# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email hn.gopi@iiserpune.ac.in _publ_contact_author_name 'Gopi, Hosahudya' loop_ _publ_author_name 'Gopi, Hosahudya' 'Bandyopadhyay, Anupam' 'Jadhav, Sandip' data_P1 _database_code_depnum_ccdc_archive 'CCDC 878071' #TrackingRef '- All peptide.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic 'Alpha gamma helix' _chemical_name_common 'Tetra peptide' _chemical_formula_moiety 'C39 H58 N4 O7, (C H4 O)' _chemical_formula_sum 'C40 H62 N4 O8' _chemical_compound_source synthesis _exptl_crystal_recrystallization_method methanol _chemical_melting_point ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colorless _diffrn_ambient_temperature 100(2) _diffrn_ambient_pressure 101.325 _chemical_formula_weight 726.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_int_tables_number 4 _chemical_absolute_configuration syn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.132(2) _cell_length_b 20.141(4) _cell_length_c 21.010(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.384(5) _cell_angle_gamma 90.00 _cell_volume 4230.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'graphite monochromator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42078 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.28 _reflns_number_total 14908 _reflns_number_gt 6991 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0904P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.7(10) _refine_ls_number_reflns 14908 _refine_ls_number_parameters 952 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 2.496 _refine_ls_shift/su_mean 0.051 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 0.2149(3) 0.86739(13) 0.43139(14) 0.0659(8) Uani 1 1 d . . . O2 O 0.3222(3) 0.76895(13) 0.42686(14) 0.0637(7) Uani 1 1 d . . . O3 O 0.6627(3) 0.73301(12) 0.50960(13) 0.0594(7) Uani 1 1 d . . . O4 O 0.3688(3) 0.57548(15) 0.57364(14) 0.0779(9) Uani 1 1 d . . . O5 O 0.5832(3) 0.49148(12) 0.48090(13) 0.0657(8) Uani 1 1 d . . . O6 O 0.7104(8) 0.4740(2) 0.7506(2) 0.182(3) Uani 1 1 d . . . O7 O 0.6560(4) 0.57913(18) 0.73648(15) 0.0907(10) Uani 1 1 d . . . O8 O 0.7889(3) 0.97256(13) 1.03211(14) 0.0619(7) Uani 1 1 d . . . O9 O 0.6825(3) 0.87806(13) 1.05404(13) 0.0624(7) Uani 1 1 d . . . O10 O 0.3455(3) 0.83315(12) 0.98936(13) 0.0602(7) Uani 1 1 d . . . O11 O 0.6142(3) 0.66308(14) 0.94447(15) 0.0764(9) Uani 1 1 d . . . O12 O 0.4296(3) 0.59618(12) 1.05916(13) 0.0630(7) Uani 1 1 d . . . O13 O 0.2671(6) 0.6683(2) 0.78246(19) 0.1374(17) Uani 1 1 d . . . O14 O 0.2893(4) 0.55988(17) 0.79080(15) 0.0983(12) Uani 1 1 d . . . O15 O 0.4127(8) 0.4911(2) 0.1407(2) 0.136(2) Uani 1 1 d . . . H15A H 0.4289 0.5271 0.1255 0.205 Uiso 1 1 calc R . . O16 O 0.7317(14) 0.4131(8) 0.3743(6) 0.313(5) Uiso 1 1 d . . . H16A H 0.8018 0.4079 0.3994 0.469 Uiso 1 1 calc R . . N1 N 0.4342(3) 0.86394(15) 0.45888(15) 0.0515(8) Uani 1 1 d . . . H1 H 0.4251 0.9051 0.4680 0.062 Uiso 1 1 calc R . . N2 N 0.5223(3) 0.78579(15) 0.56587(15) 0.0547(8) Uani 1 1 d . . . H2 H 0.4704 0.8195 0.5663 0.066 Uiso 1 1 calc R . . N3 N 0.3967(3) 0.63988(16) 0.48993(16) 0.0594(8) Uani 1 1 d . . . H3 H 0.3960 0.6796 0.4747 0.071 Uiso 1 1 calc R . . N4 N 0.6652(3) 0.59039(15) 0.51771(15) 0.0558(8) Uani 1 1 d . . . H4 H 0.6518 0.6326 0.5179 0.067 Uiso 1 1 calc R . . N5 N 0.5699(3) 0.96946(14) 1.01225(14) 0.0501(8) Uani 1 1 d . . . H5 H 0.5778 1.0087 0.9971 0.060 Uiso 1 1 calc R . . N6 N 0.4697(3) 0.87591(15) 0.91940(14) 0.0569(8) Uani 1 1 d . . . H6 H 0.5190 0.9087 0.9115 0.068 Uiso 1 1 calc R . . N7 N 0.6120(3) 0.73860(15) 1.02289(15) 0.0514(8) Uani 1 1 d . . . H7 H 0.6201 0.7797 1.0339 0.062 Uiso 1 1 calc R . . N8 N 0.3475(3) 0.69074(15) 1.00954(15) 0.0508(8) Uani 1 1 d . . . H8 H 0.3649 0.7313 1.0010 0.061 Uiso 1 1 calc R . . C1 C 0.0794(5) 0.8414(3) 0.4091(3) 0.0789(14) Uani 1 1 d . . . C2 C -0.0049(5) 0.9032(3) 0.4109(3) 0.1046(19) Uani 1 1 d . . . H2A H -0.0975 0.8923 0.3976 0.157 Uiso 1 1 calc R . . H2B H 0.0216 0.9360 0.3823 0.157 Uiso 1 1 calc R . . H2C H 0.0079 0.9205 0.4541 0.157 Uiso 1 1 calc R . . C3 C 0.0448(6) 0.7916(3) 0.4579(4) 0.123(2) Uani 1 1 d . . . H3A H 0.0917 0.7508 0.4539 0.184 Uiso 1 1 calc R . . H3B H -0.0498 0.7835 0.4502 0.184 Uiso 1 1 calc R . . H3C H 0.0706 0.8091 0.5006 0.184 Uiso 1 1 calc R . . C4 C 0.0735(8) 0.8140(5) 0.3429(3) 0.151(3) Uani 1 1 d . . . H4A H 0.1243 0.7736 0.3450 0.227 Uiso 1 1 calc R . . H4B H 0.1104 0.8457 0.3165 0.227 Uiso 1 1 calc R . . H4C H -0.0178 0.8051 0.3246 0.227 Uiso 1 1 calc R . . C5 C 0.3235(4) 0.8281(2) 0.43822(19) 0.0559(10) Uani 1 1 d . . . C6 C 0.5691(4) 0.83613(17) 0.46648(19) 0.0502(9) Uani 1 1 d . . . C7 C 0.5990(5) 0.8119(2) 0.4012(2) 0.0667(12) Uani 1 1 d . . . H7A H 0.5888 0.8481 0.3710 0.100 Uiso 1 1 calc R . . H7B H 0.5379 0.7770 0.3853 0.100 Uiso 1 1 calc R . . H7C H 0.6891 0.7954 0.4062 0.100 Uiso 1 1 calc R . . C8 C 0.6646(4) 0.8921(2) 0.4914(2) 0.0658(11) Uani 1 1 d . . . H8A H 0.6434 0.9083 0.5315 0.099 Uiso 1 1 calc R . . H8B H 0.6559 0.9275 0.4604 0.099 Uiso 1 1 calc R . . H8C H 0.7548 0.8758 0.4981 0.099 Uiso 1 1 calc R . . C9 C 0.5870(4) 0.77936(18) 0.51597(18) 0.0478(9) Uani 1 1 d . . . C10 C 0.5334(5) 0.7394(2) 0.62012(18) 0.0627(11) Uani 1 1 d . . . H10 H 0.5815 0.6999 0.6091 0.075 Uiso 1 1 calc R . . C11 C 0.6167(6) 0.7720(3) 0.6805(2) 0.0869(15) Uani 1 1 d . . . H11A H 0.5765 0.8144 0.6880 0.104 Uiso 1 1 calc R . . H11B H 0.6113 0.7440 0.7176 0.104 Uiso 1 1 calc R . . C12 C 0.7582(7) 0.7829(3) 0.6765(2) 0.0861(16) Uani 1 1 d . . . C13 C 0.8069(7) 0.8418(3) 0.6538(3) 0.114(2) Uani 1 1 d . . . H13 H 0.7479 0.8770 0.6434 0.136 Uiso 1 1 calc R . . C14 C 0.9384(9) 0.8501(4) 0.6460(5) 0.154(3) Uani 1 1 d . . . H14 H 0.9675 0.8902 0.6312 0.185 Uiso 1 1 calc R . . C15 C 1.0261(9) 0.7976(7) 0.6608(5) 0.162(3) Uani 1 1 d . . . H15 H 1.1139 0.8017 0.6536 0.195 Uiso 1 1 calc R . . C16 C 0.9857(12) 0.7406(5) 0.6855(5) 0.155(4) Uani 1 1 d . . . H16 H 1.0464 0.7067 0.6984 0.186 Uiso 1 1 calc R . . C17 C 0.8559(10) 0.7340(3) 0.6910(3) 0.120(2) Uani 1 1 d . . . H17 H 0.8291 0.6934 0.7057 0.144 Uiso 1 1 calc R . . C18 C 0.3994(5) 0.7178(2) 0.6339(2) 0.0762(13) Uani 1 1 d . . . H18A H 0.3570 0.7555 0.6511 0.091 Uiso 1 1 calc R . . H18B H 0.4132 0.6841 0.6673 0.091 Uiso 1 1 calc R . . C19 C 0.3040(5) 0.6904(2) 0.5765(2) 0.0726(13) Uani 1 1 d . . . H19A H 0.2200 0.6790 0.5903 0.087 Uiso 1 1 calc R . . H19B H 0.2856 0.7248 0.5439 0.087 Uiso 1 1 calc R . . C20 C 0.3575(4) 0.6302(2) 0.5470(2) 0.0640(11) Uani 1 1 d . . . C21 C 0.4406(4) 0.58575(19) 0.45266(18) 0.0558(10) Uani 1 1 d . . . H21 H 0.3696 0.5522 0.4458 0.067 Uiso 1 1 calc R . . C22 C 0.4596(5) 0.6132(2) 0.38699(19) 0.0649(11) Uani 1 1 d . . . H22A H 0.3757 0.6330 0.3669 0.078 Uiso 1 1 calc R . . H22B H 0.5253 0.6486 0.3941 0.078 Uiso 1 1 calc R . . C23 C 0.5031(5) 0.5647(2) 0.3399(2) 0.0712(12) Uani 1 1 d . . . H23 H 0.5867 0.5438 0.3603 0.085 Uiso 1 1 calc R . . C24 C 0.5292(6) 0.6008(3) 0.2798(2) 0.0932(16) Uani 1 1 d . . . H24A H 0.5949 0.6349 0.2916 0.140 Uiso 1 1 calc R . . H24B H 0.4476 0.6206 0.2585 0.140 Uiso 1 1 calc R . . H24C H 0.5615 0.5699 0.2512 0.140 Uiso 1 1 calc R . . C25 C 0.3980(6) 0.5096(3) 0.3207(2) 0.0988(18) Uani 1 1 d . . . H25A H 0.3140 0.5294 0.3026 0.148 Uiso 1 1 calc R . . H25B H 0.3871 0.4843 0.3583 0.148 Uiso 1 1 calc R . . H25C H 0.4275 0.4808 0.2894 0.148 Uiso 1 1 calc R . . C26 C 0.5693(4) 0.55240(19) 0.48570(18) 0.0544(10) Uani 1 1 d . . . C27 C 0.7919(4) 0.5651(2) 0.55257(19) 0.0593(10) Uani 1 1 d . . . H27 H 0.8046 0.5197 0.5380 0.071 Uiso 1 1 calc R . . C28 C 0.9079(5) 0.6077(2) 0.5380(2) 0.0728(12) Uani 1 1 d . . . H28A H 0.8865 0.6541 0.5434 0.087 Uiso 1 1 calc R . . H28B H 0.9870 0.5973 0.5691 0.087 Uiso 1 1 calc R . . C29 C 0.9392(5) 0.5979(2) 0.4717(2) 0.0674(12) Uani 1 1 d . . . C30 C 0.8729(6) 0.6319(3) 0.4208(3) 0.0986(17) Uani 1 1 d . . . H30 H 0.8078 0.6626 0.4274 0.118 Uiso 1 1 calc R . . C31 C 0.9002(9) 0.6220(6) 0.3599(4) 0.157(4) Uani 1 1 d . . . H31 H 0.8542 0.6458 0.3253 0.188 Uiso 1 1 calc R . . C32 C 0.9975(12) 0.5760(8) 0.3501(4) 0.181(6) Uani 1 1 d . . . H32 H 1.0145 0.5677 0.3086 0.218 Uiso 1 1 calc R . . C33 C 1.0669(8) 0.5434(4) 0.4010(5) 0.139(3) Uani 1 1 d . . . H33 H 1.1330 0.5132 0.3945 0.167 Uiso 1 1 calc R . . C34 C 1.0407(5) 0.5544(3) 0.4619(3) 0.0924(16) Uani 1 1 d . . . H34 H 1.0909 0.5328 0.4968 0.111 Uiso 1 1 calc R . . C35 C 0.7880(5) 0.5635(2) 0.6249(2) 0.0696(12) Uani 1 1 d . . . H35A H 0.8746 0.5491 0.6472 0.083 Uiso 1 1 calc R . . H35B H 0.7732 0.6083 0.6392 0.083 Uiso 1 1 calc R . . C36 C 0.6812(5) 0.5185(2) 0.6444(2) 0.0753(13) Uani 1 1 d . . . H36A H 0.5936 0.5328 0.6232 0.090 Uiso 1 1 calc R . . H36B H 0.6952 0.4733 0.6309 0.090 Uiso 1 1 calc R . . C37 C 0.6867(6) 0.5204(3) 0.7154(2) 0.0897(16) Uani 1 1 d . . . C38 C 0.6648(8) 0.5890(4) 0.8055(3) 0.116(2) Uani 1 1 d . . . H38A H 0.6548 0.5467 0.8263 0.139 Uiso 1 1 calc R . . H38B H 0.5933 0.6181 0.8138 0.139 Uiso 1 1 calc R . . C39 C 0.7952(8) 0.6186(4) 0.8322(3) 0.128(3) Uani 1 1 d . . . H39A H 0.8039 0.6609 0.8122 0.193 Uiso 1 1 calc R . . H39B H 0.8658 0.5897 0.8238 0.193 Uiso 1 1 calc R . . H39C H 0.8008 0.6244 0.8779 0.193 Uiso 1 1 calc R . . C40 C 0.9246(4) 0.9476(2) 1.0572(2) 0.0692(12) Uani 1 1 d . . . C41 C 0.9566(6) 0.8888(3) 1.0179(3) 0.1020(18) Uani 1 1 d . . . H41A H 0.9144 0.8498 1.0316 0.153 Uiso 1 1 calc R . . H41B H 1.0517 0.8823 1.0242 0.153 Uiso 1 1 calc R . . H41C H 0.9241 0.8969 0.9731 0.153 Uiso 1 1 calc R . . C42 C 1.0100(5) 1.0063(3) 1.0449(3) 0.1008(18) Uani 1 1 d . . . H42A H 1.1013 0.9981 1.0638 0.151 Uiso 1 1 calc R . . H42B H 0.9785 1.0454 1.0638 0.151 Uiso 1 1 calc R . . H42C H 1.0043 1.0127 0.9992 0.151 Uiso 1 1 calc R . . C43 C 0.9367(6) 0.9341(3) 1.1275(3) 0.1079(19) Uani 1 1 d . . . H43A H 0.8815 0.8968 1.1342 0.162 Uiso 1 1 calc R . . H43B H 0.9082 0.9724 1.1488 0.162 Uiso 1 1 calc R . . H43C H 1.0282 0.9243 1.1448 0.162 Uiso 1 1 calc R . . C44 C 0.6797(4) 0.93539(19) 1.03474(19) 0.0540(10) Uani 1 1 d . . . C45 C 0.4357(4) 0.94240(18) 1.01239(19) 0.0524(10) Uani 1 1 d . . . C46 C 0.3356(4) 0.9939(2) 0.9795(2) 0.0716(13) Uani 1 1 d . . . H46A H 0.3621 1.0080 0.9398 0.107 Uiso 1 1 calc R . . H46B H 0.3341 1.0315 1.0075 0.107 Uiso 1 1 calc R . . H46C H 0.2480 0.9745 0.9707 0.107 Uiso 1 1 calc R . . C47 C 0.4117(5) 0.9297(2) 1.0807(2) 0.0712(13) Uani 1 1 d . . . H47A H 0.4323 0.9691 1.1061 0.107 Uiso 1 1 calc R . . H47B H 0.4679 0.8940 1.0992 0.107 Uiso 1 1 calc R . . H47C H 0.3196 0.9181 1.0800 0.107 Uiso 1 1 calc R . . C48 C 0.4146(4) 0.87797(18) 0.97278(18) 0.0487(9) Uani 1 1 d . . . C49 C 0.4507(5) 0.82096(19) 0.87382(18) 0.0621(11) Uani 1 1 d . . . H49 H 0.3986 0.7867 0.8917 0.074 Uiso 1 1 calc R . . C50 C 0.3700(6) 0.8437(3) 0.8090(2) 0.0880(16) Uani 1 1 d . . . H50A H 0.4268 0.8719 0.7876 0.106 Uiso 1 1 calc R . . H50B H 0.3479 0.8048 0.7821 0.106 Uiso 1 1 calc R . . C51 C 0.2444(8) 0.8802(3) 0.8132(2) 0.0938(18) Uani 1 1 d . . . C52 C 0.1335(10) 0.8464(4) 0.8222(3) 0.134(3) Uani 1 1 d . . . H52 H 0.1368 0.8004 0.8254 0.161 Uiso 1 1 calc R . . C53 C 0.0140(12) 0.8794(7) 0.8269(5) 0.176(4) Uani 1 1 d . . . H53 H -0.0623 0.8557 0.8323 0.211 Uiso 1 1 calc R . . C54 C 0.0120(14) 0.9470(9) 0.8233(6) 0.188(6) Uani 1 1 d . . . H54 H -0.0667 0.9696 0.8265 0.226 Uiso 1 1 calc R . . C55 C 0.1175(16) 0.9805(6) 0.8156(6) 0.195(6) Uani 1 1 d . . . H55 H 0.1143 1.0267 0.8143 0.234 Uiso 1 1 calc R . . C56 C 0.2354(10) 0.9478(3) 0.8093(4) 0.148(3) Uani 1 1 d . . . H56 H 0.3094 0.9723 0.8023 0.177 Uiso 1 1 calc R . . C57 C 0.5825(5) 0.7901(2) 0.8637(2) 0.0765(14) Uani 1 1 d . . . H57A H 0.5631 0.7493 0.8394 0.092 Uiso 1 1 calc R . . H57B H 0.6255 0.8201 0.8373 0.092 Uiso 1 1 calc R . . C58 C 0.6813(5) 0.7744(2) 0.9242(2) 0.0686(12) Uani 1 1 d . . . H58A H 0.7654 0.7607 0.9118 0.082 Uiso 1 1 calc R . . H58B H 0.6978 0.8144 0.9499 0.082 Uiso 1 1 calc R . . C59 C 0.6336(4) 0.72043(19) 0.9649(2) 0.0583(10) Uani 1 1 d . . . C60 C 0.5747(4) 0.69023(18) 1.06839(18) 0.0501(9) Uani 1 1 d . . . H60 H 0.6455 0.6567 1.0762 0.060 Uiso 1 1 calc R . . C61 C 0.5658(4) 0.7243(2) 1.13233(18) 0.0614(10) Uani 1 1 d . . . H61A H 0.4981 0.7587 1.1244 0.074 Uiso 1 1 calc R . . H61B H 0.5353 0.6920 1.1609 0.074 Uiso 1 1 calc R . . C62 C 0.6940(5) 0.7555(3) 1.1672(2) 0.0842(15) Uani 1 1 d . . . H62 H 0.7236 0.7891 1.1389 0.101 Uiso 1 1 calc R . . C63 C 0.8039(6) 0.7048(4) 1.1831(3) 0.132(3) Uani 1 1 d . . . H63A H 0.8239 0.6857 1.1439 0.197 Uiso 1 1 calc R . . H63B H 0.7752 0.6705 1.2094 0.197 Uiso 1 1 calc R . . H63C H 0.8825 0.7259 1.2060 0.197 Uiso 1 1 calc R . . C64 C 0.6656(8) 0.7899(4) 1.2278(3) 0.131(2) Uani 1 1 d . . . H64A H 0.7442 0.8132 1.2478 0.197 Uiso 1 1 calc R . . H64B H 0.6412 0.7575 1.2573 0.197 Uiso 1 1 calc R . . H64C H 0.5935 0.8209 1.2167 0.197 Uiso 1 1 calc R . . C65 C 0.4442(4) 0.65513(18) 1.04377(18) 0.0513(9) Uani 1 1 d . . . C66 C 0.2154(4) 0.66599(19) 0.98570(19) 0.0578(10) Uani 1 1 d . . . H66 H 0.2109 0.6200 1.0005 0.069 Uiso 1 1 calc R . . C67 C 0.1110(4) 0.7062(2) 1.0141(2) 0.0706(12) Uani 1 1 d . . . H67A H 0.1117 0.7516 0.9988 0.085 Uiso 1 1 calc R . . H67B H 0.0230 0.6878 0.9989 0.085 Uiso 1 1 calc R . . C68 C 0.1357(5) 0.7062(2) 1.0859(3) 0.0759(13) Uani 1 1 d . . . C69 C 0.1130(6) 0.6497(3) 1.1205(3) 0.1050(19) Uani 1 1 d . . . H69 H 0.0775 0.6119 1.0988 0.126 Uiso 1 1 calc R . . C70 C 0.1429(9) 0.6497(5) 1.1863(4) 0.141(3) Uani 1 1 d . . . H70 H 0.1285 0.6113 1.2087 0.169 Uiso 1 1 calc R . . C71 C 0.1914(8) 0.7026(6) 1.2190(3) 0.128(3) Uani 1 1 d . . . H71 H 0.2073 0.7015 1.2639 0.154 Uiso 1 1 calc R . . C72 C 0.2188(7) 0.7596(5) 1.1871(4) 0.119(2) Uani 1 1 d . . . H72 H 0.2565 0.7965 1.2099 0.143 Uiso 1 1 calc R . . C73 C 0.1885(6) 0.7606(3) 1.1201(3) 0.0937(16) Uani 1 1 d . . . H73 H 0.2044 0.7991 1.0980 0.112 Uiso 1 1 calc R . . C74 C 0.1929(4) 0.6652(2) 0.9129(2) 0.0677(11) Uani 1 1 d . . . H74A H 0.2051 0.7098 0.8973 0.081 Uiso 1 1 calc R . . H74B H 0.1013 0.6521 0.8971 0.081 Uiso 1 1 calc R . . C75 C 0.2863(5) 0.6186(2) 0.88562(19) 0.0681(12) Uani 1 1 d . . . H75A H 0.3776 0.6301 0.9039 0.082 Uiso 1 1 calc R . . H75B H 0.2701 0.5738 0.8995 0.082 Uiso 1 1 calc R . . C76 C 0.2741(6) 0.6189(2) 0.8147(2) 0.0816(14) Uani 1 1 d . . . C77 C 0.2847(8) 0.5542(3) 0.7210(2) 0.116(2) Uani 1 1 d . . . H77A H 0.1991 0.5695 0.6982 0.139 Uiso 1 1 calc R . . H77B H 0.3550 0.5807 0.7073 0.139 Uiso 1 1 calc R . . C78 C 0.3038(12) 0.4840(4) 0.7079(4) 0.190(5) Uani 1 1 d . . . H78A H 0.2351 0.4584 0.7228 0.284 Uiso 1 1 calc R . . H78B H 0.3898 0.4699 0.7298 0.284 Uiso 1 1 calc R . . H78C H 0.2991 0.4775 0.6623 0.284 Uiso 1 1 calc R . . C79 C 0.2983(11) 0.4852(6) 0.1378(7) 0.205(6) Uani 1 1 d . . . H79A H 0.2575 0.4795 0.0936 0.307 Uiso 1 1 calc R . . H79B H 0.2625 0.5242 0.1551 0.307 Uiso 1 1 calc R . . H79C H 0.2800 0.4471 0.1624 0.307 Uiso 1 1 calc R . . C80 C 0.6439(7) 0.3968(2) 0.3983(3) 0.099(2) Uani 1 1 d . . . H80A H 0.5817 0.3719 0.3681 0.149 Uiso 1 1 calc R . . H80B H 0.6001 0.4352 0.4121 0.149 Uiso 1 1 calc R . . H80C H 0.6762 0.3695 0.4350 0.149 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 0.0533(17) 0.0469(15) 0.097(2) -0.0045(15) 0.0096(15) 0.0043(14) O2 0.0675(19) 0.0390(14) 0.0828(19) -0.0078(14) 0.0073(15) -0.0019(13) O3 0.0699(18) 0.0404(14) 0.0713(17) 0.0024(13) 0.0218(14) 0.0090(13) O4 0.102(2) 0.0610(19) 0.075(2) 0.0106(17) 0.0283(17) -0.0084(18) O5 0.093(2) 0.0327(13) 0.0696(18) 0.0016(13) 0.0092(15) -0.0057(14) O6 0.361(9) 0.093(3) 0.101(3) 0.032(3) 0.066(4) 0.055(4) O7 0.131(3) 0.079(2) 0.065(2) -0.0060(18) 0.0251(18) 0.003(2) O8 0.0523(17) 0.0419(14) 0.091(2) -0.0031(14) 0.0093(14) 0.0025(13) O9 0.077(2) 0.0381(14) 0.0691(17) 0.0005(13) 0.0019(14) 0.0006(14) O10 0.0746(19) 0.0389(14) 0.0700(17) 0.0019(13) 0.0201(15) -0.0067(14) O11 0.106(2) 0.0455(16) 0.085(2) -0.0145(16) 0.0384(18) -0.0021(17) O12 0.081(2) 0.0300(13) 0.0780(19) 0.0038(13) 0.0121(15) 0.0017(13) O13 0.244(6) 0.086(3) 0.081(2) 0.021(2) 0.026(3) 0.019(3) O14 0.169(4) 0.062(2) 0.063(2) -0.0088(17) 0.017(2) -0.024(2) O15 0.250(7) 0.069(3) 0.094(3) 0.005(2) 0.038(4) 0.030(4) N1 0.051(2) 0.0352(15) 0.068(2) -0.0028(15) 0.0094(16) 0.0000(15) N2 0.069(2) 0.0396(16) 0.0581(19) -0.0011(15) 0.0189(16) 0.0019(16) N3 0.068(2) 0.0424(17) 0.071(2) 0.0015(17) 0.0225(18) -0.0033(17) N4 0.073(2) 0.0352(16) 0.059(2) -0.0041(15) 0.0099(17) -0.0034(17) N5 0.053(2) 0.0345(15) 0.0615(19) 0.0018(15) 0.0052(15) -0.0012(15) N6 0.079(2) 0.0395(16) 0.0524(19) -0.0021(15) 0.0128(17) -0.0108(17) N7 0.060(2) 0.0371(15) 0.0597(19) -0.0042(15) 0.0189(16) 0.0013(15) N8 0.055(2) 0.0317(14) 0.0642(19) 0.0019(15) 0.0067(16) -0.0023(15) C1 0.057(3) 0.070(3) 0.105(4) 0.001(3) -0.001(3) -0.002(3) C2 0.061(3) 0.084(4) 0.164(6) 0.012(4) 0.005(3) 0.013(3) C3 0.071(4) 0.099(4) 0.198(7) 0.025(5) 0.025(4) -0.019(3) C4 0.130(6) 0.190(8) 0.117(5) -0.048(6) -0.029(4) 0.021(6) C5 0.063(3) 0.048(2) 0.057(2) -0.001(2) 0.010(2) 0.006(2) C6 0.054(2) 0.0358(17) 0.065(2) -0.0006(18) 0.0196(19) 0.0003(17) C7 0.081(3) 0.058(2) 0.066(3) 0.009(2) 0.027(2) 0.005(2) C8 0.059(3) 0.045(2) 0.095(3) 0.007(2) 0.017(2) -0.006(2) C9 0.052(2) 0.0364(18) 0.056(2) -0.0030(17) 0.0130(18) -0.0023(18) C10 0.089(3) 0.050(2) 0.050(2) 0.0010(19) 0.011(2) -0.003(2) C11 0.119(5) 0.085(4) 0.054(3) -0.014(3) 0.009(3) -0.006(3) C12 0.119(5) 0.058(3) 0.068(3) -0.007(2) -0.024(3) 0.007(3) C13 0.102(5) 0.079(4) 0.148(6) 0.018(4) -0.017(4) 0.009(4) C14 0.102(6) 0.117(6) 0.236(10) 0.007(6) 0.003(6) -0.006(5) C15 0.100(6) 0.167(9) 0.205(10) -0.018(8) -0.020(5) 0.023(7) C16 0.152(9) 0.118(7) 0.166(8) -0.045(6) -0.061(7) 0.050(7) C17 0.170(7) 0.070(4) 0.099(4) -0.014(3) -0.045(5) 0.014(5) C18 0.106(4) 0.063(3) 0.069(3) -0.005(2) 0.044(3) -0.004(3) C19 0.076(3) 0.069(3) 0.080(3) -0.003(3) 0.037(3) -0.005(3) C20 0.067(3) 0.060(3) 0.068(3) 0.007(2) 0.021(2) -0.012(2) C21 0.064(3) 0.045(2) 0.060(2) 0.000(2) 0.011(2) -0.008(2) C22 0.086(3) 0.052(2) 0.058(2) 0.007(2) 0.014(2) 0.005(2) C23 0.089(3) 0.060(3) 0.066(3) 0.008(2) 0.016(2) 0.004(3) C24 0.126(4) 0.088(4) 0.070(3) 0.006(3) 0.032(3) -0.003(3) C25 0.135(5) 0.090(4) 0.076(3) -0.022(3) 0.030(3) -0.036(4) C26 0.077(3) 0.041(2) 0.048(2) -0.0018(19) 0.019(2) -0.008(2) C27 0.070(3) 0.049(2) 0.058(2) -0.005(2) 0.009(2) 0.005(2) C28 0.073(3) 0.067(3) 0.077(3) -0.007(2) 0.007(2) -0.008(2) C29 0.067(3) 0.062(3) 0.073(3) -0.001(2) 0.011(2) -0.019(2) C30 0.099(4) 0.115(5) 0.084(4) 0.025(4) 0.020(3) -0.007(4) C31 0.116(6) 0.250(12) 0.103(6) 0.047(6) 0.018(5) -0.060(7) C32 0.145(8) 0.330(17) 0.078(5) -0.020(7) 0.046(5) -0.105(10) C33 0.122(6) 0.159(7) 0.157(7) -0.053(6) 0.084(6) -0.032(5) C34 0.081(4) 0.084(4) 0.118(4) -0.003(3) 0.035(3) -0.004(3) C35 0.084(3) 0.063(3) 0.060(3) -0.009(2) 0.009(2) 0.000(2) C36 0.101(4) 0.061(3) 0.065(3) -0.003(2) 0.014(2) 0.000(3) C37 0.135(5) 0.064(3) 0.073(3) 0.017(3) 0.025(3) 0.010(3) C38 0.170(7) 0.114(5) 0.074(4) -0.017(4) 0.051(4) -0.019(5) C39 0.145(6) 0.168(7) 0.069(4) -0.032(4) 0.008(4) 0.039(5) C40 0.059(3) 0.059(3) 0.087(3) -0.007(2) 0.002(2) 0.010(2) C41 0.082(4) 0.080(4) 0.140(5) -0.031(4) 0.006(3) 0.031(3) C42 0.060(3) 0.077(3) 0.166(5) -0.016(4) 0.021(3) 0.001(3) C43 0.094(4) 0.111(5) 0.106(4) -0.013(4) -0.022(3) 0.004(4) C44 0.063(3) 0.039(2) 0.058(2) -0.0055(19) 0.006(2) 0.001(2) C45 0.056(3) 0.0354(18) 0.067(3) -0.0021(18) 0.016(2) 0.0010(18) C46 0.058(3) 0.043(2) 0.115(4) 0.001(2) 0.017(2) 0.007(2) C47 0.092(3) 0.057(2) 0.072(3) -0.016(2) 0.035(3) -0.010(2) C48 0.057(2) 0.0341(17) 0.055(2) 0.0005(17) 0.0086(19) -0.0003(18) C49 0.096(3) 0.044(2) 0.046(2) -0.0058(19) 0.014(2) -0.010(2) C50 0.133(5) 0.070(3) 0.057(3) 0.001(2) 0.004(3) -0.004(3) C51 0.139(6) 0.067(3) 0.064(3) 0.005(3) -0.017(3) -0.006(4) C52 0.148(7) 0.119(6) 0.127(6) 0.041(5) -0.006(5) 0.045(6) C53 0.175(10) 0.170(10) 0.174(8) 0.057(8) 0.006(7) 0.031(9) C54 0.172(11) 0.211(16) 0.161(9) 0.000(10) -0.031(9) 0.078(11) C55 0.231(13) 0.109(7) 0.203(11) -0.008(7) -0.089(11) 0.064(9) C56 0.177(8) 0.074(4) 0.164(7) 0.010(4) -0.054(6) 0.019(5) C57 0.123(4) 0.052(2) 0.061(3) -0.005(2) 0.035(3) -0.003(3) C58 0.086(3) 0.054(2) 0.074(3) -0.006(2) 0.035(3) -0.001(2) C59 0.065(3) 0.043(2) 0.070(3) -0.007(2) 0.023(2) 0.003(2) C60 0.054(2) 0.0384(18) 0.058(2) -0.0006(18) 0.0095(18) 0.0023(18) C61 0.071(3) 0.057(2) 0.055(2) 0.000(2) 0.006(2) -0.003(2) C62 0.100(4) 0.082(3) 0.065(3) 0.012(3) -0.003(3) -0.017(3) C63 0.091(4) 0.173(7) 0.119(5) -0.007(5) -0.019(4) 0.010(5) C64 0.187(7) 0.117(5) 0.076(4) -0.030(4) -0.018(4) -0.036(5) C65 0.068(3) 0.040(2) 0.049(2) -0.0031(18) 0.0169(19) 0.003(2) C66 0.065(3) 0.0388(19) 0.068(3) 0.0034(19) 0.006(2) -0.006(2) C67 0.057(3) 0.062(3) 0.092(3) 0.009(3) 0.011(2) 0.009(2) C68 0.072(3) 0.064(3) 0.098(4) 0.000(3) 0.034(3) 0.015(3) C69 0.133(5) 0.086(4) 0.108(5) 0.019(4) 0.055(4) 0.012(4) C70 0.192(8) 0.135(7) 0.119(6) 0.030(6) 0.092(6) 0.040(6) C71 0.148(6) 0.161(8) 0.083(5) 0.004(5) 0.042(4) 0.067(6) C72 0.119(5) 0.140(6) 0.101(5) -0.018(5) 0.025(4) 0.034(5) C73 0.096(4) 0.088(4) 0.100(4) -0.003(3) 0.024(3) 0.024(3) C74 0.074(3) 0.051(2) 0.074(3) 0.005(2) -0.001(2) -0.007(2) C75 0.092(3) 0.049(2) 0.061(3) 0.001(2) 0.004(2) -0.003(2) C76 0.119(4) 0.056(3) 0.067(3) 0.007(3) 0.006(3) 0.000(3) C77 0.191(7) 0.098(4) 0.059(3) -0.011(3) 0.024(3) -0.024(5) C78 0.363(14) 0.113(6) 0.111(5) -0.054(5) 0.092(7) -0.071(7) C79 0.149(9) 0.133(8) 0.321(16) 0.021(9) 0.005(10) 0.010(8) C80 0.175(6) 0.045(2) 0.102(4) -0.025(2) 0.094(4) -0.043(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 C5 1.344(5) . ? O1 C1 1.473(5) . ? O2 C5 1.214(5) . ? O3 C9 1.229(4) . ? O4 C20 1.233(5) . ? O5 C26 1.241(4) . ? O6 C37 1.193(6) . ? O7 C37 1.317(6) . ? O7 C38 1.452(6) . ? O8 C44 1.344(5) . ? O8 C40 1.478(5) . ? O9 C44 1.223(4) . ? O10 C48 1.227(4) . ? O11 C59 1.237(5) . ? O12 C65 1.246(4) . ? O13 C76 1.199(6) . ? O14 C76 1.309(6) . ? O14 C77 1.465(6) . ? O15 C79 1.156(10) . ? O15 H15A 0.8200 . ? O16 C80 1.141(13) . ? O16 H16A 0.8381 . ? N1 C5 1.345(5) . ? N1 C6 1.462(5) . ? N1 H1 0.8600 . ? N2 C9 1.330(5) . ? N2 C10 1.464(5) . ? N2 H2 0.8600 . ? N3 C20 1.337(5) . ? N3 C21 1.454(5) . ? N3 H3 0.8600 . ? N4 C26 1.330(5) . ? N4 C27 1.461(5) . ? N4 H4 0.8600 . ? N5 C44 1.326(5) . ? N5 C45 1.466(5) . ? N5 H5 0.8600 . ? N6 C48 1.333(5) . ? N6 C49 1.456(5) . ? N6 H6 0.8600 . ? N7 C59 1.323(5) . ? N7 C60 1.457(5) . ? N7 H7 0.8600 . ? N8 C65 1.327(5) . ? N8 C66 1.439(5) . ? N8 H8 0.8600 . ? C1 C4 1.487(8) . ? C1 C2 1.513(7) . ? C1 C3 1.516(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 C8 1.522(6) . ? C6 C7 1.533(5) . ? C6 C9 1.536(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C10 C18 1.498(6) . ? C10 C11 1.550(6) . ? C10 H10 0.9800 . ? C11 C12 1.466(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.395(9) . ? C12 C13 1.397(8) . ? C13 C14 1.378(10) . ? C13 H13 0.9300 . ? C14 C15 1.383(12) . ? C14 H14 0.9300 . ? C15 C16 1.350(13) . ? C15 H15 0.9300 . ? C16 C17 1.346(12) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.522(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.504(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 C22 1.528(5) . ? C21 C26 1.529(6) . ? C21 H21 0.9800 . ? C22 C23 1.507(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.518(6) . ? C23 C25 1.546(7) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C27 C28 1.525(6) . ? C27 C35 1.527(6) . ? C27 H27 0.9800 . ? C28 C29 1.491(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.353(7) . ? C29 C34 1.392(7) . ? C30 C31 1.367(10) . ? C30 H30 0.9300 . ? C31 C32 1.393(15) . ? C31 H31 0.9300 . ? C32 C33 1.351(14) . ? C32 H32 0.9300 . ? C33 C34 1.367(9) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.519(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.485(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C38 C39 1.474(9) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C43 1.486(7) . ? C40 C41 1.509(6) . ? C40 C42 1.512(7) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C45 C47 1.516(6) . ? C45 C46 1.533(6) . ? C45 C48 1.538(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C49 C57 1.519(7) . ? C49 C50 1.539(6) . ? C49 H49 0.9800 . ? C50 C51 1.485(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.353(10) . ? C51 C56 1.366(9) . ? C52 C53 1.398(13) . ? C52 H52 0.9300 . ? C53 C54 1.365(16) . ? C53 H53 0.9300 . ? C54 C55 1.296(17) . ? C54 H54 0.9300 . ? C55 C56 1.390(15) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.517(7) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.511(6) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C60 C65 1.514(6) . ? C60 C61 1.525(5) . ? C60 H60 0.9800 . ? C61 C62 1.520(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.507(8) . ? C62 C64 1.518(8) . ? C62 H62 0.9800 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C66 C74 1.510(6) . ? C66 C67 1.528(6) . ? C66 H66 0.9800 . ? C67 C68 1.488(7) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 C73 1.371(8) . ? C68 C69 1.389(7) . ? C69 C70 1.367(10) . ? C69 H69 0.9300 . ? C70 C71 1.318(11) . ? C70 H70 0.9300 . ? C71 C72 1.380(11) . ? C71 H71 0.9300 . ? C72 C73 1.392(8) . ? C72 H72 0.9300 . ? C73 H73 0.9300 . ? C74 C75 1.511(6) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C76 1.476(6) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C77 C78 1.460(10) . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 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 C5 O1 C1 121.9(3) . . ? C37 O7 C38 118.6(4) . . ? C44 O8 C40 121.3(3) . . ? C76 O14 C77 117.9(4) . . ? C79 O15 H15A 109.5 . . ? C80 O16 H16A 112.5 . . ? C5 N1 C6 123.0(3) . . ? C5 N1 H1 118.5 . . ? C6 N1 H1 118.5 . . ? C9 N2 C10 124.5(3) . . ? C9 N2 H2 117.8 . . ? C10 N2 H2 117.7 . . ? C20 N3 C21 122.3(3) . . ? C20 N3 H3 118.8 . . ? C21 N3 H3 118.8 . . ? C26 N4 C27 124.2(3) . . ? C26 N4 H4 117.9 . . ? C27 N4 H4 117.9 . . ? C44 N5 C45 122.1(3) . . ? C44 N5 H5 119.0 . . ? C45 N5 H5 118.9 . . ? C48 N6 C49 123.3(3) . . ? C48 N6 H6 118.4 . . ? C49 N6 H6 118.4 . . ? C59 N7 C60 121.2(3) . . ? C59 N7 H7 119.4 . . ? C60 N7 H7 119.4 . . ? C65 N8 C66 124.3(3) . . ? C65 N8 H8 117.8 . . ? C66 N8 H8 117.8 . . ? O1 C1 C4 108.8(5) . . ? O1 C1 C2 101.5(4) . . ? C4 C1 C2 113.1(5) . . ? O1 C1 C3 109.0(4) . . ? C4 C1 C3 114.1(6) . . ? C2 C1 C3 109.4(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.4 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.4 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.4 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 O1 125.1(4) . . ? O2 C5 N1 124.9(4) . . ? O1 C5 N1 110.0(3) . . ? N1 C6 C8 106.6(3) . . ? N1 C6 C7 110.0(3) . . ? C8 C6 C7 109.7(3) . . ? N1 C6 C9 111.4(3) . . ? C8 C6 C9 108.6(3) . . ? C7 C6 C9 110.5(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 N2 123.8(3) . . ? O3 C9 C6 119.9(3) . . ? N2 C9 C6 116.2(3) . . ? N2 C10 C18 112.3(4) . . ? N2 C10 C11 109.3(4) . . ? C18 C10 C11 110.7(4) . . ? N2 C10 H10 108.2 . . ? C18 C10 H10 108.2 . . ? C11 C10 H10 108.2 . . ? C12 C11 C10 115.0(4) . . ? C12 C11 H11A 108.5 . . ? C10 C11 H11A 108.5 . . ? C12 C11 H11B 108.5 . . ? C10 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C17 C12 C13 113.3(7) . . ? C17 C12 C11 123.1(6) . . ? C13 C12 C11 123.4(5) . . ? C14 C13 C12 123.1(6) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C15 118.6(9) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C16 C15 C14 120.8(10) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 118.6(9) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C16 C17 C12 125.4(8) . . ? C16 C17 H17 117.3 . . ? C12 C17 H17 117.3 . . ? C10 C18 C19 115.5(3) . . ? C10 C18 H18A 108.4 . . ? C19 C18 H18A 108.4 . . ? C10 C18 H18B 108.4 . . ? C19 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? C20 C19 C18 113.2(4) . . ? C20 C19 H19A 108.9 . . ? C18 C19 H19A 108.9 . . ? C20 C19 H19B 108.9 . . ? C18 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? O4 C20 N3 121.3(4) . . ? O4 C20 C19 123.1(4) . . ? N3 C20 C19 115.6(4) . . ? N3 C21 C22 108.0(3) . . ? N3 C21 C26 113.4(3) . . ? C22 C21 C26 110.2(3) . . ? N3 C21 H21 108.3 . . ? C22 C21 H21 108.4 . . ? C26 C21 H21 108.3 . . ? C23 C22 C21 116.9(3) . . ? C23 C22 H22A 108.1 . . ? C21 C22 H22A 108.1 . . ? C23 C22 H22B 108.1 . . ? C21 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? C22 C23 C24 110.2(4) . . ? C22 C23 C25 111.9(4) . . ? C24 C23 C25 109.5(4) . . ? C22 C23 H23 108.4 . . ? C24 C23 H23 108.4 . . ? C25 C23 H23 108.4 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.4 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O5 C26 N4 121.8(4) . . ? O5 C26 C21 119.8(4) . . ? N4 C26 C21 118.4(3) . . ? N4 C27 C28 110.3(3) . . ? N4 C27 C35 110.1(3) . . ? C28 C27 C35 110.9(4) . . ? N4 C27 H27 108.5 . . ? C28 C27 H27 108.5 . . ? C35 C27 H27 108.5 . . ? C29 C28 C27 113.6(4) . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C30 C29 C34 119.0(5) . . ? C30 C29 C28 121.2(5) . . ? C34 C29 C28 119.8(5) . . ? C29 C30 C31 121.0(7) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C30 C31 C32 119.5(8) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.3 . . ? C33 C32 C31 119.7(8) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.5(9) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.8 . . ? C33 C34 C29 120.2(7) . . ? C33 C34 H34 119.9 . . ? C29 C34 H34 119.9 . . ? C36 C35 C27 114.6(4) . . ? C36 C35 H35A 108.6 . . ? C27 C35 H35A 108.6 . . ? C36 C35 H35B 108.6 . . ? C27 C35 H35B 108.6 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C35 110.1(4) . . ? C37 C36 H36A 109.7 . . ? C35 C36 H36A 109.6 . . ? C37 C36 H36B 109.6 . . ? C35 C36 H36B 109.6 . . ? H36A C36 H36B 108.2 . . ? O6 C37 O7 122.1(5) . . ? O6 C37 C36 125.0(5) . . ? O7 C37 C36 112.9(4) . . ? O7 C38 C39 109.9(5) . . ? O7 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? O7 C38 H38B 109.6 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? 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 . . ? O8 C40 C43 109.7(4) . . ? O8 C40 C41 110.0(4) . . ? C43 C40 C41 114.1(5) . . ? O8 C40 C42 101.4(4) . . ? C43 C40 C42 110.9(5) . . ? C41 C40 C42 109.9(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O9 C44 N5 125.4(4) . . ? O9 C44 O8 124.4(4) . . ? N5 C44 O8 110.2(3) . . ? N5 C45 C47 110.9(3) . . ? N5 C45 C46 107.0(3) . . ? C47 C45 C46 110.1(3) . . ? N5 C45 C48 111.1(3) . . ? C47 C45 C48 109.9(3) . . ? C46 C45 C48 107.7(3) . . ? 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 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O10 C48 N6 123.6(3) . . ? O10 C48 C45 120.2(3) . . ? N6 C48 C45 116.2(3) . . ? N6 C49 C57 112.2(4) . . ? N6 C49 C50 110.5(3) . . ? C57 C49 C50 110.5(4) . . ? N6 C49 H49 107.8 . . ? C57 C49 H49 107.8 . . ? C50 C49 H49 107.8 . . ? C51 C50 C49 115.6(4) . . ? C51 C50 H50A 108.4 . . ? C49 C50 H50A 108.4 . . ? C51 C50 H50B 108.4 . . ? C49 C50 H50B 108.4 . . ? H50A C50 H50B 107.4 . . ? C52 C51 C56 117.4(8) . . ? C52 C51 C50 119.9(6) . . ? C56 C51 C50 122.7(8) . . ? C51 C52 C53 121.4(9) . . ? C51 C52 H52 119.3 . . ? C53 C52 H52 119.3 . . ? C54 C53 C52 118.4(12) . . ? C54 C53 H53 120.8 . . ? C52 C53 H53 120.8 . . ? C55 C54 C53 121.4(14) . . ? C55 C54 H54 119.3 . . ? C53 C54 H54 119.3 . . ? C54 C55 C56 120.3(12) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.8 . . ? C51 C56 C55 121.2(10) . . ? C51 C56 H56 119.4 . . ? C55 C56 H56 119.4 . . ? C58 C57 C49 116.3(3) . . ? C58 C57 H57A 108.3 . . ? C49 C57 H57A 108.2 . . ? C58 C57 H57B 108.2 . . ? C49 C57 H57B 108.2 . . ? H57A C57 H57B 107.4 . . ? C59 C58 C57 113.4(4) . . ? C59 C58 H58A 108.9 . . ? C57 C58 H58A 108.9 . . ? C59 C58 H58B 108.9 . . ? C57 C58 H58B 108.9 . . ? H58A C58 H58B 107.7 . . ? O11 C59 N7 122.5(4) . . ? O11 C59 C58 121.5(4) . . ? N7 C59 C58 116.0(3) . . ? N7 C60 C65 113.2(3) . . ? N7 C60 C61 109.6(3) . . ? C65 C60 C61 109.7(3) . . ? N7 C60 H60 108.1 . . ? C65 C60 H60 108.1 . . ? C61 C60 H60 108.1 . . ? C62 C61 C60 116.2(4) . . ? C62 C61 H61A 108.2 . . ? C60 C61 H61A 108.2 . . ? C62 C61 H61B 108.2 . . ? C60 C61 H61B 108.2 . . ? H61A C61 H61B 107.4 . . ? C63 C62 C64 111.0(5) . . ? C63 C62 C61 111.7(5) . . ? C64 C62 C61 109.2(5) . . ? C63 C62 H62 108.3 . . ? C64 C62 H62 108.2 . . ? C61 C62 H62 108.3 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.4 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O12 C65 N8 123.2(4) . . ? O12 C65 C60 119.3(4) . . ? N8 C65 C60 117.3(3) . . ? N8 C66 C74 109.5(3) . . ? N8 C66 C67 110.1(3) . . ? C74 C66 C67 113.6(3) . . ? N8 C66 H66 107.8 . . ? C74 C66 H66 107.8 . . ? C67 C66 H66 107.8 . . ? C68 C67 C66 112.5(3) . . ? C68 C67 H67A 109.1 . . ? C66 C67 H67A 109.1 . . ? C68 C67 H67B 109.1 . . ? C66 C67 H67B 109.1 . . ? H67A C67 H67B 107.8 . . ? C73 C68 C69 117.6(5) . . ? C73 C68 C67 121.3(5) . . ? C69 C68 C67 121.0(5) . . ? C70 C69 C68 120.1(7) . . ? C70 C69 H69 120.0 . . ? C68 C69 H69 119.9 . . ? C71 C70 C69 122.0(7) . . ? C71 C70 H70 119.0 . . ? C69 C70 H70 118.9 . . ? C70 C71 C72 120.4(7) . . ? C70 C71 H71 119.7 . . ? C72 C71 H71 119.9 . . ? C71 C72 C73 118.3(7) . . ? C71 C72 H72 120.8 . . ? C73 C72 H72 120.9 . . ? C68 C73 C72 121.5(6) . . ? C68 C73 H73 119.2 . . ? C72 C73 H73 119.3 . . ? C66 C74 C75 112.9(3) . . ? C66 C74 H74A 109.0 . . ? C75 C74 H74A 109.0 . . ? C66 C74 H74B 109.0 . . ? C75 C74 H74B 109.0 . . ? H74A C74 H74B 107.8 . . ? C76 C75 C74 115.2(4) . . ? C76 C75 H75A 108.5 . . ? C74 C75 H75A 108.5 . . ? C76 C75 H75B 108.5 . . ? C74 C75 H75B 108.5 . . ? H75A C75 H75B 107.5 . . ? O13 C76 O14 122.5(5) . . ? O13 C76 C75 124.1(5) . . ? O14 C76 C75 112.8(4) . . ? C78 C77 O14 106.3(5) . . ? C78 C77 H77A 110.5 . . ? O14 C77 H77A 110.5 . . ? C78 C77 H77B 110.5 . . ? O14 C77 H77B 110.4 . . ? H77A C77 H77B 108.7 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O15 C79 H79A 109.5 . . ? O15 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? O15 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O16 C80 H80A 110.0 . . ? O16 C80 H80B 108.1 . . ? H80A C80 H80B 109.5 . . ? O16 C80 H80C 110.3 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.210 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.044 #===End data_P2 _database_code_depnum_ccdc_archive 'CCDC 878072' #TrackingRef '- All peptide.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic 'ALPHA-GAMMA mixed peptide' _chemical_name_common hexaM _chemical_formula_moiety '2(C54 H76 N6 O9), O' _chemical_formula_sum 'C108 H152 N12 O19' _chemical_compound_source synthesis _exptl_crystal_recrystallization_method EtOAc/hexane _chemical_melting_point ? _exptl_crystal_description 'ractangular plates' _exptl_crystal_colour colorless _diffrn_ambient_temperature 100(2) _diffrn_ambient_pressure 101.325 _chemical_formula_weight 1922.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_int_tables_number 4 _chemical_absolute_configuration syn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.850(6) _cell_length_b 18.173(7) _cell_length_c 24.075(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.254(7) _cell_angle_gamma 90.00 _cell_volume 6204(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.976 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Graphite monochromator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 64901 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_sigmaI/netI 0.1074 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 28.28 _reflns_number_total 28846 _reflns_number_gt 13821 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(7) _refine_ls_number_reflns 28846 _refine_ls_number_parameters 1272 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1256 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1406 _refine_ls_goodness_of_fit_ref 0.784 _refine_ls_restrained_S_all 0.788 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1940(2) 0.93974(19) 0.61983(13) 0.0585(8) Uani 1 1 d . . . C2 C -0.1799(3) 0.8756(2) 0.66183(16) 0.0769(10) Uani 1 1 d . . . H2A H -0.1293 0.8866 0.6963 0.115 Uiso 1 1 calc R . . H2B H -0.1646 0.8322 0.6437 0.115 Uiso 1 1 calc R . . H2C H -0.2368 0.8674 0.6721 0.115 Uiso 1 1 calc R . . C3 C -0.2702(3) 0.9216(3) 0.56354(17) 0.0956(15) Uani 1 1 d . . . H3A H -0.3270 0.9077 0.5722 0.143 Uiso 1 1 calc R . . H3B H -0.2495 0.8817 0.5443 0.143 Uiso 1 1 calc R . . H3C H -0.2823 0.9641 0.5387 0.143 Uiso 1 1 calc R . . C4 C -0.1041(3) 0.9614(2) 0.60807(15) 0.0707(9) Uani 1 1 d . . . H4A H -0.1170 0.9986 0.5784 0.106 Uiso 1 1 calc R . . H4B H -0.0770 0.9191 0.5952 0.106 Uiso 1 1 calc R . . H4C H -0.0607 0.9803 0.6430 0.106 Uiso 1 1 calc R . . C5 C -0.1910(2) 1.03416(16) 0.69283(11) 0.0455(7) Uani 1 1 d . . . C6 C -0.20553(19) 1.13972(15) 0.75305(11) 0.0455(7) Uani 1 1 d . . . C7 C -0.2866(2) 1.18807(18) 0.75627(13) 0.0590(9) Uani 1 1 d . . . H7A H -0.3061 1.2185 0.7222 0.088 Uiso 1 1 calc R . . H7B H -0.2669 1.2186 0.7902 0.088 Uiso 1 1 calc R . . H7C H -0.3385 1.1578 0.7584 0.088 Uiso 1 1 calc R . . C8 C -0.1262(2) 1.18631(19) 0.74411(14) 0.0618(8) Uani 1 1 d . . . H8A H -0.0769 1.1548 0.7397 0.093 Uiso 1 1 calc R . . H8B H -0.1018 1.2178 0.7772 0.093 Uiso 1 1 calc R . . H8C H -0.1498 1.2158 0.7098 0.093 Uiso 1 1 calc R . . C9 C -0.17061(19) 1.09629(16) 0.81001(11) 0.0439(7) Uani 1 1 d . . . C10 C -0.2072(2) 1.00501(17) 0.87440(12) 0.0518(7) Uani 1 1 d . . . H10 H -0.1386 1.0073 0.8918 0.062 Uiso 1 1 calc R . . C11 C -0.2510(2) 1.0417(2) 0.91819(14) 0.0626(9) Uani 1 1 d . . . H11A H -0.2309 1.0150 0.9547 0.075 Uiso 1 1 calc R . . H11B H -0.2271 1.0915 0.9256 0.075 Uiso 1 1 calc R . . C12 C -0.3561(2) 1.0443(2) 0.89806(14) 0.0620(9) Uani 1 1 d . . . C13 C -0.4019(3) 1.1069(2) 0.87052(15) 0.0720(10) Uani 1 1 d . . . H13 H -0.3666 1.1469 0.8649 0.086 Uiso 1 1 calc R . . C14 C -0.4999(3) 1.1105(3) 0.85126(17) 0.0906(13) Uani 1 1 d . . . H14 H -0.5302 1.1526 0.8329 0.109 Uiso 1 1 calc R . . C15 C -0.5516(3) 1.0508(4) 0.8597(2) 0.1027(15) Uani 1 1 d . . . H15 H -0.6171 1.0526 0.8459 0.123 Uiso 1 1 calc R . . C16 C -0.5084(4) 0.9889(3) 0.8879(2) 0.1054(15) Uani 1 1 d . . . H16 H -0.5438 0.9494 0.8944 0.126 Uiso 1 1 calc R . . C17 C -0.4090(3) 0.9866(3) 0.90689(18) 0.0831(11) Uani 1 1 d . . . H17 H -0.3789 0.9448 0.9259 0.100 Uiso 1 1 calc R . . C18 C -0.2321(2) 0.92444(17) 0.86299(14) 0.0573(8) Uani 1 1 d . . . H18A H -0.2989 0.9199 0.8426 0.069 Uiso 1 1 calc R . . H18B H -0.2197 0.8986 0.8998 0.069 Uiso 1 1 calc R . . C19 C -0.1752(2) 0.88922(18) 0.82669(13) 0.0566(8) Uani 1 1 d . . . H19A H -0.1928 0.8379 0.8200 0.068 Uiso 1 1 calc R . . H19B H -0.1899 0.9136 0.7892 0.068 Uiso 1 1 calc R . . C20 C -0.0718(2) 0.89452(17) 0.85625(13) 0.0500(7) Uani 1 1 d . . . C21 C 0.0803(2) 0.94136(18) 0.85285(12) 0.0502(7) Uani 1 1 d . . . H21 H 0.1050 0.8910 0.8567 0.060 Uiso 1 1 calc R . . C22 C 0.1209(3) 0.9808(3) 0.81124(15) 0.0801(11) Uani 1 1 d . . . H22A H 0.1866 0.9910 0.8312 0.096 Uiso 1 1 calc R . . H22B H 0.0890 1.0278 0.8023 0.096 Uiso 1 1 calc R . . C23 C 0.1161(4) 0.9435(5) 0.75447(19) 0.136(3) Uani 1 1 d . . . H23 H 0.0496 0.9380 0.7321 0.163 Uiso 1 1 calc R . . C24 C 0.1625(5) 0.8642(5) 0.7650(3) 0.163(3) Uani 1 1 d . . . H24A H 0.2283 0.8687 0.7857 0.244 Uiso 1 1 calc R . . H24B H 0.1554 0.8408 0.7282 0.244 Uiso 1 1 calc R . . H24C H 0.1318 0.8352 0.7873 0.244 Uiso 1 1 calc R . . C25 C 0.1639(5) 0.9927(6) 0.7199(3) 0.196(4) Uani 1 1 d . . . H25A H 0.1269 1.0364 0.7077 0.294 Uiso 1 1 calc R . . H25B H 0.1690 0.9665 0.6863 0.294 Uiso 1 1 calc R . . H25C H 0.2257 1.0060 0.7439 0.294 Uiso 1 1 calc R . . C26 C 0.1163(2) 0.97735(17) 0.91238(12) 0.0466(7) Uani 1 1 d . . . C27 C 0.0978(2) 1.07126(17) 0.97970(12) 0.0527(8) Uani 1 1 d . . . H27 H 0.1590 1.0513 1.0023 0.063 Uiso 1 1 calc R . . C28 C 0.1105(3) 1.1525(2) 0.96660(17) 0.0707(10) Uani 1 1 d . . . H28A H 0.0488 1.1736 0.9481 0.085 Uiso 1 1 calc R . . H28B H 0.1370 1.1781 1.0032 0.085 Uiso 1 1 calc R . . C29 C 0.1715(3) 1.16663(19) 0.92893(18) 0.0712(10) Uani 1 1 d . . . C30 C 0.1335(3) 1.1845(3) 0.8724(2) 0.0880(12) Uani 1 1 d . . . H30 H 0.0681 1.1857 0.8575 0.106 Uiso 1 1 calc R . . C31 C 0.1857(4) 1.2009(3) 0.8358(3) 0.1194(18) Uani 1 1 d . . . H31 H 0.1562 1.2139 0.7973 0.143 Uiso 1 1 calc R . . C32 C 0.2808(5) 1.1980(3) 0.8565(3) 0.1257(19) Uani 1 1 d . . . H32 H 0.3180 1.2089 0.8326 0.151 Uiso 1 1 calc R . . C33 C 0.3220(3) 1.1781(4) 0.9148(3) 0.1215(19) Uani 1 1 d . . . H33 H 0.3873 1.1751 0.9295 0.146 Uiso 1 1 calc R . . C34 C 0.2683(3) 1.1630(3) 0.9504(2) 0.0978(14) Uani 1 1 d . . . H34 H 0.2968 1.1503 0.9891 0.117 Uiso 1 1 calc R . . C35 C 0.0293(2) 1.06500(19) 1.01585(14) 0.0616(9) Uani 1 1 d . . . H35A H 0.0593 1.0852 1.0542 0.074 Uiso 1 1 calc R . . H35B H -0.0257 1.0950 0.9978 0.074 Uiso 1 1 calc R . . C36 C -0.0030(2) 0.9879(2) 1.02271(14) 0.0611(9) Uani 1 1 d . . . H36A H -0.0508 0.9902 1.0427 0.073 Uiso 1 1 calc R . . H36B H -0.0322 0.9675 0.9844 0.073 Uiso 1 1 calc R . . C37 C 0.0734(2) 0.93665(18) 1.05538(12) 0.0495(7) Uani 1 1 d . . . C38 C 0.1436(2) 0.81414(16) 1.05563(11) 0.0499(7) Uani 1 1 d . . . C39 C 0.1068(3) 0.7832(2) 1.10335(14) 0.0729(10) Uani 1 1 d . . . H39A H 0.1160 0.8186 1.1341 0.109 Uiso 1 1 calc R . . H39B H 0.1404 0.7388 1.1184 0.109 Uiso 1 1 calc R . . H39C H 0.0408 0.7725 1.0877 0.109 Uiso 1 1 calc R . . C40 C 0.1379(3) 0.7578(2) 1.00850(14) 0.0739(10) Uani 1 1 d . . . H40A H 0.0749 0.7387 0.9948 0.111 Uiso 1 1 calc R . . H40B H 0.1810 0.7183 1.0239 0.111 Uiso 1 1 calc R . . H40C H 0.1542 0.7806 0.9768 0.111 Uiso 1 1 calc R . . C41 C 0.2470(2) 0.83631(17) 1.07979(12) 0.0495(7) Uani 1 1 d . . . C42 C 0.3749(2) 0.90871(19) 1.06276(13) 0.0590(8) Uani 1 1 d . . . H42 H 0.4127 0.8759 1.0930 0.071 Uiso 1 1 calc R . . C43 C 0.4065(2) 0.8977(2) 1.00836(16) 0.0719(10) Uani 1 1 d . . . H43A H 0.3753 0.9340 0.9795 0.086 Uiso 1 1 calc R . . H43B H 0.4738 0.9067 1.0184 0.086 Uiso 1 1 calc R . . C44 C 0.3864(2) 0.8226(2) 0.98169(15) 0.0678(9) Uani 1 1 d . . . C45 C 0.3313(3) 0.8136(3) 0.92584(18) 0.0845(12) Uani 1 1 d . . . H45 H 0.3064 0.8548 0.9037 0.101 Uiso 1 1 calc R . . C46 C 0.3114(4) 0.7438(3) 0.9013(2) 0.1023(15) Uani 1 1 d . . . H46 H 0.2751 0.7389 0.8627 0.123 Uiso 1 1 calc R . . C47 C 0.3445(4) 0.6835(3) 0.9331(3) 0.1104(16) Uani 1 1 d . . . H47 H 0.3308 0.6370 0.9167 0.132 Uiso 1 1 calc R . . C48 C 0.3988(4) 0.6908(3) 0.9901(2) 0.1078(16) Uani 1 1 d . . . H48 H 0.4204 0.6490 1.0125 0.129 Uiso 1 1 calc R . . C49 C 0.4210(3) 0.7585(3) 1.01391(19) 0.0915(13) Uani 1 1 d . . . H49 H 0.4597 0.7627 1.0520 0.110 Uiso 1 1 calc R . . C50 C 0.3918(3) 0.9858(2) 1.08531(14) 0.0637(9) Uani 1 1 d . . . H50 H 0.4440 1.0102 1.0805 0.076 Uiso 1 1 calc R . . C51 C 0.3396(3) 1.0213(2) 1.11102(13) 0.0625(9) Uani 1 1 d . . . H51 H 0.2842 0.9988 1.1127 0.075 Uiso 1 1 calc R . . C52 C 0.3611(3) 1.0934(2) 1.13732(15) 0.0714(10) Uani 1 1 d . . . C53 C 0.4452(5) 1.2046(3) 1.1390(2) 0.127(2) Uani 1 1 d D . . H53A H 0.4328 1.2085 1.1762 0.152 Uiso 1 1 calc R . . H53B H 0.5127 1.2091 1.1456 0.152 Uiso 1 1 calc R . . C54 C 0.3991(9) 1.2601(4) 1.1028(4) 0.263(7) Uani 1 1 d D . . H54A H 0.3364 1.2443 1.0821 0.394 Uiso 1 1 calc R . . H54B H 0.4328 1.2718 1.0755 0.394 Uiso 1 1 calc R . . H54C H 0.3958 1.3029 1.1254 0.394 Uiso 1 1 calc R . . C55 C 0.9939(2) 0.65828(19) 0.80930(13) 0.0599(9) Uani 1 1 d . . . C56 C 1.0388(3) 0.6758(3) 0.87285(15) 0.0951(15) Uani 1 1 d . . . H56A H 0.9909 0.6899 0.8901 0.143 Uiso 1 1 calc R . . H56B H 1.0829 0.7155 0.8764 0.143 Uiso 1 1 calc R . . H56C H 1.0713 0.6331 0.8924 0.143 Uiso 1 1 calc R . . C57 C 0.9332(3) 0.7222(2) 0.77939(17) 0.0808(11) Uani 1 1 d . . . H57A H 0.9087 0.7122 0.7385 0.121 Uiso 1 1 calc R . . H57B H 0.9705 0.7662 0.7852 0.121 Uiso 1 1 calc R . . H57C H 0.8818 0.7286 0.7955 0.121 Uiso 1 1 calc R . . C58 C 1.0669(2) 0.6356(2) 0.78104(17) 0.0769(10) Uani 1 1 d . . . H58A H 1.1043 0.5964 0.8029 0.115 Uiso 1 1 calc R . . H58B H 1.1068 0.6768 0.7799 0.115 Uiso 1 1 calc R . . H58C H 1.0364 0.6191 0.7421 0.115 Uiso 1 1 calc R . . C59 C 0.8764(2) 0.56436(16) 0.76370(12) 0.0466(7) Uani 1 1 d . . . C60 C 0.7713(2) 0.45973(16) 0.73165(11) 0.0457(7) Uani 1 1 d . . . C61 C 0.8336(2) 0.41485(18) 0.70457(14) 0.0626(9) Uani 1 1 d . . . H61A H 0.8689 0.4474 0.6875 0.094 Uiso 1 1 calc R . . H61B H 0.7950 0.3832 0.6751 0.094 Uiso 1 1 calc R . . H61C H 0.8763 0.3856 0.7341 0.094 Uiso 1 1 calc R . . C62 C 0.7164(2) 0.40996(17) 0.76083(13) 0.0581(8) Uani 1 1 d . . . H62A H 0.7596 0.3823 0.7912 0.087 Uiso 1 1 calc R . . H62B H 0.6779 0.3768 0.7326 0.087 Uiso 1 1 calc R . . H62C H 0.6769 0.4394 0.7772 0.087 Uiso 1 1 calc R . . C64 C 0.56968(19) 0.59212(16) 0.65978(12) 0.0480(7) Uani 1 1 d . . . H64 H 0.5831 0.5916 0.6223 0.058 Uiso 1 1 calc R . . C65 C 0.4748(2) 0.5531(2) 0.65082(14) 0.0614(9) Uani 1 1 d . . . H65A H 0.4281 0.5777 0.6194 0.074 Uiso 1 1 calc R . . H65B H 0.4808 0.5031 0.6381 0.074 Uiso 1 1 calc R . . C66 C 0.4378(2) 0.5496(2) 0.70239(16) 0.0664(9) Uani 1 1 d . . . C67 C 0.3819(3) 0.6036(3) 0.7130(2) 0.1025(15) Uani 1 1 d . . . H67 H 0.3662 0.6440 0.6882 0.123 Uiso 1 1 calc R . . C68 C 0.3476(4) 0.5983(5) 0.7620(3) 0.134(2) Uani 1 1 d . . . H68 H 0.3110 0.6360 0.7701 0.161 Uiso 1 1 calc R . . C69 C 0.3684(6) 0.5374(6) 0.7974(3) 0.136(3) Uani 1 1 d . . . H69 H 0.3451 0.5331 0.8291 0.163 Uiso 1 1 calc R . . C70 C 0.4214(4) 0.4856(4) 0.7859(2) 0.114(2) Uani 1 1 d . . . H70 H 0.4356 0.4443 0.8098 0.137 Uiso 1 1 calc R . . C71 C 0.4568(3) 0.4908(3) 0.73911(17) 0.0824(12) Uani 1 1 d . . . H71 H 0.4947 0.4531 0.7325 0.099 Uiso 1 1 calc R . . C72 C 0.5705(2) 0.67167(18) 0.67841(14) 0.0553(8) Uani 1 1 d . . . H72A H 0.5624 0.6739 0.7169 0.066 Uiso 1 1 calc R . . H72B H 0.5180 0.6974 0.6518 0.066 Uiso 1 1 calc R . . C73 C 0.6624(2) 0.70959(17) 0.67935(12) 0.0524(7) Uani 1 1 d . . . H73A H 0.6604 0.7603 0.6914 0.063 Uiso 1 1 calc R . . H73B H 0.7143 0.6855 0.7078 0.063 Uiso 1 1 calc R . . C74 C 0.6801(2) 0.70792(15) 0.62116(12) 0.0446(7) Uani 1 1 d . . . C75 C 0.78382(19) 0.66859(17) 0.56530(12) 0.0474(7) Uani 1 1 d . . . H75 H 0.7908 0.7197 0.5543 0.057 Uiso 1 1 calc R . . C76 C 0.8799(2) 0.6312(2) 0.57563(14) 0.0606(8) Uani 1 1 d . . . H76A H 0.8777 0.5842 0.5943 0.073 Uiso 1 1 calc R . . H76B H 0.8885 0.6210 0.5380 0.073 Uiso 1 1 calc R . . C77 C 0.9646(2) 0.6716(3) 0.61115(16) 0.0770(11) Uani 1 1 d . . . H77 H 0.9550 0.6838 0.6487 0.092 Uiso 1 1 calc R . . C78 C 1.0507(3) 0.6233(4) 0.6224(2) 0.1175(19) Uani 1 1 d . . . H78A H 1.0677 0.6178 0.5871 0.176 Uiso 1 1 calc R . . H78B H 1.0372 0.5758 0.6355 0.176 Uiso 1 1 calc R . . H78C H 1.1021 0.6454 0.6516 0.176 Uiso 1 1 calc R . . C79 C 0.9780(3) 0.7437(3) 0.5814(2) 0.1104(17) Uani 1 1 d . . . H79A H 0.9948 0.7328 0.5468 0.166 Uiso 1 1 calc R . . H79B H 1.0273 0.7720 0.6074 0.166 Uiso 1 1 calc R . . H79C H 0.9203 0.7713 0.5714 0.166 Uiso 1 1 calc R . . C80 C 0.71378(18) 0.63229(17) 0.51396(12) 0.0456(7) Uani 1 1 d . . . C81 C 0.6017(2) 0.53374(17) 0.47581(12) 0.0500(7) Uani 1 1 d . . . H81 H 0.6005 0.5580 0.4392 0.060 Uiso 1 1 calc R . . C82 C 0.6411(3) 0.4565(2) 0.47532(17) 0.0746(10) Uani 1 1 d . . . H82A H 0.6320 0.4290 0.5078 0.089 Uiso 1 1 calc R . . H82B H 0.6059 0.4319 0.4398 0.089 Uiso 1 1 calc R . . C83 C 0.7452(3) 0.4558(2) 0.47939(15) 0.0738(10) Uani 1 1 d . . . C84 C 0.7779(4) 0.4807(4) 0.4345(2) 0.1150(18) Uani 1 1 d . . . H84 H 0.7355 0.4952 0.3994 0.138 Uiso 1 1 calc R . . C85 C 0.8743(4) 0.4838(4) 0.4423(3) 0.144(3) Uani 1 1 d . . . H85 H 0.8962 0.5028 0.4128 0.173 Uiso 1 1 calc R . . C86 C 0.9367(4) 0.4597(4) 0.4920(3) 0.130(2) Uani 1 1 d . . . H86 H 1.0010 0.4597 0.4960 0.155 Uiso 1 1 calc R . . C87 C 0.9050(4) 0.4355(3) 0.5361(2) 0.1005(15) Uani 1 1 d . . . H87 H 0.9476 0.4198 0.5708 0.121 Uiso 1 1 calc R . . C88 C 0.8100(3) 0.4340(2) 0.52961(17) 0.0794(11) Uani 1 1 d . . . H88 H 0.7892 0.4177 0.5603 0.095 Uiso 1 1 calc R . . C89 C 0.5016(2) 0.53071(18) 0.47957(15) 0.0582(8) Uani 1 1 d . . . H89A H 0.5005 0.4986 0.5115 0.070 Uiso 1 1 calc R . . H89B H 0.4616 0.5088 0.4441 0.070 Uiso 1 1 calc R . . C90 C 0.4601(2) 0.60451(19) 0.48836(13) 0.0570(8) Uani 1 1 d . . . H90A H 0.3978 0.5966 0.4926 0.068 Uiso 1 1 calc R . . H90B H 0.4992 0.6262 0.5242 0.068 Uiso 1 1 calc R . . C91 C 0.45227(18) 0.65787(17) 0.43928(12) 0.0465(7) Uani 1 1 d . . . C92 C 0.4941(2) 0.78164(16) 0.41308(12) 0.0502(7) Uani 1 1 d . . . C93 C 0.5692(3) 0.83775(19) 0.44489(14) 0.0706(10) Uani 1 1 d . . . H93A H 0.5549 0.8552 0.4790 0.106 Uiso 1 1 calc R . . H93B H 0.5695 0.8784 0.4195 0.106 Uiso 1 1 calc R . . H93C H 0.6301 0.8147 0.4561 0.106 Uiso 1 1 calc R . . C94 C 0.3957(2) 0.8145(2) 0.39901(14) 0.0686(10) Uani 1 1 d . . . H94A H 0.3502 0.7789 0.3783 0.103 Uiso 1 1 calc R . . H94B H 0.3921 0.8575 0.3754 0.103 Uiso 1 1 calc R . . H94C H 0.3827 0.8276 0.4345 0.103 Uiso 1 1 calc R . . C95 C 0.5168(2) 0.76023(16) 0.35750(12) 0.0464(7) Uani 1 1 d . . . C96 C 0.6206(2) 0.6873(2) 0.31653(13) 0.0616(9) Uani 1 1 d . . . H96 H 0.5924 0.7189 0.2829 0.074 Uiso 1 1 calc R . . C97 C 0.7279(2) 0.6988(2) 0.33437(15) 0.0692(10) Uani 1 1 d . . . H97A H 0.7576 0.6643 0.3651 0.083 Uiso 1 1 calc R . . H97B H 0.7504 0.6880 0.3013 0.083 Uiso 1 1 calc R . . C98 C 0.7575(2) 0.7757(2) 0.35523(17) 0.0734(10) Uani 1 1 d . . . C99 C 0.8092(3) 0.7875(3) 0.4114(2) 0.0890(13) Uani 1 1 d . . . H99 H 0.8262 0.7476 0.4365 0.107 Uiso 1 1 calc R . . C100 C 0.8370(4) 0.8567(4) 0.4318(3) 0.1187(18) Uani 1 1 d . . . H100 H 0.8733 0.8637 0.4702 0.142 Uiso 1 1 calc R . . C101 C 0.8112(4) 0.9138(4) 0.3960(3) 0.129(2) Uani 1 1 d . . . H101 H 0.8294 0.9610 0.4098 0.155 Uiso 1 1 calc R . . C102 C 0.7587(4) 0.9047(4) 0.3395(4) 0.148(3) Uani 1 1 d . . . H102 H 0.7415 0.9452 0.3149 0.178 Uiso 1 1 calc R . . C103 C 0.7311(3) 0.8341(3) 0.3189(2) 0.1090(16) Uani 1 1 d . . . H103 H 0.6947 0.8270 0.2806 0.131 Uiso 1 1 calc R . . C104 C 0.5941(3) 0.6091(2) 0.29852(13) 0.0634(9) Uani 1 1 d . . . H104 H 0.6338 0.5833 0.2820 0.076 Uiso 1 1 calc R . . C105 C 0.5211(3) 0.5745(2) 0.30391(14) 0.0666(10) Uani 1 1 d . . . H105 H 0.4856 0.5979 0.3247 0.080 Uiso 1 1 calc R . . C106 C 0.4895(3) 0.5016(2) 0.28003(17) 0.0784(11) Uani 1 1 d . . . C107 C 0.5316(5) 0.3826(4) 0.2549(4) 0.196(4) Uani 1 1 d D . . H10A H 0.4807 0.3660 0.2694 0.235 Uiso 1 1 calc R . . H10B H 0.5082 0.3840 0.2128 0.235 Uiso 1 1 calc R . . C108 C 0.6043(8) 0.3340(5) 0.2714(6) 0.297(8) Uani 1 1 d D . . H10C H 0.6187 0.3244 0.3123 0.446 Uiso 1 1 calc R . . H10D H 0.6588 0.3545 0.2634 0.446 Uiso 1 1 calc R . . H10E H 0.5869 0.2889 0.2502 0.446 Uiso 1 1 calc R . . N1 N -0.24216(16) 1.08951(13) 0.70352(9) 0.0469(6) Uani 1 1 d . . . H1 H -0.2984 1.0961 0.6808 0.056 Uiso 1 1 calc R . . N2 N -0.22864(16) 1.04547(14) 0.82015(10) 0.0479(6) Uani 1 1 d . . . H2 H -0.2806 1.0364 0.7936 0.057 Uiso 1 1 calc R . . N3 N -0.02101(17) 0.93637(14) 0.83066(10) 0.0511(6) Uani 1 1 d . . . H3 H -0.0498 0.9610 0.8001 0.061 Uiso 1 1 calc R . . N4 N 0.06500(16) 1.03066(13) 0.92538(10) 0.0472(6) Uani 1 1 d . . . H4 H 0.0112 1.0415 0.9012 0.057 Uiso 1 1 calc R . . N5 N 0.08480(16) 0.87605(13) 1.02768(9) 0.0470(6) Uani 1 1 d . . . H5 H 0.0559 0.8730 0.9911 0.056 Uiso 1 1 calc R . . N6 N 0.27732(16) 0.88728(14) 1.05098(10) 0.0502(6) Uani 1 1 d . . . H6 H 0.2362 0.9094 1.0232 0.060 Uiso 1 1 calc R . . N7 N 0.82754(16) 0.50960(13) 0.77625(9) 0.0469(6) Uani 1 1 d . . . H7 H 0.8288 0.5030 0.8118 0.056 Uiso 1 1 calc R . . N8 N 0.64576(16) 0.55169(13) 0.70119(10) 0.0474(6) Uani 1 1 d . . . H8 H 0.6566 0.5595 0.7378 0.057 Uiso 1 1 calc R . . N9 N 0.75549(16) 0.67040(13) 0.61796(9) 0.0456(6) Uani 1 1 d . . . H9 H 0.7883 0.6466 0.6480 0.055 Uiso 1 1 calc R . . N10 N 0.66352(16) 0.57623(13) 0.52381(10) 0.0456(6) Uani 1 1 d . . . H10F H 0.6673 0.5646 0.5590 0.055 Uiso 1 1 calc R . . N11 N 0.50322(15) 0.71952(13) 0.45317(9) 0.0441(5) Uani 1 1 d . . . H11 H 0.5432 0.7229 0.4872 0.053 Uiso 1 1 calc R . . N12 N 0.58310(17) 0.70966(14) 0.36269(10) 0.0513(6) Uani 1 1 d . . . H12 H 0.6053 0.6887 0.3960 0.062 Uiso 1 1 calc R . . O1 O -0.23510(14) 1.00272(12) 0.64098(8) 0.0613(6) Uani 1 1 d . . . O2 O -0.11538(14) 1.01433(11) 0.72465(8) 0.0521(5) Uani 1 1 d . . . O3 O -0.09477(13) 1.11134(11) 0.84628(8) 0.0523(5) Uani 1 1 d . . . O4 O -0.03443(15) 0.86119(12) 0.90198(9) 0.0588(5) Uani 1 1 d . . . O5 O 0.19309(14) 0.95751(13) 0.94429(9) 0.0590(5) Uani 1 1 d . . . O6 O 0.12295(16) 0.95087(13) 1.10532(8) 0.0620(6) Uani 1 1 d . . . O7 O 0.29832(16) 0.80235(13) 1.12218(9) 0.0672(6) Uani 1 1 d . . . O8 O 0.3376(2) 1.11449(16) 1.17819(12) 0.0955(9) Uani 1 1 d . . . O9 O 0.4130(2) 1.13424(16) 1.11281(12) 0.0997(9) Uani 1 1 d . . . O10 O 0.93332(15) 0.59472(12) 0.81235(8) 0.0596(6) Uani 1 1 d . . . O11 O 0.86979(13) 0.58566(11) 0.71474(8) 0.0522(5) Uani 1 1 d . . . O12 O 0.68654(14) 0.48989(11) 0.63191(8) 0.0526(5) Uani 1 1 d . . . O13 O 0.62763(14) 0.73896(11) 0.57855(8) 0.0542(5) Uani 1 1 d . . . O14 O 0.70962(14) 0.65437(12) 0.46487(8) 0.0566(5) Uani 1 1 d . . . O15 O 0.40185(14) 0.64537(12) 0.38967(8) 0.0584(5) Uani 1 1 d . . . O16 O 0.47771(15) 0.79238(13) 0.31145(9) 0.0631(6) Uani 1 1 d . . . O18 O 0.5612(2) 0.45863(17) 0.27757(15) 0.1102(11) Uani 1 1 d . . . O17 O 0.4096(2) 0.48224(17) 0.26308(14) 0.1001(10) Uani 1 1 d . . . C63 C 0.6985(2) 0.50323(15) 0.68370(11) 0.0424(6) Uani 1 1 d . . . O24 O 0.48503(19) 0.7962(2) 0.19483(11) 0.0991(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0606(18) 0.064(2) 0.0465(17) -0.0236(16) 0.0087(14) 0.0013(16) C2 0.104(3) 0.055(2) 0.069(2) -0.0117(19) 0.021(2) 0.000(2) C3 0.084(3) 0.113(4) 0.070(2) -0.054(2) -0.007(2) 0.019(2) C4 0.085(2) 0.073(2) 0.055(2) -0.0063(18) 0.0224(18) -0.003(2) C5 0.0557(17) 0.0440(17) 0.0325(14) -0.0029(12) 0.0065(13) -0.0023(14) C6 0.0559(16) 0.0341(16) 0.0379(15) -0.0003(12) 0.0004(12) 0.0072(13) C7 0.073(2) 0.0464(18) 0.0422(16) -0.0039(14) -0.0065(14) 0.0212(16) C8 0.071(2) 0.058(2) 0.0497(18) 0.0045(16) 0.0067(15) -0.0059(17) C9 0.0511(15) 0.0367(16) 0.0371(15) -0.0046(12) 0.0027(12) 0.0074(13) C10 0.0572(17) 0.0512(19) 0.0444(16) -0.0032(14) 0.0112(13) 0.0018(14) C11 0.075(2) 0.064(2) 0.0472(18) 0.0015(16) 0.0164(16) 0.0050(18) C12 0.067(2) 0.074(2) 0.0521(19) 0.0031(17) 0.0277(16) 0.0064(19) C13 0.077(2) 0.081(3) 0.064(2) 0.0031(19) 0.0298(18) 0.015(2) C14 0.089(3) 0.117(4) 0.068(2) 0.003(2) 0.028(2) 0.032(3) C15 0.079(3) 0.127(5) 0.109(4) -0.021(3) 0.038(3) -0.005(3) C16 0.101(4) 0.107(4) 0.127(4) -0.020(3) 0.063(3) -0.016(3) C17 0.095(3) 0.083(3) 0.083(3) 0.010(2) 0.045(2) 0.004(2) C18 0.0606(18) 0.051(2) 0.0565(19) 0.0076(15) 0.0116(15) 0.0007(15) C19 0.0643(18) 0.0476(19) 0.0493(17) -0.0028(14) 0.0037(14) 0.0036(15) C20 0.0609(17) 0.0407(17) 0.0420(16) -0.0044(14) 0.0055(14) 0.0083(15) C21 0.0550(16) 0.0542(19) 0.0386(15) 0.0056(13) 0.0094(13) 0.0117(14) C22 0.084(2) 0.109(3) 0.051(2) 0.016(2) 0.0263(18) -0.001(2) C23 0.088(3) 0.268(9) 0.052(3) 0.010(4) 0.023(2) -0.002(4) C24 0.186(6) 0.190(7) 0.142(5) -0.046(5) 0.095(5) 0.034(6) C25 0.178(6) 0.330(13) 0.103(4) 0.045(6) 0.079(4) -0.023(7) C26 0.0497(16) 0.0480(18) 0.0410(15) 0.0088(13) 0.0117(13) 0.0028(14) C27 0.0638(18) 0.0422(18) 0.0434(16) -0.0046(13) 0.0025(14) 0.0081(14) C28 0.075(2) 0.051(2) 0.080(2) 0.0004(18) 0.0148(19) 0.0020(17) C29 0.067(2) 0.048(2) 0.090(3) 0.0020(19) 0.009(2) 0.0034(17) C30 0.078(2) 0.088(3) 0.096(3) 0.023(2) 0.022(2) 0.008(2) C31 0.110(4) 0.129(5) 0.132(4) 0.048(4) 0.056(4) 0.029(3) C32 0.119(4) 0.129(5) 0.144(5) 0.028(4) 0.062(4) 0.014(4) C33 0.063(3) 0.145(5) 0.160(5) -0.013(4) 0.037(3) -0.005(3) C34 0.081(3) 0.105(4) 0.100(3) 0.000(3) 0.016(3) 0.007(3) C35 0.068(2) 0.060(2) 0.0524(19) -0.0033(16) 0.0122(16) 0.0117(17) C36 0.0614(18) 0.072(2) 0.0485(17) 0.0000(16) 0.0147(15) 0.0082(17) C37 0.0573(17) 0.054(2) 0.0333(15) 0.0024(13) 0.0082(13) -0.0068(14) C38 0.0653(18) 0.0373(17) 0.0353(14) 0.0025(12) -0.0032(13) -0.0079(14) C39 0.094(3) 0.065(2) 0.0509(19) 0.0109(17) 0.0076(18) -0.029(2) C40 0.092(2) 0.056(2) 0.053(2) -0.0090(16) -0.0109(18) -0.0013(19) C41 0.0671(18) 0.0444(18) 0.0309(14) -0.0037(13) 0.0052(14) 0.0054(15) C42 0.0550(17) 0.065(2) 0.0460(17) 0.0054(15) -0.0017(14) -0.0036(15) C43 0.0605(19) 0.092(3) 0.063(2) 0.010(2) 0.0184(16) 0.0002(19) C44 0.0610(19) 0.080(3) 0.059(2) 0.0006(19) 0.0128(17) 0.0118(18) C45 0.077(2) 0.091(3) 0.077(3) -0.005(2) 0.010(2) 0.015(2) C46 0.114(3) 0.109(4) 0.079(3) -0.025(3) 0.020(3) 0.007(3) C47 0.141(4) 0.091(4) 0.106(4) -0.024(3) 0.048(3) 0.011(3) C48 0.150(4) 0.078(3) 0.099(4) -0.003(3) 0.043(3) 0.020(3) C49 0.106(3) 0.092(4) 0.074(3) 0.012(3) 0.023(2) 0.026(3) C50 0.066(2) 0.066(2) 0.0510(18) 0.0033(17) 0.0040(16) -0.0176(18) C51 0.075(2) 0.063(2) 0.0399(17) 0.0024(15) 0.0010(16) -0.0187(18) C52 0.091(2) 0.072(3) 0.0414(19) 0.0006(18) 0.0050(18) -0.017(2) C53 0.197(6) 0.078(4) 0.100(4) -0.017(3) 0.034(4) -0.064(4) C54 0.407(16) 0.065(4) 0.208(8) -0.021(5) -0.074(9) 0.005(6) C55 0.071(2) 0.059(2) 0.0455(17) -0.0084(15) 0.0109(15) -0.0247(17) C56 0.113(3) 0.115(4) 0.048(2) -0.017(2) 0.010(2) -0.059(3) C57 0.099(3) 0.055(2) 0.079(3) -0.010(2) 0.014(2) -0.010(2) C58 0.066(2) 0.087(3) 0.074(2) -0.007(2) 0.0156(18) -0.012(2) C59 0.0552(16) 0.0437(17) 0.0318(15) -0.0008(12) -0.0012(13) -0.0034(13) C60 0.0615(17) 0.0339(15) 0.0343(14) -0.0001(12) 0.0029(12) -0.0029(13) C61 0.074(2) 0.0465(19) 0.0523(18) -0.0015(15) -0.0035(16) 0.0098(16) C62 0.075(2) 0.0390(17) 0.0484(17) 0.0083(14) -0.0003(15) -0.0156(15) C64 0.0523(16) 0.0467(18) 0.0417(15) 0.0050(13) 0.0088(12) 0.0055(14) C65 0.0533(17) 0.072(2) 0.0511(19) 0.0018(16) 0.0044(14) -0.0036(16) C66 0.0596(19) 0.074(3) 0.063(2) -0.0072(19) 0.0142(16) -0.0184(19) C67 0.102(3) 0.081(3) 0.148(5) -0.010(3) 0.074(3) -0.010(3) C68 0.129(4) 0.138(6) 0.166(6) -0.060(5) 0.092(4) -0.035(4) C69 0.147(6) 0.172(7) 0.109(5) -0.031(5) 0.069(4) -0.064(5) C70 0.095(3) 0.165(6) 0.074(3) 0.014(3) 0.013(3) -0.055(4) C71 0.063(2) 0.110(3) 0.066(2) 0.018(2) 0.0065(18) -0.018(2) C72 0.0655(19) 0.051(2) 0.0484(17) 0.0055(14) 0.0160(14) 0.0048(15) C73 0.0629(18) 0.0446(18) 0.0455(17) -0.0021(13) 0.0096(14) -0.0021(14) C74 0.0521(16) 0.0344(16) 0.0432(16) 0.0014(12) 0.0078(13) -0.0071(13) C75 0.0506(15) 0.0471(18) 0.0398(15) 0.0109(13) 0.0062(12) 0.0043(13) C76 0.0519(16) 0.074(2) 0.0510(18) 0.0078(16) 0.0070(14) 0.0109(16) C77 0.0516(18) 0.119(4) 0.058(2) -0.004(2) 0.0110(16) -0.001(2) C78 0.057(2) 0.188(6) 0.095(3) -0.002(3) 0.004(2) 0.027(3) C79 0.073(3) 0.121(4) 0.139(4) -0.028(4) 0.036(3) -0.031(3) C80 0.0420(14) 0.0498(18) 0.0426(16) 0.0097(13) 0.0091(12) 0.0049(13) C81 0.0615(18) 0.0446(18) 0.0393(15) -0.0009(13) 0.0080(13) 0.0029(14) C82 0.094(3) 0.059(2) 0.066(2) 0.0038(18) 0.0167(19) 0.017(2) C83 0.094(3) 0.068(2) 0.059(2) 0.0007(18) 0.0214(19) 0.030(2) C84 0.112(4) 0.172(5) 0.064(3) 0.025(3) 0.032(3) 0.052(4) C85 0.108(4) 0.240(8) 0.102(4) 0.019(5) 0.058(3) 0.054(5) C86 0.092(3) 0.196(6) 0.103(4) 0.012(4) 0.034(3) 0.066(4) C87 0.101(3) 0.112(4) 0.085(3) 0.013(3) 0.022(3) 0.046(3) C88 0.097(3) 0.071(3) 0.072(2) 0.0127(19) 0.028(2) 0.028(2) C89 0.0602(18) 0.0486(19) 0.061(2) 0.0065(15) 0.0109(15) -0.0074(15) C90 0.0551(17) 0.062(2) 0.0513(18) 0.0068(15) 0.0116(14) -0.0042(15) C91 0.0417(14) 0.0473(18) 0.0438(16) -0.0044(13) 0.0024(13) 0.0016(13) C92 0.0650(18) 0.0419(17) 0.0340(14) -0.0029(12) -0.0005(13) 0.0072(14) C93 0.104(3) 0.0454(19) 0.0491(18) -0.0067(15) 0.0020(18) -0.0131(18) C94 0.080(2) 0.065(2) 0.0538(19) 0.0000(17) 0.0086(17) 0.0295(19) C95 0.0492(15) 0.0398(16) 0.0409(16) 0.0027(13) -0.0011(13) -0.0050(13) C96 0.0624(19) 0.076(2) 0.0408(17) 0.0021(16) 0.0062(14) 0.0084(17) C97 0.065(2) 0.087(3) 0.057(2) 0.0093(19) 0.0204(16) 0.0062(19) C98 0.0542(19) 0.086(3) 0.075(3) 0.016(2) 0.0108(18) -0.0033(19) C99 0.083(3) 0.098(4) 0.086(3) 0.011(2) 0.024(2) -0.029(2) C100 0.113(4) 0.115(5) 0.120(4) 0.013(4) 0.022(3) -0.042(4) C101 0.087(3) 0.105(5) 0.172(6) -0.019(4) 0.004(4) -0.030(3) C102 0.104(4) 0.091(4) 0.212(7) 0.042(4) -0.012(4) -0.016(3) C103 0.084(3) 0.098(4) 0.116(4) 0.025(3) -0.015(2) -0.007(3) C104 0.065(2) 0.075(2) 0.0437(17) -0.0101(16) 0.0050(15) 0.0143(19) C105 0.060(2) 0.078(3) 0.0500(19) -0.0146(17) -0.0009(15) 0.0153(19) C106 0.074(2) 0.074(3) 0.072(2) -0.018(2) -0.0028(19) 0.016(2) C107 0.140(5) 0.115(5) 0.270(9) -0.134(6) -0.037(5) 0.038(4) C108 0.246(12) 0.086(5) 0.47(2) -0.002(8) -0.037(12) 0.004(7) N1 0.0489(12) 0.0440(14) 0.0365(12) -0.0049(10) -0.0048(10) 0.0080(11) N2 0.0494(13) 0.0493(15) 0.0375(13) -0.0009(11) 0.0017(10) 0.0023(12) N3 0.0630(15) 0.0484(15) 0.0354(12) 0.0048(11) 0.0045(11) 0.0114(12) N4 0.0450(12) 0.0477(15) 0.0411(13) 0.0025(11) 0.0006(10) 0.0082(11) N5 0.0563(13) 0.0469(15) 0.0283(11) -0.0015(11) -0.0021(10) -0.0080(11) N6 0.0541(14) 0.0500(15) 0.0382(13) 0.0098(11) 0.0008(11) -0.0002(12) N7 0.0622(14) 0.0450(15) 0.0269(11) -0.0004(10) 0.0033(10) -0.0079(12) N8 0.0583(14) 0.0460(15) 0.0329(12) 0.0049(10) 0.0059(11) 0.0017(12) N9 0.0504(13) 0.0445(14) 0.0360(12) 0.0062(10) 0.0039(10) 0.0010(11) N10 0.0540(13) 0.0442(15) 0.0352(12) 0.0065(10) 0.0082(10) -0.0015(11) N11 0.0483(12) 0.0439(14) 0.0322(11) -0.0014(10) -0.0004(9) 0.0025(11) N12 0.0630(15) 0.0519(16) 0.0327(12) 0.0044(11) 0.0042(11) 0.0049(13) O1 0.0597(12) 0.0622(14) 0.0470(12) -0.0204(10) -0.0072(9) 0.0150(11) O2 0.0579(12) 0.0501(13) 0.0379(10) -0.0017(9) -0.0019(9) 0.0132(10) O3 0.0558(11) 0.0444(12) 0.0433(11) -0.0022(9) -0.0057(9) 0.0029(9) O4 0.0710(13) 0.0521(13) 0.0449(12) 0.0062(10) 0.0040(10) 0.0035(11) O5 0.0548(12) 0.0687(15) 0.0471(12) 0.0118(10) 0.0055(9) 0.0218(11) O6 0.0758(13) 0.0635(14) 0.0380(11) -0.0081(10) 0.0036(10) -0.0035(11) O7 0.0756(14) 0.0652(15) 0.0436(12) 0.0162(10) -0.0090(10) -0.0004(12) O8 0.139(2) 0.080(2) 0.0658(17) -0.0106(15) 0.0284(17) -0.0328(18) O9 0.151(3) 0.0714(18) 0.0754(17) -0.0060(15) 0.0321(18) -0.0459(19) O10 0.0722(13) 0.0623(14) 0.0360(11) -0.0041(10) 0.0032(9) -0.0240(11) O11 0.0581(11) 0.0506(13) 0.0377(11) 0.0025(9) -0.0016(9) -0.0080(10) O12 0.0700(13) 0.0477(12) 0.0312(10) 0.0003(9) 0.0010(9) 0.0015(10) O13 0.0581(11) 0.0510(13) 0.0466(11) 0.0082(10) 0.0050(9) 0.0070(10) O14 0.0560(11) 0.0679(15) 0.0410(11) 0.0172(10) 0.0070(9) -0.0008(10) O15 0.0561(11) 0.0622(14) 0.0446(12) -0.0065(10) -0.0040(9) -0.0077(10) O16 0.0697(13) 0.0680(15) 0.0405(11) 0.0135(10) -0.0010(10) 0.0105(11) O18 0.0880(19) 0.080(2) 0.137(3) -0.0405(19) -0.0063(17) 0.0208(17) O17 0.0769(18) 0.093(2) 0.108(2) -0.0301(17) -0.0076(16) 0.0009(16) C63 0.0536(15) 0.0327(15) 0.0346(14) -0.0008(12) 0.0036(12) -0.0073(13) O24 0.0813(17) 0.142(3) 0.0643(15) 0.0212(17) 0.0063(13) 0.0072(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.458(4) . ? C1 C4 1.496(5) . ? C1 C2 1.516(5) . ? C1 C3 1.522(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O2 1.212(3) . ? C5 N1 1.331(4) . ? C5 O1 1.352(3) . ? C6 N1 1.471(3) . ? C6 C7 1.511(4) . ? C6 C8 1.517(5) . ? C6 C9 1.533(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O3 1.234(3) . ? C9 N2 1.334(4) . ? C10 N2 1.449(4) . ? C10 C18 1.515(5) . ? C10 C11 1.545(4) . ? C10 H10 0.9800 . ? C11 C12 1.491(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.363(5) . ? C12 C13 1.389(5) . ? C13 C14 1.392(6) . ? C13 H13 0.9300 . ? C14 C15 1.377(7) . ? C14 H14 0.9300 . ? C15 C16 1.371(7) . ? C15 H15 0.9300 . ? C16 C17 1.411(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.526(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.492(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O4 1.235(3) . ? C20 N3 1.342(4) . ? C21 N3 1.443(4) . ? C21 C22 1.495(5) . ? C21 C26 1.521(4) . ? C21 H21 0.9800 . ? C22 C23 1.508(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C25 1.532(9) . ? C23 C24 1.585(10) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O5 1.225(3) . ? C26 N4 1.326(4) . ? C27 N4 1.454(4) . ? C27 C35 1.527(5) . ? C27 C28 1.534(5) . ? C27 H27 0.9800 . ? C28 C29 1.482(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.348(5) . ? C29 C34 1.377(6) . ? C30 C31 1.370(7) . ? C30 H30 0.9300 . ? C31 C32 1.352(8) . ? C31 H31 0.9300 . ? C32 C33 1.404(8) . ? C32 H32 0.9300 . ? C33 C34 1.361(7) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.505(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.498(4) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 O6 1.236(3) . ? C37 N5 1.324(4) . ? C38 N5 1.460(4) . ? C38 C40 1.512(4) . ? C38 C39 1.519(5) . ? C38 C41 1.526(4) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 O7 1.242(3) . ? C41 N6 1.314(4) . ? C42 N6 1.445(4) . ? C42 C50 1.496(5) . ? C42 C43 1.530(5) . ? C42 H42 0.9800 . ? C43 C44 1.501(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.361(5) . ? C44 C49 1.409(6) . ? C45 C46 1.394(7) . ? C45 H45 0.9300 . ? C46 C47 1.344(7) . ? C46 H46 0.9300 . ? C47 C48 1.376(7) . ? C47 H47 0.9300 . ? C48 C49 1.356(7) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C51 1.299(5) . ? C50 H50 0.9300 . ? C51 C52 1.449(5) . ? C51 H51 0.9300 . ? C52 O8 1.200(4) . ? C52 O9 1.327(5) . ? C53 C54 1.375(8) . ? C53 O9 1.443(5) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 O10 1.479(4) . ? C55 C58 1.498(5) . ? C55 C56 1.511(4) . ? C55 C57 1.516(5) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 O11 1.216(3) . ? C59 N7 1.319(4) . ? C59 O10 1.343(3) . ? C60 N7 1.463(3) . ? C60 C61 1.518(5) . ? C60 C62 1.522(4) . ? C60 C63 1.545(4) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C64 N8 1.464(3) . ? C64 C72 1.513(4) . ? C64 C65 1.534(4) . ? C64 H64 0.9800 . ? C65 C66 1.501(5) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.357(6) . ? C66 C71 1.361(5) . ? C67 C68 1.420(8) . ? C67 H67 0.9300 . ? C68 C69 1.375(10) . ? C68 H68 0.9300 . ? C69 C70 1.309(9) . ? C69 H69 0.9300 . ? C70 C71 1.380(7) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 C73 1.523(4) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.501(4) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 O13 1.226(3) . ? C74 N9 1.332(4) . ? C75 N9 1.450(4) . ? C75 C80 1.511(4) . ? C75 C76 1.532(4) . ? C75 H75 0.9800 . ? C76 C77 1.488(5) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C78 1.509(6) . ? C77 C79 1.533(7) . ? C77 H77 0.9800 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 O14 1.232(3) . ? C80 N10 1.325(4) . ? C81 N10 1.464(4) . ? C81 C89 1.517(4) . ? C81 C82 1.521(5) . ? C81 H81 0.9800 . ? C82 C83 1.520(6) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C88 1.361(5) . ? C83 C84 1.384(6) . ? C84 C85 1.389(7) . ? C84 H84 0.9300 . ? C85 C86 1.352(7) . ? C85 H85 0.9300 . ? C86 C87 1.356(7) . ? C86 H86 0.9300 . ? C87 C88 1.373(6) . ? C87 H87 0.9300 . ? C88 H88 0.9300 . ? C89 C90 1.517(5) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 C91 1.506(4) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 O15 1.228(3) . ? C91 N11 1.338(4) . ? C92 N11 1.465(4) . ? C92 C94 1.521(4) . ? C92 C95 1.524(4) . ? C92 C93 1.537(4) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 O16 1.235(3) . ? C95 N12 1.325(4) . ? C96 N12 1.441(4) . ? C96 C104 1.503(5) . ? C96 C97 1.537(5) . ? C96 H96 0.9800 . ? C97 C98 1.505(6) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 C99 1.359(6) . ? C98 C103 1.358(6) . ? C99 C100 1.368(7) . ? C99 H99 0.9300 . ? C100 C101 1.332(8) . ? C100 H100 0.9300 . ? C101 C102 1.363(8) . ? C101 H101 0.9300 . ? C102 C103 1.393(8) . ? C102 H102 0.9300 . ? C103 H103 0.9300 . ? C104 C105 1.292(5) . ? C104 H104 0.9300 . ? C105 C106 1.466(6) . ? C105 H105 0.9300 . ? C106 O17 1.187(4) . ? C106 O18 1.335(5) . ? C107 C108 1.359(9) . ? C107 O18 1.502(6) . ? C107 H10A 0.9700 . ? C107 H10B 0.9700 . ? C108 H10C 0.9600 . ? C108 H10D 0.9600 . ? C108 H10E 0.9600 . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 H4 0.8600 . ? N5 H5 0.8600 . ? N6 H6 0.8600 . ? N7 H7 0.8600 . ? N8 C63 1.327(4) . ? N8 H8 0.8600 . ? N9 H9 0.8600 . ? N10 H10F 0.8600 . ? N11 H11 0.8600 . ? N12 H12 0.8600 . ? O12 C63 1.231(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C4 110.4(3) . . ? O1 C1 C2 111.1(3) . . ? C4 C1 C2 111.9(3) . . ? O1 C1 C3 101.7(3) . . ? C4 C1 C3 111.0(3) . . ? C2 C1 C3 110.3(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 N1 125.3(2) . . ? O2 C5 O1 124.2(3) . . ? N1 C5 O1 110.5(2) . . ? N1 C6 C7 107.1(2) . . ? N1 C6 C8 110.3(2) . . ? C7 C6 C8 110.3(3) . . ? N1 C6 C9 110.6(2) . . ? C7 C6 C9 108.5(2) . . ? C8 C6 C9 110.1(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 N2 121.8(3) . . ? O3 C9 C6 121.0(3) . . ? N2 C9 C6 117.0(2) . . ? N2 C10 C18 110.5(2) . . ? N2 C10 C11 111.8(3) . . ? C18 C10 C11 114.2(3) . . ? N2 C10 H10 106.6 . . ? C18 C10 H10 106.6 . . ? C11 C10 H10 106.6 . . ? C12 C11 C10 113.8(3) . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C17 C12 C13 118.8(3) . . ? C17 C12 C11 121.4(3) . . ? C13 C12 C11 119.8(3) . . ? C12 C13 C14 120.9(4) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C15 C14 C13 119.2(5) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 121.3(5) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 118.4(5) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C12 C17 C16 121.5(4) . . ? C12 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C10 C18 C19 111.2(3) . . ? C10 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C10 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C20 C19 C18 111.5(2) . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? O4 C20 N3 121.5(3) . . ? O4 C20 C19 121.4(3) . . ? N3 C20 C19 117.2(3) . . ? N3 C21 C22 111.4(2) . . ? N3 C21 C26 114.3(2) . . ? C22 C21 C26 109.1(3) . . ? N3 C21 H21 107.2 . . ? C22 C21 H21 107.2 . . ? C26 C21 H21 107.2 . . ? C21 C22 C23 118.2(4) . . ? C21 C22 H22A 107.8 . . ? C23 C22 H22A 107.8 . . ? C21 C22 H22B 107.8 . . ? C23 C22 H22B 107.8 . . ? H22A C22 H22B 107.1 . . ? C22 C23 C25 109.0(6) . . ? C22 C23 C24 111.3(4) . . ? C25 C23 C24 111.5(6) . . ? C22 C23 H23 108.3 . . ? C25 C23 H23 108.3 . . ? C24 C23 H23 108.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O5 C26 N4 124.1(3) . . ? O5 C26 C21 117.8(3) . . ? N4 C26 C21 118.1(2) . . ? N4 C27 C35 111.9(3) . . ? N4 C27 C28 109.4(3) . . ? C35 C27 C28 109.4(3) . . ? N4 C27 H27 108.7 . . ? C35 C27 H27 108.7 . . ? C28 C27 H27 108.7 . . ? C29 C28 C27 115.3(3) . . ? C29 C28 H28A 108.5 . . ? C27 C28 H28A 108.5 . . ? C29 C28 H28B 108.5 . . ? C27 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C30 C29 C34 118.0(4) . . ? C30 C29 C28 120.6(3) . . ? C34 C29 C28 121.4(4) . . ? C29 C30 C31 123.7(4) . . ? C29 C30 H30 118.2 . . ? C31 C30 H30 118.2 . . ? C32 C31 C30 118.9(5) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? C31 C32 C33 118.5(5) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C34 C33 C32 121.3(5) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C29 119.7(5) . . ? C33 C34 H34 120.2 . . ? C29 C34 H34 120.2 . . ? C36 C35 C27 114.8(3) . . ? C36 C35 H35A 108.6 . . ? C27 C35 H35A 108.6 . . ? C36 C35 H35B 108.6 . . ? C27 C35 H35B 108.6 . . ? H35A C35 H35B 107.5 . . ? C37 C36 C35 114.9(3) . . ? C37 C36 H36A 108.6 . . ? C35 C36 H36A 108.6 . . ? C37 C36 H36B 108.6 . . ? C35 C36 H36B 108.6 . . ? H36A C36 H36B 107.5 . . ? O6 C37 N5 122.4(3) . . ? O6 C37 C36 121.3(3) . . ? N5 C37 C36 116.3(3) . . ? N5 C38 C40 106.4(2) . . ? N5 C38 C39 109.5(3) . . ? C40 C38 C39 111.3(3) . . ? N5 C38 C41 111.6(2) . . ? C40 C38 C41 106.9(3) . . ? C39 C38 C41 110.9(2) . . ? 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 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O7 C41 N6 124.1(3) . . ? O7 C41 C38 119.0(3) . . ? N6 C41 C38 116.6(2) . . ? N6 C42 C50 112.0(3) . . ? N6 C42 C43 110.0(2) . . ? C50 C42 C43 111.8(3) . . ? N6 C42 H42 107.6 . . ? C50 C42 H42 107.6 . . ? C43 C42 H42 107.6 . . ? C44 C43 C42 114.4(3) . . ? C44 C43 H43A 108.7 . . ? C42 C43 H43A 108.7 . . ? C44 C43 H43B 108.7 . . ? C42 C43 H43B 108.7 . . ? H43A C43 H43B 107.6 . . ? C45 C44 C49 117.3(4) . . ? C45 C44 C43 121.1(4) . . ? C49 C44 C43 121.5(3) . . ? C44 C45 C46 121.2(4) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C47 C46 C45 120.3(5) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C48 119.9(5) . . ? C46 C47 H47 120.1 . . ? C48 C47 H47 120.1 . . ? C49 C48 C47 120.3(5) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C48 C49 C44 121.0(4) . . ? C48 C49 H49 119.5 . . ? C44 C49 H49 119.5 . . ? C51 C50 C42 125.3(3) . . ? C51 C50 H50 117.3 . . ? C42 C50 H50 117.3 . . ? C50 C51 C52 124.9(4) . . ? C50 C51 H51 117.6 . . ? C52 C51 H51 117.6 . . ? O8 C52 O9 122.3(4) . . ? O8 C52 C51 124.5(4) . . ? O9 C52 C51 113.2(3) . . ? C54 C53 O9 109.5(5) . . ? C54 C53 H53A 109.8 . . ? O9 C53 H53A 109.8 . . ? C54 C53 H53B 109.8 . . ? O9 C53 H53B 109.8 . . ? H53A C53 H53B 108.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O10 C55 C58 109.9(3) . . ? O10 C55 C56 101.9(3) . . ? C58 C55 C56 110.9(3) . . ? O10 C55 C57 109.7(3) . . ? C58 C55 C57 113.8(3) . . ? C56 C55 C57 110.0(3) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O11 C59 N7 124.8(2) . . ? O11 C59 O10 124.3(3) . . ? N7 C59 O10 110.9(2) . . ? N7 C60 C61 111.1(2) . . ? N7 C60 C62 107.3(2) . . ? C61 C60 C62 110.9(3) . . ? N7 C60 C63 110.6(2) . . ? C61 C60 C63 109.6(2) . . ? C62 C60 C63 107.3(2) . . ? 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 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N8 C64 C72 109.9(2) . . ? N8 C64 C65 110.8(3) . . ? C72 C64 C65 114.2(3) . . ? N8 C64 H64 107.2 . . ? C72 C64 H64 107.2 . . ? C65 C64 H64 107.2 . . ? C66 C65 C64 116.7(3) . . ? C66 C65 H65A 108.1 . . ? C64 C65 H65A 108.1 . . ? C66 C65 H65B 108.1 . . ? C64 C65 H65B 108.1 . . ? H65A C65 H65B 107.3 . . ? C67 C66 C71 117.8(4) . . ? C67 C66 C65 121.2(4) . . ? C71 C66 C65 121.0(4) . . ? C66 C67 C68 119.8(6) . . ? C66 C67 H67 120.1 . . ? C68 C67 H67 120.1 . . ? C69 C68 C67 120.0(6) . . ? C69 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C70 C69 C68 119.1(6) . . ? C70 C69 H69 120.5 . . ? C68 C69 H69 120.5 . . ? C69 C70 C71 121.5(6) . . ? C69 C70 H70 119.3 . . ? C71 C70 H70 119.3 . . ? C66 C71 C70 121.9(5) . . ? C66 C71 H71 119.0 . . ? C70 C71 H71 119.0 . . ? C64 C72 C73 111.4(3) . . ? C64 C72 H72A 109.3 . . ? C73 C72 H72A 109.3 . . ? C64 C72 H72B 109.3 . . ? C73 C72 H72B 109.3 . . ? H72A C72 H72B 108.0 . . ? C74 C73 C72 112.4(2) . . ? C74 C73 H73A 109.1 . . ? C72 C73 H73A 109.1 . . ? C74 C73 H73B 109.1 . . ? C72 C73 H73B 109.1 . . ? H73A C73 H73B 107.8 . . ? O13 C74 N9 121.6(3) . . ? O13 C74 C73 121.8(3) . . ? N9 C74 C73 116.6(2) . . ? N9 C75 C80 114.7(2) . . ? N9 C75 C76 111.5(2) . . ? C80 C75 C76 108.7(2) . . ? N9 C75 H75 107.2 . . ? C80 C75 H75 107.2 . . ? C76 C75 H75 107.2 . . ? C77 C76 C75 117.5(3) . . ? C77 C76 H76A 107.9 . . ? C75 C76 H76A 107.9 . . ? C77 C76 H76B 107.9 . . ? C75 C76 H76B 107.9 . . ? H76A C76 H76B 107.2 . . ? C76 C77 C78 110.0(4) . . ? C76 C77 C79 111.0(3) . . ? C78 C77 C79 111.1(4) . . ? C76 C77 H77 108.2 . . ? C78 C77 H77 108.2 . . ? C79 C77 H77 108.2 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O14 C80 N10 123.5(3) . . ? O14 C80 C75 118.0(3) . . ? N10 C80 C75 118.5(2) . . ? N10 C81 C89 111.6(2) . . ? N10 C81 C82 109.9(2) . . ? C89 C81 C82 110.6(3) . . ? N10 C81 H81 108.2 . . ? C89 C81 H81 108.2 . . ? C82 C81 H81 108.2 . . ? C83 C82 C81 113.1(3) . . ? C83 C82 H82A 109.0 . . ? C81 C82 H82A 109.0 . . ? C83 C82 H82B 109.0 . . ? C81 C82 H82B 109.0 . . ? H82A C82 H82B 107.8 . . ? C88 C83 C84 118.0(4) . . ? C88 C83 C82 119.8(4) . . ? C84 C83 C82 122.1(3) . . ? C83 C84 C85 119.6(4) . . ? C83 C84 H84 120.2 . . ? C85 C84 H84 120.2 . . ? C86 C85 C84 120.9(5) . . ? C86 C85 H85 119.5 . . ? C84 C85 H85 119.5 . . ? C85 C86 C87 119.5(5) . . ? C85 C86 H86 120.2 . . ? C87 C86 H86 120.2 . . ? C86 C87 C88 120.0(4) . . ? C86 C87 H87 120.0 . . ? C88 C87 H87 120.0 . . ? C83 C88 C87 121.8(4) . . ? C83 C88 H88 119.1 . . ? C87 C88 H88 119.1 . . ? C81 C89 C90 115.0(3) . . ? C81 C89 H89A 108.5 . . ? C90 C89 H89A 108.5 . . ? C81 C89 H89B 108.5 . . ? C90 C89 H89B 108.5 . . ? H89A C89 H89B 107.5 . . ? C91 C90 C89 113.5(3) . . ? C91 C90 H90A 108.9 . . ? C89 C90 H90A 108.9 . . ? C91 C90 H90B 108.9 . . ? C89 C90 H90B 108.9 . . ? H90A C90 H90B 107.7 . . ? O15 C91 N11 122.3(3) . . ? O15 C91 C90 121.8(3) . . ? N11 C91 C90 115.9(2) . . ? N11 C92 C94 110.1(3) . . ? N11 C92 C95 112.4(2) . . ? C94 C92 C95 110.6(2) . . ? N11 C92 C93 105.8(2) . . ? C94 C92 C93 111.0(3) . . ? C95 C92 C93 106.9(3) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C92 C94 H94A 109.5 . . ? C92 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C92 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? O16 C95 N12 123.4(3) . . ? O16 C95 C92 120.0(3) . . ? N12 C95 C92 116.5(2) . . ? N12 C96 C104 111.2(3) . . ? N12 C96 C97 110.6(3) . . ? C104 C96 C97 111.8(3) . . ? N12 C96 H96 107.7 . . ? C104 C96 H96 107.7 . . ? C97 C96 H96 107.7 . . ? C98 C97 C96 113.3(3) . . ? C98 C97 H97A 108.9 . . ? C96 C97 H97A 108.9 . . ? C98 C97 H97B 108.9 . . ? C96 C97 H97B 108.9 . . ? H97A C97 H97B 107.7 . . ? C99 C98 C103 119.1(4) . . ? C99 C98 C97 120.1(4) . . ? C103 C98 C97 120.7(4) . . ? C98 C99 C100 121.7(5) . . ? C98 C99 H99 119.2 . . ? C100 C99 H99 119.2 . . ? C101 C100 C99 119.0(5) . . ? C101 C100 H100 120.5 . . ? C99 C100 H100 120.5 . . ? C100 C101 C102 121.5(6) . . ? C100 C101 H101 119.3 . . ? C102 C101 H101 119.3 . . ? C101 C102 C103 119.2(6) . . ? C101 C102 H102 120.4 . . ? C103 C102 H102 120.4 . . ? C98 C103 C102 119.6(5) . . ? C98 C103 H103 120.2 . . ? C102 C103 H103 120.2 . . ? C105 C104 C96 125.9(3) . . ? C105 C104 H104 117.1 . . ? C96 C104 H104 117.1 . . ? C104 C105 C106 125.5(4) . . ? C104 C105 H105 117.3 . . ? C106 C105 H105 117.3 . . ? O17 C106 O18 122.6(4) . . ? O17 C106 C105 125.0(4) . . ? O18 C106 C105 112.3(3) . . ? C108 C107 O18 111.7(6) . . ? C108 C107 H10A 109.3 . . ? O18 C107 H10A 109.3 . . ? C108 C107 H10B 109.3 . . ? O18 C107 H10B 109.3 . . ? H10A C107 H10B 107.9 . . ? C107 C108 H10C 109.5 . . ? C107 C108 H10D 109.5 . . ? H10C C108 H10D 109.5 . . ? C107 C108 H10E 109.5 . . ? H10C C108 H10E 109.5 . . ? H10D C108 H10E 109.5 . . ? C5 N1 C6 122.0(2) . . ? C5 N1 H1 119.0 . . ? C6 N1 H1 119.0 . . ? C9 N2 C10 122.3(2) . . ? C9 N2 H2 118.8 . . ? C10 N2 H2 118.8 . . ? C20 N3 C21 122.1(2) . . ? C20 N3 H3 118.9 . . ? C21 N3 H3 118.9 . . ? C26 N4 C27 121.4(2) . . ? C26 N4 H4 119.3 . . ? C27 N4 H4 119.3 . . ? C37 N5 C38 123.8(2) . . ? C37 N5 H5 118.1 . . ? C38 N5 H5 118.1 . . ? C41 N6 C42 124.5(2) . . ? C41 N6 H6 117.7 . . ? C42 N6 H6 117.7 . . ? C59 N7 C60 122.2(2) . . ? C59 N7 H7 118.9 . . ? C60 N7 H7 118.9 . . ? C63 N8 C64 121.7(2) . . ? C63 N8 H8 119.1 . . ? C64 N8 H8 119.1 . . ? C74 N9 C75 121.9(2) . . ? C74 N9 H9 119.0 . . ? C75 N9 H9 119.0 . . ? C80 N10 C81 121.2(2) . . ? C80 N10 H10F 119.4 . . ? C81 N10 H10F 119.4 . . ? C91 N11 C92 123.1(2) . . ? C91 N11 H11 118.5 . . ? C92 N11 H11 118.5 . . ? C95 N12 C96 124.7(2) . . ? C95 N12 H12 117.7 . . ? C96 N12 H12 117.7 . . ? C5 O1 C1 121.1(2) . . ? C52 O9 C53 117.5(4) . . ? C59 O10 C55 120.8(2) . . ? C106 O18 C107 113.8(4) . . ? O12 C63 N8 122.1(2) . . ? O12 C63 C60 121.0(3) . . ? N8 C63 C60 116.8(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.204 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.039 #===End data_P3 _database_code_depnum_ccdc_archive 'CCDC 878073' #TrackingRef '- All peptide.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic 'Alpha-Gamma mixed peptide' _chemical_name_common HexaD _chemical_formula_moiety '2(C54 H78 N6 O9), O' _chemical_formula_sum 'C108 H156 N12 O19' _chemical_compound_source synthesis _exptl_crystal_recrystallization_method Acetone _chemical_melting_point ? _exptl_crystal_description 'square plate' _exptl_crystal_colour colorless _diffrn_ambient_temperature 100(2) _diffrn_ambient_pressure 101.325 _chemical_formula_weight 1926.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 _chemical_absolute_configuration syn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 18.113(14) _cell_length_b 24.50(2) _cell_length_c 27.36(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12140(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.054 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.976 _exptl_absorpt_correction_T_max 0.991 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Graphite monochromator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54184 _diffrn_reflns_av_R_equivalents 0.1117 _diffrn_reflns_av_sigmaI/netI 0.2367 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 28.28 _reflns_number_total 26203 _reflns_number_gt 8437 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^2^+0.7694P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.7(13) _refine_ls_number_reflns 26203 _refine_ls_number_parameters 1272 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.2236 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.2378 _refine_ls_wR_factor_gt 0.1896 _refine_ls_goodness_of_fit_ref 0.794 _refine_ls_restrained_S_all 0.798 _refine_ls_shift/su_max 2.090 _refine_ls_shift/su_mean 0.033 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3877(3) 0.6849(2) 0.15933(17) 0.0452(14) Uani 1 1 d . . . C2 C 0.4166(3) 0.6788(3) 0.10806(19) 0.0699(18) Uani 1 1 d . . . H2A H 0.4502 0.7080 0.1010 0.105 Uiso 1 1 calc R . . H2B H 0.3761 0.6800 0.0854 0.105 Uiso 1 1 calc R . . H2C H 0.4418 0.6445 0.1050 0.105 Uiso 1 1 calc R . . C3 C 0.3655(4) 0.7452(3) 0.1692(2) 0.078(2) Uani 1 1 d . . . H3A H 0.3501 0.7490 0.2026 0.118 Uiso 1 1 calc R . . H3B H 0.3257 0.7553 0.1480 0.118 Uiso 1 1 calc R . . H3C H 0.4072 0.7685 0.1632 0.118 Uiso 1 1 calc R . . C4 C 0.3236(3) 0.6479(3) 0.1713(2) 0.0691(18) Uani 1 1 d . . . H4A H 0.3364 0.6109 0.1634 0.104 Uiso 1 1 calc R . . H4B H 0.2812 0.6588 0.1527 0.104 Uiso 1 1 calc R . . H4C H 0.3125 0.6506 0.2056 0.104 Uiso 1 1 calc R . . C5 C 0.4825(3) 0.6269(3) 0.1961(2) 0.0461(14) Uani 1 1 d . . . C6 C 0.5915(2) 0.5832(2) 0.23160(17) 0.0410(13) Uani 1 1 d . . . C7 C 0.6338(3) 0.5768(2) 0.18271(19) 0.0587(16) Uani 1 1 d . . . H7A H 0.5993 0.5697 0.1568 0.088 Uiso 1 1 calc R . . H7B H 0.6678 0.5469 0.1852 0.088 Uiso 1 1 calc R . . H7C H 0.6605 0.6097 0.1758 0.088 Uiso 1 1 calc R . . C8 C 0.6458(3) 0.5957(2) 0.27319(19) 0.0542(15) Uani 1 1 d . . . H8A H 0.6730 0.6283 0.2656 0.081 Uiso 1 1 calc R . . H8B H 0.6795 0.5657 0.2769 0.081 Uiso 1 1 calc R . . H8C H 0.6190 0.6009 0.3031 0.081 Uiso 1 1 calc R . . C9 C 0.5514(2) 0.5297(2) 0.24377(16) 0.0324(11) Uani 1 1 d . . . C10 C 0.4652(3) 0.4839(2) 0.29836(17) 0.0461(14) Uani 1 1 d . . . H10A H 0.4688 0.4563 0.2726 0.055 Uiso 1 1 calc R . . C11 C 0.5028(3) 0.4600(3) 0.34417(18) 0.0556(16) Uani 1 1 d . . . H11A H 0.4782 0.4261 0.3525 0.067 Uiso 1 1 calc R . . H11B H 0.5535 0.4511 0.3359 0.067 Uiso 1 1 calc R . . C12 C 0.5036(4) 0.4954(3) 0.38825(19) 0.0638(18) Uani 1 1 d . . . C13 C 0.4458(4) 0.4973(4) 0.4209(2) 0.095(3) Uani 1 1 d . . . H13 H 0.4041 0.4762 0.4149 0.114 Uiso 1 1 calc R . . C14 C 0.4478(5) 0.5282(5) 0.4608(3) 0.123(4) Uani 1 1 d . . . H14 H 0.4088 0.5276 0.4829 0.147 Uiso 1 1 calc R . . C15 C 0.5064(8) 0.5603(4) 0.4691(3) 0.119(4) Uani 1 1 d . . . H15 H 0.5065 0.5825 0.4967 0.143 Uiso 1 1 calc R . . C16 C 0.5660(5) 0.5617(3) 0.4386(3) 0.095(3) Uani 1 1 d . . . H16 H 0.6060 0.5844 0.4450 0.115 Uiso 1 1 calc R . . C17 C 0.5645(4) 0.5276(3) 0.3972(2) 0.0729(19) Uani 1 1 d . . . H17 H 0.6046 0.5267 0.3760 0.087 Uiso 1 1 calc R . . C18 C 0.3829(2) 0.4958(2) 0.30583(17) 0.0451(13) Uani 1 1 d . . . H18A H 0.3774 0.5245 0.3301 0.054 Uiso 1 1 calc R . . H18B H 0.3588 0.4633 0.3183 0.054 Uiso 1 1 calc R . . C19 C 0.3449(3) 0.5134(2) 0.25869(16) 0.0470(14) Uani 1 1 d . . . H19A H 0.3679 0.5465 0.2467 0.056 Uiso 1 1 calc R . . H19B H 0.2935 0.5215 0.2655 0.056 Uiso 1 1 calc R . . C20 C 0.3491(3) 0.4698(2) 0.21967(19) 0.0433(13) Uani 1 1 d . . . C21 C 0.3949(3) 0.4461(2) 0.13813(16) 0.0460(14) Uani 1 1 d . . . H21 H 0.3443 0.4373 0.1281 0.055 Uiso 1 1 calc R . . C22 C 0.4332(4) 0.4739(3) 0.09494(19) 0.0660(17) Uani 1 1 d . . . H22A H 0.4444 0.4463 0.0707 0.079 Uiso 1 1 calc R . . H22B H 0.4798 0.4887 0.1064 0.079 Uiso 1 1 calc R . . C23 C 0.3905(5) 0.5197(3) 0.0699(2) 0.095(3) Uani 1 1 d . . . H23 H 0.3801 0.5478 0.0944 0.114 Uiso 1 1 calc R . . C24 C 0.3139(5) 0.4978(4) 0.0497(3) 0.126(3) Uani 1 1 d . . . H24A H 0.2928 0.5243 0.0280 0.188 Uiso 1 1 calc R . . H24B H 0.2808 0.4915 0.0766 0.188 Uiso 1 1 calc R . . H24C H 0.3216 0.4642 0.0324 0.188 Uiso 1 1 calc R . . C25 C 0.4379(7) 0.5451(4) 0.0303(2) 0.161(5) Uani 1 1 d . . . H25A H 0.4855 0.5540 0.0435 0.242 Uiso 1 1 calc R . . H25B H 0.4146 0.5778 0.0186 0.242 Uiso 1 1 calc R . . H25C H 0.4436 0.5198 0.0039 0.242 Uiso 1 1 calc R . . C26 C 0.4344(3) 0.3924(2) 0.14882(18) 0.0417(13) Uani 1 1 d . . . C27 C 0.5302(3) 0.3434(2) 0.19345(18) 0.0479(14) Uani 1 1 d . . . H27 H 0.5126 0.3139 0.1723 0.057 Uiso 1 1 calc R . . C28 C 0.6120(3) 0.3528(3) 0.18228(18) 0.0570(16) Uani 1 1 d . . . H28A H 0.6311 0.3797 0.2050 0.068 Uiso 1 1 calc R . . H28B H 0.6386 0.3190 0.1879 0.068 Uiso 1 1 calc R . . C29 C 0.6271(3) 0.3715(3) 0.1319(2) 0.0497(15) Uani 1 1 d . . . C30 C 0.6273(3) 0.3398(3) 0.0917(2) 0.0706(19) Uani 1 1 d . . . H30 H 0.6152 0.3032 0.0955 0.085 Uiso 1 1 calc R . . C31 C 0.6434(4) 0.3571(3) 0.0469(2) 0.083(2) Uani 1 1 d . . . H31 H 0.6410 0.3329 0.0208 0.100 Uiso 1 1 calc R . . C32 C 0.6639(4) 0.4107(4) 0.0389(2) 0.098(3) Uani 1 1 d . . . H32 H 0.6775 0.4230 0.0080 0.118 Uiso 1 1 calc R . . C33 C 0.6631(4) 0.4451(4) 0.0787(3) 0.093(2) Uani 1 1 d . . . H33 H 0.6742 0.4818 0.0745 0.112 Uiso 1 1 calc R . . C34 C 0.6461(3) 0.4259(3) 0.1249(2) 0.078(2) Uani 1 1 d . . . H34 H 0.6475 0.4495 0.1515 0.093 Uiso 1 1 calc R . . C35 C 0.5206(3) 0.3252(2) 0.24624(17) 0.0518(15) Uani 1 1 d . . . H35A H 0.5499 0.3491 0.2669 0.062 Uiso 1 1 calc R . . H35B H 0.5406 0.2887 0.2495 0.062 Uiso 1 1 calc R . . C36 C 0.4411(3) 0.3250(2) 0.26574(17) 0.0524(15) Uani 1 1 d . . . H36A H 0.4423 0.3175 0.3005 0.063 Uiso 1 1 calc R . . H36B H 0.4201 0.3611 0.2614 0.063 Uiso 1 1 calc R . . C37 C 0.3914(3) 0.2841(3) 0.24159(17) 0.0418(13) Uani 1 1 d . . . C38 C 0.2690(2) 0.2731(2) 0.2022(2) 0.0482(14) Uani 1 1 d . . . C39 C 0.2332(3) 0.2406(3) 0.2452(2) 0.0731(19) Uani 1 1 d . . . H39A H 0.2680 0.2146 0.2577 0.110 Uiso 1 1 calc R . . H39B H 0.1901 0.2218 0.2336 0.110 Uiso 1 1 calc R . . H39C H 0.2194 0.2655 0.2707 0.110 Uiso 1 1 calc R . . C40 C 0.2139(3) 0.3123(3) 0.1786(2) 0.0693(18) Uani 1 1 d . . . H40A H 0.1952 0.3369 0.2030 0.104 Uiso 1 1 calc R . . H40B H 0.1737 0.2919 0.1648 0.104 Uiso 1 1 calc R . . H40C H 0.2381 0.3327 0.1533 0.104 Uiso 1 1 calc R . . C41 C 0.2941(3) 0.2334(2) 0.1621(2) 0.0474(14) Uani 1 1 d . . . C42 C 0.3725(3) 0.2249(3) 0.0889(2) 0.0598(16) Uani 1 1 d . . . H42 H 0.3457 0.1904 0.0856 0.072 Uiso 1 1 calc R . . C43 C 0.3558(3) 0.2595(3) 0.0438(2) 0.0678(18) Uani 1 1 d . . . H43A H 0.3625 0.2371 0.0150 0.081 Uiso 1 1 calc R . . H43B H 0.3913 0.2890 0.0422 0.081 Uiso 1 1 calc R . . C44 C 0.2786(4) 0.2837(3) 0.04262(19) 0.0614(17) Uani 1 1 d . . . C45 C 0.2678(4) 0.3401(3) 0.0418(3) 0.079(2) Uani 1 1 d . . . H45 H 0.3081 0.3637 0.0421 0.095 Uiso 1 1 calc R . . C46 C 0.1985(5) 0.3603(4) 0.0405(3) 0.102(3) Uani 1 1 d . . . H46 H 0.1917 0.3979 0.0393 0.123 Uiso 1 1 calc R . . C47 C 0.1374(5) 0.3264(5) 0.0410(3) 0.101(3) Uani 1 1 d . . . H47 H 0.0903 0.3416 0.0408 0.122 Uiso 1 1 calc R . . C48 C 0.1455(4) 0.2709(4) 0.0416(3) 0.101(3) Uani 1 1 d . . . H48 H 0.1047 0.2478 0.0414 0.122 Uiso 1 1 calc R . . C49 C 0.2143(4) 0.2511(3) 0.0425(2) 0.079(2) Uani 1 1 d . . . H49 H 0.2202 0.2134 0.0431 0.095 Uiso 1 1 calc R . . C50 C 0.4543(3) 0.2118(2) 0.0917(2) 0.0601(16) Uani 1 1 d . . . H50A H 0.4821 0.2456 0.0930 0.072 Uiso 1 1 calc R . . H50B H 0.4689 0.1924 0.0624 0.072 Uiso 1 1 calc R . . C51 C 0.4732(3) 0.1774(3) 0.1363(2) 0.0623(17) Uani 1 1 d . . . H51A H 0.4597 0.1981 0.1652 0.075 Uiso 1 1 calc R . . H51B H 0.4423 0.1451 0.1356 0.075 Uiso 1 1 calc R . . C52 C 0.5502(4) 0.1595(3) 0.1421(3) 0.085(2) Uani 1 1 d . . . C53 C 0.6809(5) 0.1864(6) 0.1336(5) 0.189(6) Uani 1 1 d D . . H53A H 0.6990 0.2191 0.1495 0.227 Uiso 1 1 calc R . . H53B H 0.6900 0.1550 0.1544 0.227 Uiso 1 1 calc R . . C54 C 0.7102(9) 0.1800(10) 0.0903(6) 0.341(15) Uani 1 1 d D . . H54A H 0.6942 0.1459 0.0766 0.512 Uiso 1 1 calc R . . H54B H 0.7631 0.1800 0.0930 0.512 Uiso 1 1 calc R . . H54C H 0.6950 0.2093 0.0693 0.512 Uiso 1 1 calc R . . C55 C 0.8845(3) 0.0005(2) 0.34394(19) 0.0541(15) Uani 1 1 d . . . C56 C 0.8672(4) -0.0586(3) 0.3325(3) 0.080(2) Uani 1 1 d . . . H56A H 0.8577 -0.0625 0.2982 0.120 Uiso 1 1 calc R . . H56B H 0.8244 -0.0698 0.3507 0.120 Uiso 1 1 calc R . . H56C H 0.9085 -0.0810 0.3415 0.120 Uiso 1 1 calc R . . C57 C 0.9087(3) 0.0068(3) 0.39631(18) 0.0689(18) Uani 1 1 d . . . H57A H 0.9482 -0.0183 0.4030 0.103 Uiso 1 1 calc R . . H57B H 0.8679 -0.0009 0.4176 0.103 Uiso 1 1 calc R . . H57C H 0.9256 0.0434 0.4017 0.103 Uiso 1 1 calc R . . C58 C 0.8204(3) 0.0368(3) 0.3302(2) 0.0674(18) Uani 1 1 d . . . H58A H 0.8275 0.0723 0.3442 0.101 Uiso 1 1 calc R . . H58B H 0.7754 0.0213 0.3425 0.101 Uiso 1 1 calc R . . H58C H 0.8176 0.0398 0.2953 0.101 Uiso 1 1 calc R . . C59 C 0.9809(3) 0.0601(3) 0.3099(2) 0.0486(15) Uani 1 1 d . . . C60 C 1.0897(3) 0.1052(2) 0.2768(2) 0.0517(14) Uani 1 1 d . . . C61 C 1.1451(3) 0.0941(2) 0.2358(2) 0.0626(17) Uani 1 1 d . . . H61A H 1.1718 0.0611 0.2428 0.094 Uiso 1 1 calc R . . H61B H 1.1791 0.1240 0.2335 0.094 Uiso 1 1 calc R . . H61C H 1.1193 0.0901 0.2054 0.094 Uiso 1 1 calc R . . C62 C 1.1314(3) 0.1120(2) 0.3253(2) 0.0631(17) Uani 1 1 d . . . H62A H 1.0965 0.1144 0.3516 0.095 Uiso 1 1 calc R . . H62B H 1.1606 0.1446 0.3242 0.095 Uiso 1 1 calc R . . H62C H 1.1630 0.0810 0.3303 0.095 Uiso 1 1 calc R . . C63 C 1.0496(3) 0.1606(3) 0.2651(2) 0.0467(14) Uani 1 1 d . . . C64 C 0.9624(3) 0.2069(2) 0.21002(19) 0.0493(14) Uani 1 1 d . . . H64 H 0.9654 0.2343 0.2361 0.059 Uiso 1 1 calc R . . C65 C 1.0010(3) 0.2308(3) 0.1661(2) 0.0640(17) Uani 1 1 d . . . H65A H 0.9761 0.2645 0.1572 0.077 Uiso 1 1 calc R . . H65B H 1.0510 0.2402 0.1754 0.077 Uiso 1 1 calc R . . C66 C 1.0045(4) 0.1955(3) 0.1220(2) 0.0669(18) Uani 1 1 d . . . C67 C 1.0661(4) 0.1641(3) 0.1124(2) 0.0689(19) Uani 1 1 d . . . H67 H 1.1060 0.1671 0.1336 0.083 Uiso 1 1 calc R . . C68 C 1.0722(5) 0.1289(3) 0.0738(2) 0.084(2) Uani 1 1 d . . . H68 H 1.1151 0.1087 0.0690 0.101 Uiso 1 1 calc R . . C69 C 1.0117(5) 0.1241(4) 0.0417(3) 0.100(3) Uani 1 1 d . . . H69 H 1.0148 0.1011 0.0147 0.121 Uiso 1 1 calc R . . C70 C 0.9482(5) 0.1534(4) 0.0499(2) 0.097(3) Uani 1 1 d . . . H70 H 0.9080 0.1494 0.0291 0.116 Uiso 1 1 calc R . . C71 C 0.9439(4) 0.1898(3) 0.0901(2) 0.082(2) Uani 1 1 d . . . H71 H 0.9011 0.2099 0.0954 0.098 Uiso 1 1 calc R . . C72 C 0.8811(3) 0.1945(2) 0.20255(18) 0.0550(15) Uani 1 1 d . . . H72A H 0.8566 0.2272 0.1910 0.066 Uiso 1 1 calc R . . H72B H 0.8764 0.1669 0.1773 0.066 Uiso 1 1 calc R . . C73 C 0.8419(3) 0.1744(2) 0.24845(16) 0.0494(14) Uani 1 1 d . . . H73A H 0.7908 0.1660 0.2409 0.059 Uiso 1 1 calc R . . H73B H 0.8654 0.1413 0.2603 0.059 Uiso 1 1 calc R . . C74 C 0.8453(3) 0.2174(3) 0.28669(19) 0.0494(15) Uani 1 1 d . . . C75 C 0.8886(3) 0.2395(2) 0.37010(17) 0.0449(14) Uani 1 1 d . . . H75 H 0.8379 0.2488 0.3795 0.054 Uiso 1 1 calc R . . C76 C 0.9235(3) 0.2117(2) 0.41302(18) 0.0581(16) Uani 1 1 d . . . H76A H 0.9707 0.1969 0.4028 0.070 Uiso 1 1 calc R . . H76B H 0.9331 0.2388 0.4380 0.070 Uiso 1 1 calc R . . C77 C 0.8781(5) 0.1659(3) 0.4355(2) 0.097(3) Uani 1 1 d . . . H77 H 0.8654 0.1396 0.4098 0.116 Uiso 1 1 calc R . . C78 C 0.8072(5) 0.1880(4) 0.4576(3) 0.118(3) Uani 1 1 d . . . H78A H 0.8189 0.2158 0.4811 0.177 Uiso 1 1 calc R . . H78B H 0.7809 0.1589 0.4734 0.177 Uiso 1 1 calc R . . H78C H 0.7770 0.2033 0.4322 0.177 Uiso 1 1 calc R . . C79 C 0.9259(6) 0.1360(3) 0.4755(3) 0.131(3) Uani 1 1 d . . . H79A H 0.9735 0.1271 0.4621 0.196 Uiso 1 1 calc R . . H79B H 0.9014 0.1031 0.4854 0.196 Uiso 1 1 calc R . . H79C H 0.9321 0.1595 0.5032 0.196 Uiso 1 1 calc R . . C80 C 0.9289(3) 0.2935(3) 0.35889(18) 0.0479(14) Uani 1 1 d . . . C81 C 1.0267(3) 0.3444(3) 0.3179(2) 0.0561(15) Uani 1 1 d . . . H81 H 1.0048 0.3747 0.3363 0.067 Uiso 1 1 calc R . . C82 C 1.1054(3) 0.3354(3) 0.3366(2) 0.0746(19) Uani 1 1 d . . . H82A H 1.1309 0.3117 0.3138 0.090 Uiso 1 1 calc R . . H82B H 1.1308 0.3703 0.3366 0.090 Uiso 1 1 calc R . . C83 C 1.1114(4) 0.3113(4) 0.3864(2) 0.082(2) Uani 1 1 d . . . C84 C 1.1316(5) 0.2592(3) 0.3913(3) 0.098(3) Uani 1 1 d . . . H84 H 1.1449 0.2384 0.3643 0.117 Uiso 1 1 calc R . . C85 C 1.1321(5) 0.2371(4) 0.4376(4) 0.130(3) Uani 1 1 d . . . H85 H 1.1453 0.2007 0.4418 0.156 Uiso 1 1 calc R . . C86 C 1.1136(8) 0.2677(5) 0.4775(3) 0.196(7) Uani 1 1 d . . . H86 H 1.1163 0.2522 0.5084 0.235 Uiso 1 1 calc R . . C87 C 1.0916(10) 0.3198(5) 0.4730(3) 0.240(9) Uani 1 1 d . . . H87 H 1.0742 0.3396 0.4997 0.288 Uiso 1 1 calc R . . C88 C 1.0961(6) 0.3437(4) 0.4253(3) 0.154(5) Uani 1 1 d . . . H88 H 1.0886 0.3809 0.4211 0.185 Uiso 1 1 calc R . . C89 C 1.0257(3) 0.3590(3) 0.26460(18) 0.0566(16) Uani 1 1 d . . . H89A H 1.0488 0.3945 0.2609 0.068 Uiso 1 1 calc R . . H89B H 1.0562 0.3328 0.2473 0.068 Uiso 1 1 calc R . . C90 C 0.9512(3) 0.3610(3) 0.23956(19) 0.0589(16) Uani 1 1 d . . . H90A H 0.9586 0.3692 0.2052 0.071 Uiso 1 1 calc R . . H90B H 0.9284 0.3252 0.2417 0.071 Uiso 1 1 calc R . . C91 C 0.8994(3) 0.4025(3) 0.26088(19) 0.0513(15) Uani 1 1 d . . . C92 C 0.7767(3) 0.4177(2) 0.2976(2) 0.0570(16) Uani 1 1 d . . . C93 C 0.7437(3) 0.4472(3) 0.2540(2) 0.0741(19) Uani 1 1 d . . . H93A H 0.7373 0.4219 0.2275 0.111 Uiso 1 1 calc R . . H93B H 0.7762 0.4760 0.2440 0.111 Uiso 1 1 calc R . . H93C H 0.6966 0.4622 0.2630 0.111 Uiso 1 1 calc R . . C94 C 0.7189(3) 0.3774(2) 0.3208(3) 0.085(2) Uani 1 1 d . . . H94A H 0.7013 0.3527 0.2962 0.127 Uiso 1 1 calc R . . H94B H 0.6782 0.3978 0.3338 0.127 Uiso 1 1 calc R . . H94C H 0.7420 0.3570 0.3466 0.127 Uiso 1 1 calc R . . C95 C 0.7981(3) 0.4586(3) 0.3384(2) 0.0539(15) Uani 1 1 d . . . C96 C 0.8762(4) 0.4700(3) 0.41236(18) 0.0676(19) Uani 1 1 d . . . H96 H 0.8502 0.5050 0.4139 0.081 Uiso 1 1 calc R . . C97 C 0.8595(5) 0.4401(3) 0.4593(2) 0.093(3) Uani 1 1 d . . . H97A H 0.8713 0.4638 0.4866 0.112 Uiso 1 1 calc R . . H97B H 0.8912 0.4083 0.4614 0.112 Uiso 1 1 calc R . . C98 C 0.7808(5) 0.4221(4) 0.4639(3) 0.096(3) Uani 1 1 d . . . C99 C 0.7598(10) 0.3683(6) 0.4551(4) 0.190(6) Uani 1 1 d . . . H99 H 0.7963 0.3421 0.4500 0.228 Uiso 1 1 calc R . . C100 C 0.6826(11) 0.3515(6) 0.4537(5) 0.198(7) Uani 1 1 d . . . H100 H 0.6679 0.3176 0.4420 0.237 Uiso 1 1 calc R . . C101 C 0.6358(9) 0.3874(8) 0.4698(5) 0.195(7) Uani 1 1 d . . . H101 H 0.5875 0.3762 0.4757 0.235 Uiso 1 1 calc R . . C102 C 0.6528(8) 0.4384(6) 0.4782(5) 0.161(5) Uani 1 1 d . . . H102 H 0.6154 0.4630 0.4860 0.193 Uiso 1 1 calc R . . C103 C 0.7238(6) 0.4565(4) 0.4758(3) 0.112(3) Uani 1 1 d . . . H103 H 0.7339 0.4930 0.4825 0.134 Uiso 1 1 calc R . . C104 C 0.9568(3) 0.4827(3) 0.4052(2) 0.0660(17) Uani 1 1 d . . . H10B H 0.9842 0.4487 0.4052 0.079 Uiso 1 1 calc R . . H10C H 0.9738 0.5040 0.4329 0.079 Uiso 1 1 calc R . . C105 C 0.9751(4) 0.5135(3) 0.3588(2) 0.0707(19) Uani 1 1 d . . . H10D H 0.9588 0.4915 0.3314 0.085 Uiso 1 1 calc R . . H10E H 0.9460 0.5467 0.3586 0.085 Uiso 1 1 calc R . . C106 C 1.0536(4) 0.5289(3) 0.3500(3) 0.079(2) Uani 1 1 d . . . C107 C 1.1810(5) 0.5131(6) 0.3666(5) 0.216(8) Uani 1 1 d D . . H10H H 1.1992 0.5015 0.3349 0.260 Uiso 1 1 calc R . . H10I H 1.1870 0.5523 0.3695 0.260 Uiso 1 1 calc R . . C108 C 1.2175(6) 0.4864(10) 0.4036(5) 0.369(17) Uani 1 1 d D . . H10J H 1.2286 0.4498 0.3935 0.554 Uiso 1 1 calc R . . H10K H 1.1868 0.4855 0.4322 0.554 Uiso 1 1 calc R . . H10L H 1.2625 0.5054 0.4109 0.554 Uiso 1 1 calc R . . N1 N 0.5398(2) 0.62860(17) 0.22840(13) 0.0378(10) Uani 1 1 d . . . H1 H 0.5455 0.6566 0.2470 0.045 Uiso 1 1 calc R . . N2 N 0.5030(2) 0.53241(19) 0.28053(14) 0.0461(11) Uani 1 1 d . . . H2 H 0.4941 0.5634 0.2940 0.055 Uiso 1 1 calc R . . N3 N 0.3904(2) 0.48318(17) 0.18032(14) 0.0424(11) Uani 1 1 d . . . H3 H 0.4142 0.5136 0.1799 0.051 Uiso 1 1 calc R . . N4 N 0.4861(2) 0.39231(18) 0.18295(14) 0.0430(11) Uani 1 1 d . . . H4 H 0.4940 0.4216 0.1994 0.052 Uiso 1 1 calc R . . N5 N 0.3308(2) 0.30607(17) 0.22160(14) 0.0426(11) Uani 1 1 d . . . H5 H 0.3277 0.3411 0.2200 0.051 Uiso 1 1 calc R . . N6 N 0.3459(2) 0.25204(18) 0.13255(14) 0.0444(11) Uani 1 1 d . . . H6 H 0.3656 0.2829 0.1399 0.053 Uiso 1 1 calc R . . N7 N 1.0372(2) 0.06023(18) 0.27905(16) 0.0478(11) Uani 1 1 d . . . H7 H 1.0430 0.0329 0.2597 0.057 Uiso 1 1 calc R . . N8 N 1.0008(2) 0.15837(18) 0.22782(15) 0.0464(11) Uani 1 1 d . . . H8 H 0.9920 0.1274 0.2142 0.056 Uiso 1 1 calc R . . N9 N 0.8840(2) 0.20495(18) 0.32733(14) 0.0469(11) Uani 1 1 d . . . H9 H 0.9075 0.1745 0.3278 0.056 Uiso 1 1 calc R . . N10 N 0.9821(2) 0.29485(18) 0.32709(14) 0.0452(11) Uani 1 1 d . . . H10 H 0.9918 0.2658 0.3107 0.054 Uiso 1 1 calc R . . N11 N 0.8379(3) 0.38248(19) 0.28150(15) 0.0543(12) Uani 1 1 d . . . H11 H 0.8340 0.3478 0.2855 0.065 Uiso 1 1 calc R . . N12 N 0.8480(2) 0.44122(19) 0.37041(16) 0.0551(12) Uani 1 1 d . . . H19E H 0.8655 0.4090 0.3655 0.066 Uiso 1 1 calc R . . O1 O 0.44896(18) 0.67722(15) 0.19405(12) 0.0505(9) Uani 1 1 d . . . O2 O 0.46276(18) 0.58708(15) 0.17359(13) 0.0467(9) Uani 1 1 d . . . O3 O 0.56732(18) 0.48719(15) 0.22333(12) 0.0477(9) Uani 1 1 d . . . O4 O 0.31680(19) 0.42727(15) 0.22318(12) 0.0492(9) Uani 1 1 d . . . O5 O 0.41641(19) 0.35305(16) 0.12361(12) 0.0538(10) Uani 1 1 d . . . O6 O 0.4046(2) 0.23518(18) 0.24083(13) 0.0570(10) Uani 1 1 d . . . O7 O 0.2626(2) 0.18835(17) 0.15759(13) 0.0610(11) Uani 1 1 d . . . O8 O 0.5703(3) 0.1230(2) 0.1671(2) 0.0945(16) Uani 1 1 d . . . O9 O 0.5976(3) 0.1915(3) 0.1200(3) 0.169(3) Uani 1 1 d D . . O10 O 0.9475(2) 0.01141(15) 0.31114(13) 0.0544(10) Uani 1 1 d . . . O11 O 0.95895(19) 0.09975(16) 0.33243(13) 0.0492(9) Uani 1 1 d . . . O12 O 1.06426(18) 0.20309(15) 0.28546(13) 0.0504(9) Uani 1 1 d . . . O13 O 0.81524(19) 0.26226(16) 0.28335(12) 0.0515(9) Uani 1 1 d . . . O14 O 0.9085(2) 0.33393(16) 0.38365(12) 0.0570(10) Uani 1 1 d . . . O15 O 0.9120(2) 0.45251(17) 0.25986(13) 0.0603(10) Uani 1 1 d . . . O16 O 0.7689(2) 0.50293(17) 0.34037(15) 0.0652(11) Uani 1 1 d . . . O17 O 1.0743(3) 0.5647(2) 0.32367(19) 0.1014(17) Uani 1 1 d . . . O18 O 1.1019(3) 0.4972(3) 0.3730(2) 0.120(2) Uani 1 1 d . . . O21 O 0.7492(3) 0.5946(2) 0.40194(15) 0.0982(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.049(3) 0.036(4) 0.051(3) -0.005(3) -0.012(3) 0.005(3) C2 0.082(4) 0.064(5) 0.063(3) 0.006(3) -0.009(3) 0.000(4) C3 0.087(4) 0.042(5) 0.106(5) -0.004(4) -0.025(4) 0.032(4) C4 0.038(3) 0.058(5) 0.111(5) -0.003(4) -0.013(3) 0.004(3) C5 0.032(3) 0.051(5) 0.055(3) 0.006(3) 0.010(3) -0.006(3) C6 0.034(3) 0.034(4) 0.056(3) -0.011(3) 0.005(2) 0.004(3) C7 0.061(3) 0.041(4) 0.074(4) -0.008(3) 0.005(3) -0.010(3) C8 0.054(3) 0.032(4) 0.077(4) -0.001(3) -0.019(3) 0.009(3) C9 0.031(2) 0.030(4) 0.036(2) -0.003(2) -0.004(2) 0.002(2) C10 0.055(3) 0.039(4) 0.045(3) -0.005(3) -0.004(2) -0.006(3) C11 0.057(3) 0.053(4) 0.056(3) 0.000(3) -0.009(3) 0.002(3) C12 0.075(4) 0.068(5) 0.048(3) 0.008(3) -0.009(3) 0.015(4) C13 0.093(5) 0.145(8) 0.047(3) 0.001(4) 0.002(4) 0.008(6) C14 0.098(6) 0.190(12) 0.080(6) -0.030(7) -0.009(5) 0.063(8) C15 0.206(11) 0.108(9) 0.044(4) -0.018(5) -0.012(6) 0.067(8) C16 0.151(8) 0.066(6) 0.069(5) 0.003(4) -0.032(5) 0.005(6) C17 0.093(5) 0.064(5) 0.061(4) 0.009(4) -0.020(4) 0.008(4) C18 0.038(3) 0.042(4) 0.056(3) 0.002(3) 0.007(2) -0.010(3) C19 0.039(3) 0.048(4) 0.054(3) 0.010(3) 0.000(2) -0.005(3) C20 0.041(3) 0.027(4) 0.061(3) 0.000(3) -0.012(3) 0.012(3) C21 0.049(3) 0.047(4) 0.041(3) -0.005(3) 0.001(2) -0.010(3) C22 0.093(4) 0.045(4) 0.060(3) 0.008(3) 0.019(3) -0.006(4) C23 0.180(8) 0.043(5) 0.063(4) 0.003(4) 0.004(5) 0.034(5) C24 0.149(8) 0.130(9) 0.099(5) -0.001(6) -0.053(5) 0.021(7) C25 0.301(13) 0.119(8) 0.064(4) 0.039(5) 0.064(7) 0.045(9) C26 0.043(3) 0.030(4) 0.052(3) 0.011(3) -0.008(3) -0.007(3) C27 0.055(3) 0.028(4) 0.060(3) -0.008(3) -0.003(3) 0.011(3) C28 0.052(3) 0.057(4) 0.062(3) 0.010(3) 0.006(3) 0.011(3) C29 0.033(3) 0.047(4) 0.069(4) -0.009(3) -0.004(3) -0.003(3) C30 0.076(4) 0.076(5) 0.060(4) -0.014(4) 0.006(3) -0.006(4) C31 0.108(6) 0.077(6) 0.065(4) -0.028(4) 0.002(4) -0.008(5) C32 0.124(6) 0.122(8) 0.049(4) -0.014(5) 0.008(4) -0.026(6) C33 0.090(5) 0.111(7) 0.077(5) 0.003(5) 0.007(4) -0.023(5) C34 0.075(4) 0.094(7) 0.064(4) -0.020(4) -0.003(3) 0.002(5) C35 0.054(3) 0.046(4) 0.055(3) 0.009(3) -0.007(3) -0.006(3) C36 0.068(4) 0.043(4) 0.047(3) 0.007(3) -0.005(3) -0.006(3) C37 0.037(3) 0.039(4) 0.049(3) 0.004(3) 0.000(2) -0.002(3) C38 0.028(2) 0.029(4) 0.087(4) 0.005(3) 0.008(3) -0.005(3) C39 0.071(4) 0.049(5) 0.100(4) -0.009(4) 0.037(3) -0.009(3) C40 0.055(3) 0.050(5) 0.103(4) -0.012(4) -0.004(3) 0.013(3) C41 0.043(3) 0.028(4) 0.071(3) 0.000(3) 0.010(3) 0.002(3) C42 0.055(3) 0.050(4) 0.074(4) -0.001(3) 0.008(3) -0.012(3) C43 0.064(4) 0.071(5) 0.068(4) -0.011(4) 0.000(3) 0.003(4) C44 0.079(5) 0.059(5) 0.046(3) -0.004(3) -0.005(3) -0.004(4) C45 0.061(4) 0.060(6) 0.115(5) -0.015(5) -0.013(4) -0.006(4) C46 0.113(7) 0.076(7) 0.117(6) 0.005(5) -0.008(5) -0.018(6) C47 0.077(5) 0.119(9) 0.109(6) 0.023(6) -0.012(5) 0.016(6) C48 0.068(5) 0.112(8) 0.124(6) 0.036(6) -0.027(5) -0.008(5) C49 0.085(5) 0.061(5) 0.092(4) 0.028(4) -0.030(4) -0.018(4) C50 0.068(4) 0.035(4) 0.078(4) -0.004(3) 0.024(3) -0.007(3) C51 0.055(4) 0.046(4) 0.086(4) 0.000(4) 0.013(3) 0.002(3) C52 0.068(5) 0.062(6) 0.124(6) 0.016(5) 0.046(4) 0.006(4) C53 0.124(9) 0.194(14) 0.250(14) 0.122(12) 0.014(9) 0.026(9) C54 0.198(14) 0.61(4) 0.220(15) -0.11(2) 0.038(12) 0.21(2) C55 0.062(4) 0.036(4) 0.064(3) 0.000(3) 0.015(3) -0.002(3) C56 0.080(4) 0.052(5) 0.108(5) 0.001(4) 0.036(4) -0.020(4) C57 0.080(4) 0.065(5) 0.061(3) 0.016(3) 0.013(3) 0.004(4) C58 0.045(3) 0.048(4) 0.109(5) -0.009(4) 0.002(3) -0.006(3) C59 0.041(3) 0.042(5) 0.063(3) 0.004(3) -0.004(3) 0.006(3) C60 0.046(3) 0.026(4) 0.084(4) 0.002(3) 0.004(3) 0.008(3) C61 0.034(3) 0.040(4) 0.113(5) -0.010(4) 0.016(3) -0.003(3) C62 0.078(4) 0.032(4) 0.079(4) -0.002(3) -0.025(3) 0.006(3) C63 0.033(3) 0.038(4) 0.069(3) 0.003(3) 0.008(3) -0.010(3) C64 0.061(3) 0.025(4) 0.061(3) 0.003(3) 0.002(3) 0.006(3) C65 0.063(4) 0.050(4) 0.079(4) 0.013(4) 0.010(3) 0.004(3) C66 0.078(4) 0.068(5) 0.055(3) 0.023(4) 0.006(3) -0.010(4) C67 0.078(4) 0.071(5) 0.058(4) 0.020(4) 0.018(3) 0.006(4) C68 0.119(6) 0.077(6) 0.055(4) 0.006(4) 0.013(4) 0.003(5) C69 0.118(6) 0.107(8) 0.076(5) -0.001(5) 0.008(5) -0.010(6) C70 0.096(5) 0.142(8) 0.052(4) 0.010(5) -0.016(4) -0.012(6) C71 0.084(5) 0.092(6) 0.068(4) 0.014(4) 0.007(4) 0.010(5) C72 0.059(3) 0.050(4) 0.057(3) 0.008(3) 0.002(3) 0.011(3) C73 0.058(3) 0.044(4) 0.047(3) 0.000(3) -0.009(3) -0.007(3) C74 0.041(3) 0.058(5) 0.049(3) 0.006(3) -0.005(3) -0.011(3) C75 0.040(3) 0.043(4) 0.052(3) 0.003(3) 0.007(2) -0.007(3) C76 0.084(4) 0.038(4) 0.053(3) 0.009(3) 0.004(3) 0.006(3) C77 0.146(7) 0.083(6) 0.062(4) 0.014(4) -0.010(4) -0.014(6) C78 0.120(6) 0.125(8) 0.108(6) 0.015(6) 0.031(5) -0.007(7) C79 0.213(10) 0.084(7) 0.096(5) 0.034(5) -0.052(6) -0.001(7) C80 0.061(3) 0.043(4) 0.040(3) 0.001(3) -0.007(3) 0.020(3) C81 0.054(3) 0.044(4) 0.070(4) -0.003(3) -0.005(3) 0.001(3) C82 0.063(4) 0.062(5) 0.099(5) -0.012(4) -0.004(4) 0.013(4) C83 0.083(5) 0.096(7) 0.068(4) -0.014(5) -0.014(4) 0.021(5) C84 0.131(7) 0.069(6) 0.093(5) -0.023(5) -0.035(5) 0.055(5) C85 0.171(8) 0.094(8) 0.124(7) -0.017(6) -0.064(6) 0.053(7) C86 0.356(17) 0.145(11) 0.087(6) -0.034(7) -0.110(8) 0.129(12) C87 0.48(2) 0.155(12) 0.084(6) -0.055(7) -0.118(10) 0.185(15) C88 0.272(13) 0.076(7) 0.113(7) -0.031(6) -0.091(8) 0.074(8) C89 0.054(3) 0.057(4) 0.059(3) 0.000(3) 0.008(3) -0.006(3) C90 0.077(4) 0.048(4) 0.052(3) 0.004(3) 0.008(3) 0.010(4) C91 0.058(4) 0.045(5) 0.052(3) 0.012(3) -0.010(3) -0.011(3) C92 0.040(3) 0.033(4) 0.098(4) 0.003(4) -0.003(3) -0.004(3) C93 0.077(4) 0.046(5) 0.099(4) 0.004(4) -0.034(4) -0.004(4) C94 0.044(3) 0.024(4) 0.187(7) 0.000(4) 0.032(4) -0.001(3) C95 0.046(3) 0.048(5) 0.067(4) 0.001(4) 0.009(3) -0.007(3) C96 0.114(6) 0.046(4) 0.043(3) -0.008(3) 0.002(3) 0.021(4) C97 0.141(8) 0.061(6) 0.077(4) -0.007(4) -0.002(5) 0.032(5) C98 0.115(7) 0.078(7) 0.096(5) 0.038(5) 0.038(5) 0.026(6) C99 0.269(19) 0.118(12) 0.184(10) 0.064(9) 0.132(12) 0.019(11) C100 0.244(16) 0.143(14) 0.206(12) -0.023(10) 0.134(12) -0.071(13) C101 0.200(14) 0.162(16) 0.225(14) 0.014(13) 0.136(11) -0.039(13) C102 0.128(10) 0.124(12) 0.231(13) 0.058(11) 0.031(9) 0.048(9) C103 0.120(7) 0.095(8) 0.120(6) -0.012(6) -0.011(6) 0.033(7) C104 0.076(4) 0.054(5) 0.068(4) -0.008(3) -0.020(3) 0.011(4) C105 0.097(5) 0.051(5) 0.064(4) 0.002(3) -0.029(3) 0.007(4) C106 0.073(5) 0.071(6) 0.092(5) 0.016(4) -0.028(4) -0.017(5) C107 0.060(5) 0.338(19) 0.250(13) 0.196(14) 0.000(7) 0.014(9) C108 0.070(6) 0.85(5) 0.190(12) 0.10(2) -0.013(7) 0.001(17) N1 0.041(2) 0.024(3) 0.049(2) -0.008(2) -0.004(2) 0.003(2) N2 0.052(2) 0.029(3) 0.058(2) -0.005(2) -0.001(2) 0.004(2) N3 0.047(2) 0.027(3) 0.053(2) 0.004(2) 0.001(2) -0.001(2) N4 0.043(2) 0.029(3) 0.057(2) -0.002(2) -0.005(2) -0.013(2) N5 0.041(2) 0.016(3) 0.071(3) 0.002(2) 0.005(2) -0.004(2) N6 0.041(2) 0.028(3) 0.064(3) -0.006(2) 0.005(2) -0.005(2) N7 0.039(2) 0.034(3) 0.070(3) 0.001(2) 0.002(2) -0.003(2) N8 0.049(2) 0.026(3) 0.064(3) -0.006(2) 0.002(2) 0.003(2) N9 0.052(2) 0.028(3) 0.060(3) -0.003(2) 0.005(2) 0.007(2) N10 0.053(3) 0.028(3) 0.054(2) -0.010(2) -0.001(2) -0.003(2) N11 0.067(3) 0.023(3) 0.073(3) 0.002(2) -0.009(3) 0.001(3) N12 0.067(3) 0.032(3) 0.066(3) 0.001(2) -0.002(3) 0.018(3) O1 0.0418(19) 0.034(3) 0.075(2) -0.005(2) -0.0097(18) 0.0079(19) O2 0.051(2) 0.023(2) 0.066(2) -0.0042(19) -0.0076(18) -0.0072(19) O3 0.0424(19) 0.033(2) 0.067(2) -0.0083(19) 0.0000(17) 0.0009(18) O4 0.047(2) 0.029(3) 0.072(2) 0.003(2) 0.0012(18) -0.0092(19) O5 0.067(2) 0.037(3) 0.058(2) -0.0074(19) -0.0155(19) -0.017(2) O6 0.060(2) 0.037(3) 0.074(2) 0.010(2) 0.002(2) 0.007(2) O7 0.060(2) 0.039(3) 0.084(3) -0.006(2) 0.002(2) -0.019(2) O8 0.082(3) 0.060(4) 0.141(4) 0.039(3) 0.026(3) 0.018(3) O9 0.055(3) 0.136(6) 0.316(8) 0.148(6) 0.058(4) 0.034(3) O10 0.063(2) 0.027(2) 0.073(2) -0.0001(19) 0.015(2) -0.012(2) O11 0.049(2) 0.027(2) 0.072(2) -0.001(2) 0.0076(18) 0.0015(19) O12 0.041(2) 0.030(2) 0.080(2) -0.009(2) -0.0018(18) -0.0099(18) O13 0.050(2) 0.037(3) 0.068(2) 0.001(2) -0.0036(18) 0.011(2) O14 0.074(3) 0.035(3) 0.062(2) -0.003(2) 0.003(2) 0.012(2) O15 0.073(3) 0.033(3) 0.075(2) 0.009(2) 0.001(2) -0.009(2) O16 0.072(3) 0.025(3) 0.099(3) -0.002(2) -0.010(2) 0.020(2) O17 0.114(4) 0.069(4) 0.121(4) 0.038(3) -0.033(3) -0.034(3) O18 0.078(3) 0.127(5) 0.155(4) 0.073(4) -0.020(3) 0.007(4) O21 0.146(4) 0.071(4) 0.078(3) -0.002(3) 0.000(3) 0.010(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 C1 O1 1.474(6) . ? C1 C2 1.504(7) . ? C1 C4 1.508(7) . ? C1 C3 1.555(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O2 1.208(6) . ? C5 N1 1.364(6) . ? C5 O1 1.375(7) . ? C6 N1 1.456(6) . ? C6 C8 1.535(7) . ? C6 C7 1.550(7) . ? C6 C9 1.536(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O3 1.217(6) . ? C9 N2 1.335(6) . ? C10 N2 1.456(6) . ? C10 C18 1.533(7) . ? C10 C11 1.542(7) . ? C10 H10A 0.9800 . ? C11 C12 1.486(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.378(9) . ? C12 C13 1.377(8) . ? C13 C14 1.329(11) . ? C13 H13 0.9300 . ? C14 C15 1.340(13) . ? C14 H14 0.9300 . ? C15 C16 1.363(12) . ? C15 H15 0.9300 . ? C16 C17 1.409(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.524(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.512(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 O4 1.199(6) . ? C20 N3 1.351(6) . ? C21 N3 1.472(6) . ? C21 C26 1.526(7) . ? C21 C22 1.530(7) . ? C21 H21 0.9800 . ? C22 C23 1.524(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C25 1.516(11) . ? C23 C24 1.587(11) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 O5 1.229(6) . ? C26 N4 1.322(6) . ? C27 N4 1.470(6) . ? C27 C35 1.521(7) . ? C27 C28 1.529(7) . ? C27 H27 0.9800 . ? C28 C29 1.478(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.347(8) . ? C29 C34 1.389(9) . ? C30 C31 1.328(8) . ? C30 H30 0.9300 . ? C31 C32 1.382(10) . ? C31 H31 0.9300 . ? C32 C33 1.377(10) . ? C32 H32 0.9300 . ? C33 C34 1.383(9) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.536(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.500(7) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 O6 1.222(6) . ? C37 N5 1.339(6) . ? C38 N5 1.479(6) . ? C38 C40 1.528(7) . ? C38 C39 1.561(7) . ? C38 C41 1.535(7) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 O7 1.248(6) . ? C41 N6 1.320(6) . ? C42 N6 1.448(7) . ? C42 C43 1.526(8) . ? C42 C50 1.518(8) . ? C42 H42 0.9800 . ? C43 C44 1.518(8) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.397(9) . ? C44 C49 1.411(9) . ? C45 C46 1.349(10) . ? C45 H45 0.9300 . ? C46 C47 1.384(11) . ? C46 H46 0.9300 . ? C47 C48 1.368(11) . ? C47 H47 0.9300 . ? C48 C49 1.338(10) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C51 1.521(8) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.471(9) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O8 1.183(8) . ? C52 O9 1.310(8) . ? C53 C54 1.308(12) . ? C53 O9 1.559(10) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9665 . ? C54 H54B 0.9666 . ? C54 H54C 0.9665 . ? C55 O10 1.476(6) . ? C55 C57 1.506(7) . ? C55 C56 1.515(8) . ? C55 C58 1.509(8) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 O11 1.217(6) . ? C59 N7 1.323(7) . ? C59 O10 1.339(7) . ? C60 N7 1.457(7) . ? C60 C62 1.536(7) . ? C60 C61 1.529(7) . ? C60 C63 1.573(8) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 O12 1.209(6) . ? C63 N8 1.352(6) . ? C64 N8 1.461(6) . ? C64 C65 1.509(7) . ? C64 C72 1.517(7) . ? C64 H64 0.9800 . ? C65 C66 1.486(8) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 C67 1.380(9) . ? C66 C71 1.409(8) . ? C67 C68 1.367(9) . ? C67 H67 0.9300 . ? C68 C69 1.411(10) . ? C68 H68 0.9300 . ? C69 C70 1.374(10) . ? C69 H69 0.9300 . ? C70 C71 1.417(10) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 C73 1.525(7) . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C73 C74 1.487(8) . ? C73 H73A 0.9700 . ? C73 H73B 0.9700 . ? C74 O13 1.230(7) . ? C74 N9 1.349(6) . ? C75 N9 1.446(6) . ? C75 C76 1.498(7) . ? C75 C80 1.543(7) . ? C75 H75 0.9800 . ? C76 C77 1.520(9) . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C78 1.520(10) . ? C77 C79 1.576(10) . ? C77 H77 0.9800 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 O14 1.255(6) . ? C80 N10 1.298(6) . ? C81 N10 1.480(7) . ? C81 C89 1.501(7) . ? C81 C82 1.531(8) . ? C81 H81 0.9800 . ? C82 C83 1.488(9) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C88 1.357(10) . ? C83 C84 1.336(10) . ? C84 C85 1.377(11) . ? C84 H84 0.9300 . ? C85 C86 1.367(12) . ? C85 H85 0.9300 . ? C86 C87 1.343(13) . ? C86 H86 0.9300 . ? C87 C88 1.431(14) . ? C87 H87 0.9300 . ? C88 H88 0.9300 . ? C89 C90 1.513(7) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C90 C91 1.501(8) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 O15 1.248(7) . ? C91 N11 1.341(7) . ? C92 N11 1.471(7) . ? C92 C93 1.516(8) . ? C92 C94 1.573(8) . ? C92 C95 1.551(8) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 O16 1.208(7) . ? C95 N12 1.330(7) . ? C96 N12 1.441(7) . ? C96 C104 1.506(9) . ? C96 C97 1.509(9) . ? C96 H96 0.9800 . ? C97 C98 1.496(11) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 C103 1.371(11) . ? C98 C99 1.395(16) . ? C99 C100 1.46(2) . ? C99 H99 0.9300 . ? C100 C101 1.299(17) . ? C100 H100 0.9300 . ? C101 C102 1.307(17) . ? C101 H101 0.9300 . ? C102 C103 1.363(15) . ? C102 H102 0.9300 . ? C103 H103 0.9300 . ? C104 C105 1.513(8) . ? C104 H10B 0.9700 . ? C104 H10C 0.9700 . ? C105 C106 1.490(9) . ? C105 H10D 0.9700 . ? C105 H10E 0.9700 . ? C106 O17 1.195(8) . ? C106 O18 1.329(8) . ? C107 C108 1.374(13) . ? C107 O18 1.494(10) . ? C107 H10H 0.9700 . ? C107 H10I 0.9700 . ? C108 H10J 0.9755 . ? C108 H10K 0.9756 . ? C108 H10L 0.9752 . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 H4 0.8600 . ? N5 H5 0.8600 . ? N6 H6 0.8600 . ? N7 H7 0.8600 . ? N8 H8 0.8600 . ? N9 H9 0.8600 . ? N10 H10 0.8600 . ? N11 H11 0.8600 . ? N12 H19E 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 109.0(4) . . ? O1 C1 C4 111.2(4) . . ? C2 C1 C4 114.3(5) . . ? O1 C1 C3 101.7(4) . . ? C2 C1 C3 110.3(5) . . ? C4 C1 C3 109.6(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.4 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 N1 125.5(5) . . ? O2 C5 O1 124.9(5) . . ? N1 C5 O1 109.6(5) . . ? N1 C6 C8 107.7(4) . . ? N1 C6 C7 110.1(4) . . ? C8 C6 C7 110.1(4) . . ? N1 C6 C9 111.1(4) . . ? C8 C6 C9 108.3(4) . . ? C7 C6 C9 109.5(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 N2 123.0(5) . . ? O3 C9 C6 121.3(4) . . ? N2 C9 C6 115.5(4) . . ? N2 C10 C18 110.3(4) . . ? N2 C10 C11 112.0(4) . . ? C18 C10 C11 113.2(4) . . ? N2 C10 H10A 107.0 . . ? C18 C10 H10A 107.0 . . ? C11 C10 H10A 107.0 . . ? C12 C11 C10 116.2(5) . . ? C12 C11 H11A 108.2 . . ? C10 C11 H11A 108.2 . . ? C12 C11 H11B 108.3 . . ? C10 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? C17 C12 C13 118.3(6) . . ? C17 C12 C11 119.1(6) . . ? C13 C12 C11 122.6(7) . . ? C14 C13 C12 122.1(8) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 118.9 . . ? C15 C14 C13 119.6(8) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 122.6(8) . . ? C14 C15 H15 118.6 . . ? C16 C15 H15 118.8 . . ? C15 C16 C17 117.5(8) . . ? C15 C16 H16 121.2 . . ? C17 C16 H16 121.3 . . ? C12 C17 C16 119.9(7) . . ? C12 C17 H17 120.0 . . ? C16 C17 H17 120.1 . . ? C10 C18 C19 112.4(4) . . ? C10 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? C10 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 112.0(4) . . ? C18 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? O4 C20 N3 123.0(5) . . ? O4 C20 C19 122.2(5) . . ? N3 C20 C19 114.8(5) . . ? N3 C21 C26 114.1(4) . . ? N3 C21 C22 110.8(5) . . ? C26 C21 C22 108.7(4) . . ? N3 C21 H21 107.7 . . ? C26 C21 H21 107.7 . . ? C22 C21 H21 107.7 . . ? C21 C22 C23 116.4(5) . . ? C21 C22 H22A 108.2 . . ? C23 C22 H22A 108.2 . . ? C21 C22 H22B 108.2 . . ? C23 C22 H22B 108.2 . . ? H22A C22 H22B 107.3 . . ? C25 C23 C22 109.6(7) . . ? C25 C23 C24 112.7(7) . . ? C22 C23 C24 110.5(6) . . ? C25 C23 H23 107.9 . . ? C22 C23 H23 107.9 . . ? C24 C23 H23 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O5 C26 N4 125.7(5) . . ? O5 C26 C21 116.3(4) . . ? N4 C26 C21 117.9(5) . . ? N4 C27 C35 111.2(4) . . ? N4 C27 C28 111.4(4) . . ? C35 C27 C28 110.2(4) . . ? N4 C27 H27 108.0 . . ? C35 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C29 C28 C27 114.3(4) . . ? C29 C28 H28A 108.7 . . ? C27 C28 H28A 108.7 . . ? C29 C28 H28B 108.6 . . ? C27 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C30 C29 C34 116.1(6) . . ? C30 C29 C28 125.7(6) . . ? C34 C29 C28 118.1(6) . . ? C31 C30 C29 124.8(7) . . ? C31 C30 H30 117.6 . . ? C29 C30 H30 117.6 . . ? C30 C31 C32 120.6(7) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C33 116.9(7) . . ? C31 C32 H32 121.6 . . ? C33 C32 H32 121.6 . . ? C32 C33 C34 121.2(8) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C29 C34 C33 120.4(7) . . ? C29 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C27 C35 C36 116.0(4) . . ? C27 C35 H35A 108.3 . . ? C36 C35 H35A 108.3 . . ? C27 C35 H35B 108.3 . . ? C36 C35 H35B 108.3 . . ? H35A C35 H35B 107.4 . . ? C37 C36 C35 114.4(4) . . ? C37 C36 H36A 108.6 . . ? C35 C36 H36A 108.7 . . ? C37 C36 H36B 108.7 . . ? C35 C36 H36B 108.7 . . ? H36A C36 H36B 107.6 . . ? O6 C37 N5 123.2(5) . . ? O6 C37 C36 123.0(5) . . ? N5 C37 C36 113.8(5) . . ? N5 C38 C40 107.6(5) . . ? N5 C38 C39 108.8(4) . . ? C40 C38 C39 111.5(4) . . ? N5 C38 C41 112.3(4) . . ? C40 C38 C41 106.9(5) . . ? C39 C38 C41 109.8(5) . . ? 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 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O7 C41 N6 124.8(5) . . ? O7 C41 C38 119.7(5) . . ? N6 C41 C38 115.4(5) . . ? N6 C42 C43 110.2(5) . . ? N6 C42 C50 112.3(5) . . ? C43 C42 C50 110.6(5) . . ? N6 C42 H42 107.8 . . ? C43 C42 H42 107.9 . . ? C50 C42 H42 107.9 . . ? C42 C43 C44 114.7(5) . . ? C42 C43 H43A 108.6 . . ? C44 C43 H43A 108.6 . . ? C42 C43 H43B 108.6 . . ? C44 C43 H43B 108.6 . . ? H43A C43 H43B 107.6 . . ? C45 C44 C49 116.3(7) . . ? C45 C44 C43 121.1(6) . . ? C49 C44 C43 122.6(7) . . ? C46 C45 C44 119.6(7) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 121.6(9) . . ? C45 C46 H46 119.2 . . ? C47 C46 H46 119.2 . . ? C48 C47 C46 120.7(9) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C49 C48 C47 117.4(8) . . ? C49 C48 H48 121.3 . . ? C47 C48 H48 121.3 . . ? C48 C49 C44 124.4(8) . . ? C48 C49 H49 117.8 . . ? C44 C49 H49 117.8 . . ? C42 C50 C51 112.2(5) . . ? C42 C50 H50A 109.2 . . ? C51 C50 H50A 109.2 . . ? C42 C50 H50B 109.2 . . ? C51 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? C52 C51 C50 117.8(5) . . ? C52 C51 H51A 107.9 . . ? C50 C51 H51A 107.9 . . ? C52 C51 H51B 107.8 . . ? C50 C51 H51B 107.9 . . ? H51A C51 H51B 107.2 . . ? O8 C52 O9 121.2(7) . . ? O8 C52 C51 125.4(7) . . ? O9 C52 C51 113.1(7) . . ? C54 C53 O9 100.7(11) . . ? C54 C53 H53A 111.5 . . ? O9 C53 H53A 111.6 . . ? C54 C53 H53B 111.7 . . ? O9 C53 H53B 111.6 . . ? H53A C53 H53B 109.4 . . ? C53 C54 H54A 110.2 . . ? C53 C54 H54B 110.4 . . ? H54A C54 H54B 108.7 . . ? C53 C54 H54C 110.2 . . ? H54A C54 H54C 108.7 . . ? H54B C54 H54C 108.7 . . ? O10 C55 C57 109.5(5) . . ? O10 C55 C56 102.0(4) . . ? C57 C55 C56 110.7(5) . . ? O10 C55 C58 109.7(4) . . ? C57 C55 C58 113.6(5) . . ? C56 C55 C58 110.7(5) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 H57A 109.5 . . ? C55 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C55 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C55 C58 H58A 109.5 . . ? C55 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C55 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O11 C59 N7 125.0(6) . . ? O11 C59 O10 123.4(5) . . ? N7 C59 O10 111.5(5) . . ? N7 C60 C62 111.4(4) . . ? N7 C60 C61 109.0(4) . . ? C62 C60 C61 109.3(4) . . ? N7 C60 C63 111.1(4) . . ? C62 C60 C63 108.0(5) . . ? C61 C60 C63 107.9(4) . . ? 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 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O12 C63 N8 121.8(5) . . ? O12 C63 C60 123.3(5) . . ? N8 C63 C60 114.8(5) . . ? N8 C64 C65 111.2(4) . . ? N8 C64 C72 110.0(4) . . ? C65 C64 C72 114.8(4) . . ? N8 C64 H64 106.8 . . ? C65 C64 H64 106.8 . . ? C72 C64 H64 106.8 . . ? C66 C65 C64 116.1(5) . . ? C66 C65 H65A 108.3 . . ? C64 C65 H65A 108.3 . . ? C66 C65 H65B 108.3 . . ? C64 C65 H65B 108.3 . . ? H65A C65 H65B 107.4 . . ? C67 C66 C71 117.2(7) . . ? C67 C66 C65 120.9(6) . . ? C71 C66 C65 121.8(6) . . ? C66 C67 C68 124.3(7) . . ? C66 C67 H67 117.9 . . ? C68 C67 H67 117.9 . . ? C69 C68 C67 118.1(7) . . ? C69 C68 H68 120.9 . . ? C67 C68 H68 120.9 . . ? C70 C69 C68 120.3(7) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.8 . . ? C69 C70 C71 120.1(7) . . ? C69 C70 H70 119.9 . . ? C71 C70 H70 120.0 . . ? C66 C71 C70 120.0(7) . . ? C66 C71 H71 120.0 . . ? C70 C71 H71 120.0 . . ? C73 C72 C64 114.0(4) . . ? C73 C72 H72A 108.7 . . ? C64 C72 H72A 108.7 . . ? C73 C72 H72B 108.8 . . ? C64 C72 H72B 108.8 . . ? H72A C72 H72B 107.6 . . ? C74 C73 C72 109.3(5) . . ? C74 C73 H73A 109.8 . . ? C72 C73 H73A 109.8 . . ? C74 C73 H73B 109.8 . . ? C72 C73 H73B 109.8 . . ? H73A C73 H73B 108.3 . . ? O13 C74 N9 119.6(5) . . ? O13 C74 C73 124.3(5) . . ? N9 C74 C73 116.1(6) . . ? N9 C75 C76 113.1(5) . . ? N9 C75 C80 111.6(4) . . ? C76 C75 C80 110.3(4) . . ? N9 C75 H75 107.2 . . ? C76 C75 H75 107.2 . . ? C80 C75 H75 107.2 . . ? C77 C76 C75 115.1(5) . . ? C77 C76 H76A 108.5 . . ? C75 C76 H76A 108.5 . . ? C77 C76 H76B 108.5 . . ? C75 C76 H76B 108.5 . . ? H76A C76 H76B 107.5 . . ? C76 C77 C78 110.8(7) . . ? C76 C77 C79 109.1(6) . . ? C78 C77 C79 110.8(6) . . ? C76 C77 H77 108.7 . . ? C78 C77 H77 108.7 . . ? C79 C77 H77 108.7 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O14 C80 N10 124.0(6) . . ? O14 C80 C75 115.5(5) . . ? N10 C80 C75 120.4(5) . . ? N10 C81 C89 110.7(5) . . ? N10 C81 C82 109.5(5) . . ? C89 C81 C82 111.7(5) . . ? N10 C81 H81 108.3 . . ? C89 C81 H81 108.3 . . ? C82 C81 H81 108.3 . . ? C83 C82 C81 115.5(5) . . ? C83 C82 H82A 108.4 . . ? C81 C82 H82A 108.4 . . ? C83 C82 H82B 108.4 . . ? C81 C82 H82B 108.4 . . ? H82A C82 H82B 107.5 . . ? C88 C83 C84 122.4(7) . . ? C88 C83 C82 118.1(8) . . ? C84 C83 C82 119.5(7) . . ? C83 C84 C85 118.1(8) . . ? C83 C84 H84 121.0 . . ? C85 C84 H84 120.9 . . ? C84 C85 C86 121.1(9) . . ? C84 C85 H85 119.5 . . ? C86 C85 H85 119.5 . . ? C87 C86 C85 121.5(9) . . ? C87 C86 H86 119.2 . . ? C85 C86 H86 119.2 . . ? C86 C87 C88 117.0(9) . . ? C86 C87 H87 121.5 . . ? C88 C87 H87 121.5 . . ? C83 C88 C87 119.3(8) . . ? C83 C88 H88 120.4 . . ? C87 C88 H88 120.4 . . ? C90 C89 C81 117.3(4) . . ? C90 C89 H89A 108.0 . . ? C81 C89 H89A 108.0 . . ? C90 C89 H89B 108.0 . . ? C81 C89 H89B 108.0 . . ? H89A C89 H89B 107.2 . . ? C91 C90 C89 113.8(5) . . ? C91 C90 H90A 108.8 . . ? C89 C90 H90A 108.8 . . ? C91 C90 H90B 108.8 . . ? C89 C90 H90B 108.8 . . ? H90A C90 H90B 107.7 . . ? O15 C91 N11 121.3(6) . . ? O15 C91 C90 122.8(6) . . ? N11 C91 C90 115.8(6) . . ? N11 C92 C93 110.0(5) . . ? N11 C92 C94 104.7(5) . . ? C93 C92 C94 110.7(5) . . ? N11 C92 C95 114.0(4) . . ? C93 C92 C95 110.8(5) . . ? C94 C92 C95 106.3(5) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C92 C94 H94A 109.5 . . ? C92 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C92 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? O16 C95 N12 123.7(6) . . ? O16 C95 C92 120.4(6) . . ? N12 C95 C92 115.9(6) . . ? N12 C96 C104 110.0(5) . . ? N12 C96 C97 111.6(6) . . ? C104 C96 C97 113.9(6) . . ? N12 C96 H96 107.0 . . ? C104 C96 H96 107.0 . . ? C97 C96 H96 107.0 . . ? C96 C97 C98 114.0(6) . . ? C96 C97 H97A 108.8 . . ? C98 C97 H97A 108.7 . . ? C96 C97 H97B 108.8 . . ? C98 C97 H97B 108.8 . . ? H97A C97 H97B 107.6 . . ? C103 C98 C99 114.6(11) . . ? C103 C98 C97 123.8(10) . . ? C99 C98 C97 121.6(10) . . ? C100 C99 C98 122.2(13) . . ? C100 C99 H99 118.8 . . ? C98 C99 H99 119.0 . . ? C101 C100 C99 115.3(14) . . ? C101 C100 H100 122.2 . . ? C99 C100 H100 122.5 . . ? C100 C101 C102 123.5(15) . . ? C100 C101 H101 118.3 . . ? C102 C101 H101 118.1 . . ? C101 C102 C103 121.7(13) . . ? C101 C102 H102 119.2 . . ? C103 C102 H102 119.1 . . ? C98 C103 C102 121.5(11) . . ? C98 C103 H103 119.2 . . ? C102 C103 H103 119.3 . . ? C96 C104 C105 115.1(5) . . ? C96 C104 H10B 108.5 . . ? C105 C104 H10B 108.5 . . ? C96 C104 H10C 108.5 . . ? C105 C104 H10C 108.5 . . ? H10B C104 H10C 107.5 . . ? C106 C105 C104 118.1(5) . . ? C106 C105 H10D 107.8 . . ? C104 C105 H10D 107.8 . . ? C106 C105 H10E 107.8 . . ? C104 C105 H10E 107.8 . . ? H10D C105 H10E 107.1 . . ? O17 C106 O18 120.5(7) . . ? O17 C106 C105 125.6(7) . . ? O18 C106 C105 113.8(7) . . ? C108 C107 O18 104.5(8) . . ? C108 C107 H10H 110.9 . . ? O18 C107 H10H 110.8 . . ? C108 C107 H10I 110.8 . . ? O18 C107 H10I 110.9 . . ? H10H C107 H10I 108.9 . . ? C107 C108 H10J 111.2 . . ? C107 C108 H10K 111.3 . . ? H10J C108 H10K 107.7 . . ? C107 C108 H10L 111.0 . . ? H10J C108 H10L 107.7 . . ? H10K C108 H10L 107.8 . . ? C5 N1 C6 120.3(4) . . ? C5 N1 H1 119.8 . . ? C6 N1 H1 119.8 . . ? C9 N2 C10 121.4(4) . . ? C9 N2 H2 119.3 . . ? C10 N2 H2 119.3 . . ? C20 N3 C21 120.4(4) . . ? C20 N3 H3 119.8 . . ? C21 N3 H3 119.8 . . ? C26 N4 C27 121.6(4) . . ? C26 N4 H4 119.2 . . ? C27 N4 H4 119.2 . . ? C37 N5 C38 123.1(5) . . ? C37 N5 H5 118.4 . . ? C38 N5 H5 118.4 . . ? C41 N6 C42 125.6(5) . . ? C41 N6 H6 117.2 . . ? C42 N6 H6 117.2 . . ? C59 N7 C60 122.2(5) . . ? C59 N7 H7 118.9 . . ? C60 N7 H7 118.9 . . ? C63 N8 C64 122.0(5) . . ? C63 N8 H8 119.0 . . ? C64 N8 H8 119.0 . . ? C74 N9 C75 124.3(5) . . ? C74 N9 H9 117.8 . . ? C75 N9 H9 117.8 . . ? C80 N10 C81 122.6(5) . . ? C80 N10 H10 118.7 . . ? C81 N10 H10 118.7 . . ? C91 N11 C92 122.5(5) . . ? C91 N11 H11 118.7 . . ? C92 N11 H11 118.8 . . ? C95 N12 C96 127.5(5) . . ? C95 N12 H19E 116.2 . . ? C96 N12 H19E 116.2 . . ? C5 O1 C1 118.3(4) . . ? C52 O9 C53 118.3(6) . . ? C59 O10 C55 121.8(4) . . ? C106 O18 C107 115.1(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.292 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.055