5) Uani 1 1 d . . . C91 C 0.37832(17) 0.49943(15) 0.11114(13) 0.0293(6) Uani 1 1 d . . . H91A H 0.3489 0.5039 0.0769 0.035 Uiso 1 1 calc R . . H91B H 0.3716 0.4521 0.1431 0.035 Uiso 1 1 calc R . . C92 C 0.46427(18) 0.49377(18) 0.08943(15) 0.0420(8) Uani 1 1 d . . . H92A H 0.4708 0.5381 0.0550 0.063 Uiso 1 1 calc R . . H92B H 0.4824 0.4476 0.0772 0.063 Uiso 1 1 calc R . . H92C H 0.4936 0.4921 0.1225 0.063 Uiso 1 1 calc R . . C93 C 0.32281(14) 0.64537(14) 0.10035(11) 0.0206(5) Uani 1 1 d . . . C94 C 0.32306(17) 0.67552(16) 0.03172(12) 0.0284(6) Uani 1 1 d . . . H94A H 0.2716 0.6821 0.0192 0.043 Uiso 1 1 calc R . . H94B H 0.3581 0.6394 0.0139 0.043 Uiso 1 1 calc R . . H94C H 0.3396 0.7244 0.0180 0.043 Uiso 1 1 calc R . . C95 C 0.29790(14) 0.68793(13) 0.14199(11) 0.0188(5) Uani 1 1 d . . . C96 C 0.26894(13) 0.77093(14) 0.13052(11) 0.0192(5) Uani 1 1 d . . . C97 C 0.25665(14) 0.91981(14) 0.19254(11) 0.0199(5) Uani 1 1 d . . . C98 C 0.20598(14) 0.99697(14) 0.19109(12) 0.0230(5) Uani 1 1 d . . . H98A H 0.1878 0.9971 0.2329 0.028 Uiso 1 1 calc R . . H98B H 0.1609 1.0045 0.1683 0.028 Uiso 1 1 calc R . . C99 C 0.24884(16) 1.06375(14) 0.16134(12) 0.0270(6) Uani 1 1 d . . . H99A H 0.2705 1.0613 0.1207 0.032 Uiso 1 1 calc R . . H99B H 0.2915 1.0585 0.1860 0.032 Uiso 1 1 calc R . . C100 C 0.19555(19) 1.14225(16) 0.15549(15) 0.0400(7) Uani 1 1 d . . . H10C H 0.1507 1.1457 0.1345 0.060 Uiso 1 1 calc R . . H10D H 0.2230 1.1827 0.1324 0.060 Uiso 1 1 calc R . . H10E H 0.1795 1.1477 0.1958 0.060 Uiso 1 1 calc R . . O17 O 0.17708(11) 0.65002(11) 0.30050(8) 0.0290(4) Uani 1 1 d . . . O18 O 0.96732(12) 0.10608(13) 0.30428(10) 0.0414(5) Uani 1 1 d . . . O19 O 0.91376(18) 0.2400(2) 0.09126(18) 0.0931(11) Uani 1 1 d . . . O21 O 0.51000(10) 0.04356(11) 0.83637(8) 0.0277(4) Uani 1 1 d . . . O22 O 0.29750(11) 0.33628(11) 0.20179(9) 0.0324(4) Uani 1 1 d . . . O23 O 0.20273(13) 0.45855(13) 0.55061(10) 0.0437(5) Uani 1 1 d . . . O24 O 0.3516(3) 0.0683(2) 0.58505(19) 0.1240(15) Uani 1 1 d . . . C101 C 0.10805(17) 0.69730(17) 0.27083(14) 0.0348(7) Uani 1 1 d . . . H10F H 0.0702 0.6656 0.2731 0.042 Uiso 1 1 calc R . . H10G H 0.1208 0.7226 0.2278 0.042 Uiso 1 1 calc R . . C102 C 0.07530(19) 0.75738(19) 0.30483(15) 0.0419(8) Uani 1 1 d . . . H10H H 0.0600 0.8083 0.2761 0.050 Uiso 1 1 calc R . . H10I H 0.0309 0.7436 0.3325 0.050 Uiso 1 1 calc R . . C103 C 0.14310(19) 0.75476(17) 0.34045(14) 0.0378(7) Uani 1 1 d . . . H10J H 0.1783 0.7874 0.3152 0.045 Uiso 1 1 calc R . . H10K H 0.1254 0.7703 0.3774 0.045 Uiso 1 1 calc R . . C104 C 0.18047(17) 0.67042(17) 0.35578(12) 0.0311(6) Uani 1 1 d . . . H10L H 0.2338 0.6625 0.3659 0.037 Uiso 1 1 calc R . . H10M H 0.1521 0.6397 0.3903 0.037 Uiso 1 1 calc R . . C105 C 1.0156(2) 0.0952(3) 0.2511(2) 0.0761(15) Uani 1 1 d . . . H10N H 1.0630 0.0584 0.2640 0.091 Uiso 1 1 calc R . . H10O H 1.0296 0.1439 0.2262 0.091 Uiso 1 1 calc R . . C106 C 0.9745(2) 0.0668(3) 0.21499(17) 0.0622(11) Uani 1 1 d . . . H10P H 1.0012 0.0158 0.2131 0.075 Uiso 1 1 calc R . . H10Q H 0.9705 0.1015 0.1733 0.075 Uiso 1 1 calc R . . C107 C 0.89490(18) 0.0633(2) 0.24755(14) 0.0419(8) Uani 1 1 d . . . H10R H 0.8904 0.0103 0.2700 0.050 Uiso 1 1 calc R . . H10S H 0.8547 0.0851 0.2184 0.050 Uiso 1 1 calc R . . C108 C 0.88912(17) 0.11109(18) 0.29125(15) 0.0377(7) Uani 1 1 d . . . H10T H 0.8651 0.1644 0.2722 0.045 Uiso 1 1 calc R . . H10U H 0.8586 0.0905 0.3288 0.045 Uiso 1 1 calc R . . C109 C 0.8426(2) 0.2856(2) 0.10319(18) 0.0565(10) Uani 1 1 d . . . H10V H 0.8303 0.3311 0.0682 0.068 Uiso 1 1 calc R . . H10W H 0.8445 0.3022 0.1391 0.068 Uiso 1 1 calc R . . C110 C 0.78320(19) 0.23563(19) 0.11456(15) 0.0440(8) Uani 1 1 d . . . H11D H 0.7342 0.2655 0.0983 0.053 Uiso 1 1 calc R . . H11E H 0.7747 0.2102 0.1582 0.053 Uiso 1 1 calc R . . C111 C 0.8959(2) 0.1992(3) 0.0536(2) 0.0756(13) Uani 1 1 d . . . H11H H 0.9360 0.1539 0.0544 0.091 Uiso 1 1 calc R . . H11I H 0.8919 0.2320 0.0113 0.091 Uiso 1 1 calc R . . C112 C 0.8204(2) 0.1762(2) 0.07935(19) 0.0586(10) Uani 1 1 d . . . H11F H 0.8280 0.1239 0.1070 0.070 Uiso 1 1 calc R . . H11G H 0.7885 0.1797 0.0468 0.070 Uiso 1 1 calc R . . O20A O 0.7362(2) 0.4875(3) 0.0144(2) 0.0526(12) Uani 0.621(5) 1 d PDU C 1 C13A C 0.7908(3) 0.5307(3) 0.0186(3) 0.0440(14) Uani 0.621(5) 1 d PDU C 1 H13C H 0.8123 0.5558 -0.0221 0.053 Uiso 0.621(5) 1 calc PR C 1 H13D H 0.8330 0.4975 0.0432 0.053 Uiso 0.621(5) 1 calc PR C 1 C14A C 0.7454(4) 0.5910(4) 0.0496(3) 0.0414(18) Uani 0.621(5) 1 d PDU C 1 H14A H 0.7790 0.6060 0.0721 0.050 Uiso 0.621(5) 1 calc PR C 1 H14B H 0.7199 0.6368 0.0196 0.050 Uiso 0.621(5) 1 calc PR C 1 C15A C 0.6880(3) 0.5488(3) 0.0919(2) 0.0410(14) Uani 0.621(5) 1 d PDU C 1 H15A H 0.6414 0.5842 0.1000 0.049 Uiso 0.621(5) 1 calc PR C 1 H15B H 0.7098 0.5175 0.1307 0.049 Uiso 0.621(5) 1 calc PR C 1 C16A C 0.6708(4) 0.4983(4) 0.0556(3) 0.0473(16) Uani 0.621(5) 1 d PDU C 1 H16C H 0.6621 0.4488 0.0834 0.057 Uiso 0.621(5) 1 calc PR C 1 H16D H 0.6248 0.5236 0.0329 0.057 Uiso 0.621(5) 1 calc PR C 1 O20B O 0.6948(3) 0.6132(3) 0.0187(3) 0.0414(18) Uani 0.379(5) 1 d PDU C 2 C13B C 0.7717(6) 0.5932(6) 0.0340(9) 0.072(6) Uani 0.379(5) 1 d PDU C 2 H13E H 0.7787 0.6185 0.0636 0.086 Uiso 0.379(5) 1 calc PR C 2 H13F H 0.8056 0.6096 -0.0024 0.086 Uiso 0.379(5) 1 calc PR C 2 C14B C 0.7913(5) 0.5054(5) 0.0618(6) 0.061(3) Uani 0.379(5) 1 d PDU C 2 H14C H 0.8371 0.4834 0.0404 0.074 Uiso 0.379(5) 1 calc PR C 2 H14D H 0.8005 0.4916 0.1052 0.074 Uiso 0.379(5) 1 calc PR C 2 C15B C 0.7220(6) 0.4776(5) 0.0536(6) 0.055(3) Uani 0.379(5) 1 d PDU C 2 H15C H 0.7106 0.4354 0.0891 0.066 Uiso 0.379(5) 1 calc PR C 2 H15D H 0.7290 0.4607 0.0169 0.066 Uiso 0.379(5) 1 calc PR C 2 C16B C 0.6579(5) 0.5495(5) 0.0473(5) 0.055(3) Uani 0.379(5) 1 d PDU C 2 H16E H 0.6180 0.5490 0.0222 0.066 Uiso 0.379(5) 1 calc PR C 2 H16F H 0.6342 0.5519 0.0875 0.066 Uiso 0.379(5) 1 calc PR C 2 C117 C 0.53466(16) 0.01564(17) 0.78354(13) 0.0304(6) Uani 1 1 d . . . H1G H 0.5214 -0.0346 0.7906 0.037 Uiso 1 1 calc R . . H1H H 0.5903 0.0113 0.7746 0.037 Uiso 1 1 calc R . . C118 C 0.49140(19) 0.07524(17) 0.73144(13) 0.0393(7) Uani 1 1 d . . . H1E H 0.4877 0.0539 0.6985 0.047 Uiso 1 1 calc R . . H1F H 0.5158 0.1201 0.7149 0.047 Uiso 1 1 calc R . . C119 C 0.41212(19) 0.09512(19) 0.76370(14) 0.0420(8) Uani 1 1 d . . . H11J H 0.3857 0.1470 0.7430 0.050 Uiso 1 1 calc R . . H11K H 0.3796 0.0586 0.7654 0.050 Uiso 1 1 calc R . . C120 C 0.43224(15) 0.08916(16) 0.82752(13) 0.0293(6) Uani 1 1 d . . . H12A H 0.4303 0.1403 0.8311 0.035 Uiso 1 1 calc R . . H12B H 0.3956 0.0644 0.8584 0.035 Uiso 1 1 calc R . . C121 C 0.36789(18) 0.28330(18) 0.22317(14) 0.0371(7) Uani 1 1 d . . . H12C H 0.3601 0.2525 0.2656 0.044 Uiso 1 1 calc R . . H12D H 0.4095 0.3109 0.2202 0.044 Uiso 1 1 calc R . . C122 C 0.3860(3) 0.2330(2) 0.18047(18) 0.0787(15) Uani 1 1 d . . . H12E H 0.4415 0.2148 0.1755 0.094 Uiso 1 1 calc R . . H12F H 0.3607 0.1887 0.1962 0.094 Uiso 1 1 calc R . . C123 C 0.3554(2) 0.2840(3) 0.12203(18) 0.0645(11) Uani 1 1 d . . . H12G H 0.3428 0.2545 0.0976 0.077 Uiso 1 1 calc R . . H12H H 0.3925 0.3153 0.0982 0.077 Uiso 1 1 calc R . . C124 C 0.28490(18) 0.3326(2) 0.14168(13) 0.0385(7) Uani 1 1 d . . . H12I H 0.2765 0.3841 0.1126 0.046 Uiso 1 1 calc R . . H12J H 0.2398 0.3099 0.1440 0.046 Uiso 1 1 calc R . . C125 C 0.28473(18) 0.43814(18) 0.54152(14) 0.0391(7) Uani 1 1 d . . . H12K H 0.2987 0.3949 0.5245 0.047 Uiso 1 1 calc R . . H12L H 0.3090 0.4239 0.5802 0.047 Uiso 1 1 calc R . . C126 C 0.31017(19) 0.50929(17) 0.49687(14) 0.0398(7) Uani 1 1 d . . . H12M H 0.3024 0.5137 0.4546 0.048 Uiso 1 1 calc R . . H12N H 0.3642 0.5093 0.5004 0.048 Uiso 1 1 calc R . . C127 C 0.2562(2) 0.57303(18) 0.51855(15) 0.0432(8) Uani 1 1 d . . . H12O H 0.2776 0.5830 0.5516 0.052 Uiso 1 1 calc R . . H12P H 0.2464 0.6206 0.4849 0.052 Uiso 1 1 calc R . . C128 C 0.1828(2) 0.5403(2) 0.54124(16) 0.0500(9) Uani 1 1 d . . . H12Q H 0.1616 0.5510 0.5796 0.060 Uiso 1 1 calc R . . H12R H 0.1440 0.5638 0.5110 0.060 Uiso 1 1 calc R . . C129 C 0.3782(4) 0.1394(3) 0.5679(2) 0.0996(18) Uani 1 1 d . . . H12S H 0.3718 0.1657 0.5244 0.120 Uiso 1 1 calc R . . H12T H 0.4329 0.1298 0.5749 0.120 Uiso 1 1 calc R . . C130 C 0.3313(3) 0.1895(3) 0.60633(18) 0.0704(12) Uani 1 1 d . . . H13M H 0.3122 0.2416 0.5808 0.084 Uiso 1 1 calc R . . H13N H 0.3617 0.1919 0.6378 0.084 Uiso 1 1 calc R . . C131 C 0.2644(4) 0.1463(4) 0.6350(2) 0.110(2) Uani 1 1 d . . . H13O H 0.2147 0.1816 0.6306 0.133 Uiso 1 1 calc R . . H13P H 0.2708 0.1192 0.6783 0.133 Uiso 1 1 calc R . . C132 C 0.2713(4) 0.0888(3) 0.5971(3) 0.0974(18) Uani 1 1 d . . . H13G H 0.2495 0.0439 0.6206 0.117 Uiso 1 1 calc R . . H13H H 0.2451 0.1133 0.5591 0.117 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0225(10) 0.0435(12) 0.0285(10) -0.0096(9) -0.0033(8) -0.0099(9) O2 0.0166(9) 0.0240(9) 0.0353(10) -0.0061(8) -0.0064(8) -0.0004(8) O3 0.0225(9) 0.0178(9) 0.0244(9) -0.0039(7) -0.0035(7) -0.0015(7) O4 0.0181(9) 0.0286(10) 0.0238(9) -0.0063(8) -0.0039(7) -0.0006(8) O5 0.0169(9) 0.0260(10) 0.0297(10) -0.0115(8) -0.0015(7) -0.0023(7) O6 0.0218(9) 0.0196(9) 0.0250(9) -0.0015(7) -0.0063(7) -0.0018(7) O7 0.0155(9) 0.0317(10) 0.0267(10) -0.0049(8) -0.0057(7) 0.0012(8) O8 0.0223(10) 0.0382(11) 0.0354(11) -0.0170(9) 0.0002(8) -0.0032(9) O9 0.0206(9) 0.0256(9) 0.0255(9) -0.0057(8) -0.0044(7) -0.0042(8) O10 0.0229(9) 0.0189(9) 0.0242(9) -0.0030(7) -0.0056(7) 0.0004(7) O11 0.0160(9) 0.0251(10) 0.0353(10) -0.0081(8) -0.0063(8) 0.0009(8) O12 0.0255(10) 0.0466(12) 0.0317(11) -0.0093(9) -0.0063(8) -0.0086(9) O13 0.0221(10) 0.0329(11) 0.0397(11) -0.0151(9) 0.0018(8) -0.0043(8) O14 0.0176(9) 0.0259(9) 0.0249(9) -0.0057(7) -0.0054(7) -0.0005(7) O15 0.0232(9) 0.0208(9) 0.0243(9) -0.0029(7) -0.0067(7) 0.0003(7) O16 0.0189(9) 0.0226(9) 0.0316(10) -0.0094(8) -0.0047(8) -0.0013(7) N1 0.0170(11) 0.0285(12) 0.0258(12) -0.0026(9) -0.0038(9) -0.0085(9) N2 0.0118(10) 0.0248(11) 0.0291(12) 0.0008(9) -0.0035(9) -0.0025(9) N3 0.0183(11) 0.0146(10) 0.0199(10) -0.0028(8) -0.0029(8) -0.0023(8) N4 0.0183(11) 0.0193(10) 0.0208(10) -0.0060(8) 0.0007(8) -0.0043(8) N5 0.0264(12) 0.0210(11) 0.0176(10) -0.0029(9) -0.0021(9) -0.0013(9) N6 0.0199(11) 0.0281(12) 0.0180(10) -0.0030(9) -0.0042(9) -0.0003(9) N7 0.0162(11) 0.0164(10) 0.0341(12) -0.0086(9) -0.0026(9) 0.0010(8) N8 0.0236(11) 0.0147(10) 0.0269(11) -0.0042(9) -0.0089(9) 0.0007(9) N9 0.0190(11) 0.0172(10) 0.0192(10) -0.0031(8) -0.0051(8) -0.0026(8) N10 0.0173(11) 0.0180(10) 0.0187(10) -0.0018(8) -0.0042(8) -0.0024(8) N11 0.0152(11) 0.0274(12) 0.0226(11) -0.0028(9) -0.0025(8) -0.0065(9) N12 0.0144(11) 0.0291(12) 0.0257(11) -0.0101(9) 0.0030(9) -0.0051(9) N13 0.0184(11) 0.0244(11) 0.0162(10) -0.0007(8) -0.0040(8) -0.0006(9) N14 0.0247(11) 0.0176(10) 0.0162(10) -0.0008(8) -0.0021(8) -0.0007(9) N15 0.0174(10) 0.0181(10) 0.0170(10) -0.0037(8) -0.0015(8) -0.0008(8) N16 0.0155(10) 0.0146(10) 0.0247(11) -0.0032(8) -0.0030(8) -0.0019(8) N17 0.0141(11) 0.0237(11) 0.0339(12) -0.0065(9) -0.0024(9) -0.0024(9) N18 0.0170(11) 0.0281(12) 0.0321(12) -0.0071(10) -0.0057(9) -0.0090(9) N19 0.0131(10) 0.0263(12) 0.0280(12) -0.0054(9) 0.0017(9) -0.0055(9) N20 0.0163(11) 0.0235(11) 0.0251(11) 0.0005(9) -0.0039(9) -0.0064(9) N21 0.0169(10) 0.0169(10) 0.0181(10) -0.0008(8) -0.0030(8) -0.0031(8) N22 0.0202(11) 0.0169(10) 0.0188(10) -0.0053(8) -0.0028(8) -0.0030(8) N23 0.0244(11) 0.0152(10) 0.0245(11) -0.0048(9) -0.0064(9) 0.0001(9) N24 0.0193(11) 0.0158(10) 0.0300(12) -0.0064(9) -0.0087(9) 0.0016(8) C1 0.0290(17) 0.056(2) 0.057(2) -0.0200(17) 0.0114(15) -0.0141(15) C2 0.0257(16) 0.056(2) 0.0419(18) -0.0218(15) 0.0077(13) -0.0149(14) C3 0.0213(14) 0.0294(14) 0.0282(14) -0.0055(11) -0.0005(11) -0.0091(11) C4 0.0181(13) 0.0213(13) 0.0295(14) -0.0061(11) -0.0033(11) -0.0031(10) C5 0.0179(13) 0.0204(12) 0.0198(12) -0.0058(10) -0.0053(10) -0.0014(10) C6 0.0159(12) 0.0178(12) 0.0202(12) -0.0050(10) -0.0041(10) -0.0002(10) C7 0.0204(13) 0.0188(12) 0.0170(12) -0.0052(10) -0.0020(10) -0.0025(10) C8 0.0213(14) 0.0193(13) 0.0339(15) -0.0037(11) -0.0036(11) -0.0020(11) C9 0.0211(13) 0.0177(12) 0.0194(12) -0.0056(10) -0.0004(10) -0.0033(10) C10 0.0216(13) 0.0175(12) 0.0267(13) -0.0012(10) 0.0014(11) -0.0038(10) C11 0.0336(16) 0.0268(15) 0.0450(17) -0.0150(13) 0.0062(13) -0.0137(13) C12 0.0183(12) 0.0202(12) 0.0182(12) -0.0058(10) -0.0003(10) -0.0048(10) C13 0.0179(13) 0.0174(12) 0.0281(14) -0.0045(10) 0.0004(10) -0.0021(10) C14 0.0152(12) 0.0171(12) 0.0211(12) -0.0013(10) -0.0003(10) -0.0021(10) C15 0.0245(14) 0.0221(13) 0.0215(13) -0.0030(10) -0.0011(11) -0.0021(11) C16 0.056(2) 0.0218(14) 0.0228(14) -0.0019(11) -0.0040(13) 0.0034(13) C17 0.036(3) 0.037(2) 0.028(2) -0.0071(18) 0.0013(18) -0.007(2) C17' 0.047(5) 0.047(5) 0.028(4) -0.007(4) -0.014(4) -0.009(4) C18 0.0195(13) 0.0199(13) 0.0213(13) -0.0043(10) -0.0010(10) -0.0015(10) C19 0.0373(16) 0.0206(13) 0.0266(14) -0.0078(11) -0.0035(12) -0.0002(12) C20 0.0156(12) 0.0172(12) 0.0204(12) -0.0046(10) -0.0009(10) -0.0017(10) C21 0.0125(12) 0.0214(13) 0.0212(12) -0.0045(10) 0.0003(9) -0.0036(10) C22 0.0241(14) 0.0220(13) 0.0182(12) -0.0092(10) -0.0015(10) -0.0032(11) C23 0.0235(14) 0.0265(14) 0.0201(13) -0.0062(11) -0.0029(10) 0.0020(11) C24 0.0319(16) 0.0410(17) 0.0216(14) -0.0092(12) -0.0044(12) 0.0032(13) C25 0.0438(19) 0.068(2) 0.0225(15) -0.0068(15) -0.0045(14) 0.0051(17) C26 0.0463(19) 0.0243(15) 0.0366(16) -0.0108(13) -0.0013(14) 0.0013(13) C27 0.0293(15) 0.0214(13) 0.0265(14) -0.0079(11) -0.0022(11) -0.0025(11) C28 0.0199(13) 0.0220(13) 0.0222(13) -0.0089(10) -0.0014(10) -0.0021(10) C29 0.0203(13) 0.0205(13) 0.0160(12) -0.0055(10) -0.0026(10) -0.0027(10) C30 0.0139(12) 0.0217(13) 0.0263(13) -0.0049(11) -0.0038(10) -0.0043(10) C31 0.0169(12) 0.0165(12) 0.0219(12) -0.0024(10) -0.0040(10) -0.0028(10) C32 0.0176(13) 0.0206(13) 0.0252(13) -0.0058(10) -0.0040(10) -0.0057(10) C33 0.0310(15) 0.0302(15) 0.0251(14) -0.0047(11) -0.0058(11) -0.0062(12) C34 0.0175(13) 0.0210(13) 0.0233(13) -0.0053(10) -0.0027(10) -0.0034(10) C35 0.0344(16) 0.0238(14) 0.0293(14) -0.0104(11) -0.0035(12) -0.0048(12) C36 0.0424(19) 0.053(2) 0.060(2) -0.0371(18) -0.0025(16) 0.0069(16) C37 0.0135(12) 0.0174(12) 0.0262(13) -0.0041(10) -0.0062(10) -0.0033(10) C38 0.0193(13) 0.0192(13) 0.0266(13) -0.0021(10) -0.0053(10) -0.0047(10) C39 0.0168(12) 0.0185(12) 0.0230(13) -0.0065(10) -0.0015(10) -0.0026(10) C40 0.0217(13) 0.0196(12) 0.0200(12) -0.0036(10) -0.0014(10) -0.0034(10) C41 0.0239(14) 0.0272(14) 0.0246(14) 0.0035(11) -0.0048(11) -0.0078(11) C42 0.0348(17) 0.067(2) 0.0292(16) -0.0123(15) 0.0069(13) -0.0198(16) C43 0.0223(13) 0.0215(13) 0.0179(12) -0.0034(10) -0.0031(10) -0.0004(10) C44 0.0269(15) 0.0388(17) 0.0237(14) 0.0074(12) -0.0063(12) -0.0027(13) C45 0.0154(12) 0.0197(12) 0.0202(12) -0.0048(10) -0.0035(10) 0.0002(10) C46 0.0173(12) 0.0198(12) 0.0204(12) -0.0080(10) -0.0005(10) 0.0002(10) C47 0.0200(13) 0.0257(14) 0.0235(13) -0.0031(11) -0.0026(11) -0.0028(11) C48 0.0219(14) 0.0290(14) 0.0276(14) -0.0075(11) -0.0021(11) -0.0055(11) C49 0.0292(15) 0.0366(16) 0.0336(16) -0.0094(13) -0.0058(12) -0.0055(13) C50 0.0280(16) 0.0443(18) 0.0501(19) -0.0168(15) -0.0130(14) -0.0041(14) C51 0.0406(17) 0.0362(16) 0.0292(15) -0.0102(13) -0.0122(13) -0.0016(14) C52 0.0274(14) 0.0252(14) 0.0195(13) -0.0047(11) -0.0032(11) 0.0036(11) C53 0.0254(14) 0.0227(13) 0.0196(13) -0.0048(10) 0.0004(10) -0.0009(11) C54 0.0202(13) 0.0172(12) 0.0202(12) -0.0071(10) -0.0007(10) -0.0010(10) C55 0.0135(12) 0.0205(13) 0.0201(12) -0.0025(10) -0.0021(9) -0.0036(10) C56 0.0117(12) 0.0176(12) 0.0234(13) -0.0042(10) -0.0009(9) -0.0016(9) C57 0.0145(12) 0.0208(12) 0.0194(12) -0.0041(10) -0.0006(9) -0.0044(10) C58 0.0287(15) 0.0247(14) 0.0247(13) -0.0079(11) -0.0012(11) -0.0045(11) C59 0.0179(12) 0.0222(13) 0.0178(12) -0.0032(10) -0.0014(10) -0.0052(10) C60 0.0334(15) 0.0263(14) 0.0174(13) -0.0029(11) 0.0013(11) -0.0059(12) C61 0.062(2) 0.068(2) 0.0234(15) -0.0042(15) -0.0122(15) -0.0308(19) C62 0.0128(12) 0.0211(13) 0.0189(12) -0.0008(10) -0.0008(9) -0.0050(10) C63 0.0172(13) 0.0171(12) 0.0229(13) -0.0015(10) -0.0011(10) -0.0020(10) C64 0.0185(13) 0.0204(12) 0.0169(12) -0.0037(10) -0.0019(10) -0.0033(10) C65 0.0199(13) 0.0195(12) 0.0202(12) -0.0017(10) -0.0044(10) -0.0031(10) C66 0.0241(14) 0.0190(13) 0.0370(15) -0.0025(11) -0.0071(12) -0.0045(11) C67 0.0349(16) 0.0229(14) 0.0338(15) -0.0026(12) 0.0023(12) -0.0050(12) C68 0.0214(13) 0.0180(12) 0.0220(13) -0.0032(10) -0.0043(10) -0.0011(10) C69 0.0255(14) 0.0217(14) 0.0382(16) -0.0055(12) -0.0085(12) -0.0010(11) C70 0.0146(12) 0.0207(12) 0.0218(12) -0.0039(10) -0.0051(10) 0.0003(10) C71 0.0193(13) 0.0216(13) 0.0198(12) -0.0039(10) -0.0054(10) -0.0011(10) C72 0.0216(14) 0.0216(13) 0.0297(14) -0.0046(11) -0.0059(11) -0.0032(11) C73 0.0248(14) 0.0337(15) 0.0315(15) -0.0044(12) -0.0035(12) -0.0099(12) C74 0.0243(16) 0.0486(19) 0.067(2) -0.0291(17) 0.0058(15) -0.0085(14) C75 0.0278(17) 0.062(2) 0.061(2) -0.0232(18) 0.0059(15) -0.0105(16) C76 0.0324(18) 0.068(2) 0.055(2) -0.0187(18) -0.0116(15) -0.0170(17) C77 0.0255(15) 0.0456(18) 0.0361(16) -0.0068(14) -0.0067(12) -0.0099(13) C78 0.0219(14) 0.0299(14) 0.0296(14) -0.0050(12) -0.0015(11) -0.0088(11) C79 0.0238(14) 0.0245(14) 0.0218(13) -0.0003(11) -0.0043(11) -0.0042(11) C80 0.0156(12) 0.0180(12) 0.0229(13) -0.0088(10) -0.0008(10) 0.0010(10) C81 0.0172(12) 0.0164(12) 0.0225(12) -0.0054(10) -0.0026(10) -0.0014(10) C82 0.0192(13) 0.0165(12) 0.0209(12) -0.0038(10) -0.0026(10) 0.0009(10) C83 0.0268(14) 0.0247(14) 0.0220(13) -0.0003(11) -0.0047(11) -0.0028(11) C84 0.0179(13) 0.0184(12) 0.0227(13) -0.0045(10) 0.0002(10) -0.0030(10) C85 0.0204(13) 0.0240(13) 0.0248(13) 0.0005(11) -0.0015(10) -0.0069(11) C86 0.0408(18) 0.0280(15) 0.0417(17) -0.0066(13) 0.0010(14) -0.0140(13) C87 0.0166(12) 0.0168(12) 0.0234(13) -0.0062(10) -0.0006(10) -0.0029(10) C88 0.0189(13) 0.0193(13) 0.0269(13) -0.0050(10) -0.0033(10) -0.0044(10) C89 0.0159(12) 0.0173(12) 0.0227(13) -0.0031(10) -0.0027(10) -0.0054(10) C90 0.0169(12) 0.0198(12) 0.0241(13) -0.0070(10) 0.0001(10) -0.0051(10) C91 0.0393(16) 0.0195(13) 0.0285(14) -0.0078(11) 0.0007(12) -0.0046(12) C92 0.0398(18) 0.0329(17) 0.0503(19) -0.0181(15) 0.0085(15) 0.0012(14) C93 0.0185(13) 0.0212(13) 0.0234(13) -0.0058(10) -0.0041(10) -0.0057(10) C94 0.0362(16) 0.0281(14) 0.0215(13) -0.0062(11) -0.0018(11) -0.0086(12) C95 0.0160(12) 0.0162(12) 0.0222(12) -0.0020(10) -0.0032(10) -0.0031(10) C96 0.0132(12) 0.0193(12) 0.0247(13) -0.0060(10) -0.0034(10) -0.0017(10) C97 0.0192(13) 0.0216(13) 0.0180(12) -0.0051(10) -0.0011(10) -0.0027(10) C98 0.0209(13) 0.0229(13) 0.0256(13) -0.0100(11) -0.0041(10) 0.0006(11) C99 0.0313(15) 0.0210(13) 0.0260(14) -0.0052(11) -0.0036(11) -0.0013(11) C100 0.0480(19) 0.0214(15) 0.0485(19) -0.0109(13) -0.0052(15) -0.0007(13) O17 0.0323(11) 0.0304(10) 0.0266(10) -0.0128(8) 0.0018(8) -0.0067(8) O18 0.0345(12) 0.0527(13) 0.0504(13) -0.0343(11) 0.0083(10) -0.0143(10) O19 0.0565(19) 0.123(3) 0.124(3) -0.070(2) 0.0019(18) -0.0238(19) O21 0.0252(10) 0.0317(10) 0.0276(10) -0.0110(8) -0.0018(8) -0.0053(8) O22 0.0335(11) 0.0362(11) 0.0290(10) -0.0117(9) -0.0005(8) -0.0078(9) O23 0.0400(13) 0.0485(13) 0.0385(12) -0.0045(10) -0.0061(10) -0.0101(10) O24 0.175(5) 0.087(3) 0.092(3) -0.027(2) -0.016(3) 0.018(3) C101 0.0319(16) 0.0390(17) 0.0370(16) -0.0145(13) 0.0002(13) -0.0104(13) C102 0.0451(19) 0.0415(18) 0.0369(17) -0.0162(14) 0.0008(14) 0.0010(15) C103 0.0505(19) 0.0358(17) 0.0335(16) -0.0188(13) 0.0090(14) -0.0157(15) C104 0.0330(16) 0.0395(16) 0.0255(14) -0.0137(12) 0.0042(12) -0.0142(13) C105 0.047(2) 0.137(4) 0.086(3) -0.088(3) 0.030(2) -0.043(3) C106 0.0363(19) 0.113(3) 0.048(2) -0.043(2) 0.0014(16) -0.009(2) C107 0.0346(17) 0.059(2) 0.0349(17) -0.0182(15) -0.0073(13) -0.0048(15) C108 0.0300(16) 0.0353(17) 0.0482(18) -0.0168(14) 0.0052(14) -0.0051(13) C109 0.063(2) 0.060(2) 0.054(2) -0.0278(19) 0.0071(18) -0.017(2) C110 0.0450(19) 0.0454(19) 0.0365(17) -0.0064(14) -0.0031(14) -0.0062(15) C111 0.062(3) 0.100(4) 0.066(3) -0.046(3) -0.004(2) 0.014(3) C112 0.065(3) 0.040(2) 0.075(3) -0.0179(18) -0.033(2) 0.0008(18) O20A 0.045(2) 0.066(3) 0.063(3) -0.039(2) 0.009(2) -0.022(2) C13A 0.033(3) 0.045(3) 0.059(4) -0.024(3) 0.003(3) -0.010(2) C14A 0.042(4) 0.033(3) 0.053(4) -0.020(3) 0.002(4) -0.006(3) C15A 0.045(3) 0.045(3) 0.032(3) -0.014(2) -0.007(2) 0.000(2) C16A 0.045(4) 0.063(4) 0.045(3) -0.024(3) 0.005(3) -0.025(3) O20B 0.031(3) 0.034(3) 0.051(4) -0.002(3) -0.010(3) 0.000(2) C13B 0.045(8) 0.071(8) 0.094(10) -0.019(6) -0.012(7) -0.003(6) C14B 0.060(6) 0.061(6) 0.062(6) -0.029(5) -0.032(5) 0.022(5) C15B 0.046(6) 0.048(5) 0.056(6) -0.002(5) 0.013(5) -0.003(5) C16B 0.044(5) 0.053(6) 0.068(6) -0.024(5) 0.010(4) -0.008(5) C117 0.0240(14) 0.0385(16) 0.0338(15) -0.0177(13) 0.0018(12) -0.0080(12) C118 0.060(2) 0.0350(17) 0.0261(15) -0.0080(13) -0.0004(14) -0.0192(15) C119 0.049(2) 0.0368(17) 0.0390(17) -0.0129(14) -0.0156(15) 0.0042(15) C120 0.0238(14) 0.0287(15) 0.0339(15) -0.0071(12) -0.0001(12) -0.0066(12) C121 0.0385(17) 0.0378(17) 0.0312(16) -0.0077(13) -0.0041(13) -0.0023(14) C122 0.113(4) 0.054(2) 0.048(2) -0.0192(19) -0.005(2) 0.032(2) C123 0.051(2) 0.100(3) 0.057(2) -0.047(2) 0.0007(18) -0.011(2) C124 0.0372(17) 0.056(2) 0.0285(15) -0.0136(14) 0.0013(13) -0.0211(15) C125 0.0413(18) 0.0376(17) 0.0352(16) -0.0085(13) 0.0013(14) -0.0062(14) C126 0.0448(19) 0.0361(17) 0.0358(17) -0.0062(13) 0.0002(14) -0.0100(14) C127 0.064(2) 0.0317(16) 0.0367(17) -0.0141(14) -0.0173(16) -0.0014(15) C128 0.052(2) 0.055(2) 0.0440(19) -0.0253(17) -0.0016(16) 0.0022(17) C129 0.141(5) 0.070(3) 0.068(3) -0.019(3) -0.005(3) 0.017(3) C130 0.079(3) 0.083(3) 0.045(2) -0.020(2) -0.025(2) 0.006(2) C131 0.103(4) 0.160(6) 0.065(3) -0.037(4) -0.004(3) -0.010(4) C132 0.133(5) 0.059(3) 0.093(4) -0.027(3) -0.027(4) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C4 1.236(3) . ? O2 C5 1.243(3) . ? O3 C21 1.242(3) . ? O4 C22 1.229(3) . ? O5 C29 1.234(3) . ? O6 C30 1.248(3) . ? O7 C46 1.247(3) . ? O8 C47 1.228(3) . ? O9 C54 1.236(3) . ? O10 C55 1.246(3) . ? O11 C71 1.245(3) . ? O12 C72 1.232(3) . ? O13 C79 1.234(3) . ? O14 C80 1.250(3) . ? O15 C96 1.244(3) . ? O16 C97 1.236(3) . ? N1 C4 1.344(3) . ? N1 N2 1.387(3) . ? N1 H1 0.8600 . ? N2 C5 1.355(3) . ? N2 H2 0.8600 . ? N3 C12 1.364(3) . ? N3 C6 1.390(3) . ? N3 H3 0.8600 . ? N4 C14 1.364(3) . ? N4 C20 1.389(3) . ? N4 H4 0.8600 . ? N5 C21 1.367(3) . ? N5 N6 1.391(3) . ? N5 H5 0.8600 . ? N6 C22 1.353(3) . ? N6 H6 0.8600 . ? N7 C29 1.348(3) . ? N7 N8 1.397(3) . ? N7 H7 0.8600 . ? N8 C30 1.361(3) . ? N8 H8 0.8600 . ? N9 C37 1.361(3) . ? N9 C31 1.385(3) . ? N9 H9 0.8600 . ? N10 C39 1.360(3) . ? N10 C45 1.387(3) . ? N10 H10 0.8600 . ? N11 C46 1.369(3) . ? N11 N12 1.396(3) . ? N11 H11 0.8600 . ? N12 C47 1.359(3) . ? N12 H12 0.8600 . ? N13 C54 1.344(3) . ? N13 N14 1.394(3) . ? N13 H13 0.8600 . ? N14 C55 1.364(3) . ? N14 H14 0.8600 . ? N15 C62 1.369(3) . ? N15 C56 1.385(3) . ? N15 H15 0.8600 . ? N16 C64 1.361(3) . ? N16 C70 1.393(3) . ? N16 H16 0.8600 . ? N17 C71 1.365(3) . ? N17 N18 1.392(3) . ? N17 H17 0.8600 . ? N18 C72 1.348(3) . ? N18 H18 0.8600 . ? N19 C79 1.351(3) . ? N19 N20 1.392(3) . ? N19 H19 0.8600 . ? N20 C80 1.364(3) . ? N20 H20 0.8600 . ? N21 C87 1.362(3) . ? N21 C81 1.394(3) . ? N21 H21 0.8600 . ? N22 C89 1.366(3) . ? N22 C95 1.381(3) . ? N22 H22 0.8600 . ? N23 C96 1.358(3) . ? N23 N24 1.394(3) . ? N23 H23 0.8600 . ? N24 C97 1.344(3) . ? N24 H24 0.8600 . ? C1 C2 1.525(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.514(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.513(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.450(3) . ? C6 C7 1.393(3) . ? C7 C9 1.418(3) . ? C7 C8 1.507(3) . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C8 H8E 0.9600 . ? C9 C12 1.388(3) . ? C9 C10 1.505(3) . ? C10 C11 1.529(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.504(3) . ? C13 C14 1.504(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.379(4) . ? C15 C18 1.424(3) . ? C15 C16 1.505(4) . ? C16 C17' 1.357(8) . ? C16 C17 1.418(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C18 C20 1.389(3) . ? C18 C19 1.502(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.455(3) . ? C22 C23 1.508(3) . ? C23 C24 1.515(4) . ? C23 H23C 0.9700 . ? C23 H23D 0.9700 . ? C24 C25 1.522(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.522(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.516(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.512(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C30 C31 1.445(3) . ? C31 C32 1.394(3) . ? C32 C34 1.420(3) . ? C32 C33 1.500(4) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C37 1.388(3) . ? C34 C35 1.503(4) . ? C35 C36 1.513(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.492(3) . ? C38 C39 1.502(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.383(3) . ? C40 C43 1.415(4) . ? C40 C41 1.509(4) . ? C41 C42 1.517(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C45 1.397(3) . ? C43 C44 1.497(3) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.446(3) . ? C47 C48 1.513(4) . ? C48 C49 1.524(4) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 C50 1.527(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.525(4) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.525(4) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.511(3) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C55 C56 1.454(3) . ? C56 C57 1.395(3) . ? C57 C59 1.418(3) . ? C57 C58 1.499(3) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C62 1.388(4) . ? C59 C60 1.504(3) . ? C60 C61 1.518(4) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 C63 1.499(3) . ? C63 C64 1.500(3) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C65 1.394(3) . ? C65 C68 1.422(3) . ? C65 C66 1.504(3) . ? C66 C67 1.525(4) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 C70 1.392(3) . ? C68 C69 1.501(3) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 C71 1.451(3) . ? C72 C73 1.510(4) . ? C73 C74 1.511(4) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 C75 1.525(4) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 C77 1.520(4) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 C78 1.521(4) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C79 1.510(4) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C80 C81 1.449(3) . ? C81 C82 1.391(3) . ? C82 C84 1.424(3) . ? C82 C83 1.503(3) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 C87 1.385(3) . ? C84 C85 1.509(3) . ? C85 C86 1.530(4) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 C88 1.506(3) . ? C88 C89 1.501(3) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C89 C90 1.385(3) . ? C90 C93 1.424(3) . ? C90 C91 1.501(4) . ? C91 C92 1.528(4) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 C95 1.391(4) . ? C93 C94 1.493(3) . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 C96 1.460(3) . ? C97 C98 1.504(3) . ? C98 C99 1.524(4) . ? C98 H98A 0.9700 . ? C98 H98B 0.9700 . ? C99 C100 1.526(4) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 H10C 0.9600 . ? C100 H10D 0.9600 . ? C100 H10E 0.9600 . ? O17 C104 1.442(3) . ? O17 C101 1.445(3) . ? O18 C108 1.430(4) . ? O18 C105 1.436(4) . ? O19 C109 1.400(5) . ? O19 C111 1.415(5) . ? O21 C117 1.441(3) . ? O21 C120 1.449(3) . ? O22 C121 1.439(3) . ? O22 C124 1.447(3) . ? O23 C125 1.421(4) . ? O23 C128 1.432(4) . ? O24 C132 1.400(7) . ? O24 C129 1.421(7) . ? C101 C102 1.525(4) . ? C101 H10F 0.9700 . ? C101 H10G 0.9700 . ? C102 C103 1.519(4) . ? C102 H10H 0.9700 . ? C102 H10I 0.9700 . ? C103 C104 1.505(4) . ? C103 H10J 0.9700 . ? C103 H10K 0.9700 . ? C104 H10L 0.9700 . ? C104 H10M 0.9700 . ? C105 C106 1.444(5) . ? C105 H10N 0.9700 . ? C105 H10O 0.9700 . ? C106 C107 1.510(5) . ? C106 H10P 0.9700 . ? C106 H10Q 0.9700 . ? C107 C108 1.513(4) . ? C107 H10R 0.9700 . ? C107 H10S 0.9700 . ? C108 H10T 0.9700 . ? C108 H10U 0.9700 . ? C109 C110 1.497(5) . ? C109 H10V 0.9700 . ? C109 H10W 0.9700 . ? C110 C112 1.548(5) . ? C110 H11D 0.9700 . ? C110 H11E 0.9700 . ? C111 C112 1.484(6) . ? C111 H11H 0.9700 . ? C111 H11I 0.9700 . ? C112 H11F 0.9700 . ? C112 H11G 0.9700 . ? O20A C16A 1.414(6) . ? O20A C13A 1.415(6) . ? C13A C14A 1.534(7) . ? C13A H13C 0.9700 . ? C13A H13D 0.9700 . ? C14A C15A 1.484(8) . ? C14A H14A 0.9700 . ? C14A H14B 0.9700 . ? C15A C16A 1.528(7) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C16A H16C 0.9700 . ? C16A H16D 0.9700 . ? O20B C13B 1.388(9) . ? O20B C16B 1.413(8) . ? C13B C14B 1.528(10) . ? C13B H13E 0.9700 . ? C13B H13F 0.9700 . ? C14B C15B 1.485(10) . ? C14B H14C 0.9700 . ? C14B H14D 0.9700 . ? C15B C16B 1.529(9) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16B H16E 0.9700 . ? C16B H16F 0.9700 . ? C117 C118 1.505(4) . ? C117 H1G 0.9700 . ? C117 H1H 0.9700 . ? C118 C119 1.524(5) . ? C118 H1E 0.9700 . ? C118 H1F 0.9700 . ? C119 C120 1.513(4) . ? C119 H11J 0.9700 . ? C119 H11K 0.9700 . ? C120 H12A 0.9700 . ? C120 H12B 0.9700 . ? C121 C122 1.512(5) . ? C121 H12C 0.9700 . ? C121 H12D 0.9700 . ? C122 C123 1.464(6) . ? C122 H12E 0.9700 . ? C122 H12F 0.9700 . ? C123 C124 1.477(5) . ? C123 H12G 0.9700 . ? C123 H12H 0.9700 . ? C124 H12I 0.9700 . ? C124 H12J 0.9700 . ? C125 C126 1.511(4) . ? C125 H12K 0.9700 . ? C125 H12L 0.9700 . ? C126 C127 1.518(4) . ? C126 H12M 0.9700 . ? C126 H12N 0.9700 . ? C127 C128 1.516(5) . ? C127 H12O 0.9700 . ? C127 H12P 0.9700 . ? C128 H12Q 0.9700 . ? C128 H12R 0.9700 . ? C129 C130 1.520(6) . ? C129 H12S 0.9700 . ? C129 H12T 0.9700 . ? C130 C131 1.536(7) . ? C130 H13M 0.9700 . ? C130 H13N 0.9700 . ? C131 C132 1.550(7) . ? C131 H13O 0.9700 . ? C131 H13P 0.9700 . ? C132 H13G 0.9700 . ? C132 H13H 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 N1 N2 120.0(2) . . ? C4 N1 H1 120.0 . . ? N2 N1 H1 120.0 . . ? C5 N2 N1 119.2(2) . . ? C5 N2 H2 120.4 . . ? N1 N2 H2 120.4 . . ? C12 N3 C6 109.37(19) . . ? C12 N3 H3 125.3 . . ? C6 N3 H3 125.3 . . ? C14 N4 C20 109.3(2) . . ? C14 N4 H4 125.4 . . ? C20 N4 H4 125.4 . . ? C21 N5 N6 119.1(2) . . ? C21 N5 H5 120.4 . . ? N6 N5 H5 120.4 . . ? C22 N6 N5 120.5(2) . . ? C22 N6 H6 119.8 . . ? N5 N6 H6 119.8 . . ? C29 N7 N8 122.1(2) . . ? C29 N7 H7 118.9 . . ? N8 N7 H7 118.9 . . ? C30 N8 N7 118.7(2) . . ? C30 N8 H8 120.6 . . ? N7 N8 H8 120.6 . . ? C37 N9 C31 109.3(2) . . ? C37 N9 H9 125.4 . . ? C31 N9 H9 125.4 . . ? C39 N10 C45 109.5(2) . . ? C39 N10 H10 125.3 . . ? C45 N10 H10 125.3 . . ? C46 N11 N12 118.4(2) . . ? C46 N11 H11 120.8 . . ? N12 N11 H11 120.8 . . ? C47 N12 N11 119.0(2) . . ? C47 N12 H12 120.5 . . ? N11 N12 H12 120.5 . . ? C54 N13 N14 119.6(2) . . ? C54 N13 H13 120.2 . . ? N14 N13 H13 120.2 . . ? C55 N14 N13 119.3(2) . . ? C55 N14 H14 120.4 . . ? N13 N14 H14 120.4 . . ? C62 N15 C56 109.3(2) . . ? C62 N15 H15 125.3 . . ? C56 N15 H15 125.3 . . ? C64 N16 C70 109.6(2) . . ? C64 N16 H16 125.2 . . ? C70 N16 H16 125.2 . . ? C71 N17 N18 118.3(2) . . ? C71 N17 H17 120.9 . . ? N18 N17 H17 120.9 . . ? C72 N18 N17 119.7(2) . . ? C72 N18 H18 120.2 . . ? N17 N18 H18 120.2 . . ? C79 N19 N20 120.0(2) . . ? C79 N19 H19 120.0 . . ? N20 N19 H19 120.0 . . ? C80 N20 N19 119.1(2) . . ? C80 N20 H20 120.5 . . ? N19 N20 H20 120.5 . . ? C87 N21 C81 109.31(19) . . ? C87 N21 H21 125.3 . . ? C81 N21 H21 125.3 . . ? C89 N22 C95 109.4(2) . . ? C89 N22 H22 125.3 . . ? C95 N22 H22 125.3 . . ? C96 N23 N24 119.5(2) . . ? C96 N23 H23 120.3 . . ? N24 N23 H23 120.3 . . ? C97 N24 N23 121.1(2) . . ? C97 N24 H24 119.5 . . ? N23 N24 H24 119.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C1 112.7(3) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 112.7(2) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? O1 C4 N1 123.3(2) . . ? O1 C4 C3 122.2(2) . . ? N1 C4 C3 114.5(2) . . ? O2 C5 N2 120.7(2) . . ? O2 C5 C6 122.1(2) . . ? N2 C5 C6 117.1(2) . . ? N3 C6 C7 107.3(2) . . ? N3 C6 C5 124.7(2) . . ? C7 C6 C5 127.9(2) . . ? C6 C7 C9 107.6(2) . . ? C6 C7 C8 127.3(2) . . ? C9 C7 C8 125.0(2) . . ? C7 C8 H8C 109.5 . . ? C7 C8 H8D 109.5 . . ? H8C C8 H8D 109.5 . . ? C7 C8 H8E 109.5 . . ? H8C C8 H8E 109.5 . . ? H8D C8 H8E 109.5 . . ? C12 C9 C7 107.1(2) . . ? C12 C9 C10 126.2(2) . . ? C7 C9 C10 126.5(2) . . ? C9 C10 C11 113.1(2) . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C9 108.6(2) . . ? N3 C12 C13 122.9(2) . . ? C9 C12 C13 128.1(2) . . ? C14 C13 C12 118.0(2) . . ? C14 C13 H13A 107.8 . . ? C12 C13 H13A 107.8 . . ? C14 C13 H13B 107.8 . . ? C12 C13 H13B 107.8 . . ? H13A C13 H13B 107.1 . . ? N4 C14 C15 108.4(2) . . ? N4 C14 C13 121.1(2) . . ? C15 C14 C13 130.3(2) . . ? C14 C15 C18 107.8(2) . . ? C14 C15 C16 125.7(2) . . ? C18 C15 C16 126.5(2) . . ? C17' C16 C17 124.7(5) . . ? C17' C16 C15 119.0(5) . . ? C17 C16 C15 115.9(3) . . ? C17' C16 H16A 59.5 . . ? C17 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? C17' C16 H16B 48.0 . . ? C17 C16 H16B 108.3 . . ? C15 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C17' H17D 109.5 . . ? C16 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C16 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C20 C18 C15 106.8(2) . . ? C20 C18 C19 126.6(2) . . ? C15 C18 C19 126.6(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 N4 107.8(2) . . ? C18 C20 C21 129.8(2) . . ? N4 C20 C21 122.1(2) . . ? O3 C21 N5 121.9(2) . . ? O3 C21 C20 123.2(2) . . ? N5 C21 C20 114.8(2) . . ? O4 C22 N6 123.4(2) . . ? O4 C22 C23 122.7(2) . . ? N6 C22 C23 113.9(2) . . ? C22 C23 C24 112.0(2) . . ? C22 C23 H23C 109.2 . . ? C24 C23 H23C 109.2 . . ? C22 C23 H23D 109.2 . . ? C24 C23 H23D 109.2 . . ? H23C C23 H23D 107.9 . . ? C23 C24 C25 111.5(2) . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C26 111.4(2) . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? C26 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C29 C28 C27 113.3(2) . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28B 108.9 . . ? C27 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? O5 C29 N7 123.0(2) . . ? O5 C29 C28 123.3(2) . . ? N7 C29 C28 113.6(2) . . ? O6 C30 N8 121.7(2) . . ? O6 C30 C31 121.9(2) . . ? N8 C30 C31 116.3(2) . . ? N9 C31 C32 107.9(2) . . ? N9 C31 C30 122.6(2) . . ? C32 C31 C30 129.5(2) . . ? C31 C32 C34 106.9(2) . . ? C31 C32 C33 126.3(2) . . ? C34 C32 C33 126.7(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C37 C34 C32 107.3(2) . . ? C37 C34 C35 125.6(2) . . ? C32 C34 C35 127.1(2) . . ? C34 C35 C36 114.3(2) . . ? C34 C35 H35A 108.7 . . ? C36 C35 H35A 108.7 . . ? C34 C35 H35B 108.7 . . ? C36 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N9 C37 C34 108.6(2) . . ? N9 C37 C38 120.5(2) . . ? C34 C37 C38 130.8(2) . . ? C37 C38 C39 115.9(2) . . ? C37 C38 H38A 108.3 . . ? C39 C38 H38A 108.3 . . ? C37 C38 H38B 108.3 . . ? C39 C38 H38B 108.3 . . ? H38A C38 H38B 107.4 . . ? N10 C39 C40 108.5(2) . . ? N10 C39 C38 123.9(2) . . ? C40 C39 C38 127.5(2) . . ? C39 C40 C43 107.5(2) . . ? C39 C40 C41 125.0(2) . . ? C43 C40 C41 127.3(2) . . ? C40 C41 C42 111.6(2) . . ? C40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? C40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 108.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C45 C43 C40 107.2(2) . . ? C45 C43 C44 127.5(2) . . ? C40 C43 C44 125.4(2) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N10 C45 C43 107.3(2) . . ? N10 C45 C46 124.9(2) . . ? C43 C45 C46 127.8(2) . . ? O7 C46 N11 120.5(2) . . ? O7 C46 C45 121.7(2) . . ? N11 C46 C45 117.8(2) . . ? O8 C47 N12 123.1(2) . . ? O8 C47 C48 121.7(2) . . ? N12 C47 C48 115.2(2) . . ? C47 C48 C49 111.9(2) . . ? C47 C48 H48A 109.2 . . ? C49 C48 H48A 109.2 . . ? C47 C48 H48B 109.2 . . ? C49 C48 H48B 109.2 . . ? H48A C48 H48B 107.9 . . ? C48 C49 C50 112.4(2) . . ? C48 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? C48 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C51 C52 C53 114.1(2) . . ? C51 C52 H52A 108.7 . . ? C53 C52 H52A 108.7 . . ? C51 C52 H52B 108.7 . . ? C53 C52 H52B 108.7 . . ? H52A C52 H52B 107.6 . . ? C54 C53 C52 119.6(2) . . ? C54 C53 H53A 107.4 . . ? C52 C53 H53A 107.4 . . ? C54 C53 H53B 107.4 . . ? C52 C53 H53B 107.4 . . ? H53A C53 H53B 107.0 . . ? O9 C54 N13 121.5(2) . . ? O9 C54 C53 120.6(2) . . ? N13 C54 C53 117.9(2) . . ? O10 C55 N14 122.1(2) . . ? O10 C55 C56 121.9(2) . . ? N14 C55 C56 115.9(2) . . ? N15 C56 C57 107.7(2) . . ? N15 C56 C55 123.3(2) . . ? C57 C56 C55 129.0(2) . . ? C56 C57 C59 107.1(2) . . ? C56 C57 C58 126.6(2) . . ? C59 C57 C58 126.1(2) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C62 C59 C57 107.6(2) . . ? C62 C59 C60 125.8(2) . . ? C57 C59 C60 126.6(2) . . ? C59 C60 C61 113.8(2) . . ? C59 C60 H60A 108.8 . . ? C61 C60 H60A 108.8 . . ? C59 C60 H60B 108.8 . . ? C61 C60 H60B 108.8 . . ? H60A C60 H60B 107.7 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N15 C62 C59 108.3(2) . . ? N15 C62 C63 120.8(2) . . ? C59 C62 C63 130.9(2) . . ? C62 C63 C64 116.6(2) . . ? C62 C63 H63A 108.1 . . ? C64 C63 H63A 108.1 . . ? C62 C63 H63B 108.1 . . ? C64 C63 H63B 108.1 . . ? H63A C63 H63B 107.3 . . ? N16 C64 C65 108.4(2) . . ? N16 C64 C63 123.7(2) . . ? C65 C64 C63 127.9(2) . . ? C64 C65 C68 107.2(2) . . ? C64 C65 C66 126.0(2) . . ? C68 C65 C66 126.8(2) . . ? C65 C66 C67 114.1(2) . . ? C65 C66 H66A 108.7 . . ? C67 C66 H66A 108.7 . . ? C65 C66 H66B 108.7 . . ? C67 C66 H66B 108.7 . . ? H66A C66 H66B 107.6 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C70 C68 C65 107.4(2) . . ? C70 C68 C69 127.7(2) . . ? C65 C68 C69 124.9(2) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 N16 107.5(2) . . ? C68 C70 C71 128.3(2) . . ? N16 C70 C71 124.3(2) . . ? O11 C71 N17 120.6(2) . . ? O11 C71 C70 122.0(2) . . ? N17 C71 C70 117.3(2) . . ? O12 C72 N18 122.7(2) . . ? O12 C72 C73 122.2(2) . . ? N18 C72 C73 115.2(2) . . ? C72 C73 C74 111.1(2) . . ? C72 C73 H73A 109.4 . . ? C74 C73 H73A 109.4 . . ? C72 C73 H73B 109.4 . . ? C74 C73 H73B 109.4 . . ? H73A C73 H73B 108.0 . . ? C73 C74 C75 113.6(3) . . ? C73 C74 H74A 108.8 . . ? C75 C74 H74A 108.8 . . ? C73 C74 H74B 108.8 . . ? C75 C74 H74B 108.8 . . ? H74A C74 H74B 107.7 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 C76 H76A 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C77 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C76 C77 C78 112.4(3) . . ? C76 C77 H77A 109.1 . . ? C78 C77 H77A 109.1 . . ? C76 C77 H77B 109.1 . . ? C78 C77 H77B 109.1 . . ? H77A C77 H77B 107.9 . . ? C79 C78 C77 111.3(2) . . ? C79 C78 H78A 109.4 . . ? C77 C78 H78A 109.4 . . ? C79 C78 H78B 109.4 . . ? C77 C78 H78B 109.4 . . ? H78A C78 H78B 108.0 . . ? O13 C79 N19 122.8(2) . . ? O13 C79 C78 122.7(2) . . ? N19 C79 C78 114.4(2) . . ? O14 C80 N20 120.9(2) . . ? O14 C80 C81 121.9(2) . . ? N20 C80 C81 117.1(2) . . ? C82 C81 N21 107.4(2) . . ? C82 C81 C80 128.0(2) . . ? N21 C81 C80 124.6(2) . . ? C81 C82 C84 107.5(2) . . ? C81 C82 C83 127.4(2) . . ? C84 C82 C83 125.1(2) . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C87 C84 C82 107.0(2) . . ? C87 C84 C85 126.5(2) . . ? C82 C84 C85 126.4(2) . . ? C84 C85 C86 113.0(2) . . ? C84 C85 H85A 109.0 . . ? C86 C85 H85A 109.0 . . ? C84 C85 H85B 109.0 . . ? C86 C85 H85B 109.0 . . ? H85A C85 H85B 107.8 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N21 C87 C84 108.8(2) . . ? N21 C87 C88 123.7(2) . . ? C84 C87 C88 127.5(2) . . ? C89 C88 C87 116.3(2) . . ? C89 C88 H88A 108.2 . . ? C87 C88 H88A 108.2 . . ? C89 C88 H88B 108.2 . . ? C87 C88 H88B 108.2 . . ? H88A C88 H88B 107.4 . . ? N22 C89 C90 108.3(2) . . ? N22 C89 C88 120.5(2) . . ? C90 C89 C88 131.1(2) . . ? C89 C90 C93 107.5(2) . . ? C89 C90 C91 126.2(2) . . ? C93 C90 C91 126.4(2) . . ? C90 C91 C92 113.4(2) . . ? C90 C91 H91A 108.9 . . ? C92 C91 H91A 108.9 . . ? C90 C91 H91B 108.9 . . ? C92 C91 H91B 108.9 . . ? H91A C91 H91B 107.7 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C95 C93 C90 106.8(2) . . ? C95 C93 C94 126.8(2) . . ? C90 C93 C94 126.4(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 . . ? N22 C95 C93 108.0(2) . . ? N22 C95 C96 122.3(2) . . ? C93 C95 C96 129.7(2) . . ? O15 C96 N23 122.1(2) . . ? O15 C96 C95 123.0(2) . . ? N23 C96 C95 114.9(2) . . ? O16 C97 N24 122.6(2) . . ? O16 C97 C98 122.9(2) . . ? N24 C97 C98 114.5(2) . . ? C97 C98 C99 112.2(2) . . ? C97 C98 H98A 109.2 . . ? C99 C98 H98A 109.2 . . ? C97 C98 H98B 109.2 . . ? C99 C98 H98B 109.2 . . ? H98A C98 H98B 107.9 . . ? C98 C99 C100 112.0(2) . . ? C98 C99 H99A 109.2 . . ? C100 C99 H99A 109.2 . . ? C98 C99 H99B 109.2 . . ? C100 C99 H99B 109.2 . . ? H99A C99 H99B 107.9 . . ? C99 C100 H10C 109.5 . . ? C99 C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? C99 C100 H10E 109.5 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C104 O17 C101 107.6(2) . . ? C108 O18 C105 106.7(2) . . ? C109 O19 C111 104.4(3) . . ? C117 O21 C120 107.8(2) . . ? C121 O22 C124 109.0(2) . . ? C125 O23 C128 108.0(2) . . ? C132 O24 C129 104.4(4) . . ? O17 C101 C102 107.1(2) . . ? O17 C101 H10F 110.3 . . ? C102 C101 H10F 110.3 . . ? O17 C101 H10G 110.3 . . ? C102 C101 H10G 110.3 . . ? H10F C101 H10G 108.6 . . ? C103 C102 C101 103.0(2) . . ? C103 C102 H10H 111.2 . . ? C101 C102 H10H 111.2 . . ? C103 C102 H10I 111.2 . . ? C101 C102 H10I 111.2 . . ? H10H C102 H10I 109.1 . . ? C104 C103 C102 101.4(2) . . ? C104 C103 H10J 111.5 . . ? C102 C103 H10J 111.5 . . ? C104 C103 H10K 111.5 . . ? C102 C103 H10K 111.5 . . ? H10J C103 H10K 109.3 . . ? O17 C104 C103 104.5(2) . . ? O17 C104 H10L 110.9 . . ? C103 C104 H10L 110.9 . . ? O17 C104 H10M 110.9 . . ? C103 C104 H10M 110.9 . . ? H10L C104 H10M 108.9 . . ? O18 C105 C106 109.8(3) . . ? O18 C105 H10N 109.7 . . ? C106 C105 H10N 109.7 . . ? O18 C105 H10O 109.7 . . ? C106 C105 H10O 109.7 . . ? H10N C105 H10O 108.2 . . ? C105 C106 C107 105.7(3) . . ? C105 C106 H10P 110.6 . . ? C107 C106 H10P 110.6 . . ? C105 C106 H10Q 110.6 . . ? C107 C106 H10Q 110.6 . . ? H10P C106 H10Q 108.7 . . ? C106 C107 C108 104.0(3) . . ? C106 C107 H10R 111.0 . . ? C108 C107 H10R 111.0 . . ? C106 C107 H10S 111.0 . . ? C108 C107 H10S 111.0 . . ? H10R C107 H10S 109.0 . . ? O18 C108 C107 105.5(2) . . ? O18 C108 H10T 110.6 . . ? C107 C108 H10T 110.6 . . ? O18 C108 H10U 110.6 . . ? C107 C108 H10U 110.6 . . ? H10T C108 H10U 108.8 . . ? O19 C109 C110 106.1(3) . . ? O19 C109 H10V 110.5 . . ? C110 C109 H10V 110.5 . . ? O19 C109 H10W 110.5 . . ? C110 C109 H10W 110.5 . . ? H10V C109 H10W 108.7 . . ? C109 C110 C112 102.9(3) . . ? C109 C110 H11D 111.2 . . ? C112 C110 H11D 111.2 . . ? C109 C110 H11E 111.2 . . ? C112 C110 H11E 111.2 . . ? H11D C110 H11E 109.1 . . ? O19 C111 C112 106.3(3) . . ? O19 C111 H11H 110.5 . . ? C112 C111 H11H 110.5 . . ? O19 C111 H11I 110.5 . . ? C112 C111 H11I 110.5 . . ? H11H C111 H11I 108.7 . . ? C111 C112 C110 103.3(3) . . ? C111 C112 H11F 111.1 . . ? C110 C112 H11F 111.1 . . ? C111 C112 H11G 111.1 . . ? C110 C112 H11G 111.1 . . ? H11F C112 H11G 109.1 . . ? C16A O20A C13A 109.9(4) . . ? O20A C13A C14A 105.4(5) . . ? O20A C13A H13C 110.7 . . ? C14A C13A H13C 110.7 . . ? O20A C13A H13D 110.7 . . ? C14A C13A H13D 110.7 . . ? H13C C13A H13D 108.8 . . ? C15A C14A C13A 102.4(5) . . ? C15A C14A H14A 111.3 . . ? C13A C14A H14A 111.3 . . ? C15A C14A H14B 111.3 . . ? C13A C14A H14B 111.3 . . ? H14A C14A H14B 109.2 . . ? C14A C15A C16A 102.5(4) . . ? C14A C15A H15A 111.3 . . ? C16A C15A H15A 111.3 . . ? C14A C15A H15B 111.3 . . ? C16A C15A H15B 111.3 . . ? H15A C15A H15B 109.2 . . ? O20A C16A C15A 107.1(4) . . ? O20A C16A H16C 110.3 . . ? C15A C16A H16C 110.3 . . ? O20A C16A H16D 110.3 . . ? C15A C16A H16D 110.3 . . ? H16C C16A H16D 108.5 . . ? C13B O20B C16B 109.1(6) . . ? O20B C13B C14B 108.0(8) . . ? O20B C13B H13E 110.1 . . ? C14B C13B H13E 110.1 . . ? O20B C13B H13F 110.1 . . ? C14B C13B H13F 110.1 . . ? H13E C13B H13F 108.4 . . ? C15B C14B C13B 104.8(7) . . ? C15B C14B H14C 110.8 . . ? C13B C14B H14C 110.8 . . ? C15B C14B H14D 110.8 . . ? C13B C14B H14D 110.8 . . ? H14C C14B H14D 108.9 . . ? C14B C15B C16B 102.5(7) . . ? C14B C15B H15C 111.3 . . ? C16B C15B H15C 111.3 . . ? C14B C15B H15D 111.3 . . ? C16B C15B H15D 111.3 . . ? H15C C15B H15D 109.2 . . ? O20B C16B C15B 105.7(6) . . ? O20B C16B H16E 110.6 . . ? C15B C16B H16E 110.6 . . ? O20B C16B H16F 110.6 . . ? C15B C16B H16F 110.6 . . ? H16E C16B H16F 108.7 . . ? O21 C117 C118 104.9(2) . . ? O21 C117 H1G 110.8 . . ? C118 C117 H1G 110.8 . . ? O21 C117 H1H 110.8 . . ? C118 C117 H1H 110.8 . . ? H1G C117 H1H 108.8 . . ? C117 C118 C119 101.5(2) . . ? C117 C118 H1E 111.5 . . ? C119 C118 H1E 111.5 . . ? C117 C118 H1F 111.5 . . ? C119 C118 H1F 111.5 . . ? H1E C118 H1F 109.3 . . ? C120 C119 C118 102.9(2) . . ? C120 C119 H11J 111.2 . . ? C118 C119 H11J 111.2 . . ? C120 C119 H11K 111.2 . . ? C118 C119 H11K 111.2 . . ? H11J C119 H11K 109.1 . . ? O21 C120 C119 107.4(2) . . ? O21 C120 H12A 110.2 . . ? C119 C120 H12A 110.2 . . ? O21 C120 H12B 110.2 . . ? C119 C120 H12B 110.2 . . ? H12A C120 H12B 108.5 . . ? O22 C121 C122 104.1(3) . . ? O22 C121 H12C 110.9 . . ? C122 C121 H12C 110.9 . . ? O22 C121 H12D 110.9 . . ? C122 C121 H12D 110.9 . . ? H12C C121 H12D 108.9 . . ? C123 C122 C121 104.3(3) . . ? C123 C122 H12E 110.9 . . ? C121 C122 H12E 110.9 . . ? C123 C122 H12F 110.9 . . ? C121 C122 H12F 110.9 . . ? H12E C122 H12F 108.9 . . ? C122 C123 C124 103.3(3) . . ? C122 C123 H12G 111.1 . . ? C124 C123 H12G 111.1 . . ? C122 C123 H12H 111.1 . . ? C124 C123 H12H 111.1 . . ? H12G C123 H12H 109.1 . . ? O22 C124 C123 106.8(3) . . ? O22 C124 H12I 110.4 . . ? C123 C124 H12I 110.4 . . ? O22 C124 H12J 110.4 . . ? C123 C124 H12J 110.4 . . ? H12I C124 H12J 108.6 . . ? O23 C125 C126 105.7(3) . . ? O23 C125 H12K 110.6 . . ? C126 C125 H12K 110.6 . . ? O23 C125 H12L 110.6 . . ? C126 C125 H12L 110.6 . . ? H12K C125 H12L 108.7 . . ? C125 C126 C127 101.1(3) . . ? C125 C126 H12M 111.5 . . ? C127 C126 H12M 111.5 . . ? C125 C126 H12N 111.5 . . ? C127 C126 H12N 111.5 . . ? H12M C126 H12N 109.4 . . ? C128 C127 C126 103.1(3) . . ? C128 C127 H12O 111.1 . . ? C126 C127 H12O 111.1 . . ? C128 C127 H12P 111.1 . . ? C126 C127 H12P 111.1 . . ? H12O C127 H12P 109.1 . . ? O23 C128 C127 107.7(3) . . ? O23 C128 H12Q 110.2 . . ? C127 C128 H12Q 110.2 . . ? O23 C128 H12R 110.2 . . ? C127 C128 H12R 110.2 . . ? H12Q C128 H12R 108.5 . . ? O24 C129 C130 108.6(5) . . ? O24 C129 H12S 110.0 . . ? C130 C129 H12S 110.0 . . ? O24 C129 H12T 110.0 . . ? C130 C129 H12T 110.0 . . ? H12S C129 H12T 108.3 . . ? C129 C130 C131 101.9(4) . . ? C129 C130 H13M 111.4 . . ? C131 C130 H13M 111.4 . . ? C129 C130 H13N 111.4 . . ? C131 C130 H13N 111.4 . . ? H13M C130 H13N 109.2 . . ? C130 C131 C132 103.1(4) . . ? C130 C131 H13O 111.1 . . ? C132 C131 H13O 111.1 . . ? C130 C131 H13P 111.1 . . ? C132 C131 H13P 111.1 . . ? H13O C131 H13P 109.1 . . ? O24 C132 C131 103.4(5) . . ? O24 C132 H13G 111.1 . . ? C131 C132 H13G 111.1 . . ? O24 C132 H13H 111.1 . . ? C131 C132 H13H 111.1 . . ? H13G C132 H13H 109.0 . . ? 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 C4 N1 N2 C5 117.8(3) . . . . ? C21 N5 N6 C22 103.0(3) . . . . ? C29 N7 N8 C30 98.8(3) . . . . ? C46 N11 N12 C47 76.6(3) . . . . ? C54 N13 N14 C55 -102.4(3) . . . . ? C71 N17 N18 C72 -81.5(3) . . . . ? C79 N19 N20 C80 -85.8(3) . . . . ? C96 N23 N24 C97 -123.2(3) . . . . ? C1 C2 C3 C4 -178.5(3) . . . . ? N2 N1 C4 O1 4.2(4) . . . . ? N2 N1 C4 C3 -177.2(2) . . . . ? C2 C3 C4 O1 -42.0(4) . . . . ? C2 C3 C4 N1 139.4(3) . . . . ? N1 N2 C5 O2 -2.6(4) . . . . ? N1 N2 C5 C6 179.3(2) . . . . ? C12 N3 C6 C7 0.7(3) . . . . ? C12 N3 C6 C5 178.5(2) . . . . ? O2 C5 C6 N3 178.8(2) . . . . ? N2 C5 C6 N3 -3.2(4) . . . . ? O2 C5 C6 C7 -3.9(4) . . . . ? N2 C5 C6 C7 174.2(2) . . . . ? N3 C6 C7 C9 -0.8(3) . . . . ? C5 C6 C7 C9 -178.5(2) . . . . ? N3 C6 C7 C8 176.5(2) . . . . ? C5 C6 C7 C8 -1.2(4) . . . . ? C6 C7 C9 C12 0.6(3) . . . . ? C8 C7 C9 C12 -176.8(2) . . . . ? C6 C7 C9 C10 175.9(2) . . . . ? C8 C7 C9 C10 -1.5(4) . . . . ? C12 C9 C10 C11 101.1(3) . . . . ? C7 C9 C10 C11 -73.3(3) . . . . ? C6 N3 C12 C9 -0.4(3) . . . . ? C6 N3 C12 C13 -174.1(2) . . . . ? C7 C9 C12 N3 -0.1(3) . . . . ? C10 C9 C12 N3 -175.5(2) . . . . ? C7 C9 C12 C13 173.2(2) . . . . ? C10 C9 C12 C13 -2.1(4) . . . . ? N3 C12 C13 C14 -23.7(3) . . . . ? C9 C12 C13 C14 163.9(2) . . . . ? C20 N4 C14 C15 0.8(3) . . . . ? C20 N4 C14 C13 176.0(2) . . . . ? C12 C13 C14 N4 95.6(3) . . . . ? C12 C13 C14 C15 -90.4(3) . . . . ? N4 C14 C15 C18 -0.7(3) . . . . ? C13 C14 C15 C18 -175.3(2) . . . . ? N4 C14 C15 C16 176.3(2) . . . . ? C13 C14 C15 C16 1.7(4) . . . . ? C14 C15 C16 C17' 104.4(6) . . . . ? C18 C15 C16 C17' -79.2(6) . . . . ? C14 C15 C16 C17 -82.1(4) . . . . ? C18 C15 C16 C17 94.3(4) . . . . ? C14 C15 C18 C20 0.4(3) . . . . ? C16 C15 C18 C20 -176.5(3) . . . . ? C14 C15 C18 C19 178.8(2) . . . . ? C16 C15 C18 C19 1.8(4) . . . . ? C15 C18 C20 N4 0.1(3) . . . . ? C19 C18 C20 N4 -178.3(2) . . . . ? C15 C18 C20 C21 174.2(2) . . . . ? C19 C18 C20 C21 -4.1(4) . . . . ? C14 N4 C20 C18 -0.5(3) . . . . ? C14 N4 C20 C21 -175.2(2) . . . . ? N6 N5 C21 O3 0.5(3) . . . . ? N6 N5 C21 C20 179.8(2) . . . . ? C18 C20 C21 O3 13.4(4) . . . . ? N4 C20 C21 O3 -173.2(2) . . . . ? C18 C20 C21 N5 -165.9(2) . . . . ? N4 C20 C21 N5 7.6(3) . . . . ? N5 N6 C22 O4 -0.4(4) . . . . ? N5 N6 C22 C23 179.0(2) . . . . ? O4 C22 C23 C24 55.1(3) . . . . ? N6 C22 C23 C24 -124.3(2) . . . . ? C22 C23 C24 C25 -179.9(2) . . . . ? C26 C27 C28 C29 -172.5(2) . . . . ? N8 N7 C29 O5 6.3(4) . . . . ? N8 N7 C29 C28 -175.5(2) . . . . ? C27 C28 C29 O5 -20.1(3) . . . . ? C27 C28 C29 N7 161.7(2) . . . . ? N7 N8 C30 O6 -10.6(3) . . . . ? N7 N8 C30 C31 166.6(2) . . . . ? C37 N9 C31 C32 0.1(3) . . . . ? C37 N9 C31 C30 -178.0(2) . . . . ? O6 C30 C31 N9 164.3(2) . . . . ? N8 C30 C31 N9 -12.9(3) . . . . ? O6 C30 C31 C32 -13.4(4) . . . . ? N8 C30 C31 C32 169.4(2) . . . . ? N9 C31 C32 C34 0.7(3) . . . . ? C30 C31 C32 C34 178.7(2) . . . . ? N9 C31 C32 C33 -176.3(2) . . . . ? C30 C31 C32 C33 1.6(4) . . . . ? C31 C32 C34 C37 -1.3(3) . . . . ? C33 C32 C34 C37 175.7(2) . . . . ? C31 C32 C34 C35 179.6(2) . . . . ? C33 C32 C34 C35 -3.4(4) . . . . ? C37 C34 C35 C36 80.8(3) . . . . ? C32 C34 C35 C36 -100.3(3) . . . . ? C31 N9 C37 C34 -1.0(3) . . . . ? C31 N9 C37 C38 176.9(2) . . . . ? C32 C34 C37 N9 1.4(3) . . . . ? C35 C34 C37 N9 -179.4(2) . . . . ? C32 C34 C37 C38 -176.2(2) . . . . ? C35 C34 C37 C38 3.0(4) . . . . ? N9 C37 C38 C39 85.9(3) . . . . ? C34 C37 C38 C39 -96.8(3) . . . . ? C45 N10 C39 C40 0.2(3) . . . . ? C45 N10 C39 C38 179.1(2) . . . . ? C37 C38 C39 N10 7.1(4) . . . . ? C37 C38 C39 C40 -174.2(2) . . . . ? N10 C39 C40 C43 -0.3(3) . . . . ? C38 C39 C40 C43 -179.2(2) . . . . ? N10 C39 C40 C41 -175.8(2) . . . . ? C38 C39 C40 C41 5.3(4) . . . . ? C39 C40 C41 C42 92.3(3) . . . . ? C43 C40 C41 C42 -82.4(3) . . . . ? C39 C40 C43 C45 0.3(3) . . . . ? C41 C40 C43 C45 175.7(2) . . . . ? C39 C40 C43 C44 -178.5(3) . . . . ? C41 C40 C43 C44 -3.1(4) . . . . ? C39 N10 C45 C43 0.0(3) . . . . ? C39 N10 C45 C46 179.0(2) . . . . ? C40 C43 C45 N10 -0.2(3) . . . . ? C44 C43 C45 N10 178.6(3) . . . . ? C40 C43 C45 C46 -179.2(2) . . . . ? C44 C43 C45 C46 -0.4(4) . . . . ? N12 N11 C46 O7 7.7(3) . . . . ? N12 N11 C46 C45 -174.0(2) . . . . ? N10 C45 C46 O7 -176.8(2) . . . . ? C43 C45 C46 O7 2.1(4) . . . . ? N10 C45 C46 N11 4.9(4) . . . . ? C43 C45 C46 N11 -176.2(2) . . . . ? N11 N12 C47 O8 10.7(4) . . . . ? N11 N12 C47 C48 -170.8(2) . . . . ? O8 C47 C48 C49 -68.5(3) . . . . ? N12 C47 C48 C49 113.0(3) . . . . ? C47 C48 C49 C50 175.6(2) . . . . ? C51 C52 C53 C54 69.7(3) . . . . ? N14 N13 C54 O9 0.2(3) . . . . ? N14 N13 C54 C53 179.7(2) . . . . ? C52 C53 C54 O9 -164.6(2) . . . . ? C52 C53 C54 N13 15.9(3) . . . . ? N13 N14 C55 O10 0.5(3) . . . . ? N13 N14 C55 C56 -176.7(2) . . . . ? C62 N15 C56 C57 -0.4(3) . . . . ? C62 N15 C56 C55 177.9(2) . . . . ? O10 C55 C56 N15 -173.6(2) . . . . ? N14 C55 C56 N15 3.6(3) . . . . ? O10 C55 C56 C57 4.3(4) . . . . ? N14 C55 C56 C57 -178.5(2) . . . . ? N15 C56 C57 C59 0.0(3) . . . . ? C55 C56 C57 C59 -178.1(2) . . . . ? N15 C56 C57 C58 175.8(2) . . . . ? C55 C56 C57 C58 -2.4(4) . . . . ? C56 C57 C59 C62 0.3(3) . . . . ? C58 C57 C59 C62 -175.4(2) . . . . ? C56 C57 C59 C60 179.5(2) . . . . ? C58 C57 C59 C60 3.7(4) . . . . ? C62 C59 C60 C61 -86.5(3) . . . . ? C57 C59 C60 C61 94.5(3) . . . . ? C56 N15 C62 C59 0.6(3) . . . . ? C56 N15 C62 C63 -175.9(2) . . . . ? C57 C59 C62 N15 -0.5(3) . . . . ? C60 C59 C62 N15 -179.7(2) . . . . ? C57 C59 C62 C63 175.4(2) . . . . ? C60 C59 C62 C63 -3.7(4) . . . . ? N15 C62 C63 C64 -84.3(3) . . . . ? C59 C62 C63 C64 100.1(3) . . . . ? C70 N16 C64 C65 -0.5(3) . . . . ? C70 N16 C64 C63 176.8(2) . . . . ? C62 C63 C64 N16 -2.8(3) . . . . ? C62 C63 C64 C65 174.0(2) . . . . ? N16 C64 C65 C68 0.9(3) . . . . ? C63 C64 C65 C68 -176.3(2) . . . . ? N16 C64 C65 C66 179.3(2) . . . . ? C63 C64 C65 C66 2.2(4) . . . . ? C64 C65 C66 C67 113.6(3) . . . . ? C68 C65 C66 C67 -68.3(4) . . . . ? C64 C65 C68 C70 -0.9(3) . . . . ? C66 C65 C68 C70 -179.3(2) . . . . ? C64 C65 C68 C69 177.6(2) . . . . ? C66 C65 C68 C69 -0.8(4) . . . . ? C65 C68 C70 N16 0.6(3) . . . . ? C69 C68 C70 N16 -177.9(2) . . . . ? C65 C68 C70 C71 -177.8(2) . . . . ? C69 C68 C70 C71 3.7(4) . . . . ? C64 N16 C70 C68 0.0(3) . . . . ? C64 N16 C70 C71 178.4(2) . . . . ? N18 N17 C71 O11 -9.0(3) . . . . ? N18 N17 C71 C70 174.0(2) . . . . ? C68 C70 C71 O11 -3.5(4) . . . . ? N16 C70 C71 O11 178.4(2) . . . . ? C68 C70 C71 N17 173.5(2) . . . . ? N16 C70 C71 N17 -4.6(4) . . . . ? N17 N18 C72 O12 -9.3(4) . . . . ? N17 N18 C72 C73 170.0(2) . . . . ? O12 C72 C73 C74 74.8(3) . . . . ? N18 C72 C73 C74 -104.5(3) . . . . ? C72 C73 C74 C75 -179.7(3) . . . . ? C76 C77 C78 C79 179.5(3) . . . . ? N20 N19 C79 O13 -6.6(4) . . . . ? N20 N19 C79 C78 173.4(2) . . . . ? C77 C78 C79 O13 81.8(3) . . . . ? C77 C78 C79 N19 -98.2(3) . . . . ? N19 N20 C80 O14 -6.9(3) . . . . ? N19 N20 C80 C81 175.5(2) . . . . ? C87 N21 C81 C82 -0.1(3) . . . . ? C87 N21 C81 C80 178.7(2) . . . . ? O14 C80 C81 C82 2.6(4) . . . . ? N20 C80 C81 C82 -179.7(2) . . . . ? O14 C80 C81 N21 -175.9(2) . . . . ? N20 C80 C81 N21 1.7(3) . . . . ? N21 C81 C82 C84 0.4(3) . . . . ? C80 C81 C82 C84 -178.4(2) . . . . ? N21 C81 C82 C83 -177.5(2) . . . . ? C80 C81 C82 C83 3.7(4) . . . . ? C81 C82 C84 C87 -0.5(3) . . . . ? C83 C82 C84 C87 177.4(2) . . . . ? C81 C82 C84 C85 177.7(2) . . . . ? C83 C82 C84 C85 -4.4(4) . . . . ? C87 C84 C85 C86 99.8(3) . . . . ? C82 C84 C85 C86 -78.0(3) . . . . ? C81 N21 C87 C84 -0.2(3) . . . . ? C81 N21 C87 C88 -179.0(2) . . . . ? C82 C84 C87 N21 0.4(3) . . . . ? C85 C84 C87 N21 -177.8(2) . . . . ? C82 C84 C87 C88 179.2(2) . . . . ? C85 C84 C87 C88 1.0(4) . . . . ? N21 C87 C88 C89 -10.9(4) . . . . ? C84 C87 C88 C89 170.5(2) . . . . ? C95 N22 C89 C90 0.2(3) . . . . ? C95 N22 C89 C88 -177.3(2) . . . . ? C87 C88 C89 N22 -80.1(3) . . . . ? C87 C88 C89 C90 103.1(3) . . . . ? N22 C89 C90 C93 -0.8(3) . . . . ? C88 C89 C90 C93 176.3(2) . . . . ? N22 C89 C90 C91 179.3(2) . . . . ? C88 C89 C90 C91 -3.6(4) . . . . ? C89 C90 C91 C92 -101.0(3) . . . . ? C93 C90 C91 C92 79.1(3) . . . . ? C89 C90 C93 C95 1.1(3) . . . . ? C91 C90 C93 C95 -179.0(2) . . . . ? C89 C90 C93 C94 -177.3(2) . . . . ? C91 C90 C93 C94 2.6(4) . . . . ? C89 N22 C95 C93 0.5(3) . . . . ? C89 N22 C95 C96 -179.7(2) . . . . ? C90 C93 C95 N22 -1.0(3) . . . . ? C94 C93 C95 N22 177.4(2) . . . . ? C90 C93 C95 C96 179.2(2) . . . . ? C94 C93 C95 C96 -2.4(4) . . . . ? N24 N23 C96 O15 6.3(3) . . . . ? N24 N23 C96 C95 -171.2(2) . . . . ? N22 C95 C96 O15 -168.9(2) . . . . ? C93 C95 C96 O15 10.8(4) . . . . ? N22 C95 C96 N23 8.6(3) . . . . ? C93 C95 C96 N23 -171.6(2) . . . . ? N23 N24 C97 O16 4.5(4) . . . . ? N23 N24 C97 C98 -174.5(2) . . . . ? O16 C97 C98 C99 44.3(3) . . . . ? N24 C97 C98 C99 -136.8(2) . . . . ? C97 C98 C99 C100 175.6(2) . . . . ? C104 O17 C101 C102 8.9(3) . . . . ? O17 C101 C102 C103 16.6(3) . . . . ? C101 C102 C103 C104 -34.3(3) . . . . ? C101 O17 C104 C103 -31.4(3) . . . . ? C102 C103 C104 O17 40.8(3) . . . . ? C108 O18 C105 C106 -19.8(5) . . . . ? O18 C105 C106 C107 2.2(5) . . . . ? C105 C106 C107 C108 15.0(4) . . . . ? C105 O18 C108 C107 28.9(4) . . . . ? C106 C107 C108 O18 -27.0(3) . . . . ? C111 O19 C109 C110 40.9(4) . . . . ? O19 C109 C110 C112 -25.0(4) . . . . ? C109 O19 C111 C112 -40.4(5) . . . . ? O19 C111 C112 C110 23.4(4) . . . . ? C109 C110 C112 C111 0.8(4) . . . . ? C16A O20A C13A C14A -18.2(7) . . . . ? O20A C13A C14A C15A 33.2(7) . . . . ? C13A C14A C15A C16A -34.1(7) . . . . ? C13A O20A C16A C15A -3.8(8) . . . . ? C14A C15A C16A O20A 24.7(7) . . . . ? C16B O20B C13B C14B 14.1(16) . . . . ? O20B C13B C14B C15B 6.6(17) . . . . ? C13B C14B C15B C16B -22.5(14) . . . . ? C13B O20B C16B C15B -28.8(13) . . . . ? C14B C15B C16B O20B 31.6(12) . . . . ? C120 O21 C117 C118 28.3(3) . . . . ? O21 C117 C118 C119 -39.3(3) . . . . ? C117 C118 C119 C120 34.9(3) . . . . ? C117 O21 C120 C119 -5.4(3) . . . . ? C118 C119 C120 O21 -19.0(3) . . . . ? C124 O22 C121 C122 -14.0(3) . . . . ? O22 C121 C122 C123 30.9(4) . . . . ? C121 C122 C123 C124 -35.5(5) . . . . ? C121 O22 C124 C123 -8.0(3) . . . . ? C122 C123 C124 O22 27.3(4) . . . . ? C128 O23 C125 C126 -27.9(3) . . . . ? O23 C125 C126 C127 37.9(3) . . . . ? C125 C126 C127 C128 -32.7(3) . . . . ? C125 O23 C128 C127 6.2(3) . . . . ? C126 C127 C128 O23 17.6(3) . . . . ? C132 O24 C129 C130 36.3(5) . . . . ? O24 C129 C130 C131 -12.7(5) . . . . ? C129 C130 C131 C132 -13.0(5) . . . . ? C129 O24 C132 C131 -43.8(5) . . . . ? C130 C131 C132 O24 35.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.784 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.059