# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Ivan Huc' 'Victor Maurizot' 'Heinz Gornitzka' 'Jean-Michel Leger' _publ_requested_journal 'Chemical Communications' _publ_contact_author_name 'Dr Ivan Huc' _publ_contact_author_address ; IECB 16, av. Pey Berland Pessac 33607 FRANCE ; _publ_contact_author_email 'I.HUC@IECB-POLYTECHNIQUE.U-BORDEAUX.FR' _publ_section_title ; Hydroxy-substituted oligopyridine-dicarboxamides helical folders ; data_1B _database_code_CSD 176827 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H25 N7 O6 S' _chemical_formula_weight 527.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.422(2) _cell_length_b 10.165(3) _cell_length_c 14.420(4) _cell_angle_alpha 93.370(7) _cell_angle_beta 91.761(5) _cell_angle_gamma 91.344(7) _cell_volume 1231.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2005 _cell_measurement_theta_min 2.553 _cell_measurement_theta_max 28.636 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5591 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0888 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3507 _reflns_number_gt 2329 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3507 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7277(5) 0.9377(4) 0.0664(2) 0.0377(11) Uani 1 1 d . . . H1A H 0.8181 0.9583 0.0281 0.057 Uiso 1 1 calc R . . H1B H 0.6370 0.9906 0.0487 0.057 Uiso 1 1 calc R . . H1C H 0.6988 0.8438 0.0567 0.057 Uiso 1 1 calc R . . C2 C 0.7726(4) 0.9690(3) 0.1672(2) 0.0271(9) Uani 1 1 d . . . C3 C 0.6829(4) 0.9291(3) 0.3261(2) 0.0227(8) Uani 1 1 d . . . C4 C 0.7869(4) 1.0146(3) 0.3785(2) 0.0276(9) Uani 1 1 d . . . H4 H 0.8554 1.0746 0.3499 0.033 Uiso 1 1 calc R . . C5 C 0.7859(4) 1.0082(3) 0.4742(2) 0.0284(9) Uani 1 1 d . . . H5 H 0.8546 1.0658 0.5121 0.034 Uiso 1 1 calc R . . C6 C 0.6871(4) 0.9200(3) 0.5163(2) 0.0250(9) Uani 1 1 d . . . H6 H 0.6881 0.9143 0.5818 0.030 Uiso 1 1 calc R . . C7 C 0.5877(4) 0.8410(3) 0.4580(2) 0.0222(8) Uani 1 1 d . . . C8 C 0.4594(4) 0.7006(3) 0.5743(2) 0.0236(9) Uani 1 1 d . . . C9 C 0.3451(4) 0.5843(3) 0.5739(2) 0.0222(8) Uani 1 1 d . . . C10 C 0.3104(4) 0.5297(3) 0.6573(2) 0.0240(9) Uani 1 1 d . . . H10 H 0.3585 0.5649 0.7142 0.029 Uiso 1 1 calc R . . C11 C 0.2047(4) 0.4230(3) 0.6563(2) 0.0230(8) Uani 1 1 d . . . C12 C 0.1385(4) 0.3738(3) 0.5707(2) 0.0237(9) Uani 1 1 d . . . H12 H 0.0656 0.3007 0.5673 0.028 Uiso 1 1 calc R . . C13 C 0.1817(4) 0.4338(3) 0.4911(2) 0.0218(8) Uani 1 1 d . . . C14 C 0.1119(4) 0.3793(3) 0.3980(2) 0.0227(8) Uani 1 1 d . . . C15 C 0.1335(4) 0.4178(3) 0.2291(2) 0.0209(8) Uani 1 1 d . . . C16 C 0.0296(4) 0.3195(3) 0.1934(2) 0.0249(9) Uani 1 1 d . . . H16 H -0.0314 0.2677 0.2327 0.030 Uiso 1 1 calc R . . C17 C 0.0184(4) 0.2999(3) 0.0973(2) 0.0273(9) Uani 1 1 d . . . H17 H -0.0510 0.2324 0.0700 0.033 Uiso 1 1 calc R . . C18 C 0.1064(4) 0.3767(3) 0.0406(2) 0.0267(9) Uani 1 1 d . . . H18 H 0.1005 0.3621 -0.0251 0.032 Uiso 1 1 calc R . . C19 C 0.2036(4) 0.4758(3) 0.0833(2) 0.0231(9) Uani 1 1 d . . . C20 C 0.3326(4) 0.5590(4) -0.0560(2) 0.0263(9) Uani 1 1 d . . . C21 C 0.4191(5) 0.6769(4) -0.0895(2) 0.0361(10) Uani 1 1 d . . . H21A H 0.5078 0.6477 -0.1273 0.054 Uiso 1 1 calc R . . H21B H 0.4600 0.7328 -0.0360 0.054 Uiso 1 1 calc R . . H21C H 0.3460 0.7272 -0.1270 0.054 Uiso 1 1 calc R . . C22 C 0.1767(5) 0.8269(4) 0.2707(2) 0.0362(10) Uani 1 1 d . . . H22A H 0.1466 0.7330 0.2639 0.054 Uiso 1 1 calc R . . H22B H 0.0879 0.8769 0.2957 0.054 Uiso 1 1 calc R . . H22C H 0.2694 0.8395 0.3133 0.054 Uiso 1 1 calc R . . C23 C 0.2833(5) 1.0480(3) 0.1971(3) 0.0369(10) Uani 1 1 d . . . H23A H 0.3690 1.0462 0.2445 0.055 Uiso 1 1 calc R . . H23B H 0.1923 1.0936 0.2235 0.055 Uiso 1 1 calc R . . H23C H 0.3209 1.0947 0.1441 0.055 Uiso 1 1 calc R . . N1 N 0.6684(4) 0.9224(3) 0.22830(18) 0.0254(8) Uani 1 1 d . . . H1N H 0.581(4) 0.882(3) 0.208(2) 0.030 Uiso 1 1 d . . . N2 N 0.5818(3) 0.8451(3) 0.36436(18) 0.0236(7) Uani 1 1 d . . . N3 N 0.4824(4) 0.7433(3) 0.48759(19) 0.0252(8) Uani 1 1 d . . . H3N H 0.430(4) 0.698(3) 0.441(2) 0.030 Uiso 1 1 d . . . N4 N 0.2825(3) 0.5378(3) 0.49019(17) 0.0214(7) Uani 1 1 d . . . N5 N 0.1648(4) 0.4465(3) 0.32487(17) 0.0240(7) Uani 1 1 d . . . H5N H 0.235(4) 0.516(3) 0.337(2) 0.029 Uiso 1 1 d . . . N6 N 0.2190(3) 0.4964(3) 0.17640(17) 0.0236(7) Uani 1 1 d . . . N7 N 0.2952(4) 0.5665(3) 0.03534(18) 0.0263(8) Uani 1 1 d . . . H7N H 0.331(4) 0.630(4) 0.072(2) 0.032 Uiso 1 1 d . . . O1 O 0.8950(3) 1.0301(3) 0.19096(17) 0.0405(7) Uani 1 1 d . . . O2 O 0.5240(3) 0.7478(2) 0.64593(16) 0.0353(7) Uani 1 1 d . . . O3 O 0.1611(3) 0.3642(2) 0.73375(16) 0.0306(7) Uani 1 1 d . . . H3O H 0.208(5) 0.405(4) 0.786(3) 0.042(12) Uiso 1 1 d . . . O4 O 0.0203(3) 0.2847(2) 0.39265(15) 0.0328(7) Uani 1 1 d . . . O5 O 0.2963(3) 0.4609(2) -0.10802(15) 0.0357(7) Uani 1 1 d . . . O6 O 0.3767(3) 0.8174(2) 0.13191(15) 0.0335(7) Uani 1 1 d . . . S1 S 0.22476(12) 0.88412(9) 0.15943(6) 0.0307(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(3) 0.043(2) 0.031(2) 0.0038(17) 0.0106(19) -0.008(2) C2 0.024(2) 0.027(2) 0.031(2) 0.0043(16) 0.0070(17) -0.0059(19) C3 0.021(2) 0.023(2) 0.0250(19) 0.0029(15) 0.0054(16) 0.0018(17) C4 0.025(2) 0.025(2) 0.032(2) -0.0002(16) 0.0065(17) -0.0063(18) C5 0.025(2) 0.029(2) 0.030(2) -0.0057(16) 0.0020(17) -0.0024(18) C6 0.024(2) 0.026(2) 0.0241(18) -0.0013(15) 0.0034(16) -0.0040(18) C7 0.022(2) 0.019(2) 0.0258(19) 0.0013(14) 0.0059(16) -0.0005(17) C8 0.025(2) 0.023(2) 0.024(2) 0.0007(15) 0.0064(16) 0.0011(17) C9 0.022(2) 0.024(2) 0.0207(18) -0.0004(15) 0.0033(16) 0.0014(17) C10 0.028(2) 0.026(2) 0.0179(17) -0.0019(15) 0.0041(16) -0.0001(18) C11 0.028(2) 0.0216(19) 0.0196(18) 0.0036(14) 0.0069(16) 0.0021(18) C12 0.023(2) 0.023(2) 0.0249(19) -0.0001(15) 0.0046(16) -0.0028(17) C13 0.022(2) 0.023(2) 0.0209(18) -0.0002(14) 0.0072(15) 0.0021(17) C14 0.024(2) 0.020(2) 0.0236(18) 0.0018(15) 0.0033(16) -0.0013(18) C15 0.020(2) 0.0215(19) 0.0212(18) -0.0024(15) 0.0034(15) 0.0007(17) C16 0.027(2) 0.023(2) 0.0254(19) 0.0025(15) 0.0035(16) 0.0003(18) C17 0.025(2) 0.029(2) 0.027(2) -0.0021(16) -0.0055(17) -0.0043(18) C18 0.028(2) 0.031(2) 0.0207(18) -0.0031(15) -0.0017(16) -0.0016(18) C19 0.022(2) 0.024(2) 0.0227(19) 0.0023(15) 0.0020(16) 0.0015(17) C20 0.023(2) 0.034(2) 0.0214(19) -0.0021(16) 0.0025(16) 0.0051(19) C21 0.038(3) 0.044(3) 0.027(2) 0.0055(17) 0.0085(18) -0.006(2) C22 0.034(2) 0.041(2) 0.034(2) 0.0044(18) 0.0090(18) -0.005(2) C23 0.040(3) 0.030(2) 0.041(2) 0.0035(18) 0.005(2) 0.002(2) N1 0.0211(18) 0.0315(18) 0.0231(16) 0.0016(13) 0.0006(14) -0.0112(15) N2 0.0217(17) 0.0251(17) 0.0241(16) 0.0031(12) 0.0027(13) -0.0046(14) N3 0.0284(19) 0.0258(17) 0.0212(16) 0.0018(13) 0.0019(14) -0.0089(15) N4 0.0204(17) 0.0231(17) 0.0207(15) 0.0006(12) 0.0045(13) -0.0011(14) N5 0.0283(18) 0.0233(17) 0.0201(16) 0.0009(12) 0.0015(13) -0.0087(15) N6 0.0267(18) 0.0253(17) 0.0184(15) -0.0008(12) 0.0032(13) -0.0041(15) N7 0.032(2) 0.0297(18) 0.0165(16) -0.0014(13) 0.0037(14) -0.0061(15) O1 0.0358(17) 0.0455(17) 0.0398(15) 0.0013(12) 0.0106(13) -0.0176(15) O2 0.0468(18) 0.0353(16) 0.0224(13) -0.0009(11) -0.0011(12) -0.0161(14) O3 0.0409(17) 0.0354(16) 0.0157(13) 0.0042(11) 0.0077(12) -0.0091(13) O4 0.0403(17) 0.0315(15) 0.0263(13) 0.0051(11) 0.0002(12) -0.0138(14) O5 0.0474(18) 0.0392(17) 0.0199(13) -0.0046(11) 0.0053(12) -0.0038(14) O6 0.0307(16) 0.0385(16) 0.0302(13) -0.0054(11) 0.0073(12) -0.0095(13) S1 0.0307(6) 0.0347(6) 0.0261(5) -0.0007(4) 0.0013(4) -0.0070(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.504(5) . ? C2 O1 1.220(4) . ? C2 N1 1.359(4) . ? C3 N2 1.344(4) . ? C3 C4 1.392(5) . ? C3 N1 1.410(4) . ? C4 C5 1.386(5) . ? C5 C6 1.386(5) . ? C6 C7 1.377(4) . ? C7 N2 1.353(4) . ? C7 N3 1.409(4) . ? C8 O2 1.220(4) . ? C8 N3 1.365(4) . ? C8 C9 1.507(5) . ? C9 N4 1.357(4) . ? C9 C10 1.391(4) . ? C10 C11 1.386(5) . ? C11 O3 1.354(4) . ? C11 C12 1.398(5) . ? C12 C13 1.386(4) . ? C13 N4 1.341(4) . ? C13 C14 1.518(4) . ? C14 O4 1.216(4) . ? C14 N5 1.370(4) . ? C15 N6 1.346(4) . ? C15 C16 1.378(4) . ? C15 N5 1.410(4) . ? C16 C17 1.389(5) . ? C17 C18 1.382(5) . ? C18 C19 1.386(5) . ? C19 N6 1.349(4) . ? C19 N7 1.413(4) . ? C20 O5 1.240(4) . ? C20 N7 1.361(4) . ? C20 C21 1.499(5) . ? C22 S1 1.793(3) . ? C23 S1 1.775(4) . ? O6 S1 1.515(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 C2 N1 123.4(3) . . ? O1 C2 C1 121.6(3) . . ? N1 C2 C1 114.9(3) . . ? N2 C3 C4 123.1(3) . . ? N2 C3 N1 112.4(3) . . ? C4 C3 N1 124.5(3) . . ? C5 C4 C3 117.0(3) . . ? C6 C5 C4 121.7(3) . . ? C7 C6 C5 116.5(3) . . ? N2 C7 C6 124.1(3) . . ? N2 C7 N3 111.2(3) . . ? C6 C7 N3 124.7(3) . . ? O2 C8 N3 125.3(3) . . ? O2 C8 C9 121.8(3) . . ? N3 C8 C9 112.9(3) . . ? N4 C9 C10 123.6(3) . . ? N4 C9 C8 117.0(3) . . ? C10 C9 C8 119.4(3) . . ? C11 C10 C9 119.0(3) . . ? O3 C11 C10 123.5(3) . . ? O3 C11 C12 118.1(3) . . ? C10 C11 C12 118.4(3) . . ? C13 C12 C11 118.5(3) . . ? N4 C13 C12 124.4(3) . . ? N4 C13 C14 117.0(3) . . ? C12 C13 C14 118.6(3) . . ? O4 C14 N5 125.9(3) . . ? O4 C14 C13 121.2(3) . . ? N5 C14 C13 112.9(3) . . ? N6 C15 C16 123.9(3) . . ? N6 C15 N5 112.0(3) . . ? C16 C15 N5 124.1(3) . . ? C15 C16 C17 116.8(3) . . ? C18 C17 C16 121.2(3) . . ? C17 C18 C19 117.5(3) . . ? N6 C19 C18 122.8(3) . . ? N6 C19 N7 112.7(3) . . ? C18 C19 N7 124.5(3) . . ? O5 C20 N7 121.8(3) . . ? O5 C20 C21 122.3(3) . . ? N7 C20 C21 115.9(3) . . ? C2 N1 C3 127.9(3) . . ? C3 N2 C7 117.6(3) . . ? C8 N3 C7 130.2(3) . . ? C13 N4 C9 116.2(3) . . ? C14 N5 C15 128.2(3) . . ? C15 N6 C19 117.8(3) . . ? C20 N7 C19 128.0(3) . . ? O6 S1 C23 105.34(17) . . ? O6 S1 C22 106.39(17) . . ? C23 S1 C22 97.79(17) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.306 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.061 #===END data_2A(nitrobenzene_heptane) _database_code_CSD 176828 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H64 N16 O16' _chemical_formula_weight 1409.39 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 37.717(3) _cell_length_b 13.1706(9) _cell_length_c 13.6264(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.3720(10) _cell_angle_gamma 90.00 _cell_volume 6763.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7076 _cell_measurement_theta_min 3.114 _cell_measurement_theta_max 27.865 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type 'semi-empirical' _exptl_absorpt_correction_T_min 0.478766 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17200 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9250 _reflns_number_gt 7544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+2.7858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(10) _refine_ls_number_reflns 9250 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 296 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1300 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.66376(11) 0.5042(4) 0.9361(3) 0.0423(10) Uani 1 1 d . . . H1A H 0.6536 0.4978 1.0009 0.063 Uiso 1 1 calc R . . H1B H 0.6480 0.4715 0.8866 0.063 Uiso 1 1 calc R . . H1C H 0.6663 0.5762 0.9199 0.063 Uiso 1 1 calc R . . C2 C 0.69971(11) 0.4536(3) 0.9376(3) 0.0317(9) Uani 1 1 d . . . C3 C 0.76338(10) 0.4901(3) 0.9115(3) 0.0260(8) Uani 1 1 d . . . C4 C 0.77732(11) 0.3920(3) 0.9171(3) 0.0338(10) Uani 1 1 d . . . H4 H 0.7630 0.3349 0.9311 0.041 Uiso 1 1 calc R . . C5 C 0.81306(12) 0.3830(3) 0.9012(3) 0.0371(10) Uani 1 1 d . . . H5 H 0.8235 0.3173 0.9019 0.045 Uiso 1 1 calc R . . C6 C 0.83418(11) 0.4665(3) 0.8843(3) 0.0331(9) Uani 1 1 d . . . H6 H 0.8588 0.4600 0.8734 0.040 Uiso 1 1 calc R . . C7 C 0.81734(10) 0.5606(3) 0.8841(3) 0.0286(8) Uani 1 1 d . . . C8 C 0.87002(10) 0.6738(3) 0.8778(3) 0.0314(9) Uani 1 1 d . . . C9 C 0.87822(10) 0.7857(3) 0.8761(3) 0.0302(8) Uani 1 1 d . . . C10 C 0.91257(11) 0.8165(3) 0.8989(3) 0.0350(9) Uani 1 1 d . . . H10 H 0.9309 0.7680 0.9105 0.042 Uiso 1 1 calc R . . C11 C 0.91980(11) 0.9201(3) 0.9044(3) 0.0348(9) Uani 1 1 d . . . C12 C 0.89248(10) 0.9894(3) 0.8865(3) 0.0321(9) Uani 1 1 d . . . H12 H 0.8966 1.0605 0.8890 0.039 Uiso 1 1 calc R . . C13 C 0.85881(10) 0.9501(3) 0.8647(3) 0.0287(8) Uani 1 1 d . . . C14 C 0.96154(11) 1.0522(3) 0.9378(4) 0.0392(10) Uani 1 1 d . . . H14A H 0.9481 1.0826 0.9914 0.047 Uiso 1 1 calc R . . H14B H 0.9544 1.0869 0.8757 0.047 Uiso 1 1 calc R . . C15 C 1.00082(11) 1.0661(3) 0.9589(3) 0.0353(9) Uani 1 1 d . . . C16 C 1.01345(12) 1.1648(3) 0.9706(3) 0.0419(11) Uani 1 1 d . . . H16 H 0.9973 1.2201 0.9676 0.050 Uiso 1 1 calc R . . C17 C 1.04945(12) 1.1833(4) 0.9865(4) 0.0487(12) Uani 1 1 d . . . H17 H 1.0578 1.2510 0.9940 0.058 Uiso 1 1 calc R . . C18 C 1.07301(12) 1.1035(4) 0.9914(4) 0.0499(12) Uani 1 1 d . . . H18 H 1.0976 1.1160 1.0028 0.060 Uiso 1 1 calc R . . C19 C 1.06082(12) 1.0054(4) 0.9797(4) 0.0488(12) Uani 1 1 d . . . H19 H 1.0771 0.9504 0.9818 0.059 Uiso 1 1 calc R . . C20 C 1.02475(11) 0.9866(3) 0.9648(4) 0.0434(11) Uani 1 1 d . . . H20 H 1.0165 0.9186 0.9585 0.052 Uiso 1 1 calc R . . C21 C 0.82853(10) 1.0238(3) 0.8519(3) 0.0290(8) Uani 1 1 d . . . C22 C 0.76299(9) 1.0242(3) 0.8235(3) 0.0229(7) Uani 1 1 d . . . C23 C 0.75736(10) 1.1277(3) 0.8352(3) 0.0305(9) Uani 1 1 d . . . H23 H 0.7765 1.1734 0.8471 0.037 Uiso 1 1 calc R . . C24 C 0.72253(10) 1.1612(3) 0.8289(3) 0.0322(9) Uani 1 1 d . . . H24 H 0.7176 1.2312 0.8386 0.039 Uiso 1 1 calc R . . C25 C 0.69455(10) 1.0946(3) 0.8086(3) 0.0280(8) Uani 1 1 d . . . H25 H 0.6706 1.1172 0.8023 0.034 Uiso 1 1 calc R . . C26 C 0.70366(10) 0.9933(3) 0.7981(3) 0.0258(8) Uani 1 1 d . . . C27 C 0.64221(10) 0.9253(3) 0.7701(3) 0.0274(8) Uani 1 1 d . . . C28 C 0.62339(9) 0.8256(3) 0.7503(3) 0.0265(8) Uani 1 1 d . . . C29 C 0.58643(10) 0.8250(3) 0.7525(3) 0.0293(8) Uani 1 1 d . . . H29 H 0.5735 0.8849 0.7657 0.035 Uiso 1 1 calc R . . C30 C 0.56930(10) 0.7326(3) 0.7345(3) 0.0314(9) Uani 1 1 d . . . C31 C 0.58954(10) 0.6471(3) 0.7147(3) 0.0321(9) Uani 1 1 d . . . H31 H 0.5784 0.5834 0.7023 0.038 Uiso 1 1 calc R . . C32 C 0.62600(9) 0.6565(3) 0.7136(3) 0.0253(8) Uani 1 1 d . . . C33 C 0.51170(10) 0.8044(3) 0.7538(3) 0.0327(9) Uani 1 1 d . . . H33A H 0.5156 0.8594 0.7058 0.039 Uiso 1 1 calc R . . H33B H 0.5174 0.8308 0.8206 0.039 Uiso 1 1 calc R . . C34 C 0.47383(10) 0.7689(3) 0.7458(3) 0.0333(9) Uani 1 1 d . . . C35 C 0.46312(11) 0.6903(3) 0.6838(3) 0.0388(10) Uani 1 1 d . . . H35 H 0.4801 0.6555 0.6468 0.047 Uiso 1 1 calc R . . C36 C 0.42766(12) 0.6621(4) 0.6754(4) 0.0456(11) Uani 1 1 d . . . H36 H 0.4206 0.6077 0.6331 0.055 Uiso 1 1 calc R . . C37 C 0.40273(11) 0.7125(4) 0.7278(4) 0.0456(12) Uani 1 1 d . . . H37 H 0.3784 0.6939 0.7211 0.055 Uiso 1 1 calc R . . C38 C 0.41335(12) 0.7904(4) 0.7903(4) 0.0512(12) Uani 1 1 d . . . H38 H 0.3964 0.8245 0.8279 0.061 Uiso 1 1 calc R . . C39 C 0.44897(11) 0.8191(3) 0.7982(4) 0.0433(11) Uani 1 1 d . . . H39 H 0.4560 0.8737 0.8400 0.052 Uiso 1 1 calc R . . C40 C 0.64720(10) 0.5635(3) 0.6938(3) 0.0263(8) Uani 1 1 d . . . C41 C 0.70905(10) 0.5032(3) 0.6817(3) 0.0252(8) Uani 1 1 d . . . C42 C 0.70145(11) 0.4002(3) 0.6719(3) 0.0311(9) Uani 1 1 d . . . H42 H 0.6780 0.3750 0.6770 0.037 Uiso 1 1 calc R . . C43 C 0.72940(10) 0.3363(3) 0.6545(3) 0.0306(9) Uani 1 1 d . . . H43 H 0.7251 0.2656 0.6467 0.037 Uiso 1 1 calc R . . C44 C 0.76367(10) 0.3730(3) 0.6481(3) 0.0294(8) Uani 1 1 d . . . H44 H 0.7831 0.3291 0.6377 0.035 Uiso 1 1 calc R . . C45 C 0.76818(10) 0.4777(3) 0.6578(3) 0.0231(7) Uani 1 1 d . . . C46 C 0.83285(10) 0.4800(3) 0.6331(3) 0.0269(8) Uani 1 1 d . . . C47 C 0.86258(10) 0.5556(3) 0.6192(3) 0.0269(8) Uani 1 1 d . . . C48 C 0.89531(10) 0.5179(3) 0.5959(3) 0.0296(8) Uani 1 1 d . . . H48 H 0.8996 0.4469 0.5939 0.036 Uiso 1 1 calc R . . C49 C 0.92191(10) 0.5876(3) 0.5754(3) 0.0336(9) Uani 1 1 d . . . C50 C 0.91402(10) 0.6917(3) 0.5804(3) 0.0341(9) Uani 1 1 d . . . H50 H 0.9315 0.7412 0.5671 0.041 Uiso 1 1 calc R . . C51 C 0.88037(10) 0.7205(3) 0.6051(3) 0.0290(8) Uani 1 1 d . . . C52 C 0.96288(10) 0.4567(3) 0.5403(3) 0.0367(10) Uani 1 1 d . . . H52A H 0.9478 0.4261 0.4869 0.044 Uiso 1 1 calc R . . H52B H 0.9576 0.4221 0.6025 0.044 Uiso 1 1 calc R . . C53 C 1.00163(11) 0.4427(3) 0.5190(3) 0.0357(9) Uani 1 1 d . . . C54 C 1.02586(12) 0.5214(4) 0.5212(4) 0.0512(13) Uani 1 1 d . . . H54 H 1.0183 0.5888 0.5338 0.061 Uiso 1 1 calc R . . C55 C 1.06130(13) 0.5016(4) 0.5050(5) 0.0636(16) Uani 1 1 d . . . H55 H 1.0779 0.5560 0.5060 0.076 Uiso 1 1 calc R . . C56 C 1.07266(13) 0.4048(4) 0.4875(4) 0.0544(13) Uani 1 1 d . . . H56 H 1.0969 0.3922 0.4755 0.065 Uiso 1 1 calc R . . C57 C 1.04873(12) 0.3255(4) 0.4876(4) 0.0464(11) Uani 1 1 d . . . H57 H 1.0566 0.2579 0.4773 0.056 Uiso 1 1 calc R . . C58 C 1.01348(12) 0.3445(3) 0.5027(3) 0.0413(10) Uani 1 1 d . . . H58 H 0.9971 0.2898 0.5020 0.050 Uiso 1 1 calc R . . C59 C 0.87138(10) 0.8318(3) 0.6071(3) 0.0296(8) Uani 1 1 d . . . C60 C 0.81816(10) 0.9438(3) 0.5995(3) 0.0265(8) Uani 1 1 d . . . C61 C 0.83540(10) 1.0370(3) 0.5978(3) 0.0301(9) Uani 1 1 d . . . H61 H 0.8604 1.0424 0.6082 0.036 Uiso 1 1 calc R . . C62 C 0.81428(11) 1.1216(3) 0.5802(3) 0.0314(9) Uani 1 1 d . . . H62 H 0.8249 1.1869 0.5793 0.038 Uiso 1 1 calc R . . C63 C 0.77816(10) 1.1127(3) 0.5640(3) 0.0275(8) Uani 1 1 d . . . H63 H 0.7637 1.1702 0.5496 0.033 Uiso 1 1 calc R . . C64 C 0.76370(10) 1.0149(3) 0.5696(3) 0.0264(8) Uani 1 1 d . . . C65 C 0.69987(11) 1.0587(3) 0.5365(3) 0.0296(8) Uani 1 1 d . . . C66 C 0.66350(11) 1.0127(3) 0.5353(4) 0.0396(10) Uani 1 1 d . . . H66A H 0.6499 1.0355 0.4766 0.059 Uiso 1 1 calc R . . H66B H 0.6514 1.0340 0.5941 0.059 Uiso 1 1 calc R . . H66C H 0.6655 0.9385 0.5345 0.059 Uiso 1 1 calc R . . N1 N 0.72736(9) 0.5145(3) 0.9207(2) 0.0299(7) Uani 1 1 d . . . H1N H 0.7220(12) 0.572(4) 0.906(3) 0.036 Uiso 1 1 d . . . N2 N 0.78275(8) 0.5728(2) 0.8961(2) 0.0266(7) Uani 1 1 d . . . N3 N 0.83493(9) 0.6533(3) 0.8705(3) 0.0311(8) Uani 1 1 d . . . H3N H 0.8226(13) 0.696(4) 0.858(4) 0.037 Uiso 1 1 d . . . N4 N 0.85118(8) 0.8498(2) 0.8597(2) 0.0267(7) Uani 1 1 d . . . N5 N 0.79659(8) 0.9791(2) 0.8317(2) 0.0251(7) Uani 1 1 d . . . H5N H 0.7960(11) 0.920(4) 0.825(3) 0.030 Uiso 1 1 d . . . N6 N 0.73693(8) 0.9573(2) 0.8049(2) 0.0236(6) Uani 1 1 d . . . N7 N 0.67833(8) 0.9159(2) 0.7788(2) 0.0279(7) Uani 1 1 d . . . H7N H 0.6890(11) 0.852(3) 0.781(3) 0.033 Uiso 1 1 d . . . N8 N 0.64320(8) 0.7449(2) 0.7304(2) 0.0251(7) Uani 1 1 d . . . N9 N 0.68297(8) 0.5763(2) 0.6989(2) 0.0274(7) Uani 1 1 d . . . H9N H 0.6903(11) 0.637(4) 0.717(3) 0.033 Uiso 1 1 d . . . N10 N 0.74173(8) 0.5416(2) 0.6745(2) 0.0241(6) Uani 1 1 d . . . N11 N 0.80135(8) 0.5245(2) 0.6501(2) 0.0256(7) Uani 1 1 d . . . H11N H 0.8008(11) 0.584(3) 0.660(3) 0.031 Uiso 1 1 d . . . N12 N 0.85424(8) 0.6545(2) 0.6243(2) 0.0261(7) Uani 1 1 d . . . N13 N 0.83639(9) 0.8508(2) 0.6124(3) 0.0279(7) Uani 1 1 d . . . H13N H 0.8248(12) 0.804(4) 0.614(3) 0.034 Uiso 1 1 d . . . N14 N 0.78308(8) 0.9322(2) 0.5864(2) 0.0247(7) Uani 1 1 d . . . N15 N 0.72705(8) 0.9931(2) 0.5587(2) 0.0272(7) Uani 1 1 d . . . H15N H 0.7225(11) 0.928(3) 0.571(3) 0.033 Uiso 1 1 d . . . O1 O 0.70252(9) 0.3616(2) 0.9529(2) 0.0463(8) Uani 1 1 d . . . O2 O 0.89331(8) 0.6105(2) 0.8861(3) 0.0474(8) Uani 1 1 d . . . O3 O 0.95369(7) 0.9461(2) 0.9300(3) 0.0429(7) Uani 1 1 d . . . O4 O 0.83342(7) 1.1152(2) 0.8613(2) 0.0362(7) Uani 1 1 d . . . O5 O 0.62593(7) 1.0035(2) 0.7782(3) 0.0443(8) Uani 1 1 d . . . O6 O 0.53384(7) 0.7183(2) 0.7336(2) 0.0382(7) Uani 1 1 d . . . O7 O 0.63228(7) 0.4829(2) 0.6752(2) 0.0423(8) Uani 1 1 d . . . O8 O 0.83843(7) 0.3893(2) 0.6266(2) 0.0384(7) Uani 1 1 d . . . O9 O 0.95506(7) 0.5635(2) 0.5481(2) 0.0398(7) Uani 1 1 d . . . O10 O 0.89460(8) 0.8959(2) 0.6006(3) 0.0417(7) Uani 1 1 d . . . O11 O 0.70425(8) 1.1493(2) 0.5193(2) 0.0373(7) Uani 1 1 d . . . O14 O 0.71597(9) 0.7248(2) 0.8603(3) 0.0457(8) Uani 1 1 d . . . O15 O 0.77334(9) 0.7436(3) 0.7164(3) 0.0575(11) Uani 1 1 d . . . O16 O 0.70464(12) 0.7880(2) 0.5929(3) 0.0545(9) Uani 1 1 d . . . H1O H 0.7690(15) 0.764(4) 0.791(5) 0.065 Uiso 1 1 d . . . H2O H 0.6989(16) 0.705(5) 0.901(5) 0.065 Uiso 1 1 d . . . H3O H 0.7107(14) 0.789(4) 0.906(4) 0.065 Uiso 1 1 d . . . H4O H 0.6834(16) 0.778(4) 0.613(5) 0.065 Uiso 1 1 d . . . H5O H 0.7206(16) 0.769(5) 0.629(5) 0.065 Uiso 1 1 d . . . H6O H 0.7609(17) 0.706(5) 0.703(5) 0.065 Uiso 1 1 d . . . C67 C 0.5125(2) 0.2089(6) 0.7459(16) 0.054(2) Uani 0.769(7) 1 d PDU A 1 C68 C 0.5449(2) 0.2536(6) 0.7413(5) 0.0588(18) Uani 0.769(7) 1 d PDU A 1 H68 H 0.5659 0.2133 0.7445 0.071 Uiso 0.769(7) 1 calc PR A 1 C69 C 0.5473(3) 0.3576(7) 0.7320(10) 0.060(2) Uani 0.769(7) 1 d PDU A 1 H69 H 0.5699 0.3898 0.7335 0.072 Uiso 0.769(7) 1 calc PR A 1 C70 C 0.5170(2) 0.4142(6) 0.7205(6) 0.0613(19) Uani 0.769(7) 1 d PDU A 1 H70 H 0.5186 0.4854 0.7109 0.074 Uiso 0.769(7) 1 calc PR A 1 C71 C 0.4844(2) 0.3690(6) 0.7229(5) 0.0633(19) Uani 0.769(7) 1 d PDU A 1 H71 H 0.4635 0.4089 0.7158 0.076 Uiso 0.769(7) 1 calc PR A 1 C72 C 0.4820(2) 0.2644(6) 0.7356(5) 0.0623(19) Uani 0.769(7) 1 d PDU A 1 H72 H 0.4595 0.2322 0.7371 0.075 Uiso 0.769(7) 1 calc PR A 1 N16 N 0.5101(3) 0.0968(5) 0.7615(8) 0.069(2) Uani 0.769(7) 1 d PDU A 1 O12 O 0.5381(2) 0.0491(5) 0.7617(6) 0.102(2) Uani 0.769(7) 1 d PDU A 1 O13 O 0.4813(3) 0.0596(7) 0.7686(6) 0.103(3) Uani 0.769(7) 1 d PDU A 1 C67' C 0.5208(5) 0.1917(16) 0.752(6) 0.049(6) Uani 0.231(7) 1 d PDU A 2 C68' C 0.5559(5) 0.1687(14) 0.7445(16) 0.048(5) Uani 0.231(7) 1 d PDU A 2 H68' H 0.5634 0.1000 0.7485 0.058 Uiso 0.231(7) 1 calc PR A 2 C69' C 0.5805(6) 0.2448(17) 0.731(2) 0.074(6) Uani 0.231(7) 1 d PDU A 2 H69' H 0.6044 0.2299 0.7174 0.089 Uiso 0.231(7) 1 calc PR A 2 C70' C 0.5686(7) 0.3430(17) 0.739(2) 0.073(6) Uani 0.231(7) 1 d PDU A 2 H70' H 0.5855 0.3965 0.7422 0.088 Uiso 0.231(7) 1 calc PR A 2 C71' C 0.5333(8) 0.367(2) 0.743(4) 0.074(7) Uani 0.231(7) 1 d PDU A 2 H71' H 0.5258 0.4355 0.7392 0.088 Uiso 0.231(7) 1 calc PR A 2 C72' C 0.5087(6) 0.2890(15) 0.7513(19) 0.061(5) Uani 0.231(7) 1 d PDU A 2 H72' H 0.4841 0.3034 0.7565 0.073 Uiso 0.231(7) 1 calc PR A 2 N16' N 0.4945(5) 0.1071(14) 0.761(3) 0.050(5) Uani 0.231(7) 1 d PDU A 2 O12' O 0.5095(6) 0.0227(12) 0.7627(17) 0.074(5) Uani 0.231(7) 1 d PDU A 2 O13' O 0.4650(4) 0.1247(15) 0.7822(14) 0.059(5) Uani 0.231(7) 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(2) 0.049(3) 0.041(3) 0.007(2) 0.0034(18) -0.008(2) C2 0.043(2) 0.029(2) 0.023(2) -0.0010(16) 0.0019(16) -0.0048(17) C3 0.031(2) 0.0214(18) 0.025(2) 0.0005(14) -0.0022(15) 0.0006(15) C4 0.044(2) 0.0194(18) 0.037(2) -0.0015(16) -0.0085(19) 0.0005(17) C5 0.043(2) 0.024(2) 0.044(3) -0.0053(17) -0.0074(19) 0.0069(17) C6 0.033(2) 0.030(2) 0.036(2) -0.0032(17) -0.0035(17) 0.0071(17) C7 0.036(2) 0.0240(18) 0.026(2) -0.0037(15) -0.0025(16) -0.0002(16) C8 0.032(2) 0.032(2) 0.031(2) 0.0015(17) -0.0033(16) 0.0014(17) C9 0.029(2) 0.033(2) 0.028(2) 0.0016(16) 0.0029(15) -0.0003(16) C10 0.026(2) 0.036(2) 0.043(2) 0.0015(18) -0.0016(17) 0.0010(17) C11 0.027(2) 0.038(2) 0.040(2) 0.0028(18) 0.0005(17) -0.0013(17) C12 0.0251(19) 0.034(2) 0.037(2) 0.0017(17) -0.0009(16) -0.0076(16) C13 0.031(2) 0.028(2) 0.027(2) -0.0040(15) 0.0034(15) -0.0013(16) C14 0.027(2) 0.035(2) 0.056(3) -0.001(2) 0.0018(19) -0.0055(17) C15 0.029(2) 0.041(2) 0.036(2) 0.0059(18) 0.0009(17) -0.0045(18) C16 0.035(2) 0.045(3) 0.045(3) 0.009(2) -0.0024(19) 0.001(2) C17 0.035(2) 0.050(3) 0.061(3) 0.007(2) -0.003(2) -0.017(2) C18 0.030(2) 0.056(3) 0.062(3) -0.007(2) -0.006(2) -0.005(2) C19 0.031(2) 0.050(3) 0.064(3) -0.005(2) -0.009(2) 0.008(2) C20 0.035(2) 0.038(2) 0.057(3) -0.006(2) -0.001(2) 0.0024(19) C21 0.0243(19) 0.031(2) 0.031(2) -0.0008(16) 0.0004(15) -0.0018(16) C22 0.0260(18) 0.0185(17) 0.0240(19) -0.0002(14) 0.0008(14) -0.0012(14) C23 0.034(2) 0.0187(18) 0.039(2) -0.0029(16) 0.0003(17) -0.0059(15) C24 0.035(2) 0.0167(18) 0.044(2) -0.0008(16) -0.0034(17) -0.0002(16) C25 0.0268(19) 0.0229(18) 0.034(2) 0.0010(15) -0.0037(16) 0.0020(15) C26 0.027(2) 0.0220(18) 0.028(2) 0.0002(15) -0.0045(15) -0.0022(15) C27 0.0207(18) 0.0259(19) 0.036(2) -0.0020(16) 0.0016(15) 0.0008(15) C28 0.0223(18) 0.0256(18) 0.031(2) -0.0019(15) -0.0016(15) -0.0006(15) C29 0.0228(18) 0.0266(19) 0.039(2) -0.0014(16) 0.0020(16) 0.0053(15) C30 0.0230(19) 0.029(2) 0.042(2) 0.0000(17) 0.0003(16) -0.0024(16) C31 0.026(2) 0.0253(19) 0.045(3) -0.0044(17) -0.0036(17) -0.0040(15) C32 0.0210(17) 0.0247(18) 0.030(2) -0.0014(15) 0.0006(14) -0.0029(14) C33 0.0231(19) 0.031(2) 0.044(3) -0.0016(17) 0.0008(17) 0.0018(16) C34 0.025(2) 0.032(2) 0.043(2) 0.0017(18) -0.0004(17) 0.0013(16) C35 0.030(2) 0.044(2) 0.043(3) -0.0062(19) 0.0046(17) -0.0001(18) C36 0.036(2) 0.048(3) 0.053(3) -0.005(2) -0.002(2) -0.007(2) C37 0.023(2) 0.051(3) 0.062(3) 0.006(2) -0.002(2) -0.0011(19) C38 0.033(2) 0.050(3) 0.070(4) -0.002(2) 0.007(2) 0.009(2) C39 0.033(2) 0.033(2) 0.064(3) -0.004(2) 0.006(2) 0.0009(18) C40 0.0246(18) 0.0208(19) 0.033(2) -0.0015(15) -0.0018(15) -0.0038(15) C41 0.029(2) 0.0238(18) 0.023(2) -0.0021(15) 0.0046(15) -0.0028(15) C42 0.031(2) 0.0214(19) 0.041(2) -0.0029(17) 0.0098(17) -0.0022(15) C43 0.037(2) 0.0199(18) 0.036(2) -0.0027(16) 0.0045(17) -0.0038(16) C44 0.030(2) 0.0193(18) 0.039(2) -0.0001(16) 0.0076(16) 0.0046(15) C45 0.0285(18) 0.0200(17) 0.0207(18) -0.0014(14) -0.0013(14) 0.0012(15) C46 0.0276(19) 0.027(2) 0.026(2) 0.0024(15) 0.0012(14) 0.0028(15) C47 0.029(2) 0.0253(19) 0.026(2) -0.0009(15) -0.0021(15) 0.0022(15) C48 0.0281(19) 0.0273(19) 0.033(2) 0.0033(16) 0.0004(15) 0.0002(16) C49 0.027(2) 0.034(2) 0.040(2) 0.0006(17) -0.0002(17) 0.0036(16) C50 0.027(2) 0.027(2) 0.048(3) 0.0018(18) 0.0050(17) -0.0015(16) C51 0.028(2) 0.029(2) 0.030(2) 0.0001(16) -0.0018(15) 0.0006(16) C52 0.028(2) 0.031(2) 0.052(3) -0.0018(19) -0.0001(18) 0.0050(16) C53 0.030(2) 0.039(2) 0.038(2) 0.0004(18) 0.0013(17) 0.0053(17) C54 0.035(3) 0.038(2) 0.081(4) -0.002(2) 0.011(2) 0.002(2) C55 0.036(3) 0.044(3) 0.111(5) -0.004(3) 0.009(3) -0.005(2) C56 0.031(2) 0.057(3) 0.075(4) -0.009(3) 0.004(2) 0.013(2) C57 0.041(2) 0.043(2) 0.056(3) -0.005(2) 0.004(2) 0.009(2) C58 0.038(2) 0.042(2) 0.043(3) -0.002(2) 0.0027(19) 0.004(2) C59 0.027(2) 0.026(2) 0.036(2) -0.0003(16) -0.0010(16) 0.0018(16) C60 0.032(2) 0.0247(19) 0.023(2) 0.0009(15) 0.0026(15) -0.0001(15) C61 0.029(2) 0.025(2) 0.037(2) -0.0032(16) 0.0050(16) -0.0066(15) C62 0.035(2) 0.0183(18) 0.041(2) -0.0062(16) 0.0052(17) -0.0047(16) C63 0.030(2) 0.0159(17) 0.037(2) -0.0018(15) 0.0047(16) 0.0049(15) C64 0.0276(19) 0.0266(19) 0.026(2) 0.0006(15) 0.0055(15) -0.0028(15) C65 0.034(2) 0.030(2) 0.024(2) -0.0009(16) 0.0008(16) 0.0017(16) C66 0.028(2) 0.045(2) 0.046(3) 0.007(2) 0.0012(18) 0.0002(18) N1 0.0385(19) 0.0189(16) 0.032(2) 0.0018(13) -0.0003(14) 0.0027(14) N2 0.0322(17) 0.0192(15) 0.0282(17) 0.0004(12) 0.0008(13) -0.0012(12) N3 0.0271(18) 0.0244(17) 0.041(2) 0.0014(14) -0.0010(15) 0.0034(13) N4 0.0249(16) 0.0273(16) 0.0280(18) -0.0011(13) 0.0006(13) -0.0010(13) N5 0.0244(15) 0.0171(15) 0.0337(19) -0.0029(13) -0.0011(12) -0.0022(13) N6 0.0260(16) 0.0186(14) 0.0261(17) 0.0003(12) 0.0005(12) -0.0005(12) N7 0.0210(16) 0.0169(15) 0.045(2) -0.0038(14) -0.0019(14) 0.0007(12) N8 0.0212(15) 0.0259(16) 0.0283(17) -0.0050(13) 0.0018(12) -0.0007(12) N9 0.0266(17) 0.0176(15) 0.038(2) -0.0043(13) 0.0065(13) -0.0020(13) N10 0.0261(16) 0.0195(15) 0.0267(17) -0.0004(12) 0.0007(12) 0.0010(12) N11 0.0250(16) 0.0158(15) 0.0361(19) 0.0003(13) 0.0033(12) -0.0024(13) N12 0.0241(15) 0.0248(16) 0.0294(18) 0.0007(13) -0.0008(12) 0.0011(12) N13 0.0284(18) 0.0174(15) 0.038(2) 0.0013(13) 0.0018(14) -0.0046(13) N14 0.0262(16) 0.0212(15) 0.0268(17) 0.0001(12) 0.0006(12) -0.0023(12) N15 0.0269(17) 0.0228(16) 0.0322(19) 0.0010(13) 0.0036(13) -0.0003(13) O1 0.058(2) 0.0300(16) 0.051(2) 0.0021(14) 0.0115(15) -0.0093(14) O2 0.0322(16) 0.0317(15) 0.078(2) 0.0012(15) -0.0049(15) 0.0079(13) O3 0.0247(15) 0.0361(15) 0.067(2) 0.0034(15) -0.0060(13) -0.0028(12) O4 0.0278(15) 0.0255(15) 0.055(2) 0.0010(12) 0.0001(13) -0.0057(11) O5 0.0292(15) 0.0259(15) 0.077(2) -0.0119(15) -0.0019(14) 0.0052(12) O6 0.0232(14) 0.0286(15) 0.063(2) -0.0074(13) 0.0032(13) -0.0009(11) O7 0.0312(15) 0.0259(15) 0.070(2) -0.0158(14) 0.0029(14) -0.0022(12) O8 0.0316(15) 0.0249(14) 0.059(2) 0.0023(13) 0.0068(13) 0.0034(12) O9 0.0268(15) 0.0299(14) 0.063(2) 0.0002(14) 0.0120(13) 0.0058(12) O10 0.0321(16) 0.0258(14) 0.068(2) 0.0020(14) 0.0059(14) -0.0018(12) O11 0.0424(17) 0.0267(14) 0.0426(18) 0.0007(12) -0.0018(13) 0.0046(12) O14 0.053(2) 0.0240(15) 0.059(2) -0.0057(14) -0.0090(16) 0.0086(14) O15 0.036(2) 0.0326(18) 0.104(3) 0.0143(19) -0.0022(19) -0.0052(14) O16 0.070(3) 0.0303(17) 0.065(3) -0.0067(16) 0.0279(19) -0.0169(18) C67 0.072(5) 0.053(4) 0.037(5) -0.007(5) 0.003(6) -0.021(3) C68 0.064(4) 0.058(4) 0.055(4) 0.001(3) 0.003(3) -0.007(3) C69 0.061(5) 0.058(4) 0.061(6) 0.000(4) -0.004(6) -0.020(4) C70 0.079(5) 0.053(4) 0.051(4) 0.003(3) -0.001(4) -0.008(3) C71 0.069(4) 0.075(4) 0.047(4) -0.009(4) 0.002(3) 0.005(4) C72 0.063(4) 0.073(4) 0.051(4) -0.008(4) 0.001(3) -0.023(3) N16 0.095(6) 0.056(4) 0.055(4) -0.002(4) -0.024(6) -0.032(4) O12 0.131(6) 0.052(3) 0.121(6) -0.010(4) -0.007(5) -0.004(4) O13 0.119(6) 0.097(6) 0.091(5) 0.018(5) -0.018(5) -0.066(6) C67' 0.057(8) 0.053(8) 0.037(13) -0.004(11) 0.010(13) -0.002(7) C68' 0.058(8) 0.040(9) 0.047(11) 0.007(9) 0.002(9) 0.000(7) C69' 0.073(11) 0.077(11) 0.074(15) -0.004(12) 0.017(12) -0.023(9) C70' 0.087(11) 0.062(9) 0.070(14) -0.018(11) -0.005(15) -0.035(11) C71' 0.096(14) 0.060(10) 0.064(15) 0.014(13) 0.005(17) -0.010(9) C72' 0.067(10) 0.060(9) 0.058(11) -0.010(10) 0.019(10) 0.007(7) N16' 0.037(8) 0.065(9) 0.045(11) 0.003(10) -0.017(11) -0.001(7) O12' 0.065(13) 0.056(9) 0.101(15) -0.010(10) 0.004(11) -0.005(8) O13' 0.042(7) 0.062(11) 0.072(12) -0.005(9) 0.004(7) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.510(6) . ? C2 O1 1.233(5) . ? C2 N1 1.343(5) . ? C3 N2 1.334(5) . ? C3 C4 1.395(5) . ? C3 N1 1.407(5) . ? C4 C5 1.379(6) . ? C5 C6 1.383(6) . ? C6 C7 1.393(5) . ? C7 N2 1.331(5) . ? C7 N3 1.405(5) . ? C8 O2 1.213(5) . ? C8 N3 1.350(5) . ? C8 C9 1.506(5) . ? C9 N4 1.336(5) . ? C9 C10 1.381(5) . ? C10 C11 1.392(6) . ? C11 O3 1.355(5) . ? C11 C12 1.391(6) . ? C12 C13 1.392(5) . ? C13 N4 1.353(5) . ? C13 C21 1.504(5) . ? C14 O3 1.432(5) . ? C14 C15 1.508(5) . ? C15 C20 1.383(6) . ? C15 C16 1.391(6) . ? C16 C17 1.388(6) . ? C17 C18 1.376(7) . ? C18 C19 1.379(7) . ? C19 C20 1.389(6) . ? C21 O4 1.224(5) . ? C21 N5 1.359(5) . ? C22 N6 1.337(4) . ? C22 C23 1.390(5) . ? C22 N5 1.400(5) . ? C23 C24 1.385(5) . ? C24 C25 1.391(5) . ? C25 C26 1.386(5) . ? C26 N6 1.341(5) . ? C26 N7 1.414(5) . ? C27 O5 1.206(4) . ? C27 N7 1.368(5) . ? C27 C28 1.512(5) . ? C28 N8 1.334(5) . ? C28 C29 1.395(5) . ? C29 C30 1.394(5) . ? C30 O6 1.350(5) . ? C30 C31 1.393(5) . ? C31 C32 1.381(5) . ? C32 N8 1.348(5) . ? C32 C40 1.493(5) . ? C33 O6 1.442(5) . ? C33 C34 1.503(5) . ? C34 C39 1.372(6) . ? C34 C35 1.385(6) . ? C35 C36 1.388(6) . ? C36 C37 1.375(7) . ? C37 C38 1.382(7) . ? C38 C39 1.395(6) . ? C40 O7 1.224(4) . ? C40 N9 1.359(5) . ? C41 N10 1.340(5) . ? C41 C42 1.392(5) . ? C41 N9 1.404(5) . ? C42 C43 1.377(5) . ? C43 C44 1.386(5) . ? C44 C45 1.394(5) . ? C45 N10 1.332(5) . ? C45 N11 1.403(5) . ? C46 O8 1.217(5) . ? C46 N11 1.354(5) . ? C46 C47 1.517(5) . ? C47 N12 1.343(5) . ? C47 C48 1.380(5) . ? C48 C49 1.397(6) . ? C49 O9 1.357(5) . ? C49 C50 1.405(6) . ? C50 C51 1.380(5) . ? C51 N12 1.348(5) . ? C51 C59 1.505(5) . ? C52 O9 1.442(5) . ? C52 C53 1.513(6) . ? C53 C54 1.381(6) . ? C53 C58 1.389(6) . ? C54 C55 1.388(7) . ? C55 C56 1.369(7) . ? C56 C57 1.381(7) . ? C57 C58 1.377(7) . ? C59 O10 1.223(5) . ? C59 N13 1.348(5) . ? C60 N14 1.336(5) . ? C60 C61 1.390(5) . ? C60 N13 1.411(5) . ? C61 C62 1.385(5) . ? C62 C63 1.376(5) . ? C63 C64 1.402(5) . ? C64 N14 1.326(5) . ? C64 N15 1.414(5) . ? C65 O11 1.228(5) . ? C65 N15 1.365(5) . ? C65 C66 1.499(6) . ? C67 C68 1.362(10) . ? C67 C72 1.367(11) . ? C67 N16 1.494(10) . ? C68 C69 1.379(11) . ? C69 C70 1.369(12) . ? C70 C71 1.367(11) . ? C71 C72 1.392(10) . ? N16 O13 1.200(11) . ? N16 O12 1.231(11) . ? C67' C72' 1.360(18) . ? C67' C68' 1.364(18) . ? C67' N16' 1.501(17) . ? C68' C69' 1.383(19) . ? C69' C70' 1.37(2) . ? C70' C71' 1.37(2) . ? C71' C72' 1.39(2) . ? N16' O13' 1.185(18) . ? N16' O12' 1.246(19) . ? 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 C2 N1 123.6(4) . . ? O1 C2 C1 120.5(4) . . ? N1 C2 C1 115.9(4) . . ? N2 C3 C4 123.9(4) . . ? N2 C3 N1 111.4(3) . . ? C4 C3 N1 124.7(3) . . ? C5 C4 C3 116.1(4) . . ? C4 C5 C6 122.0(4) . . ? C5 C6 C7 116.2(4) . . ? N2 C7 C6 123.8(4) . . ? N2 C7 N3 112.4(3) . . ? C6 C7 N3 123.7(4) . . ? O2 C8 N3 125.0(4) . . ? O2 C8 C9 121.7(4) . . ? N3 C8 C9 113.3(3) . . ? N4 C9 C10 123.6(4) . . ? N4 C9 C8 117.8(3) . . ? C10 C9 C8 118.4(3) . . ? C9 C10 C11 118.7(4) . . ? O3 C11 C12 124.3(4) . . ? O3 C11 C10 116.3(3) . . ? C12 C11 C10 119.4(4) . . ? C11 C12 C13 117.2(4) . . ? N4 C13 C12 124.3(3) . . ? N4 C13 C21 117.7(3) . . ? C12 C13 C21 117.8(3) . . ? O3 C14 C15 109.3(3) . . ? C20 C15 C16 118.8(4) . . ? C20 C15 C14 123.6(4) . . ? C16 C15 C14 117.6(4) . . ? C17 C16 C15 120.7(4) . . ? C18 C17 C16 119.9(4) . . ? C17 C18 C19 119.9(4) . . ? C18 C19 C20 120.3(4) . . ? C15 C20 C19 120.4(4) . . ? O4 C21 N5 125.2(3) . . ? O4 C21 C13 120.8(3) . . ? N5 C21 C13 114.0(3) . . ? N6 C22 C23 123.6(3) . . ? N6 C22 N5 113.1(3) . . ? C23 C22 N5 123.3(3) . . ? C24 C23 C22 117.0(3) . . ? C23 C24 C25 121.4(3) . . ? C26 C25 C24 116.0(3) . . ? N6 C26 C25 124.6(3) . . ? N6 C26 N7 112.4(3) . . ? C25 C26 N7 123.0(3) . . ? O5 C27 N7 125.3(3) . . ? O5 C27 C28 121.4(3) . . ? N7 C27 C28 113.3(3) . . ? N8 C28 C29 124.6(3) . . ? N8 C28 C27 117.8(3) . . ? C29 C28 C27 117.6(3) . . ? C30 C29 C28 117.2(3) . . ? O6 C30 C31 115.8(3) . . ? O6 C30 C29 125.1(3) . . ? C31 C30 C29 119.1(3) . . ? C32 C31 C30 118.9(3) . . ? N8 C32 C31 123.2(3) . . ? N8 C32 C40 118.8(3) . . ? C31 C32 C40 118.0(3) . . ? O6 C33 C34 107.3(3) . . ? C39 C34 C35 119.3(4) . . ? C39 C34 C33 118.7(4) . . ? C35 C34 C33 122.0(4) . . ? C34 C35 C36 120.4(4) . . ? C37 C36 C35 120.3(4) . . ? C36 C37 C38 119.4(4) . . ? C37 C38 C39 120.1(5) . . ? C34 C39 C38 120.4(4) . . ? O7 C40 N9 124.5(3) . . ? O7 C40 C32 120.3(3) . . ? N9 C40 C32 115.3(3) . . ? N10 C41 C42 123.2(3) . . ? N10 C41 N9 113.9(3) . . ? C42 C41 N9 122.8(3) . . ? C43 C42 C41 117.1(4) . . ? C42 C43 C44 121.4(3) . . ? C43 C44 C45 116.7(3) . . ? N10 C45 C44 123.5(3) . . ? N10 C45 N11 114.3(3) . . ? C44 C45 N11 122.2(3) . . ? O8 C46 N11 126.4(4) . . ? O8 C46 C47 120.3(3) . . ? N11 C46 C47 113.3(3) . . ? N12 C47 C48 125.1(4) . . ? N12 C47 C46 117.0(3) . . ? C48 C47 C46 117.8(3) . . ? C47 C48 C49 117.8(4) . . ? O9 C49 C48 125.3(4) . . ? O9 C49 C50 116.2(4) . . ? C48 C49 C50 118.4(4) . . ? C51 C50 C49 118.7(4) . . ? N12 C51 C50 123.8(3) . . ? N12 C51 C59 117.2(3) . . ? C50 C51 C59 118.9(3) . . ? O9 C52 C53 109.6(3) . . ? C54 C53 C58 119.0(4) . . ? C54 C53 C52 123.2(4) . . ? C58 C53 C52 117.6(4) . . ? C53 C54 C55 119.8(4) . . ? C56 C55 C54 120.8(5) . . ? C55 C56 C57 119.7(5) . . ? C58 C57 C56 119.9(4) . . ? C57 C58 C53 120.8(4) . . ? O10 C59 N13 125.6(3) . . ? O10 C59 C51 120.6(3) . . ? N13 C59 C51 113.8(3) . . ? N14 C60 C61 124.1(3) . . ? N14 C60 N13 113.1(3) . . ? C61 C60 N13 122.8(3) . . ? C62 C61 C60 116.6(3) . . ? C63 C62 C61 121.2(3) . . ? C62 C63 C64 117.0(3) . . ? N14 C64 C63 123.5(3) . . ? N14 C64 N15 112.4(3) . . ? C63 C64 N15 124.2(3) . . ? O11 C65 N15 123.4(4) . . ? O11 C65 C66 121.4(4) . . ? N15 C65 C66 115.2(3) . . ? C2 N1 C3 129.7(3) . . ? C7 N2 C3 117.8(3) . . ? C8 N3 C7 129.1(3) . . ? C9 N4 C13 116.7(3) . . ? C21 N5 C22 128.7(3) . . ? C22 N6 C26 117.3(3) . . ? C27 N7 C26 127.9(3) . . ? C28 N8 C32 117.0(3) . . ? C40 N9 C41 127.4(3) . . ? C45 N10 C41 118.1(3) . . ? C46 N11 C45 127.9(3) . . ? C47 N12 C51 116.2(3) . . ? C59 N13 C60 128.8(3) . . ? C64 N14 C60 117.7(3) . . ? C65 N15 C64 128.1(3) . . ? C11 O3 C14 117.1(3) . . ? C30 O6 C33 118.0(3) . . ? C49 O9 C52 116.2(3) . . ? C68 C67 C72 121.2(7) . . ? C68 C67 N16 119.6(9) . . ? C72 C67 N16 119.2(8) . . ? C67 C68 C69 119.7(8) . . ? C70 C69 C68 119.6(8) . . ? C71 C70 C69 120.6(8) . . ? C70 C71 C72 119.8(7) . . ? C67 C72 C71 118.9(7) . . ? O13 N16 O12 124.9(9) . . ? O13 N16 C67 118.4(11) . . ? O12 N16 C67 116.6(9) . . ? C72' C67' C68' 122.4(16) . . ? C72' C67' N16' 118.5(16) . . ? C68' C67' N16' 119.2(16) . . ? C67' C68' C69' 120.5(17) . . ? C70' C69' C68' 116.7(18) . . ? C71' C70' C69' 122(2) . . ? C70' C71' C72' 119(2) . . ? C67' C72' C71' 117.9(19) . . ? O13' N16' O12' 127(2) . . ? O13' N16' C67' 120.3(19) . . ? O12' N16' C67' 111.3(18) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.359 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.055 #===END data_2A(DMSO_EtOH) _database_code_CSD 176829 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C142 H142 N30 O30 S4' _chemical_formula_weight 2877.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 13.429(3) _cell_length_b 14.377(7) _cell_length_c 19.518(2) _cell_angle_alpha 87.660(10) _cell_angle_beta 70.850(10) _cell_angle_gamma 85.940(10) _cell_volume 3550.2(19) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 1.325 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6229 _exptl_absorpt_correction_T_max 0.7970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9165 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 59.94 _reflns_number_total 9165 _reflns_number_gt 5977 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2787P)^2^+7.5340P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(9) _refine_ls_number_reflns 9165 _refine_ls_number_parameters 1856 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1625 _refine_ls_R_factor_gt 0.1180 _refine_ls_wR_factor_ref 0.3794 _refine_ls_wR_factor_gt 0.3130 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 1.018 _refine_ls_shift/su_mean 0.046 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_1 C 0.7091(19) 0.0686(15) 1.0827(11) 0.096(7) Uani 1 1 d . . . H1A_1 H 0.6439 0.0557 1.0756 0.145 Uiso 1 1 calc R . . H1B_1 H 0.7007 0.1273 1.1062 0.145 Uiso 1 1 calc R . . H1C_1 H 0.7277 0.0201 1.1123 0.145 Uiso 1 1 calc R . . O2_1 O 0.8814(11) 0.0867(10) 0.9993(7) 0.092(4) Uani 1 1 d . . . C3_1 C 0.8000(18) 0.0729(13) 1.0061(9) 0.081(6) Uani 1 1 d . . . N4_1 N 0.7523(11) 0.0792(11) 0.9518(7) 0.070(4) Uani 1 1 d . . . H4_1 H 0.6844 0.0811 0.9675 0.084 Uiso 1 1 calc R . . C5_1 C 0.7945(13) 0.0824(11) 0.8818(9) 0.063(5) Uani 1 1 d . . . N6_1 N 0.7279(12) 0.0857(11) 0.8419(9) 0.076(4) Uani 1 1 d . . . C7_1 C 0.7648(14) 0.0937(12) 0.7683(8) 0.067(5) Uani 1 1 d . . . C8_1 C 0.8727(14) 0.1097(15) 0.7347(11) 0.083(6) Uani 1 1 d . . . H8_1 H 0.8980 0.1213 0.6850 0.099 Uiso 1 1 calc R . . C9_1 C 0.9380(14) 0.1086(16) 0.7720(11) 0.089(7) Uani 1 1 d . . . H9_1 H 1.0087 0.1191 0.7480 0.107 Uiso 1 1 calc R . . C10_1 C 0.9036(14) 0.0920(12) 0.8480(11) 0.072(5) Uani 1 1 d . . . H10_1 H 0.9505 0.0875 0.8742 0.087 Uiso 1 1 calc R . . N11_1 N 0.6882(10) 0.0943(10) 0.7354(7) 0.061(4) Uani 1 1 d . . . H11_1 H 0.6273 0.0800 0.7641 0.073 Uiso 1 1 calc R . . C12_1 C 0.6915(14) 0.1131(12) 0.6670(11) 0.072(5) Uani 1 1 d . . . O13_1 O 0.7699(12) 0.1376(10) 0.6199(7) 0.096(4) Uani 1 1 d . . . C14_1 C 0.5914(14) 0.1025(12) 0.6509(10) 0.068(5) Uani 1 1 d . . . N15_1 N 0.5106(10) 0.0799(9) 0.7059(7) 0.061(4) Uani 1 1 d . . . C16_1 C 0.4229(15) 0.0744(11) 0.6926(8) 0.070(5) Uani 1 1 d . . . C17_1 C 0.4076(13) 0.0921(12) 0.6241(8) 0.062(4) Uani 1 1 d . . . H17_1 H 0.3407 0.0965 0.6195 0.074 Uiso 1 1 calc R . . C18_1 C 0.4981(14) 0.1024(13) 0.5647(9) 0.072(5) Uani 1 1 d . . . C19_1 C 0.5910(15) 0.1190(13) 0.5826(10) 0.071(5) Uani 1 1 d . . . H19_1 H 0.6502 0.1409 0.5473 0.085 Uiso 1 1 calc R . . O20_1 O 0.5026(10) 0.1190(9) 0.4952(6) 0.076(4) Uani 1 1 d . . . C21_1 C 0.4093(15) 0.1062(12) 0.4789(8) 0.067(5) Uani 1 1 d . . . H21A_1 H 0.3574 0.1572 0.4978 0.081 Uiso 1 1 calc R . . H21B_1 H 0.3794 0.0484 0.5008 0.081 Uiso 1 1 calc R . . C22_1 C 0.438(2) 0.1033(19) 0.3979(11) 0.117(9) Uani 1 1 d . . . C23_1 C 0.3467(16) 0.1325(14) 0.3702(9) 0.080(5) Uani 1 1 d . . . H23_1 H 0.2795 0.1512 0.4005 0.096 Uiso 1 1 calc R . . C24_1 C 0.373(2) 0.1287(15) 0.2969(11) 0.102(7) Uani 1 1 d . . . H24_1 H 0.3194 0.1425 0.2767 0.122 Uiso 1 1 calc R . . C25_1 C 0.482(2) 0.1037(14) 0.2460(9) 0.099(8) Uani 1 1 d . . . H25_1 H 0.4972 0.1076 0.1960 0.119 Uiso 1 1 calc R . . C26_1 C 0.554(2) 0.077(2) 0.2734(11) 0.114(8) Uani 1 1 d . . . H26_1 H 0.6209 0.0570 0.2426 0.137 Uiso 1 1 calc R . . C27_1 C 0.535(2) 0.076(2) 0.3510(10) 0.112(9) Uani 1 1 d . . . H27_1 H 0.5896 0.0571 0.3690 0.134 Uiso 1 1 calc R . . C28_1 C 0.3196(12) 0.0531(12) 0.7536(8) 0.061(5) Uani 1 1 d . . . O29_1 O 0.2384(9) 0.0631(9) 0.7454(6) 0.073(3) Uani 1 1 d . . . N30_1 N 0.3387(9) 0.0168(9) 0.8147(6) 0.050(3) Uani 1 1 d . . . H30_1 H 0.4037 0.0085 0.8128 0.059 Uiso 1 1 calc R . . C31_1 C 0.2594(13) -0.0085(11) 0.8817(9) 0.060(4) Uani 1 1 d . . . N32_1 N 0.3018(9) -0.0322(8) 0.9339(6) 0.048(3) Uani 1 1 d . . . C33_1 C 0.2352(13) -0.0580(11) 0.9982(9) 0.060(4) Uani 1 1 d . . . C34_1 C 0.1283(18) -0.0610(13) 1.0123(11) 0.082(6) Uani 1 1 d . . . H34_1 H 0.0844 -0.0743 1.0590 0.099 Uiso 1 1 calc R . . C35_1 C 0.0850(13) -0.0438(13) 0.9552(10) 0.070(5) Uani 1 1 d . . . H35_1 H 0.0140 -0.0493 0.9613 0.084 Uiso 1 1 calc R . . C36_1 C 0.1612(11) -0.0172(12) 0.8869(8) 0.059(4) Uani 1 1 d . . . H36_1 H 0.1400 -0.0061 0.8463 0.071 Uiso 1 1 calc R . . N37_1 N 0.2885(11) -0.0821(10) 1.0492(7) 0.065(4) Uani 1 1 d . . . H37_1 H 0.3547 -0.0990 1.0337 0.078 Uiso 1 1 calc R . . C38_1 C 0.2360(13) -0.0789(12) 1.1234(7) 0.059(4) Uani 1 1 d . . . O39_1 O 0.1423(10) -0.0655(15) 1.1540(6) 0.123(7) Uani 1 1 d . . . C40_1 C 0.3139(15) -0.1058(16) 1.1646(8) 0.086(6) Uani 1 1 d . . . N41_1 N 0.4105(10) -0.1197(9) 1.1338(7) 0.057(3) Uani 1 1 d . . . C42_1 C 0.4747(14) -0.1402(12) 1.1682(8) 0.066(5) Uani 1 1 d . . . C43_1 C 0.4361(16) -0.1372(12) 1.2467(9) 0.075(5) Uani 1 1 d . . . H43_1 H 0.4830 -0.1493 1.2724 0.089 Uiso 1 1 calc R . . C44_1 C 0.3317(14) -0.1167(13) 1.2834(8) 0.068(5) Uani 1 1 d . . . C45_1 C 0.2637(12) -0.0934(13) 1.2445(7) 0.061(4) Uani 1 1 d . . . H45_1 H 0.1936 -0.0722 1.2659 0.073 Uiso 1 1 calc R . . O46_1 O 0.3039(9) -0.1054(10) 1.3581(6) 0.081(4) Uani 1 1 d . . . C47_1 C 0.2007(15) -0.0759(15) 1.3928(7) 0.086(6) Uani 1 1 d . . . H47A_1 H 0.1533 -0.1200 1.3864 0.103 Uiso 1 1 calc R . . H47B_1 H 0.1844 -0.0155 1.3737 0.103 Uiso 1 1 calc R . . C48_1 C 0.1895(14) -0.0693(13) 1.4742(9) 0.069(5) Uani 1 1 d . . . C49_1 C 0.1538(17) 0.0166(17) 1.5109(10) 0.088(6) Uani 1 1 d . . . H49_1 H 0.1403 0.0706 1.4868 0.106 Uiso 1 1 calc R . . C50_1 C 0.1411(14) 0.0155(16) 1.5811(9) 0.084(6) Uani 1 1 d . . . H50_1 H 0.1114 0.0705 1.6049 0.101 Uiso 1 1 calc R . . C51_1 C 0.1636(15) -0.051(2) 1.6215(11) 0.102(8) Uani 1 1 d . . . H51_1 H 0.1539 -0.0445 1.6706 0.123 Uiso 1 1 calc R . . C52_1 C 0.205(2) -0.1341(17) 1.5823(11) 0.116(9) Uani 1 1 d . . . H52_1 H 0.2231 -0.1862 1.6066 0.139 Uiso 1 1 calc R . . C53_1 C 0.219(2) -0.1396(16) 1.5089(10) 0.104(8) Uani 1 1 d . . . H53_1 H 0.2488 -0.1940 1.4843 0.125 Uiso 1 1 calc R . . C54_1 C 0.5914(15) -0.1525(13) 1.1340(11) 0.075(5) Uani 1 1 d . . . O55_1 O 0.6480(12) -0.1757(13) 1.1659(8) 0.110(5) Uani 1 1 d . . . N56_1 N 0.6156(10) -0.1533(12) 1.0600(7) 0.083(5) Uani 1 1 d . . . H56_1 H 0.5622 -0.1469 1.0448 0.099 Uiso 1 1 calc R . . C57_1 C 0.7162(15) -0.1633(12) 1.0042(12) 0.081(6) Uani 1 1 d . . . N58_1 N 0.7114(11) -0.1494(11) 0.9391(7) 0.066(4) Uani 1 1 d . . . C59_1 C 0.7989(12) -0.1580(11) 0.8869(9) 0.059(4) Uani 1 1 d . . . C60_1 C 0.9026(13) -0.1797(13) 0.8914(10) 0.069(5) Uani 1 1 d . . . H60_1 H 0.9647 -0.1820 0.8520 0.083 Uiso 1 1 calc R . . C61_1 C 0.8968(12) -0.1974(15) 0.9649(10) 0.080(6) Uani 1 1 d . . . H61_1 H 0.9587 -0.2174 0.9741 0.096 Uiso 1 1 calc R . . C62_1 C 0.8100(15) -0.1874(12) 1.0202(11) 0.076(5) Uani 1 1 d . . . H62_1 H 0.8101 -0.1957 1.0677 0.092 Uiso 1 1 calc R . . N63_1 N 0.7863(12) -0.1472(11) 0.8171(8) 0.079(5) Uani 1 1 d . . . H63_1 H 0.7221 -0.1389 0.8175 0.094 Uiso 1 1 calc R . . C64_1 C 0.8608(10) -0.1480(12) 0.7498(8) 0.060(5) Uani 1 1 d . . . O65_1 O 0.9517(9) -0.1601(11) 0.7396(7) 0.092(4) Uani 1 1 d . . . C66_1 C 0.8162(13) -0.1339(11) 0.6895(9) 0.060(4) Uani 1 1 d . . . N67_1 N 0.7159(9) -0.1480(10) 0.7012(7) 0.063(4) Uani 1 1 d . . . C68_1 C 0.6812(12) -0.1366(12) 0.6450(10) 0.064(5) Uani 1 1 d . . . C69_1 C 0.7399(14) -0.1014(12) 0.5743(9) 0.066(5) Uani 1 1 d . . . H69_1 H 0.7113 -0.0906 0.5371 0.079 Uiso 1 1 calc R . . C70_1 C 0.8411(13) -0.0854(11) 0.5673(10) 0.072(6) Uani 1 1 d . . . C71_1 C 0.8857(11) -0.1023(13) 0.6221(8) 0.062(5) Uani 1 1 d . . . H71_1 H 0.9563 -0.0934 0.6150 0.074 Uiso 1 1 calc R . . O72_1 O 0.9131(8) -0.0502(9) 0.5013(6) 0.070(3) Uani 1 1 d . . . C73_1 C 0.8832(15) -0.0018(18) 0.4466(10) 0.097(7) Uani 1 1 d . . . H73A_1 H 0.8740 -0.0491 0.4155 0.116 Uiso 1 1 calc R . . H73B_1 H 0.8135 0.0272 0.4704 0.116 Uiso 1 1 calc R . . C74_1 C 0.9331(13) 0.0580(14) 0.4060(10) 0.080(6) Uani 1 1 d . . . C75_1 C 0.9508(19) 0.1410(15) 0.4447(14) 0.104(8) Uani 1 1 d . . . H75_1 H 0.9204 0.1423 0.4949 0.125 Uiso 1 1 calc R . . C76_1 C 1.002(2) 0.206(2) 0.4150(17) 0.145(11) Uani 1 1 d . . . H76_1 H 1.0014 0.2616 0.4377 0.174 Uiso 1 1 calc R . . C77_1 C 1.0718(16) 0.1846(17) 0.3301(13) 0.112(8) Uani 1 1 d . . . H77_1 H 1.1228 0.2244 0.3033 0.134 Uiso 1 1 calc R . . C78_1 C 1.053(2) 0.107(3) 0.301(3) 0.26(3) Uani 1 1 d . . . H78_1 H 1.0896 0.0944 0.2521 0.313 Uiso 1 1 calc R . . C79_1 C 0.9894(18) 0.0551(16) 0.3355(10) 0.097(7) Uani 1 1 d . . . H79_1 H 0.9774 0.0058 0.3103 0.117 Uiso 1 1 calc R . . C80_1 C 0.5647(14) -0.1473(12) 0.6557(10) 0.069(5) Uani 1 1 d . . . O81_1 O 0.5203(9) -0.1365(10) 0.6114(7) 0.079(4) Uani 1 1 d . . . N82_1 N 0.5088(10) -0.1800(9) 0.7267(7) 0.060(4) Uani 1 1 d . . . H82_1 H 0.5461 -0.1872 0.7551 0.072 Uiso 1 1 calc R . . C83_1 C 0.4109(9) -0.2009(11) 0.7562(8) 0.049(4) Uani 1 1 d . . . N84_1 N 0.3870(13) -0.2319(11) 0.8249(7) 0.076(4) Uani 1 1 d . . . C85_1 C 0.2787(13) -0.2575(15) 0.8625(9) 0.082(6) Uani 1 1 d . . . C86_1 C 0.2111(12) -0.2598(13) 0.8316(11) 0.079(6) Uani 1 1 d . . . H86_1 H 0.1456 -0.2823 0.8570 0.094 Uiso 1 1 calc R . . C87_1 C 0.2330(15) -0.2277(14) 0.7559(9) 0.078(6) Uani 1 1 d . . . H87_1 H 0.1827 -0.2270 0.7326 0.093 Uiso 1 1 calc R . . C88_1 C 0.3327(13) -0.1990(11) 0.7222(9) 0.067(5) Uani 1 1 d . . . H88_1 H 0.3498 -0.1772 0.6745 0.081 Uiso 1 1 calc R . . N89_1 N 0.2756(12) -0.2743(16) 0.9334(8) 0.106(7) Uani 1 1 d . . . H89_1 H 0.3292 -0.2609 0.9452 0.127 Uiso 1 1 calc R . . C90_1 C 0.1930(15) -0.3104(15) 0.9853(10) 0.082(6) Uani 1 1 d . . . O91_1 O 0.1089(13) -0.3285(11) 0.9754(8) 0.110(5) Uani 1 1 d . . . C92_1 C 0.1936(16) -0.3109(17) 1.0620(11) 0.095(6) Uani 1 1 d . . . H92A_1 H 0.2621 -0.2963 1.0624 0.142 Uiso 1 1 calc R . . H92B_1 H 0.1777 -0.3716 1.0836 0.142 Uiso 1 1 calc R . . H92C_1 H 0.1414 -0.2653 1.0892 0.142 Uiso 1 1 calc R . . C1_2 C 0.965(2) 0.772(2) 0.2528(12) 0.138(12) Uani 1 1 d . . . H1A_2 H 0.8939 0.7588 0.2574 0.207 Uiso 1 1 calc R . . H1B_2 H 1.0136 0.7310 0.2179 0.207 Uiso 1 1 calc R . . H1C_2 H 0.9768 0.8354 0.2371 0.207 Uiso 1 1 calc R . . O2_2 O 1.0589(9) 0.7660(12) 0.3366(9) 0.106(5) Uani 1 1 d . . . C3_2 C 0.9818(12) 0.7564(13) 0.3256(11) 0.075(6) Uani 1 1 d . . . N4_2 N 0.8904(12) 0.7300(12) 0.3781(8) 0.084(5) Uani 1 1 d . . . H4_2 H 0.8355 0.7296 0.3646 0.100 Uiso 1 1 calc R . . C5_2 C 0.8755(9) 0.7031(10) 0.4519(8) 0.051(4) Uani 1 1 d . . . N6_2 N 0.7865(10) 0.6727(10) 0.4856(8) 0.067(4) Uani 1 1 d . . . C7_2 C 0.7702(15) 0.6490(13) 0.5562(10) 0.078(6) Uani 1 1 d . . . C8_2 C 0.8325(15) 0.6463(13) 0.5937(11) 0.078(6) Uani 1 1 d . . . H8_2 H 0.8141 0.6284 0.6424 0.094 Uiso 1 1 calc R . . C9_2 C 0.9342(12) 0.6744(13) 0.5506(10) 0.072(5) Uani 1 1 d . . . H9_2 H 0.9872 0.6712 0.5717 0.086 Uiso 1 1 calc R . . C10_2 C 0.9577(14) 0.7042(12) 0.4838(10) 0.068(5) Uani 1 1 d . . . H10_2 H 1.0239 0.7251 0.4582 0.082 Uiso 1 1 calc R . . N11_2 N 0.6549(10) 0.6212(12) 0.5865(8) 0.077(5) Uani 1 1 d . . . H11_2 H 0.6196 0.6195 0.5569 0.092 Uiso 1 1 calc R . . C12_2 C 0.6067(13) 0.5996(13) 0.6564(10) 0.068(5) Uani 1 1 d . . . O13_2 O 0.6395(12) 0.5925(11) 0.7082(6) 0.098(5) Uani 1 1 d . . . C14_2 C 0.4958(14) 0.5757(12) 0.6670(8) 0.069(5) Uani 1 1 d . . . N15_2 N 0.4554(11) 0.5924(9) 0.6131(7) 0.064(4) Uani 1 1 d . . . C16_2 C 0.3533(13) 0.5755(11) 0.6258(8) 0.062(5) Uani 1 1 d . . . C17_2 C 0.2914(15) 0.5486(11) 0.6927(11) 0.078(6) Uani 1 1 d . . . H17_2 H 0.2201 0.5431 0.7001 0.094 Uiso 1 1 calc R . . C18_2 C 0.3273(13) 0.5290(12) 0.7499(8) 0.061(5) Uani 1 1 d . . . C19_2 C 0.4296(13) 0.5471(12) 0.7363(9) 0.068(5) Uani 1 1 d . . . H19_2 H 0.4576 0.5404 0.7741 0.082 Uiso 1 1 calc R . . O20_2 O 0.2649(10) 0.4935(9) 0.8078(7) 0.085(4) Uani 1 1 d . . . C21_2 C 0.3118(13) 0.4614(11) 0.8632(9) 0.069(5) Uani 1 1 d . . . H21A_2 H 0.3114 0.5109 0.8956 0.083 Uiso 1 1 calc R . . H21B_2 H 0.3831 0.4343 0.8421 0.083 Uiso 1 1 calc R . . C22_2 C 0.2280(15) 0.3822(12) 0.9038(9) 0.071(5) Uani 1 1 d . . . C23_2 C 0.1752(17) 0.3969(18) 0.9755(16) 0.112(8) Uani 1 1 d . . . H23_2 H 0.1809 0.4501 0.9992 0.134 Uiso 1 1 calc R . . C24_2 C 0.108(2) 0.3204(15) 1.0121(11) 0.116(9) Uani 1 1 d . . . H24_2 H 0.0675 0.3236 1.0609 0.139 Uiso 1 1 calc R . . C25_2 C 0.108(3) 0.2371(16) 0.9678(18) 0.136(11) Uani 1 1 d . . . H25_2 H 0.0756 0.1834 0.9895 0.163 Uiso 1 1 calc R . . C26_2 C 0.1490(15) 0.2423(17) 0.9076(15) 0.109(9) Uani 1 1 d . . . H26_2 H 0.1330 0.1982 0.8799 0.131 Uiso 1 1 calc R . . C27_2 C 0.2203(19) 0.3064(17) 0.8698(12) 0.099(7) Uani 1 1 d . . . H27_2 H 0.2616 0.2965 0.8218 0.119 Uiso 1 1 calc R . . C28_2 C 0.3058(15) 0.5953(12) 0.5662(10) 0.076(6) Uani 1 1 d . . . O29_2 O 0.2125(10) 0.6115(12) 0.5758(7) 0.097(5) Uani 1 1 d . . . N30_2 N 0.3837(9) 0.5890(9) 0.4962(7) 0.056(3) Uani 1 1 d . . . H30_2 H 0.4473 0.5714 0.4939 0.067 Uiso 1 1 calc R . . C31_2 C 0.3640(11) 0.6094(11) 0.4312(9) 0.060(4) Uani 1 1 d . . . N32_2 N 0.4581(11) 0.5936(10) 0.3726(9) 0.072(4) Uani 1 1 d . . . C33_2 C 0.4523(11) 0.6132(12) 0.3070(7) 0.056(4) Uani 1 1 d . . . C34_2 C 0.3708(16) 0.6345(17) 0.2872(10) 0.092(7) Uani 1 1 d . . . H34_2 H 0.3733 0.6420 0.2392 0.110 Uiso 1 1 calc R . . C35_2 C 0.2712(16) 0.6458(12) 0.3509(11) 0.076(5) Uani 1 1 d . . . H35_2 H 0.2068 0.6648 0.3450 0.091 Uiso 1 1 calc R . . C36_2 C 0.2795(14) 0.6272(14) 0.4162(10) 0.075(5) Uani 1 1 d . . . H36_2 H 0.2167 0.6273 0.4550 0.090 Uiso 1 1 calc R . . N37_2 N 0.5549(14) 0.5950(11) 0.2548(9) 0.086(5) Uani 1 1 d . . . H37_2 H 0.6044 0.5746 0.2714 0.103 Uiso 1 1 calc R . . C38_2 C 0.5825(13) 0.6072(14) 0.1799(9) 0.069(5) Uani 1 1 d . . . O39_2 O 0.5172(10) 0.6248(10) 0.1485(7) 0.082(4) Uani 1 1 d . . . C40_2 C 0.6987(11) 0.5800(12) 0.1371(8) 0.058(4) Uani 1 1 d . . . N41_2 N 0.7584(11) 0.5644(12) 0.1826(8) 0.074(4) Uani 1 1 d . . . C42_2 C 0.8663(12) 0.5420(10) 0.1444(8) 0.056(4) Uani 1 1 d . . . C43_2 C 0.9004(16) 0.5445(14) 0.0709(11) 0.080(5) Uani 1 1 d . . . H43_2 H 0.9728 0.5375 0.0470 0.096 Uiso 1 1 calc R . . C44_2 C 0.8367(15) 0.5564(12) 0.0302(9) 0.066(5) Uani 1 1 d . . . C45_2 C 0.7321(13) 0.5777(14) 0.0656(9) 0.070(5) Uani 1 1 d . . . H45_2 H 0.6853 0.5904 0.0398 0.084 Uiso 1 1 calc R . . O46_2 O 0.8614(11) 0.5578(9) -0.0407(6) 0.082(4) Uani 1 1 d . . . C47_2 C 0.9772(13) 0.5221(15) -0.0872(10) 0.081(6) Uani 1 1 d . . . H47A_2 H 1.0271 0.5662 -0.0845 0.097 Uiso 1 1 calc R . . H47B_2 H 0.9954 0.4626 -0.0677 0.097 Uiso 1 1 calc R . . C48_2 C 0.9835(14) 0.5120(15) -0.1601(9) 0.076(5) Uani 1 1 d . . . C49_2 C 0.9711(16) 0.5891(17) -0.2041(10) 0.088(6) Uani 1 1 d . . . H49_2 H 0.9514 0.6465 -0.1818 0.105 Uiso 1 1 calc R . . C50_2 C 0.9845(17) 0.5873(19) -0.2725(11) 0.098(7) Uani 1 1 d . . . H50_2 H 0.9806 0.6422 -0.2986 0.118 Uiso 1 1 calc R . . C51_2 C 1.0042(18) 0.5052(14) -0.3051(10) 0.087(6) Uani 1 1 d . . . H51_2 H 1.0082 0.5043 -0.3536 0.104 Uiso 1 1 calc R . . C52_2 C 1.018(2) 0.425(2) -0.2729(13) 0.124(11) Uani 1 1 d . . . H52_2 H 1.0301 0.3681 -0.2964 0.149 Uiso 1 1 calc R . . C53_2 C 1.0138(13) 0.4322(14) -0.1956(10) 0.079(6) Uani 1 1 d . . . H53_2 H 1.0326 0.3799 -0.1718 0.095 Uiso 1 1 calc R . . C54_2 C 0.9317(15) 0.5286(16) 0.1873(12) 0.089(7) Uani 1 1 d . . . O55_2 O 1.0294(11) 0.5094(13) 0.1591(8) 0.106(5) Uani 1 1 d . . . N56_2 N 0.8892(9) 0.5227(13) 0.2610(7) 0.076(5) Uani 1 1 d . . . H56_2 H 0.8216 0.5316 0.2770 0.091 Uiso 1 1 calc R . . C57_2 C 0.9356(13) 0.5046(14) 0.3158(10) 0.074(5) Uani 1 1 d . . . N58_2 N 0.8653(11) 0.4820(11) 0.3821(7) 0.075(4) Uani 1 1 d . . . C59_2 C 0.9063(11) 0.4599(11) 0.4328(7) 0.052(4) Uani 1 1 d . . . C60_2 C 1.0161(16) 0.4633(13) 0.4257(10) 0.075(5) Uani 1 1 d . . . H60_2 H 1.0430 0.4497 0.4635 0.091 Uiso 1 1 calc R . . C61_2 C 1.0744(12) 0.4882(13) 0.3594(9) 0.069(5) Uani 1 1 d . . . H61_2 H 1.1471 0.4841 0.3500 0.083 Uiso 1 1 calc R . . C62_2 C 1.0415(10) 0.5185(13) 0.3043(8) 0.065(5) Uani 1 1 d . . . H62_2 H 1.0851 0.5461 0.2623 0.078 Uiso 1 1 calc R . . N63_2 N 0.8311(12) 0.4290(11) 0.4980(7) 0.074(4) Uani 1 1 d . . . H63_2 H 0.7664 0.4318 0.4991 0.089 Uiso 1 1 calc R . . C64_2 C 0.8499(13) 0.3955(10) 0.5590(8) 0.056(4) Uani 1 1 d . . . O65_2 O 0.9377(9) 0.3848(10) 0.5666(6) 0.082(4) Uani 1 1 d . . . C66_2 C 0.7540(11) 0.3750(11) 0.6224(8) 0.055(4) Uani 1 1 d . . . N67_2 N 0.6629(10) 0.3659(9) 0.6052(6) 0.060(4) Uani 1 1 d . . . C68_2 C 0.5756(13) 0.3430(12) 0.6613(8) 0.064(5) Uani 1 1 d . . . C69_2 C 0.5793(13) 0.3270(12) 0.7319(8) 0.061(4) Uani 1 1 d . . . H69_2 H 0.5190 0.3112 0.7693 0.073 Uiso 1 1 calc R . . C70_2 C 0.6693(14) 0.3345(10) 0.7449(8) 0.060(4) Uani 1 1 d . . . C71_2 C 0.7625(14) 0.3622(12) 0.6894(9) 0.067(5) Uani 1 1 d . . . H71_2 H 0.8248 0.3709 0.6988 0.080 Uiso 1 1 calc R . . O72_2 O 0.6684(10) 0.3229(10) 0.8160(6) 0.081(4) Uani 1 1 d . . . C73_2 C 0.7596(15) 0.3437(17) 0.8343(10) 0.089(7) Uani 1 1 d . . . H73A_2 H 0.7795 0.4061 0.8170 0.107 Uiso 1 1 calc R . . H73B_2 H 0.8182 0.3002 0.8104 0.107 Uiso 1 1 calc R . . C74_2 C 0.7372(12) 0.3370(10) 0.9168(7) 0.051(4) Uani 1 1 d . . . C75_2 C 0.6401(17) 0.3656(15) 0.9600(12) 0.088(6) Uani 1 1 d . . . H75_2 H 0.5873 0.3842 0.9403 0.105 Uiso 1 1 calc R . . C76_2 C 0.6205(19) 0.367(2) 1.0328(11) 0.113(9) Uani 1 1 d . . . H76_2 H 0.5539 0.3858 1.0639 0.136 Uiso 1 1 calc R . . C77_2 C 0.701(2) 0.3391(19) 1.0600(12) 0.106(8) Uani 1 1 d . . . H77_2 H 0.6875 0.3441 1.1096 0.127 Uiso 1 1 calc R . . C78_2 C 0.7918(18) 0.3074(15) 1.0222(9) 0.089(6) Uani 1 1 d . . . H78_2 H 0.8441 0.2849 1.0412 0.107 Uiso 1 1 calc R . . C79_2 C 0.8041(15) 0.3106(14) 0.9470(10) 0.077(5) Uani 1 1 d . . . H79_2 H 0.8703 0.2905 0.9161 0.093 Uiso 1 1 calc R . . C80_2 C 0.4730(11) 0.3305(11) 0.6460(7) 0.053(4) Uani 1 1 d . . . O81_2 O 0.3936(8) 0.3081(8) 0.6943(6) 0.067(3) Uani 1 1 d . . . N82_2 N 0.4791(12) 0.3578(10) 0.5769(8) 0.075(4) Uani 1 1 d . . . H82_2 H 0.5360 0.3829 0.5511 0.090 Uiso 1 1 calc R . . C83_2 C 0.4010(12) 0.3487(13) 0.5437(9) 0.063(5) Uani 1 1 d . . . N84_2 N 0.4418(10) 0.3612(9) 0.4715(7) 0.058(3) Uani 1 1 d . . . C85_2 C 0.3755(14) 0.3604(14) 0.4360(10) 0.080(6) Uani 1 1 d . . . C86_2 C 0.2690(14) 0.3468(16) 0.4654(9) 0.081(6) Uani 1 1 d . . . H86_2 H 0.2264 0.3405 0.4368 0.097 Uiso 1 1 calc R . . C87_2 C 0.2304(16) 0.3430(13) 0.5396(11) 0.077(5) Uani 1 1 d . . . H87_2 H 0.1578 0.3427 0.5629 0.092 Uiso 1 1 calc R . . C88_2 C 0.2993(12) 0.3395(12) 0.5819(8) 0.062(5) Uani 1 1 d . . . H88_2 H 0.2754 0.3315 0.6321 0.074 Uiso 1 1 calc R . . N89_2 N 0.4319(12) 0.3710(11) 0.3570(7) 0.077(4) Uani 1 1 d . . . H89_2 H 0.4984 0.3793 0.3444 0.092 Uiso 1 1 calc R . . C90_2 C 0.3922(12) 0.3691(12) 0.3052(9) 0.069(5) Uani 1 1 d . . . O91_2 O 0.2981(13) 0.3554(13) 0.3114(8) 0.122(7) Uani 1 1 d . . . C92_2 C 0.470(2) 0.364(2) 0.2288(12) 0.146(12) Uani 1 1 d . . . H92A_2 H 0.4316 0.3626 0.1950 0.219 Uiso 1 1 calc R . . H92B_2 H 0.5155 0.3088 0.2243 0.219 Uiso 1 1 calc R . . H92C_2 H 0.5109 0.4180 0.2187 0.219 Uiso 1 1 calc R . . S1_3 S 0.6279(6) 0.7548(5) 0.3472(4) 0.112(2) Uani 1 1 d . . . O2_3 O 0.7033(15) 0.6825(13) 0.3456(11) 0.131(6) Uani 1 1 d . . . C3_3 C 0.548(3) 0.797(3) 0.4453(15) 0.194(18) Uani 1 1 d . . . H3A_3 H 0.4950 0.7536 0.4685 0.292 Uiso 1 1 calc R . . H3B_3 H 0.5142 0.8575 0.4426 0.292 Uiso 1 1 calc R . . H3C_3 H 0.5948 0.8000 0.4729 0.292 Uiso 1 1 calc R . . C4_3 C 0.712(2) 0.871(2) 0.336(3) 0.29(4) Uani 1 1 d . . . H4A_3 H 0.7645 0.8722 0.2888 0.431 Uiso 1 1 calc R . . H4B_3 H 0.7452 0.8700 0.3726 0.431 Uiso 1 1 calc R . . H4C_3 H 0.6647 0.9259 0.3413 0.431 Uiso 1 1 calc R . . S11_3 S 0.5444(6) 0.6740(12) 0.9621(5) 0.226(7) Uani 1 1 d . . . O12_3 O 0.517(4) 0.5909(16) 0.970(2) 0.31(3) Uani 1 1 d . . . C13_3 C 0.5908(17) 0.6653(16) 0.8717(12) 0.104(7) Uani 1 1 d . . . H13A_3 H 0.6424 0.6137 0.8587 0.155 Uiso 1 1 calc R . . H13B_3 H 0.6228 0.7218 0.8506 0.155 Uiso 1 1 calc R . . H13C_3 H 0.5336 0.6553 0.8540 0.155 Uiso 1 1 calc R . . C14_3 C 0.4636(12) 0.7626(13) 0.9743(9) 0.064(5) Uani 1 1 d . . . H14A_3 H 0.4331 0.7740 1.0253 0.096 Uiso 1 1 calc R . . H14B_3 H 0.4087 0.7515 0.9548 0.096 Uiso 1 1 calc R . . H14C_3 H 0.5001 0.8160 0.9503 0.096 Uiso 1 1 calc R . . S21_3 S 0.7287(9) 0.3075(8) 0.3065(4) 0.207(6) Uani 1 1 d . . . O22_3 O 0.6587(10) 0.3914(15) 0.3125(9) 0.134(7) Uani 1 1 d . . . C23_3 C 0.728(2) 0.2581(18) 0.3807(16) 0.128(10) Uani 1 1 d . . . H23A_3 H 0.6584 0.2666 0.4158 0.192 Uiso 1 1 calc R . . H23B_3 H 0.7780 0.2850 0.3981 0.192 Uiso 1 1 calc R . . H23C_3 H 0.7460 0.1927 0.3732 0.192 Uiso 1 1 calc R . . C24_3 C 0.844(3) 0.287(3) 0.257(2) 0.24(3) Uani 1 1 d . . . H24A_3 H 0.8532 0.3144 0.2102 0.358 Uiso 1 1 calc R . . H24A_3' H 0.8588 0.2209 0.2534 0.358 Uiso 1 1 calc R . . H24A_3'' H 0.8908 0.3133 0.2783 0.358 Uiso 1 1 calc R . . S31_3 S 0.4714(7) 0.1585(7) 0.0154(6) 0.162(4) Uani 1 1 d . . . O32_3 O 0.5065(16) 0.0532(10) -0.0016(9) 0.124(6) Uani 1 1 d . . . C33_3 C 0.337(3) 0.145(3) 0.076(2) 0.214(18) Uani 1 1 d . . . H33A_3 H 0.3392 0.1231 0.1223 0.321 Uiso 1 1 calc R . . H33B_3 H 0.3042 0.1015 0.0557 0.321 Uiso 1 1 calc R . . H33C_3 H 0.2983 0.2046 0.0807 0.321 Uiso 1 1 calc R . . C34_3 C 0.465(3) 0.200(3) -0.0764(19) 0.181(16) Uani 1 1 d . . . H34A_3 H 0.5359 0.2042 -0.1096 0.272 Uiso 1 1 calc R . . H34B_3 H 0.4283 0.2601 -0.0720 0.272 Uiso 1 1 calc R . . H34C_3 H 0.4291 0.1564 -0.0942 0.272 Uiso 1 1 calc R . . O45_3 O 0.5454(10) 0.9432(11) 0.8537(7) 0.095(5) Uani 1 1 d . . . O46_3 O 0.6270(10) 0.4994(11) 0.4549(7) 0.089(4) Uani 1 1 d . . . O47_3 O 0.239(4) 0.379(6) 0.152(4) 0.29(5) Uani 0.50 1 d P . . O48_3 O 0.905(2) 0.162(2) 0.1216(14) 0.110(9) Uani 0.50 1 d P . . C49_3 C 0.962(4) 0.093(2) 0.1442(18) 0.104(16) Uani 0.50 1 d P . . H49A_3 H 1.0062 0.1211 0.1671 0.125 Uiso 0.50 1 calc PR . . H49B_3 H 1.0079 0.0600 0.1021 0.125 Uiso 0.50 1 calc PR . . C50_3 C 0.894(3) 0.022(2) 0.198(2) 0.091(12) Uani 0.50 1 d P . . H50A_3 H 0.9393 -0.0250 0.2117 0.137 Uiso 0.50 1 calc PR . . H50B_3 H 0.8508 -0.0078 0.1758 0.137 Uiso 0.50 1 calc PR . . H50C_3 H 0.8493 0.0532 0.2409 0.137 Uiso 0.50 1 calc PR . . 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_1 0.141(19) 0.084(14) 0.068(13) -0.022(11) -0.036(13) -0.012(13) O2_1 0.102(10) 0.102(11) 0.075(10) -0.028(8) -0.027(8) -0.020(9) C3_1 0.139(17) 0.066(12) 0.046(10) -0.007(8) -0.035(12) -0.046(12) N4_1 0.068(8) 0.091(11) 0.047(9) 0.003(8) -0.012(7) -0.021(8) C5_1 0.069(11) 0.055(10) 0.051(10) -0.015(8) 0.000(8) 0.004(8) N6_1 0.069(9) 0.080(11) 0.072(11) -0.004(9) -0.015(8) 0.009(8) C7_1 0.084(13) 0.058(11) 0.039(10) -0.007(8) 0.001(9) 0.029(9) C8_1 0.064(12) 0.104(16) 0.082(14) 0.004(11) -0.032(11) 0.018(10) C9_1 0.049(10) 0.125(19) 0.069(13) -0.002(12) 0.010(9) 0.013(11) C10_1 0.067(11) 0.066(12) 0.094(15) -0.029(10) -0.040(11) 0.013(9) N11_1 0.060(8) 0.078(10) 0.043(8) -0.007(7) -0.017(7) 0.016(7) C12_1 0.073(12) 0.049(11) 0.085(15) 0.024(9) -0.016(11) -0.005(9) O13_1 0.117(11) 0.092(11) 0.066(9) 0.003(8) -0.019(8) 0.025(8) C14_1 0.083(13) 0.058(11) 0.061(12) 0.017(9) -0.026(10) 0.006(9) N15_1 0.068(9) 0.056(9) 0.060(9) -0.004(7) -0.025(8) 0.008(7) C16_1 0.105(14) 0.048(10) 0.031(9) -0.007(7) 0.015(9) -0.008(9) C17_1 0.064(10) 0.076(12) 0.040(9) 0.004(8) -0.010(8) -0.009(8) C18_1 0.079(12) 0.086(13) 0.057(12) 0.016(9) -0.034(10) 0.001(10) C19_1 0.075(12) 0.073(13) 0.055(12) 0.007(9) -0.008(10) -0.008(10) O20_1 0.078(8) 0.094(10) 0.061(8) 0.016(7) -0.031(7) -0.020(7) C21_1 0.098(13) 0.057(10) 0.041(9) 0.009(8) -0.019(9) 0.011(9) C22_1 0.15(2) 0.15(2) 0.050(13) 0.051(14) -0.045(14) -0.016(18) C23_1 0.105(14) 0.090(14) 0.045(10) 0.008(9) -0.027(9) 0.003(11) C24_1 0.16(2) 0.088(15) 0.073(14) 0.028(12) -0.062(15) -0.007(14) C25_1 0.18(2) 0.078(14) 0.030(9) 0.011(9) -0.024(12) -0.016(14) C26_1 0.13(2) 0.15(2) 0.055(13) 0.006(14) -0.027(13) -0.001(17) C27_1 0.13(2) 0.16(3) 0.033(10) -0.004(12) -0.023(12) 0.011(17) C28_1 0.051(9) 0.083(12) 0.050(10) 0.000(9) -0.022(8) 0.020(8) O29_1 0.074(8) 0.094(9) 0.053(8) 0.005(6) -0.025(6) 0.003(7) N30_1 0.044(7) 0.064(8) 0.037(7) 0.001(6) -0.010(6) 0.007(6) C31_1 0.078(12) 0.047(10) 0.047(10) 0.000(8) -0.010(9) 0.004(8) N32_1 0.059(8) 0.051(8) 0.037(7) -0.007(6) -0.014(6) -0.017(6) C33_1 0.076(12) 0.052(10) 0.046(10) 0.008(8) -0.012(9) -0.004(9) C34_1 0.120(17) 0.063(12) 0.062(12) -0.011(9) -0.026(12) -0.006(11) C35_1 0.055(10) 0.076(13) 0.079(13) 0.008(10) -0.018(9) -0.022(9) C36_1 0.050(9) 0.074(12) 0.044(10) -0.015(8) -0.004(7) 0.011(8) N37_1 0.080(9) 0.069(9) 0.037(8) 0.000(7) -0.010(7) 0.004(7) C38_1 0.077(11) 0.076(11) 0.020(7) -0.007(7) -0.008(7) -0.001(9) O39_1 0.061(8) 0.27(2) 0.034(7) 0.017(10) -0.019(6) 0.013(11) C40_1 0.088(13) 0.133(18) 0.026(8) 0.004(9) -0.014(9) 0.036(12) N41_1 0.061(8) 0.052(8) 0.042(8) 0.006(6) 0.005(6) -0.009(6) C42_1 0.084(12) 0.078(12) 0.031(8) 0.007(8) -0.011(8) -0.007(10) C43_1 0.109(14) 0.063(11) 0.038(9) 0.018(8) -0.013(9) 0.019(10) C44_1 0.081(12) 0.082(13) 0.033(9) 0.015(8) -0.009(9) 0.004(10) C45_1 0.057(9) 0.089(13) 0.024(8) 0.002(8) 0.003(7) 0.002(8) O46_1 0.076(8) 0.115(11) 0.047(7) -0.018(7) -0.015(6) 0.010(7) C47_1 0.107(14) 0.117(16) 0.019(7) 0.018(8) -0.013(8) 0.037(12) C48_1 0.075(12) 0.072(13) 0.052(11) -0.006(9) -0.009(9) -0.006(9) C49_1 0.093(15) 0.116(18) 0.059(13) 0.019(12) -0.028(11) -0.023(13) C50_1 0.069(11) 0.121(17) 0.052(11) -0.015(11) -0.012(9) 0.027(11) C51_1 0.063(12) 0.19(3) 0.054(12) -0.005(14) -0.023(10) -0.004(14) C52_1 0.21(3) 0.103(18) 0.054(13) 0.015(12) -0.070(15) 0.017(17) C53_1 0.18(2) 0.077(14) 0.054(12) -0.012(10) -0.044(13) 0.020(14) C54_1 0.076(12) 0.080(13) 0.074(13) 0.039(10) -0.031(10) -0.029(10) O55_1 0.099(11) 0.160(16) 0.066(10) 0.004(9) -0.028(8) 0.029(10) N56_1 0.046(8) 0.138(15) 0.037(8) 0.019(8) 0.016(6) 0.013(8) C57_1 0.081(13) 0.056(11) 0.118(18) 0.014(11) -0.051(13) -0.001(9) N58_1 0.069(9) 0.091(11) 0.032(7) -0.007(7) -0.012(7) 0.014(8) C59_1 0.060(10) 0.058(10) 0.056(11) -0.018(8) -0.012(9) -0.010(8) C60_1 0.054(9) 0.077(13) 0.071(12) -0.011(10) -0.010(8) -0.013(8) C61_1 0.039(9) 0.117(17) 0.067(12) 0.028(11) 0.002(9) -0.004(9) C62_1 0.087(13) 0.059(12) 0.083(14) -0.013(10) -0.027(11) 0.003(9) N63_1 0.073(10) 0.084(12) 0.068(11) -0.020(9) -0.008(8) 0.002(8) C64_1 0.031(8) 0.085(12) 0.044(9) -0.028(8) 0.021(7) -0.012(8) O65_1 0.059(8) 0.133(13) 0.059(8) 0.000(8) 0.016(6) -0.012(8) C66_1 0.065(11) 0.048(10) 0.061(11) -0.010(8) -0.007(9) -0.015(8) N67_1 0.039(7) 0.087(11) 0.060(9) 0.006(8) -0.013(6) -0.007(7) C68_1 0.054(9) 0.055(10) 0.082(14) -0.008(9) -0.020(9) 0.007(7) C69_1 0.084(13) 0.059(11) 0.047(10) -0.006(8) -0.007(9) -0.027(9) C70_1 0.060(11) 0.047(10) 0.079(13) -0.010(9) 0.019(10) 0.004(8) C71_1 0.042(8) 0.100(14) 0.042(9) -0.002(8) -0.013(7) 0.006(8) O72_1 0.057(6) 0.092(9) 0.055(7) 0.012(6) -0.014(5) 0.009(6) C73_1 0.078(12) 0.15(2) 0.057(12) -0.005(13) -0.016(10) 0.012(13) C74_1 0.057(11) 0.097(16) 0.070(14) 0.030(11) -0.002(10) -0.023(10) C75_1 0.120(19) 0.069(15) 0.095(18) 0.025(13) -0.001(14) -0.013(13) C76_1 0.17(3) 0.088(19) 0.13(2) 0.013(16) -0.01(2) 0.049(17) C77_1 0.066(12) 0.111(18) 0.120(19) 0.040(15) 0.019(12) -0.013(11) C78_1 0.067(18) 0.19(4) 0.51(9) -0.13(5) -0.05(3) -0.01(2) C79_1 0.119(18) 0.102(16) 0.043(11) 0.005(10) 0.014(11) -0.028(13) C80_1 0.074(12) 0.060(11) 0.067(12) -0.034(9) -0.015(10) 0.022(9) O81_1 0.065(7) 0.107(10) 0.069(8) 0.021(7) -0.022(6) -0.035(7) N82_1 0.060(9) 0.061(9) 0.055(9) -0.015(7) -0.012(7) -0.006(7) C83_1 0.029(7) 0.073(11) 0.050(9) 0.011(8) -0.019(6) -0.006(7) N84_1 0.100(12) 0.086(12) 0.040(8) 0.004(7) -0.022(8) -0.001(9) C85_1 0.068(11) 0.118(16) 0.052(11) -0.001(10) -0.021(9) 0.053(11) C86_1 0.044(9) 0.079(13) 0.094(15) 0.011(11) -0.003(10) 0.024(8) C87_1 0.093(14) 0.102(15) 0.059(11) -0.014(10) -0.050(11) -0.010(11) C88_1 0.067(11) 0.053(10) 0.064(11) -0.016(8) 0.009(9) -0.023(8) N89_1 0.061(9) 0.19(2) 0.047(10) 0.016(11) -0.006(8) 0.044(11) C90_1 0.074(13) 0.106(16) 0.055(11) 0.036(11) -0.010(10) -0.011(11) O91_1 0.122(13) 0.123(13) 0.088(11) 0.042(9) -0.034(10) -0.057(11) C92_1 0.082(13) 0.124(18) 0.067(14) 0.022(12) -0.009(10) -0.015(12) C1_2 0.14(2) 0.20(3) 0.058(15) -0.004(16) 0.006(14) -0.06(2) O2_2 0.037(6) 0.153(14) 0.110(12) 0.015(10) -0.001(7) -0.017(8) C3_2 0.038(9) 0.079(13) 0.082(13) -0.019(10) 0.013(9) 0.012(8) N4_2 0.065(10) 0.122(14) 0.062(10) 0.015(9) -0.013(8) -0.042(9) C5_2 0.032(7) 0.053(9) 0.056(10) -0.005(7) 0.007(7) -0.023(6) N6_2 0.055(9) 0.071(10) 0.075(10) -0.005(8) -0.024(8) 0.000(7) C7_2 0.093(14) 0.058(12) 0.068(13) -0.016(10) -0.005(11) -0.005(10) C8_2 0.090(13) 0.083(13) 0.084(14) 0.033(10) -0.064(12) 0.000(10) C9_2 0.045(9) 0.101(15) 0.075(12) 0.032(11) -0.027(9) -0.018(9) C10_2 0.073(11) 0.069(12) 0.071(13) 0.010(9) -0.030(10) -0.040(10) N11_2 0.051(8) 0.117(13) 0.053(9) 0.026(8) -0.008(7) -0.009(8) C12_2 0.060(11) 0.072(12) 0.062(12) 0.006(9) -0.006(9) -0.014(9) O13_2 0.133(12) 0.119(12) 0.039(7) -0.003(7) -0.028(7) 0.015(9) C14_2 0.088(13) 0.070(12) 0.033(9) -0.002(8) -0.003(9) 0.007(9) N15_2 0.088(11) 0.046(8) 0.044(8) -0.011(6) -0.003(7) 0.001(7) C16_2 0.061(11) 0.054(10) 0.044(10) 0.004(8) 0.016(8) 0.009(8) C17_2 0.085(13) 0.027(9) 0.113(17) -0.010(9) -0.015(12) -0.019(8) C18_2 0.075(12) 0.072(12) 0.030(8) 0.009(8) -0.014(8) 0.012(9) C19_2 0.068(12) 0.069(12) 0.048(10) 0.002(8) 0.004(9) 0.014(9) O20_2 0.093(9) 0.078(9) 0.062(8) 0.018(7) 0.006(7) -0.015(7) C21_2 0.071(10) 0.055(10) 0.067(12) 0.021(8) -0.004(8) -0.012(8) C22_2 0.100(14) 0.056(11) 0.044(10) 0.003(8) -0.010(9) 0.012(9) C23_2 0.081(15) 0.106(19) 0.14(2) 0.021(17) -0.026(15) -0.007(13) C24_2 0.15(2) 0.090(16) 0.059(12) 0.039(11) 0.016(12) 0.036(14) C25_2 0.18(3) 0.059(14) 0.17(3) 0.047(17) -0.06(2) 0.000(15) C26_2 0.074(13) 0.110(19) 0.15(2) 0.062(17) -0.044(15) -0.049(13) C27_2 0.114(18) 0.12(2) 0.076(15) -0.016(14) -0.049(13) 0.022(15) C28_2 0.092(14) 0.059(11) 0.068(12) 0.019(9) -0.023(10) 0.032(9) O29_2 0.069(8) 0.141(13) 0.077(10) 0.015(9) -0.023(7) 0.016(8) N30_2 0.037(7) 0.077(9) 0.050(8) 0.014(7) -0.009(6) -0.006(6) C31_2 0.043(9) 0.059(10) 0.060(11) 0.008(8) 0.005(8) 0.007(7) N32_2 0.059(9) 0.075(10) 0.078(11) 0.022(8) -0.020(8) -0.013(7) C33_2 0.047(9) 0.073(11) 0.029(8) -0.004(7) 0.011(7) 0.006(8) C34_2 0.087(14) 0.13(2) 0.053(11) 0.026(12) -0.019(10) 0.008(13) C35_2 0.092(14) 0.059(12) 0.087(15) 0.005(10) -0.046(12) 0.000(10) C36_2 0.063(11) 0.084(14) 0.063(12) 0.003(10) -0.004(9) 0.010(9) N37_2 0.124(14) 0.079(11) 0.077(12) -0.005(9) -0.064(11) 0.002(10) C38_2 0.057(10) 0.095(14) 0.047(10) -0.016(9) -0.008(8) 0.020(9) O39_2 0.083(9) 0.102(10) 0.061(8) -0.003(7) -0.027(7) 0.016(7) C40_2 0.044(8) 0.077(12) 0.049(10) -0.013(8) -0.009(7) -0.001(8) N41_2 0.069(9) 0.103(13) 0.052(9) 0.005(8) -0.027(8) 0.011(8) C42_2 0.068(10) 0.044(9) 0.047(9) -0.001(7) -0.001(8) -0.028(7) C43_2 0.079(13) 0.090(15) 0.067(13) 0.009(11) -0.022(11) -0.005(11) C44_2 0.091(14) 0.070(12) 0.042(10) -0.001(8) -0.022(10) -0.026(10) C45_2 0.054(10) 0.116(16) 0.056(11) 0.001(10) -0.035(9) -0.031(10) O46_2 0.114(10) 0.093(10) 0.034(6) 0.021(6) -0.019(6) -0.016(8) C47_2 0.052(10) 0.109(16) 0.084(13) -0.041(11) -0.018(9) -0.020(10) C48_2 0.081(12) 0.112(16) 0.031(9) 0.000(10) -0.017(9) 0.014(11) C49_2 0.093(13) 0.110(17) 0.057(12) 0.001(11) -0.016(10) -0.027(12) C50_2 0.103(15) 0.13(2) 0.061(14) 0.000(13) -0.017(11) -0.017(14) C51_2 0.131(18) 0.071(13) 0.043(10) -0.012(9) -0.005(11) -0.004(12) C52_2 0.121(19) 0.15(3) 0.087(17) -0.041(16) 0.003(14) -0.086(19) C53_2 0.056(10) 0.085(14) 0.071(13) -0.024(11) 0.011(9) 0.023(9) C54_2 0.064(13) 0.112(18) 0.092(16) 0.020(13) -0.026(12) -0.023(12) O55_2 0.077(9) 0.161(15) 0.066(9) -0.006(9) -0.006(7) -0.007(9) N56_2 0.036(7) 0.143(15) 0.041(8) 0.012(8) -0.005(6) 0.009(8) C57_2 0.059(11) 0.100(15) 0.055(12) -0.006(10) -0.013(9) 0.016(10) N58_2 0.067(9) 0.100(12) 0.039(8) 0.015(7) -0.003(7) 0.029(8) C59_2 0.056(9) 0.064(10) 0.030(8) -0.006(7) -0.009(7) 0.020(7) C60_2 0.097(14) 0.074(13) 0.067(13) 0.015(10) -0.043(11) -0.011(10) C61_2 0.043(9) 0.101(14) 0.048(10) 0.007(9) 0.002(7) 0.016(8) C62_2 0.031(8) 0.102(13) 0.048(9) 0.024(9) 0.003(7) -0.001(8) N63_2 0.078(10) 0.092(12) 0.044(9) 0.004(8) -0.011(8) 0.001(8) C64_2 0.074(11) 0.038(9) 0.050(10) 0.004(7) -0.012(9) -0.003(8) O65_2 0.070(8) 0.121(11) 0.045(7) 0.006(7) -0.012(6) 0.011(7) C66_2 0.044(8) 0.074(11) 0.050(10) 0.014(8) -0.024(7) 0.003(7) N67_2 0.072(9) 0.058(9) 0.031(7) 0.005(6) 0.007(6) 0.007(7) C68_2 0.063(10) 0.063(11) 0.043(10) -0.007(8) 0.012(8) 0.002(8) C69_2 0.065(11) 0.067(12) 0.036(9) 0.005(8) 0.001(8) 0.006(8) C70_2 0.083(12) 0.048(9) 0.031(8) 0.002(7) 0.004(8) 0.001(8) C71_2 0.078(12) 0.059(11) 0.061(12) 0.002(8) -0.025(10) 0.019(8) O72_2 0.093(9) 0.102(10) 0.032(6) 0.018(6) -0.002(6) -0.006(7) C73_2 0.061(12) 0.128(19) 0.072(14) -0.004(13) -0.010(10) -0.028(12) C74_2 0.066(10) 0.045(9) 0.036(8) -0.013(7) -0.007(7) 0.000(7) C75_2 0.091(14) 0.088(15) 0.086(16) -0.008(12) -0.033(12) 0.005(11) C76_2 0.099(17) 0.16(2) 0.056(13) -0.043(14) 0.021(12) -0.022(16) C77_2 0.13(2) 0.13(2) 0.055(12) -0.003(13) -0.035(13) -0.024(17) C78_2 0.105(16) 0.105(17) 0.044(11) -0.008(10) -0.007(10) -0.004(13) C79_2 0.076(12) 0.090(14) 0.057(12) -0.001(10) -0.009(9) -0.009(10) C80_2 0.052(9) 0.066(10) 0.030(8) -0.018(7) -0.003(7) 0.017(8) O81_2 0.061(7) 0.088(9) 0.042(6) 0.001(6) 0.003(6) -0.029(6) N82_2 0.083(11) 0.071(10) 0.055(10) 0.006(7) 0.000(8) -0.016(8) C83_2 0.046(9) 0.078(13) 0.068(12) 0.005(9) -0.022(9) 0.001(8) N84_2 0.062(8) 0.059(9) 0.052(8) -0.002(7) -0.017(7) -0.002(6) C85_2 0.079(13) 0.093(15) 0.063(12) 0.043(10) -0.025(10) 0.013(10) C86_2 0.056(11) 0.130(18) 0.050(11) 0.003(11) -0.011(9) 0.006(10) C87_2 0.076(12) 0.076(13) 0.073(14) -0.004(10) -0.017(10) 0.001(10) C88_2 0.059(10) 0.088(13) 0.025(8) -0.013(8) 0.010(7) -0.016(9) N89_2 0.075(9) 0.088(11) 0.052(9) 0.010(8) -0.006(7) 0.024(8) C90_2 0.058(9) 0.076(12) 0.062(11) 0.013(9) -0.016(8) 0.034(8) O91_2 0.130(13) 0.167(17) 0.065(9) 0.001(9) -0.042(9) 0.071(12) C92_2 0.14(2) 0.22(3) 0.055(14) 0.070(17) -0.011(14) 0.00(2) S1_3 0.154(6) 0.094(4) 0.099(5) 0.004(3) -0.059(4) -0.011(4) O2_3 0.136(15) 0.110(14) 0.144(16) -0.007(11) -0.045(12) 0.010(11) C3_3 0.17(3) 0.33(5) 0.09(2) -0.05(3) -0.04(2) -0.03(3) C4_3 0.073(16) 0.11(2) 0.55(9) 0.16(4) 0.05(3) 0.007(15) S11_3 0.079(4) 0.48(2) 0.118(6) 0.086(9) -0.051(4) 0.016(7) O12_3 0.58(7) 0.071(14) 0.39(5) -0.08(2) -0.31(5) 0.04(2) C13_3 0.100(15) 0.095(16) 0.101(17) 0.008(13) -0.018(12) 0.017(12) C14_3 0.050(9) 0.099(14) 0.056(10) 0.009(9) -0.032(8) -0.028(9) S21_3 0.221(10) 0.219(10) 0.096(5) 0.038(6) 0.035(6) 0.114(9) O22_3 0.054(8) 0.21(2) 0.118(14) 0.042(13) -0.016(8) 0.008(10) C23_3 0.118(19) 0.094(18) 0.16(3) 0.045(17) -0.036(18) -0.029(15) C24_3 0.18(4) 0.19(4) 0.22(4) 0.07(3) 0.08(3) 0.08(3) S31_3 0.153(7) 0.147(7) 0.201(9) -0.006(7) -0.068(7) -0.060(6) O32_3 0.204(18) 0.055(9) 0.099(12) -0.004(8) -0.029(11) -0.012(10) C33_3 0.18(3) 0.13(3) 0.35(5) -0.02(3) -0.11(3) -0.08(2) C34_3 0.23(4) 0.16(3) 0.17(3) 0.00(2) -0.10(3) 0.10(3) O45_3 0.078(9) 0.146(14) 0.058(8) 0.009(8) -0.020(7) 0.008(8) O46_3 0.072(8) 0.117(12) 0.063(8) 0.000(8) -0.001(7) -0.010(8) O47_3 0.17(4) 0.46(11) 0.27(7) -0.25(8) -0.11(5) 0.16(6) O48_3 0.12(2) 0.14(3) 0.075(17) 0.014(17) -0.052(16) 0.000(19) C49_3 0.22(5) 0.05(2) 0.05(2) -0.028(17) -0.07(3) 0.05(3) C50_3 0.10(3) 0.05(2) 0.09(3) 0.007(18) 0.02(2) 0.006(17) _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_1 C3_1 1.59(3) . ? O2_1 C3_1 1.09(2) . ? C3_1 N4_1 1.40(2) . ? N4_1 C5_1 1.30(2) . ? C5_1 N6_1 1.36(2) . ? C5_1 C10_1 1.41(2) . ? N6_1 C7_1 1.36(2) . ? C7_1 N11_1 1.38(2) . ? C7_1 C8_1 1.41(3) . ? C8_1 C9_1 1.31(3) . ? C9_1 C10_1 1.42(3) . ? N11_1 C12_1 1.34(2) . ? C12_1 O13_1 1.21(2) . ? C12_1 C14_1 1.50(3) . ? C14_1 N15_1 1.30(2) . ? C14_1 C19_1 1.35(2) . ? N15_1 C16_1 1.29(2) . ? C16_1 C17_1 1.43(2) . ? C16_1 C28_1 1.54(2) . ? C17_1 C18_1 1.39(2) . ? C18_1 O20_1 1.351(19) . ? C18_1 C19_1 1.44(2) . ? O20_1 C21_1 1.41(2) . ? C21_1 C22_1 1.50(2) . ? C22_1 C27_1 1.36(3) . ? C22_1 C23_1 1.52(3) . ? C23_1 C24_1 1.36(3) . ? C24_1 C25_1 1.51(3) . ? C25_1 C26_1 1.28(3) . ? C26_1 C27_1 1.45(3) . ? C28_1 O29_1 1.151(17) . ? C28_1 N30_1 1.376(19) . ? N30_1 C31_1 1.44(2) . ? C31_1 C36_1 1.30(2) . ? C31_1 N32_1 1.34(2) . ? N32_1 C33_1 1.335(19) . ? C33_1 C34_1 1.37(3) . ? C33_1 N37_1 1.42(2) . ? C34_1 C35_1 1.42(3) . ? C35_1 C36_1 1.45(2) . ? N37_1 C38_1 1.388(17) . ? C38_1 O39_1 1.209(19) . ? C38_1 C40_1 1.54(2) . ? C40_1 N41_1 1.24(2) . ? C40_1 C45_1 1.49(2) . ? N41_1 C42_1 1.27(2) . ? C42_1 C43_1 1.45(2) . ? C42_1 C54_1 1.49(3) . ? C43_1 C44_1 1.37(2) . ? C44_1 C45_1 1.38(2) . ? C44_1 O46_1 1.395(19) . ? O46_1 C47_1 1.37(2) . ? C47_1 C48_1 1.55(2) . ? C48_1 C53_1 1.30(3) . ? C48_1 C49_1 1.42(3) . ? C49_1 C50_1 1.32(2) . ? C50_1 C51_1 1.29(3) . ? C51_1 C52_1 1.43(3) . ? C52_1 C53_1 1.39(3) . ? C54_1 O55_1 1.16(2) . ? C54_1 N56_1 1.37(2) . ? N56_1 C57_1 1.43(2) . ? C57_1 N58_1 1.30(2) . ? C57_1 C62_1 1.41(3) . ? N58_1 C59_1 1.28(2) . ? C59_1 N63_1 1.43(2) . ? C59_1 C60_1 1.44(2) . ? C60_1 C61_1 1.42(3) . ? C61_1 C62_1 1.31(2) . ? N63_1 C64_1 1.365(19) . ? C64_1 O65_1 1.171(18) . ? C64_1 C66_1 1.49(2) . ? C66_1 N67_1 1.32(2) . ? C66_1 C71_1 1.42(2) . ? N67_1 C68_1 1.32(2) . ? C68_1 C69_1 1.44(2) . ? C68_1 C80_1 1.53(2) . ? C69_1 C70_1 1.36(2) . ? C70_1 C71_1 1.39(2) . ? C70_1 O72_1 1.432(19) . ? O72_1 C73_1 1.40(2) . ? C73_1 C74_1 1.22(3) . ? C74_1 C79_1 1.34(2) . ? C74_1 C75_1 1.51(3) . ? C75_1 C76_1 1.21(3) . ? C76_1 C77_1 1.64(4) . ? C77_1 C78_1 1.35(4) . ? C78_1 C79_1 1.19(4) . ? C80_1 O81_1 1.20(2) . ? C80_1 N82_1 1.42(2) . ? N82_1 C83_1 1.303(17) . ? C83_1 N84_1 1.337(19) . ? C83_1 C88_1 1.41(2) . ? N84_1 C85_1 1.46(2) . ? C85_1 C86_1 1.25(2) . ? C85_1 N89_1 1.38(2) . ? C86_1 C87_1 1.47(3) . ? C87_1 C88_1 1.37(2) . ? N89_1 C90_1 1.35(2) . ? C90_1 O91_1 1.25(2) . ? C90_1 C92_1 1.50(3) . ? C1_2 C3_2 1.51(3) . ? O2_2 C3_2 1.14(2) . ? C3_2 N4_2 1.38(2) . ? N4_2 C5_2 1.43(2) . ? C5_2 N6_2 1.260(18) . ? C5_2 C10_2 1.44(2) . ? N6_2 C7_2 1.35(2) . ? C7_2 C8_2 1.28(2) . ? C7_2 N11_2 1.54(2) . ? C8_2 C9_2 1.43(2) . ? C9_2 C10_2 1.30(2) . ? N11_2 C12_2 1.34(2) . ? C12_2 O13_2 1.23(2) . ? C12_2 C14_2 1.50(3) . ? C14_2 N15_2 1.34(2) . ? C14_2 C19_2 1.42(2) . ? N15_2 C16_2 1.35(2) . ? C16_2 C17_2 1.35(2) . ? C16_2 C28_2 1.51(3) . ? C17_2 C18_2 1.37(3) . ? C18_2 O20_2 1.277(18) . ? C18_2 C19_2 1.35(2) . ? O20_2 C21_2 1.46(2) . ? C21_2 C22_2 1.65(2) . ? C22_2 C27_2 1.33(3) . ? C22_2 C23_2 1.36(3) . ? C23_2 C24_2 1.48(3) . ? C24_2 C25_2 1.51(4) . ? C25_2 C26_2 1.12(4) . ? C26_2 C27_2 1.38(3) . ? C28_2 O29_2 1.21(2) . ? C28_2 N30_2 1.42(2) . ? N30_2 C31_2 1.39(2) . ? C31_2 C36_2 1.27(2) . ? C31_2 N32_2 1.41(2) . ? N32_2 C33_2 1.33(2) . ? C33_2 C34_2 1.29(2) . ? C33_2 N37_2 1.43(2) . ? C34_2 C35_2 1.50(3) . ? C35_2 C36_2 1.33(3) . ? N37_2 C38_2 1.39(2) . ? C38_2 O39_2 1.23(2) . ? C38_2 C40_2 1.54(2) . ? C40_2 C45_2 1.32(2) . ? C40_2 N41_2 1.38(2) . ? N41_2 C42_2 1.42(2) . ? C42_2 C43_2 1.35(2) . ? C42_2 C54_2 1.40(3) . ? C43_2 C44_2 1.34(3) . ? C44_2 O46_2 1.313(19) . ? C44_2 C45_2 1.36(3) . ? O46_2 C47_2 1.58(2) . ? C47_2 C48_2 1.41(2) . ? C48_2 C53_2 1.33(3) . ? C48_2 C49_2 1.41(3) . ? C49_2 C50_2 1.29(3) . ? C50_2 C51_2 1.33(3) . ? C51_2 C52_2 1.33(4) . ? C52_2 C53_2 1.50(3) . ? C54_2 O55_2 1.26(2) . ? C54_2 N56_2 1.36(2) . ? N56_2 C57_2 1.41(2) . ? C57_2 N58_2 1.37(2) . ? C57_2 C62_2 1.39(2) . ? N58_2 C59_2 1.300(19) . ? C59_2 N63_2 1.42(2) . ? C59_2 C60_2 1.44(2) . ? C60_2 C61_2 1.32(2) . ? C61_2 C62_2 1.34(2) . ? N63_2 C64_2 1.36(2) . ? C64_2 O65_2 1.234(19) . ? C64_2 C66_2 1.50(2) . ? C66_2 C71_2 1.35(2) . ? C66_2 N67_2 1.387(19) . ? N67_2 C68_2 1.365(19) . ? C68_2 C69_2 1.40(2) . ? C68_2 C80_2 1.53(2) . ? C69_2 C70_2 1.33(2) . ? C70_2 O72_2 1.386(18) . ? C70_2 C71_2 1.43(2) . ? O72_2 C73_2 1.44(2) . ? C73_2 C74_2 1.54(2) . ? C74_2 C79_2 1.26(2) . ? C74_2 C75_2 1.35(2) . ? C75_2 C76_2 1.36(3) . ? C76_2 C77_2 1.38(3) . ? C77_2 C78_2 1.26(3) . ? C78_2 C79_2 1.42(3) . ? C80_2 O81_2 1.222(17) . ? C80_2 N82_2 1.37(2) . ? N82_2 C83_2 1.42(2) . ? C83_2 C88_2 1.34(2) . ? C83_2 N84_2 1.34(2) . ? N84_2 C85_2 1.30(2) . ? C85_2 C86_2 1.38(2) . ? C85_2 N89_2 1.48(2) . ? C86_2 C87_2 1.37(3) . ? C87_2 C88_2 1.43(3) . ? N89_2 C90_2 1.29(2) . ? C90_2 O91_2 1.26(2) . ? C90_2 C92_2 1.51(3) . ? S1_3 O2_3 1.393(19) . ? S1_3 C3_3 1.96(3) . ? S1_3 C4_3 2.05(4) . ? S11_3 O12_3 1.26(3) . ? S11_3 C14_3 1.59(2) . ? S11_3 C13_3 1.67(2) . ? S21_3 O22_3 1.46(2) . ? S21_3 C24_3 1.54(3) . ? S21_3 C23_3 1.58(3) . ? S31_3 O32_3 1.568(17) . ? S31_3 C33_3 1.81(4) . ? S31_3 C34_3 1.89(3) . ? O48_3 C49_3 1.35(4) . ? C49_3 C50_3 1.56(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2_1 C3_1 N4_1 126.4(18) . . ? O2_1 C3_1 C1_1 123.8(16) . . ? N4_1 C3_1 C1_1 108.1(18) . . ? C5_1 N4_1 C3_1 130.2(16) . . ? N4_1 C5_1 N6_1 117.4(15) . . ? N4_1 C5_1 C10_1 121.7(17) . . ? N6_1 C5_1 C10_1 120.7(16) . . ? C7_1 N6_1 C5_1 121.4(15) . . ? N6_1 C7_1 N11_1 114.7(15) . . ? N6_1 C7_1 C8_1 117.9(17) . . ? N11_1 C7_1 C8_1 127.1(16) . . ? C9_1 C8_1 C7_1 121.6(19) . . ? C8_1 C9_1 C10_1 121.6(18) . . ? C5_1 C10_1 C9_1 116.4(16) . . ? C12_1 N11_1 C7_1 131.7(15) . . ? O13_1 C12_1 N11_1 123.1(18) . . ? O13_1 C12_1 C14_1 120.8(18) . . ? N11_1 C12_1 C14_1 116.1(15) . . ? N15_1 C14_1 C19_1 125.6(17) . . ? N15_1 C14_1 C12_1 115.9(15) . . ? C19_1 C14_1 C12_1 118.5(16) . . ? C16_1 N15_1 C14_1 115.9(14) . . ? N15_1 C16_1 C17_1 126.0(14) . . ? N15_1 C16_1 C28_1 121.3(15) . . ? C17_1 C16_1 C28_1 112.6(16) . . ? C18_1 C17_1 C16_1 116.4(16) . . ? O20_1 C18_1 C17_1 126.6(16) . . ? O20_1 C18_1 C19_1 116.9(15) . . ? C17_1 C18_1 C19_1 114.7(15) . . ? C14_1 C19_1 C18_1 119.4(16) . . ? C18_1 O20_1 C21_1 116.4(13) . . ? O20_1 C21_1 C22_1 107.7(16) . . ? C27_1 C22_1 C21_1 126(2) . . ? C27_1 C22_1 C23_1 120.8(18) . . ? C21_1 C22_1 C23_1 114(2) . . ? C24_1 C23_1 C22_1 113.5(19) . . ? C23_1 C24_1 C25_1 124(2) . . ? C26_1 C25_1 C24_1 118.3(18) . . ? C25_1 C26_1 C27_1 122(2) . . ? C22_1 C27_1 C26_1 121(2) . . ? O29_1 C28_1 N30_1 126.0(15) . . ? O29_1 C28_1 C16_1 122.1(15) . . ? N30_1 C28_1 C16_1 111.8(13) . . ? C28_1 N30_1 C31_1 125.7(13) . . ? C36_1 C31_1 N32_1 125.2(15) . . ? C36_1 C31_1 N30_1 122.7(15) . . ? N32_1 C31_1 N30_1 111.7(14) . . ? C33_1 N32_1 C31_1 116.7(14) . . ? N32_1 C33_1 C34_1 123.3(16) . . ? N32_1 C33_1 N37_1 112.0(14) . . ? C34_1 C33_1 N37_1 124.8(15) . . ? C33_1 C34_1 C35_1 119.8(18) . . ? C34_1 C35_1 C36_1 114.0(16) . . ? C31_1 C36_1 C35_1 120.5(16) . . ? C38_1 N37_1 C33_1 121.5(14) . . ? O39_1 C38_1 N37_1 127.6(15) . . ? O39_1 C38_1 C40_1 122.3(13) . . ? N37_1 C38_1 C40_1 109.8(14) . . ? N41_1 C40_1 C45_1 124.2(16) . . ? N41_1 C40_1 C38_1 123.0(14) . . ? C45_1 C40_1 C38_1 111.7(14) . . ? C40_1 N41_1 C42_1 122.7(14) . . ? N41_1 C42_1 C43_1 118.8(16) . . ? N41_1 C42_1 C54_1 124.5(14) . . ? C43_1 C42_1 C54_1 115.9(16) . . ? C44_1 C43_1 C42_1 120.8(17) . . ? C43_1 C44_1 C45_1 119.1(15) . . ? C43_1 C44_1 O46_1 116.7(16) . . ? C45_1 C44_1 O46_1 123.3(15) . . ? C44_1 C45_1 C40_1 113.4(14) . . ? C47_1 O46_1 C44_1 115.7(13) . . ? O46_1 C47_1 C48_1 106.0(14) . . ? C53_1 C48_1 C49_1 118.8(18) . . ? C53_1 C48_1 C47_1 121.0(17) . . ? C49_1 C48_1 C47_1 120.1(18) . . ? C50_1 C49_1 C48_1 117(2) . . ? C51_1 C50_1 C49_1 130(2) . . ? C50_1 C51_1 C52_1 112.3(18) . . ? C53_1 C52_1 C51_1 122(2) . . ? C48_1 C53_1 C52_1 121(2) . . ? O55_1 C54_1 N56_1 125.9(19) . . ? O55_1 C54_1 C42_1 123.4(18) . . ? N56_1 C54_1 C42_1 109.1(15) . . ? C54_1 N56_1 C57_1 130.0(16) . . ? N58_1 C57_1 C62_1 125(2) . . ? N58_1 C57_1 N56_1 113.6(15) . . ? C62_1 C57_1 N56_1 121.8(19) . . ? C59_1 N58_1 C57_1 116.4(16) . . ? N58_1 C59_1 N63_1 113.1(15) . . ? N58_1 C59_1 C60_1 127.9(16) . . ? N63_1 C59_1 C60_1 119.0(14) . . ? C61_1 C60_1 C59_1 110.3(14) . . ? C62_1 C61_1 C60_1 124.2(18) . . ? C61_1 C62_1 C57_1 117(2) . . ? C64_1 N63_1 C59_1 129.8(15) . . ? O65_1 C64_1 N63_1 123.7(17) . . ? O65_1 C64_1 C66_1 122.4(13) . . ? N63_1 C64_1 C66_1 113.8(13) . . ? N67_1 C66_1 C71_1 123.6(16) . . ? N67_1 C66_1 C64_1 119.8(14) . . ? C71_1 C66_1 C64_1 116.5(13) . . ? C66_1 N67_1 C68_1 117.1(14) . . ? N67_1 C68_1 C69_1 125.9(15) . . ? N67_1 C68_1 C80_1 119.7(15) . . ? C69_1 C68_1 C80_1 113.8(16) . . ? C70_1 C69_1 C68_1 113.3(17) . . ? C69_1 C70_1 C71_1 124.2(16) . . ? C69_1 C70_1 O72_1 122.3(18) . . ? C71_1 C70_1 O72_1 113.5(14) . . ? C70_1 C71_1 C66_1 115.6(14) . . ? C73_1 O72_1 C70_1 124.8(14) . . ? C74_1 C73_1 O72_1 125.4(19) . . ? C73_1 C74_1 C79_1 130(2) . . ? C73_1 C74_1 C75_1 114.0(19) . . ? C79_1 C74_1 C75_1 114.4(17) . . ? C76_1 C75_1 C74_1 125(3) . . ? C75_1 C76_1 C77_1 112(3) . . ? C78_1 C77_1 C76_1 118(3) . . ? C79_1 C78_1 C77_1 121(5) . . ? C78_1 C79_1 C74_1 129(3) . . ? O81_1 C80_1 N82_1 119.6(16) . . ? O81_1 C80_1 C68_1 128.0(17) . . ? N82_1 C80_1 C68_1 112.2(16) . . ? C83_1 N82_1 C80_1 131.2(14) . . ? N82_1 C83_1 N84_1 114.1(13) . . ? N82_1 C83_1 C88_1 127.0(14) . . ? N84_1 C83_1 C88_1 118.8(13) . . ? C83_1 N84_1 C85_1 118.0(13) . . ? C86_1 C85_1 N89_1 133(2) . . ? C86_1 C85_1 N84_1 123.0(17) . . ? N89_1 C85_1 N84_1 104.2(15) . . ? C85_1 C86_1 C87_1 121.3(18) . . ? C88_1 C87_1 C86_1 115.2(15) . . ? C87_1 C88_1 C83_1 123.4(16) . . ? C90_1 N89_1 C85_1 123.8(19) . . ? O91_1 C90_1 N89_1 123.8(17) . . ? O91_1 C90_1 C92_1 117.5(16) . . ? N89_1 C90_1 C92_1 117.6(18) . . ? O2_2 C3_2 N4_2 124(2) . . ? O2_2 C3_2 C1_2 125.2(18) . . ? N4_2 C3_2 C1_2 110.9(17) . . ? C3_2 N4_2 C5_2 128.2(15) . . ? N6_2 C5_2 C10_2 122.4(15) . . ? N6_2 C5_2 N4_2 114.6(14) . . ? C10_2 C5_2 N4_2 122.9(12) . . ? C5_2 N6_2 C7_2 115.3(15) . . ? C8_2 C7_2 N6_2 130.9(18) . . ? C8_2 C7_2 N11_2 123.6(18) . . ? N6_2 C7_2 N11_2 105.5(16) . . ? C7_2 C8_2 C9_2 110.6(17) . . ? C10_2 C9_2 C8_2 124.4(15) . . ? C9_2 C10_2 C5_2 116.1(15) . . ? C12_2 N11_2 C7_2 123.4(15) . . ? O13_2 C12_2 N11_2 131.4(16) . . ? O13_2 C12_2 C14_2 119.0(15) . . ? N11_2 C12_2 C14_2 109.5(15) . . ? N15_2 C14_2 C19_2 119.7(17) . . ? N15_2 C14_2 C12_2 119.6(14) . . ? C19_2 C14_2 C12_2 120.2(16) . . ? C14_2 N15_2 C16_2 118.2(14) . . ? N15_2 C16_2 C17_2 120.8(17) . . ? N15_2 C16_2 C28_2 119.0(14) . . ? C17_2 C16_2 C28_2 119.9(16) . . ? C16_2 C17_2 C18_2 124.1(18) . . ? O20_2 C18_2 C19_2 127.3(15) . . ? O20_2 C18_2 C17_2 118.6(16) . . ? C19_2 C18_2 C17_2 114.0(15) . . ? C18_2 C19_2 C14_2 122.8(17) . . ? C18_2 O20_2 C21_2 116.3(14) . . ? O20_2 C21_2 C22_2 98.6(13) . . ? C27_2 C22_2 C23_2 123(2) . . ? C27_2 C22_2 C21_2 121.4(17) . . ? C23_2 C22_2 C21_2 115.0(17) . . ? C22_2 C23_2 C24_2 114(2) . . ? C23_2 C24_2 C25_2 118(2) . . ? C26_2 C25_2 C24_2 117(2) . . ? C25_2 C26_2 C27_2 128(3) . . ? C22_2 C27_2 C26_2 118(2) . . ? O29_2 C28_2 N30_2 123.4(16) . . ? O29_2 C28_2 C16_2 124.8(16) . . ? N30_2 C28_2 C16_2 111.8(14) . . ? C31_2 N30_2 C28_2 124.5(13) . . ? C36_2 C31_2 N30_2 132.7(15) . . ? C36_2 C31_2 N32_2 117.3(17) . . ? N30_2 C31_2 N32_2 109.4(13) . . ? C33_2 N32_2 C31_2 116.2(14) . . ? C34_2 C33_2 N32_2 129.7(14) . . ? C34_2 C33_2 N37_2 121.4(15) . . ? N32_2 C33_2 N37_2 108.4(14) . . ? C33_2 C34_2 C35_2 112.1(16) . . ? C36_2 C35_2 C34_2 116.7(17) . . ? C31_2 C36_2 C35_2 126.9(18) . . ? C38_2 N37_2 C33_2 126.5(15) . . ? O39_2 C38_2 N37_2 123.2(15) . . ? O39_2 C38_2 C40_2 121.0(15) . . ? N37_2 C38_2 C40_2 115.0(15) . . ? C45_2 C40_2 N41_2 127.4(14) . . ? C45_2 C40_2 C38_2 121.0(15) . . ? N41_2 C40_2 C38_2 111.5(13) . . ? C40_2 N41_2 C42_2 112.6(13) . . ? C43_2 C42_2 C54_2 124.9(17) . . ? C43_2 C42_2 N41_2 119.4(16) . . ? C54_2 C42_2 N41_2 115.3(15) . . ? C44_2 C43_2 C42_2 124.4(19) . . ? O46_2 C44_2 C43_2 129.1(18) . . ? O46_2 C44_2 C45_2 113.5(16) . . ? C43_2 C44_2 C45_2 117.2(16) . . ? C40_2 C45_2 C44_2 118.6(14) . . ? C44_2 O46_2 C47_2 118.0(15) . . ? C48_2 C47_2 O46_2 110.0(14) . . ? C53_2 C48_2 C49_2 114.1(17) . . ? C53_2 C48_2 C47_2 123(2) . . ? C49_2 C48_2 C47_2 122(2) . . ? C50_2 C49_2 C48_2 126(2) . . ? C49_2 C50_2 C51_2 119(2) . . ? C52_2 C51_2 C50_2 124(2) . . ? C51_2 C52_2 C53_2 115(2) . . ? C48_2 C53_2 C52_2 121(2) . . ? O55_2 C54_2 N56_2 118.0(18) . . ? O55_2 C54_2 C42_2 121(2) . . ? N56_2 C54_2 C42_2 120.4(16) . . ? C54_2 N56_2 C57_2 131.9(14) . . ? N58_2 C57_2 C62_2 123.6(16) . . ? N58_2 C57_2 N56_2 114.0(14) . . ? C62_2 C57_2 N56_2 122.0(15) . . ? C59_2 N58_2 C57_2 115.6(14) . . ? N58_2 C59_2 N63_2 112.9(14) . . ? N58_2 C59_2 C60_2 125.5(14) . . ? N63_2 C59_2 C60_2 121.6(14) . . ? C61_2 C60_2 C59_2 112.4(15) . . ? C60_2 C61_2 C62_2 127.8(15) . . ? C61_2 C62_2 C57_2 113.6(14) . . ? C64_2 N63_2 C59_2 127.2(15) . . ? O65_2 C64_2 N63_2 125.3(15) . . ? O65_2 C64_2 C66_2 118.8(14) . . ? N63_2 C64_2 C66_2 115.8(14) . . ? C71_2 C66_2 N67_2 125.2(14) . . ? C71_2 C66_2 C64_2 119.7(14) . . ? N67_2 C66_2 C64_2 114.9(12) . . ? C68_2 N67_2 C66_2 116.2(13) . . ? N67_2 C68_2 C69_2 121.6(16) . . ? N67_2 C68_2 C80_2 119.0(14) . . ? C69_2 C68_2 C80_2 119.3(13) . . ? C70_2 C69_2 C68_2 119.6(14) . . ? C69_2 C70_2 O72_2 117.8(13) . . ? C69_2 C70_2 C71_2 121.8(15) . . ? O72_2 C70_2 C71_2 120.1(16) . . ? C66_2 C71_2 C70_2 115.5(16) . . ? C70_2 O72_2 C73_2 119.7(13) . . ? O72_2 C73_2 C74_2 111.1(13) . . ? C79_2 C74_2 C75_2 117.4(16) . . ? C79_2 C74_2 C73_2 124.9(15) . . ? C75_2 C74_2 C73_2 117.6(16) . . ? C74_2 C75_2 C76_2 119(2) . . ? C75_2 C76_2 C77_2 119(2) . . ? C78_2 C77_2 C76_2 125(2) . . ? C77_2 C78_2 C79_2 112(2) . . ? C74_2 C79_2 C78_2 128.5(18) . . ? O81_2 C80_2 N82_2 126.2(14) . . ? O81_2 C80_2 C68_2 121.2(13) . . ? N82_2 C80_2 C68_2 112.1(13) . . ? C80_2 N82_2 C83_2 126.4(14) . . ? C88_2 C83_2 N84_2 126.5(15) . . ? C88_2 C83_2 N82_2 122.6(16) . . ? N84_2 C83_2 N82_2 110.5(13) . . ? C85_2 N84_2 C83_2 115.7(14) . . ? N84_2 C85_2 C86_2 126.1(17) . . ? N84_2 C85_2 N89_2 109.9(15) . . ? C86_2 C85_2 N89_2 123.9(16) . . ? C87_2 C86_2 C85_2 115.2(18) . . ? C86_2 C87_2 C88_2 121.2(17) . . ? C83_2 C88_2 C87_2 114.6(15) . . ? C90_2 N89_2 C85_2 127.1(15) . . ? O91_2 C90_2 N89_2 126.8(16) . . ? O91_2 C90_2 C92_2 115.4(18) . . ? N89_2 C90_2 C92_2 116.6(17) . . ? O2_3 S1_3 C3_3 113.5(16) . . ? O2_3 S1_3 C4_3 102.8(12) . . ? C3_3 S1_3 C4_3 87(2) . . ? O12_3 S11_3 C14_3 124(2) . . ? O12_3 S11_3 C13_3 92(2) . . ? C14_3 S11_3 C13_3 103.2(10) . . ? O22_3 S21_3 C24_3 130.5(17) . . ? O22_3 S21_3 C23_3 115.9(14) . . ? C24_3 S21_3 C23_3 102(2) . . ? O32_3 S31_3 C33_3 99.3(14) . . ? O32_3 S31_3 C34_3 99.4(13) . . ? C33_3 S31_3 C34_3 108(2) . . ? O48_3 C49_3 C50_3 114(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2_1 C3_1 N4_1 C5_1 16(3) . . . . ? C1_1 C3_1 N4_1 C5_1 -178.5(17) . . . . ? C3_1 N4_1 C5_1 N6_1 178.1(16) . . . . ? C3_1 N4_1 C5_1 C10_1 -8(3) . . . . ? N4_1 C5_1 N6_1 C7_1 176.9(15) . . . . ? C10_1 C5_1 N6_1 C7_1 3(2) . . . . ? C5_1 N6_1 C7_1 N11_1 178.9(15) . . . . ? C5_1 N6_1 C7_1 C8_1 -7(2) . . . . ? N6_1 C7_1 C8_1 C9_1 6(3) . . . . ? N11_1 C7_1 C8_1 C9_1 179.0(19) . . . . ? C7_1 C8_1 C9_1 C10_1 0(3) . . . . ? N4_1 C5_1 C10_1 C9_1 -170.9(17) . . . . ? N6_1 C5_1 C10_1 C9_1 3(2) . . . . ? C8_1 C9_1 C10_1 C5_1 -4(3) . . . . ? N6_1 C7_1 N11_1 C12_1 169.8(17) . . . . ? C8_1 C7_1 N11_1 C12_1 -3(3) . . . . ? C7_1 N11_1 C12_1 O13_1 -3(3) . . . . ? C7_1 N11_1 C12_1 C14_1 177.5(15) . . . . ? O13_1 C12_1 C14_1 N15_1 -177.1(17) . . . . ? N11_1 C12_1 C14_1 N15_1 3(2) . . . . ? O13_1 C12_1 C14_1 C19_1 1(3) . . . . ? N11_1 C12_1 C14_1 C19_1 -178.8(16) . . . . ? C19_1 C14_1 N15_1 C16_1 -1(3) . . . . ? C12_1 C14_1 N15_1 C16_1 177.3(14) . . . . ? C14_1 N15_1 C16_1 C17_1 -1(2) . . . . ? C14_1 N15_1 C16_1 C28_1 -176.9(15) . . . . ? N15_1 C16_1 C17_1 C18_1 10(3) . . . . ? C28_1 C16_1 C17_1 C18_1 -173.6(15) . . . . ? C16_1 C17_1 C18_1 O20_1 179.7(16) . . . . ? C16_1 C17_1 C18_1 C19_1 -16(2) . . . . ? N15_1 C14_1 C19_1 C18_1 -6(3) . . . . ? C12_1 C14_1 C19_1 C18_1 175.3(16) . . . . ? O20_1 C18_1 C19_1 C14_1 -179.2(17) . . . . ? C17_1 C18_1 C19_1 C14_1 15(3) . . . . ? C17_1 C18_1 O20_1 C21_1 -13(3) . . . . ? C19_1 C18_1 O20_1 C21_1 -177.4(15) . . . . ? C18_1 O20_1 C21_1 C22_1 -165.5(17) . . . . ? O20_1 C21_1 C22_1 C27_1 27(3) . . . . ? O20_1 C21_1 C22_1 C23_1 -154.5(17) . . . . ? C27_1 C22_1 C23_1 C24_1 0(3) . . . . ? C21_1 C22_1 C23_1 C24_1 -179.2(19) . . . . ? C22_1 C23_1 C24_1 C25_1 -3(3) . . . . ? C23_1 C24_1 C25_1 C26_1 6(3) . . . . ? C24_1 C25_1 C26_1 C27_1 -4(4) . . . . ? C21_1 C22_1 C27_1 C26_1 -180(2) . . . . ? C23_1 C22_1 C27_1 C26_1 2(4) . . . . ? C25_1 C26_1 C27_1 C22_1 1(4) . . . . ? N15_1 C16_1 C28_1 O29_1 166.8(17) . . . . ? C17_1 C16_1 C28_1 O29_1 -10(2) . . . . ? N15_1 C16_1 C28_1 N30_1 -17(2) . . . . ? C17_1 C16_1 C28_1 N30_1 166.9(14) . . . . ? O29_1 C28_1 N30_1 C31_1 -5(3) . . . . ? C16_1 C28_1 N30_1 C31_1 178.5(13) . . . . ? C28_1 N30_1 C31_1 C36_1 14(2) . . . . ? C28_1 N30_1 C31_1 N32_1 -173.1(14) . . . . ? C36_1 C31_1 N32_1 C33_1 -7(2) . . . . ? N30_1 C31_1 N32_1 C33_1 -179.3(12) . . . . ? C31_1 N32_1 C33_1 C34_1 0(2) . . . . ? C31_1 N32_1 C33_1 N37_1 179.6(13) . . . . ? N32_1 C33_1 C34_1 C35_1 5(3) . . . . ? N37_1 C33_1 C34_1 C35_1 -174.0(16) . . . . ? C33_1 C34_1 C35_1 C36_1 -4(2) . . . . ? N32_1 C31_1 C36_1 C35_1 8(2) . . . . ? N30_1 C31_1 C36_1 C35_1 179.2(15) . . . . ? C34_1 C35_1 C36_1 C31_1 -2(2) . . . . ? N32_1 C33_1 N37_1 C38_1 157.0(14) . . . . ? C34_1 C33_1 N37_1 C38_1 -24(2) . . . . ? C33_1 N37_1 C38_1 O39_1 8(3) . . . . ? C33_1 N37_1 C38_1 C40_1 -178.3(15) . . . . ? O39_1 C38_1 C40_1 N41_1 -180(2) . . . . ? N37_1 C38_1 C40_1 N41_1 6(3) . . . . ? O39_1 C38_1 C40_1 C45_1 -12(3) . . . . ? N37_1 C38_1 C40_1 C45_1 173.8(15) . . . . ? C45_1 C40_1 N41_1 C42_1 12(3) . . . . ? C38_1 C40_1 N41_1 C42_1 178.7(17) . . . . ? C40_1 N41_1 C42_1 C43_1 -7(3) . . . . ? C40_1 N41_1 C42_1 C54_1 -176.6(19) . . . . ? N41_1 C42_1 C43_1 C44_1 3(3) . . . . ? C54_1 C42_1 C43_1 C44_1 173.3(17) . . . . ? C42_1 C43_1 C44_1 C45_1 -4(3) . . . . ? C42_1 C43_1 C44_1 O46_1 -173.2(16) . . . . ? C43_1 C44_1 C45_1 C40_1 7(3) . . . . ? O46_1 C44_1 C45_1 C40_1 176.0(17) . . . . ? N41_1 C40_1 C45_1 C44_1 -12(3) . . . . ? C38_1 C40_1 C45_1 C44_1 -179.8(16) . . . . ? C43_1 C44_1 O46_1 C47_1 173.8(17) . . . . ? C45_1 C44_1 O46_1 C47_1 5(3) . . . . ? C44_1 O46_1 C47_1 C48_1 179.7(15) . . . . ? O46_1 C47_1 C48_1 C53_1 -53(3) . . . . ? O46_1 C47_1 C48_1 C49_1 122.9(18) . . . . ? C53_1 C48_1 C49_1 C50_1 -8(3) . . . . ? C47_1 C48_1 C49_1 C50_1 176.6(18) . . . . ? C48_1 C49_1 C50_1 C51_1 6(3) . . . . ? C49_1 C50_1 C51_1 C52_1 -2(3) . . . . ? C50_1 C51_1 C52_1 C53_1 1(4) . . . . ? C49_1 C48_1 C53_1 C52_1 7(4) . . . . ? C47_1 C48_1 C53_1 C52_1 -178(2) . . . . ? C51_1 C52_1 C53_1 C48_1 -3(4) . . . . ? N41_1 C42_1 C54_1 O55_1 -176(2) . . . . ? C43_1 C42_1 C54_1 O55_1 14(3) . . . . ? N41_1 C42_1 C54_1 N56_1 -10(2) . . . . ? C43_1 C42_1 C54_1 N56_1 -179.6(16) . . . . ? O55_1 C54_1 N56_1 C57_1 -14(3) . . . . ? C42_1 C54_1 N56_1 C57_1 -180.0(18) . . . . ? C54_1 N56_1 C57_1 N58_1 -171.9(19) . . . . ? C54_1 N56_1 C57_1 C62_1 9(3) . . . . ? C62_1 C57_1 N58_1 C59_1 0(3) . . . . ? N56_1 C57_1 N58_1 C59_1 -179.6(16) . . . . ? C57_1 N58_1 C59_1 N63_1 176.4(15) . . . . ? C57_1 N58_1 C59_1 C60_1 -1(3) . . . . ? N58_1 C59_1 C60_1 C61_1 4(3) . . . . ? N63_1 C59_1 C60_1 C61_1 -173.8(16) . . . . ? C59_1 C60_1 C61_1 C62_1 -5(3) . . . . ? C60_1 C61_1 C62_1 C57_1 4(3) . . . . ? N58_1 C57_1 C62_1 C61_1 -1(3) . . . . ? N56_1 C57_1 C62_1 C61_1 177.9(18) . . . . ? N58_1 C59_1 N63_1 C64_1 177.1(17) . . . . ? C60_1 C59_1 N63_1 C64_1 -5(3) . . . . ? C59_1 N63_1 C64_1 O65_1 1(3) . . . . ? C59_1 N63_1 C64_1 C66_1 -179.8(15) . . . . ? O65_1 C64_1 C66_1 N67_1 159.9(17) . . . . ? N63_1 C64_1 C66_1 N67_1 -19(2) . . . . ? O65_1 C64_1 C66_1 C71_1 -22(2) . . . . ? N63_1 C64_1 C66_1 C71_1 159.0(15) . . . . ? C71_1 C66_1 N67_1 C68_1 4(2) . . . . ? C64_1 C66_1 N67_1 C68_1 -178.4(15) . . . . ? C66_1 N67_1 C68_1 C69_1 -7(2) . . . . ? C66_1 N67_1 C68_1 C80_1 -177.1(14) . . . . ? N67_1 C68_1 C69_1 C70_1 4(2) . . . . ? C80_1 C68_1 C69_1 C70_1 175.2(13) . . . . ? C68_1 C69_1 C70_1 C71_1 1(2) . . . . ? C68_1 C69_1 C70_1 O72_1 -179.9(14) . . . . ? C69_1 C70_1 C71_1 C66_1 -3(2) . . . . ? O72_1 C70_1 C71_1 C66_1 177.7(14) . . . . ? N67_1 C66_1 C71_1 C70_1 1(2) . . . . ? C64_1 C66_1 C71_1 C70_1 -177.1(14) . . . . ? C69_1 C70_1 O72_1 C73_1 21(3) . . . . ? C71_1 C70_1 O72_1 C73_1 -159.7(18) . . . . ? C70_1 O72_1 C73_1 C74_1 150(2) . . . . ? O72_1 C73_1 C74_1 C79_1 108(3) . . . . ? O72_1 C73_1 C74_1 C75_1 -59(3) . . . . ? C73_1 C74_1 C75_1 C76_1 177(3) . . . . ? C79_1 C74_1 C75_1 C76_1 8(4) . . . . ? C74_1 C75_1 C76_1 C77_1 -13(4) . . . . ? C75_1 C76_1 C77_1 C78_1 10(4) . . . . ? C76_1 C77_1 C78_1 C79_1 -2(6) . . . . ? C77_1 C78_1 C79_1 C74_1 -4(7) . . . . ? C73_1 C74_1 C79_1 C78_1 -164(4) . . . . ? C75_1 C74_1 C79_1 C78_1 2(5) . . . . ? N67_1 C68_1 C80_1 O81_1 177.4(17) . . . . ? C69_1 C68_1 C80_1 O81_1 6(2) . . . . ? N67_1 C68_1 C80_1 N82_1 -7(2) . . . . ? C69_1 C68_1 C80_1 N82_1 -178.5(13) . . . . ? O81_1 C80_1 N82_1 C83_1 -1(3) . . . . ? C68_1 C80_1 N82_1 C83_1 -177.4(15) . . . . ? C80_1 N82_1 C83_1 N84_1 178.5(15) . . . . ? C80_1 N82_1 C83_1 C88_1 2(3) . . . . ? N82_1 C83_1 N84_1 C85_1 -179.7(15) . . . . ? C88_1 C83_1 N84_1 C85_1 -3(2) . . . . ? C83_1 N84_1 C85_1 C86_1 7(3) . . . . ? C83_1 N84_1 C85_1 N89_1 -172.3(16) . . . . ? N89_1 C85_1 C86_1 C87_1 173(2) . . . . ? N84_1 C85_1 C86_1 C87_1 -6(3) . . . . ? C85_1 C86_1 C87_1 C88_1 2(3) . . . . ? C86_1 C87_1 C88_1 C83_1 1(3) . . . . ? N82_1 C83_1 C88_1 C87_1 175.7(17) . . . . ? N84_1 C83_1 C88_1 C87_1 0(2) . . . . ? C86_1 C85_1 N89_1 C90_1 9(4) . . . . ? N84_1 C85_1 N89_1 C90_1 -172.1(19) . . . . ? C85_1 N89_1 C90_1 O91_1 -3(4) . . . . ? C85_1 N89_1 C90_1 C92_1 -170.8(19) . . . . ? O2_2 C3_2 N4_2 C5_2 -5(3) . . . . ? C1_2 C3_2 N4_2 C5_2 175(2) . . . . ? C3_2 N4_2 C5_2 N6_2 -172.7(17) . . . . ? C3_2 N4_2 C5_2 C10_2 3(3) . . . . ? C10_2 C5_2 N6_2 C7_2 6(2) . . . . ? N4_2 C5_2 N6_2 C7_2 -178.5(15) . . . . ? C5_2 N6_2 C7_2 C8_2 -5(3) . . . . ? C5_2 N6_2 C7_2 N11_2 176.0(13) . . . . ? N6_2 C7_2 C8_2 C9_2 1(3) . . . . ? N11_2 C7_2 C8_2 C9_2 179.0(17) . . . . ? C7_2 C8_2 C9_2 C10_2 4(3) . . . . ? C8_2 C9_2 C10_2 C5_2 -3(3) . . . . ? N6_2 C5_2 C10_2 C9_2 -2(2) . . . . ? N4_2 C5_2 C10_2 C9_2 -177.3(17) . . . . ? C8_2 C7_2 N11_2 C12_2 6(3) . . . . ? N6_2 C7_2 N11_2 C12_2 -175.1(17) . . . . ? C7_2 N11_2 C12_2 O13_2 -4(3) . . . . ? C7_2 N11_2 C12_2 C14_2 -179.8(15) . . . . ? O13_2 C12_2 C14_2 N15_2 173.0(17) . . . . ? N11_2 C12_2 C14_2 N15_2 -10(2) . . . . ? O13_2 C12_2 C14_2 C19_2 1(3) . . . . ? N11_2 C12_2 C14_2 C19_2 177.8(16) . . . . ? C19_2 C14_2 N15_2 C16_2 -4(2) . . . . ? C12_2 C14_2 N15_2 C16_2 -176.0(14) . . . . ? C14_2 N15_2 C16_2 C17_2 5(2) . . . . ? C14_2 N15_2 C16_2 C28_2 179.1(15) . . . . ? N15_2 C16_2 C17_2 C18_2 -6(2) . . . . ? C28_2 C16_2 C17_2 C18_2 179.9(16) . . . . ? C16_2 C17_2 C18_2 O20_2 -171.6(15) . . . . ? C16_2 C17_2 C18_2 C19_2 6(2) . . . . ? O20_2 C18_2 C19_2 C14_2 171.8(17) . . . . ? C17_2 C18_2 C19_2 C14_2 -5(2) . . . . ? N15_2 C14_2 C19_2 C18_2 5(3) . . . . ? C12_2 C14_2 C19_2 C18_2 176.7(16) . . . . ? C19_2 C18_2 O20_2 C21_2 -6(3) . . . . ? C17_2 C18_2 O20_2 C21_2 171.4(15) . . . . ? C18_2 O20_2 C21_2 C22_2 -154.6(14) . . . . ? O20_2 C21_2 C22_2 C27_2 65(2) . . . . ? O20_2 C21_2 C22_2 C23_2 -120.1(18) . . . . ? C27_2 C22_2 C23_2 C24_2 0(3) . . . . ? C21_2 C22_2 C23_2 C24_2 -174.6(17) . . . . ? C22_2 C23_2 C24_2 C25_2 1(3) . . . . ? C23_2 C24_2 C25_2 C26_2 -9(4) . . . . ? C24_2 C25_2 C26_2 C27_2 16(5) . . . . ? C23_2 C22_2 C27_2 C26_2 5(3) . . . . ? C21_2 C22_2 C27_2 C26_2 179.2(18) . . . . ? C25_2 C26_2 C27_2 C22_2 -15(4) . . . . ? N15_2 C16_2 C28_2 O29_2 -155.6(18) . . . . ? C17_2 C16_2 C28_2 O29_2 19(3) . . . . ? N15_2 C16_2 C28_2 N30_2 27(2) . . . . ? C17_2 C16_2 C28_2 N30_2 -158.6(15) . . . . ? O29_2 C28_2 N30_2 C31_2 7(3) . . . . ? C16_2 C28_2 N30_2 C31_2 -175.8(14) . . . . ? C28_2 N30_2 C31_2 C36_2 -8(3) . . . . ? C28_2 N30_2 C31_2 N32_2 -178.6(15) . . . . ? C36_2 C31_2 N32_2 C33_2 10(2) . . . . ? N30_2 C31_2 N32_2 C33_2 -177.7(14) . . . . ? C31_2 N32_2 C33_2 C34_2 -9(3) . . . . ? C31_2 N32_2 C33_2 N37_2 178.7(14) . . . . ? N32_2 C33_2 C34_2 C35_2 6(3) . . . . ? N37_2 C33_2 C34_2 C35_2 177.1(16) . . . . ? C33_2 C34_2 C35_2 C36_2 -4(3) . . . . ? N30_2 C31_2 C36_2 C35_2 -180.0(19) . . . . ? N32_2 C31_2 C36_2 C35_2 -10(3) . . . . ? C34_2 C35_2 C36_2 C31_2 7(3) . . . . ? C34_2 C33_2 N37_2 C38_2 7(3) . . . . ? N32_2 C33_2 N37_2 C38_2 -179.6(17) . . . . ? C33_2 N37_2 C38_2 O39_2 -9(3) . . . . ? C33_2 N37_2 C38_2 C40_2 -178.8(15) . . . . ? O39_2 C38_2 C40_2 C45_2 2(3) . . . . ? N37_2 C38_2 C40_2 C45_2 172.0(17) . . . . ? O39_2 C38_2 C40_2 N41_2 179.2(17) . . . . ? N37_2 C38_2 C40_2 N41_2 -11(2) . . . . ? C45_2 C40_2 N41_2 C42_2 -1(3) . . . . ? C38_2 C40_2 N41_2 C42_2 -178.2(14) . . . . ? C40_2 N41_2 C42_2 C43_2 5(2) . . . . ? C40_2 N41_2 C42_2 C54_2 177.9(16) . . . . ? C54_2 C42_2 C43_2 C44_2 179.2(19) . . . . ? N41_2 C42_2 C43_2 C44_2 -8(3) . . . . ? C42_2 C43_2 C44_2 O46_2 -178.4(17) . . . . ? C42_2 C43_2 C44_2 C45_2 8(3) . . . . ? N41_2 C40_2 C45_2 C44_2 1(3) . . . . ? C38_2 C40_2 C45_2 C44_2 177.7(17) . . . . ? O46_2 C44_2 C45_2 C40_2 -178.8(16) . . . . ? C43_2 C44_2 C45_2 C40_2 -4(3) . . . . ? C43_2 C44_2 O46_2 C47_2 13(3) . . . . ? C45_2 C44_2 O46_2 C47_2 -172.5(15) . . . . ? C44_2 O46_2 C47_2 C48_2 169.0(16) . . . . ? O46_2 C47_2 C48_2 C53_2 -123(2) . . . . ? O46_2 C47_2 C48_2 C49_2 66(2) . . . . ? C53_2 C48_2 C49_2 C50_2 1(3) . . . . ? C47_2 C48_2 C49_2 C50_2 173.7(19) . . . . ? C48_2 C49_2 C50_2 C51_2 5(3) . . . . ? C49_2 C50_2 C51_2 C52_2 -5(4) . . . . ? C50_2 C51_2 C52_2 C53_2 -2(3) . . . . ? C49_2 C48_2 C53_2 C52_2 -8(3) . . . . ? C47_2 C48_2 C53_2 C52_2 179.4(17) . . . . ? C51_2 C52_2 C53_2 C48_2 9(3) . . . . ? C43_2 C42_2 C54_2 O55_2 -6(3) . . . . ? N41_2 C42_2 C54_2 O55_2 -179.3(18) . . . . ? C43_2 C42_2 C54_2 N56_2 -176.8(18) . . . . ? N41_2 C42_2 C54_2 N56_2 10(3) . . . . ? O55_2 C54_2 N56_2 C57_2 5(3) . . . . ? C42_2 C54_2 N56_2 C57_2 176.0(19) . . . . ? C54_2 N56_2 C57_2 N58_2 -165(2) . . . . ? C54_2 N56_2 C57_2 C62_2 21(3) . . . . ? C62_2 C57_2 N58_2 C59_2 -10(3) . . . . ? N56_2 C57_2 N58_2 C59_2 176.4(16) . . . . ? C57_2 N58_2 C59_2 N63_2 -174.6(15) . . . . ? C57_2 N58_2 C59_2 C60_2 4(3) . . . . ? N58_2 C59_2 C60_2 C61_2 -3(3) . . . . ? N63_2 C59_2 C60_2 C61_2 175.8(16) . . . . ? C59_2 C60_2 C61_2 C62_2 8(3) . . . . ? C60_2 C61_2 C62_2 C57_2 -13(3) . . . . ? N58_2 C57_2 C62_2 C61_2 14(3) . . . . ? N56_2 C57_2 C62_2 C61_2 -173.1(18) . . . . ? N58_2 C59_2 N63_2 C64_2 175.4(16) . . . . ? C60_2 C59_2 N63_2 C64_2 -3(3) . . . . ? C59_2 N63_2 C64_2 O65_2 -2(3) . . . . ? C59_2 N63_2 C64_2 C66_2 175.2(15) . . . . ? O65_2 C64_2 C66_2 C71_2 12(2) . . . . ? N63_2 C64_2 C66_2 C71_2 -164.9(15) . . . . ? O65_2 C64_2 C66_2 N67_2 -164.5(14) . . . . ? N63_2 C64_2 C66_2 N67_2 18(2) . . . . ? C71_2 C66_2 N67_2 C68_2 1(2) . . . . ? C64_2 C66_2 N67_2 C68_2 177.1(13) . . . . ? C66_2 N67_2 C68_2 C69_2 -2(2) . . . . ? C66_2 N67_2 C68_2 C80_2 -179.1(13) . . . . ? N67_2 C68_2 C69_2 C70_2 0(2) . . . . ? C80_2 C68_2 C69_2 C70_2 177.5(14) . . . . ? C68_2 C69_2 C70_2 O72_2 176.7(14) . . . . ? C68_2 C69_2 C70_2 C71_2 3(2) . . . . ? N67_2 C66_2 C71_2 C70_2 2(2) . . . . ? C64_2 C66_2 C71_2 C70_2 -174.4(14) . . . . ? C69_2 C70_2 C71_2 C66_2 -4(2) . . . . ? O72_2 C70_2 C71_2 C66_2 -177.6(14) . . . . ? C69_2 C70_2 O72_2 C73_2 -171.0(17) . . . . ? C71_2 C70_2 O72_2 C73_2 3(2) . . . . ? C70_2 O72_2 C73_2 C74_2 173.5(14) . . . . ? O72_2 C73_2 C74_2 C79_2 146.8(19) . . . . ? O72_2 C73_2 C74_2 C75_2 -36(2) . . . . ? C79_2 C74_2 C75_2 C76_2 2(3) . . . . ? C73_2 C74_2 C75_2 C76_2 -175(2) . . . . ? C74_2 C75_2 C76_2 C77_2 0(3) . . . . ? C75_2 C76_2 C77_2 C78_2 -4(4) . . . . ? C76_2 C77_2 C78_2 C79_2 5(4) . . . . ? C75_2 C74_2 C79_2 C78_2 -1(3) . . . . ? C73_2 C74_2 C79_2 C78_2 176.0(18) . . . . ? C77_2 C78_2 C79_2 C74_2 -2(3) . . . . ? N67_2 C68_2 C80_2 O81_2 178.4(15) . . . . ? C69_2 C68_2 C80_2 O81_2 1(2) . . . . ? N67_2 C68_2 C80_2 N82_2 -9(2) . . . . ? C69_2 C68_2 C80_2 N82_2 173.8(15) . . . . ? O81_2 C80_2 N82_2 C83_2 -13(3) . . . . ? C68_2 C80_2 N82_2 C83_2 174.9(15) . . . . ? C80_2 N82_2 C83_2 C88_2 22(3) . . . . ? C80_2 N82_2 C83_2 N84_2 -165.1(15) . . . . ? C88_2 C83_2 N84_2 C85_2 -3(3) . . . . ? N82_2 C83_2 N84_2 C85_2 -175.7(15) . . . . ? C83_2 N84_2 C85_2 C86_2 -1(3) . . . . ? C83_2 N84_2 C85_2 N89_2 -177.6(14) . . . . ? N84_2 C85_2 C86_2 C87_2 7(3) . . . . ? N89_2 C85_2 C86_2 C87_2 -177.1(18) . . . . ? C85_2 C86_2 C87_2 C88_2 -9(3) . . . . ? N84_2 C83_2 C88_2 C87_2 1(3) . . . . ? N82_2 C83_2 C88_2 C87_2 172.5(16) . . . . ? C86_2 C87_2 C88_2 C83_2 6(3) . . . . ? N84_2 C85_2 N89_2 C90_2 176.7(17) . . . . ? C86_2 C85_2 N89_2 C90_2 0(3) . . . . ? C85_2 N89_2 C90_2 O91_2 -2(3) . . . . ? C85_2 N89_2 C90_2 C92_2 -169(2) . . . . ? _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 59.94 _diffrn_measured_fraction_theta_full 0.870 _refine_diff_density_max 0.785 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.117 #===END data_2B _database_code_CSD 176830 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H53 N15 O16' _chemical_formula_weight 1108.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.1333(19) _cell_length_b 25.805(3) _cell_length_c 14.0503(19) _cell_angle_alpha 90.00 _cell_angle_beta 98.046(3) _cell_angle_gamma 90.00 _cell_volume 5073.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6148 _cell_measurement_theta_min 2.368 _cell_measurement_theta_max 25.206 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22683 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 24.71 _reflns_number_total 7312 _reflns_number_gt 4529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+6.6494P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7312 _refine_ls_number_parameters 760 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1403 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6686(3) 0.52760(19) 0.4636(4) 0.0568(15) Uani 1 1 d . . . H1A H 0.6568 0.5207 0.3943 0.085 Uiso 1 1 calc R . . H1B H 0.6779 0.5649 0.4744 0.085 Uiso 1 1 calc R . . H1C H 0.6138 0.5158 0.4935 0.085 Uiso 1 1 calc R . . C2 C 0.7564(3) 0.4992(2) 0.5070(4) 0.0447(13) Uani 1 1 d . . . C3 C 0.9191(3) 0.51681(16) 0.5932(3) 0.0333(11) Uani 1 1 d . . . C4 C 0.9551(3) 0.46681(16) 0.5989(3) 0.0406(12) Uani 1 1 d . . . H4 H 0.9168 0.4382 0.5748 0.049 Uiso 1 1 calc R . . C5 C 1.0471(3) 0.46012(17) 0.6401(3) 0.0420(13) Uani 1 1 d . . . H5 H 1.0731 0.4261 0.6455 0.050 Uiso 1 1 calc R . . C6 C 1.1039(3) 0.50137(15) 0.6744(3) 0.0361(12) Uani 1 1 d . . . H6 H 1.1689 0.4968 0.7011 0.043 Uiso 1 1 calc R . . C7 C 1.0613(3) 0.54964(15) 0.6678(3) 0.0324(11) Uani 1 1 d . . . C8 C 1.2010(3) 0.60306(17) 0.7365(3) 0.0348(11) Uani 1 1 d . . . C9 C 1.2245(3) 0.65891(16) 0.7586(3) 0.0328(11) Uani 1 1 d . . . C10 C 1.3165(3) 0.67263(17) 0.7939(4) 0.0415(13) Uani 1 1 d . . . H10 H 1.3647 0.6470 0.8075 0.050 Uiso 1 1 calc R . . C11 C 1.3381(3) 0.72520(18) 0.8097(4) 0.0488(14) Uani 1 1 d . . . C12 C 1.2654(3) 0.76043(18) 0.7879(4) 0.0487(14) Uani 1 1 d . . . H12 H 1.2779 0.7965 0.7953 0.058 Uiso 1 1 calc R . . C13 C 1.1752(3) 0.74352(16) 0.7555(4) 0.0363(12) Uani 1 1 d . . . C14 C 1.0957(3) 0.78191(17) 0.7349(4) 0.0399(12) Uani 1 1 d . . . C15 C 0.9193(3) 0.78699(15) 0.7070(3) 0.0307(11) Uani 1 1 d . . . C16 C 0.9094(3) 0.84133(15) 0.7072(3) 0.0373(12) Uani 1 1 d . . . H16 H 0.9636 0.8635 0.7146 0.045 Uiso 1 1 calc R . . C17 C 0.8198(3) 0.86060(16) 0.6964(3) 0.0383(12) Uani 1 1 d . . . H17 H 0.8114 0.8971 0.6951 0.046 Uiso 1 1 calc R . . C18 C 0.7397(3) 0.82929(15) 0.6872(3) 0.0361(12) Uani 1 1 d . . . H18 H 0.6768 0.8431 0.6815 0.043 Uiso 1 1 calc R . . C19 C 0.7569(3) 0.77608(15) 0.6866(3) 0.0318(11) Uani 1 1 d . . . C20 C 0.5887(3) 0.74442(16) 0.6530(4) 0.0374(12) Uani 1 1 d . . . C21 C 0.5356(3) 0.69421(15) 0.6431(3) 0.0350(12) Uani 1 1 d . . . C22 C 0.4414(3) 0.69312(15) 0.6023(3) 0.0369(12) Uani 1 1 d . . . H22 H 0.4078 0.7243 0.5842 0.044 Uiso 1 1 calc R . . C23 C 0.3963(3) 0.64493(16) 0.5882(4) 0.0380(12) Uani 1 1 d . . . C24 C 0.4485(3) 0.60101(16) 0.6182(4) 0.0383(12) Uani 1 1 d . . . H24 H 0.4195 0.5677 0.6119 0.046 Uiso 1 1 calc R . . C25 C 0.5420(2) 0.60616(15) 0.6572(3) 0.0335(12) Uani 1 1 d . . . C26 C 0.5964(3) 0.55635(16) 0.6872(4) 0.0374(12) Uani 1 1 d . . . C27 C 0.7516(3) 0.52343(15) 0.7645(3) 0.0321(11) Uani 1 1 d . . . C28 C 0.7291(3) 0.47107(16) 0.7524(4) 0.0419(13) Uani 1 1 d . . . H28 H 0.6674 0.4602 0.7236 0.050 Uiso 1 1 calc R . . C29 C 0.7993(3) 0.43569(16) 0.7836(4) 0.0413(13) Uani 1 1 d . . . H29 H 0.7866 0.3997 0.7757 0.050 Uiso 1 1 calc R . . C30 C 0.8879(3) 0.45209(15) 0.8262(3) 0.0377(12) Uani 1 1 d . . . H30 H 0.9370 0.4280 0.8484 0.045 Uiso 1 1 calc R . . C31 C 0.9026(3) 0.50452(15) 0.8353(3) 0.0314(11) Uani 1 1 d . . . C32 C 1.0734(3) 0.50091(16) 0.9068(3) 0.0334(11) Uani 1 1 d . . . C33 C 1.1559(3) 0.53444(16) 0.9474(3) 0.0336(11) Uani 1 1 d . . . C34 C 1.2416(3) 0.51069(16) 0.9787(3) 0.0382(12) Uani 1 1 d . . . H34 H 1.2472 0.4741 0.9741 0.046 Uiso 1 1 calc R . . C35 C 1.3194(3) 0.53990(17) 1.0169(4) 0.0423(13) Uani 1 1 d . . . C36 C 1.3064(3) 0.59375(17) 1.0227(4) 0.0410(12) Uani 1 1 d . . . H36 H 1.3578 0.6156 1.0481 0.049 Uiso 1 1 calc R . . C37 C 1.2178(3) 0.61414(16) 0.9910(3) 0.0338(11) Uani 1 1 d . . . C38 C 1.2040(3) 0.67169(16) 1.0010(3) 0.0356(11) Uani 1 1 d . . . C39 C 1.0733(3) 0.73678(15) 0.9771(3) 0.0315(11) Uani 1 1 d . . . C40 C 1.1275(3) 0.78073(16) 0.9988(3) 0.0376(12) Uani 1 1 d . . . H40 H 1.1952 0.7793 1.0118 0.045 Uiso 1 1 calc R . . C41 C 1.0789(3) 0.82674(16) 1.0010(3) 0.0372(12) Uani 1 1 d . . . H41 H 1.1138 0.8580 1.0135 0.045 Uiso 1 1 calc R . . C42 C 0.9809(3) 0.82832(16) 0.9854(3) 0.0361(12) Uani 1 1 d . . . H42 H 0.9472 0.8599 0.9898 0.043 Uiso 1 1 calc R . . C43 C 0.9329(3) 0.78216(16) 0.9629(3) 0.0328(11) Uani 1 1 d . . . C44 C 0.7653(3) 0.81194(19) 0.9598(4) 0.0435(13) Uani 1 1 d . . . C45 C 0.6657(3) 0.7948(2) 0.9247(4) 0.0537(15) Uani 1 1 d . . . H45A H 0.6229 0.8070 0.9692 0.081 Uiso 1 1 calc R . . H45B H 0.6635 0.7569 0.9214 0.081 Uiso 1 1 calc R . . H45C H 0.6453 0.8093 0.8607 0.081 Uiso 1 1 calc R . . N1 N 0.8275(2) 0.53034(13) 0.5493(3) 0.0381(10) Uani 1 1 d . . . H1 H 0.8141 0.5636 0.5489 0.046 Uiso 1 1 calc R . . N2 N 0.9708(2) 0.55766(12) 0.6275(3) 0.0328(9) Uani 1 1 d . . . N3 N 1.1077(2) 0.59521(12) 0.7019(3) 0.0332(9) Uani 1 1 d . . . H3 H 1.0710 0.6228 0.7007 0.040 Uiso 1 1 calc R . . N4 N 1.1523(2) 0.69310(13) 0.7410(3) 0.0329(9) Uani 1 1 d . . . N5 N 1.0067(2) 0.76140(13) 0.7202(3) 0.0361(10) Uani 1 1 d . . . H5A H 1.0038 0.7273 0.7188 0.043 Uiso 1 1 calc R . . N6 N 0.8438(2) 0.75543(12) 0.6957(3) 0.0321(9) Uani 1 1 d . . . N7 N 0.6838(2) 0.73918(13) 0.6775(3) 0.0391(10) Uani 1 1 d . . . H7 H 0.7032 0.7072 0.6898 0.047 Uiso 1 1 calc R . . N8 N 0.5880(2) 0.65099(12) 0.6701(3) 0.0333(9) Uani 1 1 d . . . N9 N 0.6863(2) 0.56313(12) 0.7331(3) 0.0357(10) Uani 1 1 d . . . H9 H 0.7056 0.5952 0.7444 0.043 Uiso 1 1 calc R . . N10 N 0.8369(2) 0.54060(12) 0.8049(3) 0.0311(9) Uani 1 1 d . . . N11 N 0.9901(2) 0.52629(12) 0.8776(3) 0.0317(9) Uani 1 1 d . . . H11 H 0.9907 0.5601 0.8861 0.038 Uiso 1 1 calc R . . N12 N 1.1418(2) 0.58607(13) 0.9524(3) 0.0326(9) Uani 1 1 d . . . N13 N 1.1124(2) 0.68721(12) 0.9737(3) 0.0358(10) Uani 1 1 d . . . H13 H 1.0723 0.6627 0.9507 0.043 Uiso 1 1 calc R . . N14 N 0.9782(2) 0.73685(12) 0.9586(3) 0.0334(9) Uani 1 1 d . . . N15 N 0.8341(2) 0.77744(13) 0.9405(3) 0.0376(10) Uani 1 1 d . . . H15 H 0.8133 0.7489 0.9103 0.045 Uiso 1 1 calc R . . O1 O 0.7637(2) 0.45182(12) 0.5037(3) 0.0521(10) Uani 1 1 d . . . O2 O 1.26218(19) 0.56936(11) 0.7476(2) 0.0455(9) Uani 1 1 d . . . O3 O 1.4274(2) 0.74205(13) 0.8419(3) 0.0737(13) Uani 1 1 d . . . H3A H 1.4575 0.7188 0.8753 0.111 Uiso 1 1 calc R . . O4 O 1.1122(2) 0.82809(12) 0.7336(3) 0.0668(12) Uani 1 1 d . . . O5 O 0.5479(2) 0.78618(11) 0.6381(3) 0.0569(11) Uani 1 1 d . . . O6 O 0.30555(18) 0.64306(11) 0.5456(3) 0.0501(10) Uani 1 1 d . . . H6A H 0.2868 0.6121 0.5424 0.075 Uiso 1 1 calc R . . O7 O 0.5577(2) 0.51511(11) 0.6668(3) 0.0533(10) Uani 1 1 d . . . O8 O 1.08346(19) 0.45397(11) 0.9026(2) 0.0441(9) Uani 1 1 d . . . O9 O 1.4014(2) 0.51571(12) 1.0467(3) 0.0586(11) Uani 1 1 d . . . H9A H 1.4383 0.5359 1.0810 0.088 Uiso 1 1 calc R . . O10 O 1.2697(2) 0.70010(12) 1.0320(3) 0.0523(10) Uani 1 1 d . . . O11 O 0.7843(2) 0.85282(13) 1.0023(3) 0.0629(11) Uani 1 1 d . . . O12 O 0.7811(2) 0.66969(13) 0.8578(3) 0.0544(10) Uani 1 1 d . . . H12A H 0.8261 0.6644 0.8258 0.082 Uiso 1 1 calc R . . C46 C 0.8016(4) 0.64473(19) 0.9490(4) 0.0571(15) Uani 1 1 d . . . H46A H 0.8651 0.6553 0.9801 0.086 Uiso 1 1 calc R . . H46B H 0.8003 0.6071 0.9400 0.086 Uiso 1 1 calc R . . H46C H 0.7536 0.6547 0.9896 0.086 Uiso 1 1 calc R . . O13 O 0.9124(3) 0.65163(13) 0.7248(3) 0.0627(11) Uani 1 1 d D . . H13A H 0.871(4) 0.669(2) 0.677(4) 0.075 Uiso 1 1 d D . . H13B H 0.848(3) 0.644(2) 0.728(4) 0.075 Uiso 1 1 d D . . O14 O 0.5349(2) 0.57395(15) 0.1427(3) 0.0677(11) Uani 1 1 d D . . H14 H 0.5140 0.5939 0.1821 0.102 Uiso 1 1 calc R . . C47 C 0.6004(4) 0.5384(2) 0.1931(5) 0.0753(19) Uani 1 1 d D . . H47A H 0.6554 0.5573 0.2264 0.113 Uiso 1 1 calc R . . H47B H 0.6222 0.5139 0.1474 0.113 Uiso 1 1 calc R . . H47C H 0.5688 0.5193 0.2401 0.113 Uiso 1 1 calc R . . C48 C 0.4445(4) 0.8727(2) 0.8571(5) 0.0747(19) Uani 1 1 d DU . . H48A H 0.4625 0.8473 0.9083 0.112 Uiso 0.56(5) 1 calc PR A 1 H48B H 0.3747 0.8737 0.8414 0.112 Uiso 0.56(5) 1 calc PR A 1 H48C H 0.4680 0.9070 0.8789 0.112 Uiso 0.56(5) 1 calc PR A 1 H48D H 0.4663 0.8422 0.8957 0.112 Uiso 0.44(5) 1 calc PR A 2 H48E H 0.3775 0.8798 0.8634 0.112 Uiso 0.44(5) 1 calc PR A 2 H48F H 0.4837 0.9027 0.8799 0.112 Uiso 0.44(5) 1 calc PR A 2 O15 O 0.485(2) 0.8583(8) 0.7741(13) 0.106(7) Uani 0.56(5) 1 d PDU A 1 H15A H 0.4605 0.8305 0.7518 0.159 Uiso 0.56(5) 1 calc PR A 1 O15' O 0.453(2) 0.8633(7) 0.7610(12) 0.068(6) Uani 0.44(5) 1 d PDU A 2 H15' H 0.4590 0.8916 0.7329 0.102 Uiso 0.44(5) 1 calc PR A 2 C49 C 0.5485(4) 0.6194(2) 0.9276(5) 0.083(2) Uani 1 1 d DU . . H49A H 0.5945 0.6056 0.9802 0.124 Uiso 0.695(15) 1 calc PR B 1 H49B H 0.5766 0.6184 0.8677 0.124 Uiso 0.695(15) 1 calc PR B 1 H49C H 0.4903 0.5984 0.9206 0.124 Uiso 0.695(15) 1 calc PR B 1 H49D H 0.6028 0.6126 0.9775 0.124 Uiso 0.305(15) 1 calc PR B 2 H49E H 0.5422 0.5911 0.8808 0.124 Uiso 0.305(15) 1 calc PR B 2 H49F H 0.4899 0.6221 0.9572 0.124 Uiso 0.305(15) 1 calc PR B 2 O16 O 0.5265(5) 0.6698(2) 0.9478(7) 0.072(3) Uani 0.695(15) 1 d PDU B 1 H16A H 0.5438 0.6758 1.0064 0.108 Uiso 0.695(15) 1 calc PR B 1 O16' O 0.5646(9) 0.6687(5) 0.8785(15) 0.068(7) Uani 0.305(15) 1 d PDU B 2 H16' H 0.5117 0.6815 0.8555 0.102 Uiso 0.305(15) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.051(3) 0.049(3) 0.068(5) -0.007(3) -0.002(3) -0.010(2) C2 0.050(3) 0.045(3) 0.042(4) -0.004(3) 0.014(2) -0.012(2) C3 0.042(2) 0.030(3) 0.030(3) -0.003(2) 0.010(2) -0.0089(19) C4 0.056(3) 0.028(3) 0.039(4) -0.004(2) 0.011(2) -0.011(2) C5 0.060(3) 0.029(3) 0.038(4) 0.000(2) 0.009(2) 0.005(2) C6 0.041(2) 0.026(2) 0.042(4) 0.002(2) 0.008(2) 0.0000(18) C7 0.041(2) 0.026(2) 0.033(3) -0.001(2) 0.011(2) -0.0053(18) C8 0.039(2) 0.035(3) 0.031(4) 0.003(2) 0.005(2) -0.0018(19) C9 0.041(2) 0.033(3) 0.025(3) -0.002(2) 0.0074(19) -0.0029(18) C10 0.041(2) 0.036(3) 0.046(4) -0.002(2) 0.002(2) 0.001(2) C11 0.034(2) 0.043(3) 0.067(4) -0.009(3) 0.002(2) -0.008(2) C12 0.040(2) 0.034(3) 0.073(4) -0.013(3) 0.007(2) -0.007(2) C13 0.038(2) 0.028(3) 0.044(4) 0.001(2) 0.013(2) -0.0071(18) C14 0.041(2) 0.023(3) 0.057(4) 0.000(2) 0.011(2) -0.0098(18) C15 0.032(2) 0.029(2) 0.031(3) -0.001(2) 0.0061(18) -0.0033(17) C16 0.040(2) 0.026(2) 0.046(4) 0.000(2) 0.006(2) -0.0078(18) C17 0.044(2) 0.021(2) 0.051(4) 0.000(2) 0.009(2) -0.0011(18) C18 0.040(2) 0.026(2) 0.042(4) 0.002(2) 0.005(2) -0.0033(18) C19 0.037(2) 0.026(2) 0.032(3) 0.004(2) 0.0040(19) -0.0071(18) C20 0.037(2) 0.027(3) 0.047(4) 0.002(2) 0.004(2) 0.0000(19) C21 0.031(2) 0.025(2) 0.050(4) 0.003(2) 0.009(2) 0.0008(17) C22 0.031(2) 0.024(2) 0.057(4) 0.002(2) 0.009(2) 0.0035(17) C23 0.026(2) 0.032(3) 0.055(4) -0.002(2) 0.005(2) -0.0001(17) C24 0.032(2) 0.027(2) 0.056(4) -0.002(2) 0.008(2) -0.0034(17) C25 0.029(2) 0.021(2) 0.052(4) -0.001(2) 0.010(2) -0.0017(16) C26 0.034(2) 0.024(3) 0.054(4) 0.002(2) 0.008(2) -0.0011(18) C27 0.034(2) 0.027(2) 0.037(4) 0.001(2) 0.010(2) 0.0004(17) C28 0.035(2) 0.026(3) 0.064(4) -0.005(2) 0.007(2) 0.0010(18) C29 0.048(3) 0.021(2) 0.056(4) -0.003(2) 0.010(2) -0.0012(18) C30 0.039(2) 0.024(3) 0.052(4) 0.002(2) 0.013(2) 0.0074(18) C31 0.037(2) 0.027(3) 0.032(3) 0.001(2) 0.013(2) 0.0018(18) C32 0.037(2) 0.027(3) 0.037(4) 0.001(2) 0.011(2) 0.0072(18) C33 0.034(2) 0.034(3) 0.035(3) 0.006(2) 0.012(2) 0.0061(18) C34 0.044(2) 0.027(2) 0.044(4) 0.004(2) 0.011(2) 0.0108(19) C35 0.034(2) 0.037(3) 0.055(4) 0.005(2) 0.004(2) 0.0091(19) C36 0.034(2) 0.043(3) 0.047(4) 0.000(2) 0.006(2) 0.0042(19) C37 0.037(2) 0.035(3) 0.030(3) 0.005(2) 0.010(2) 0.0039(18) C38 0.037(2) 0.034(3) 0.036(4) 0.002(2) 0.007(2) 0.0018(19) C39 0.039(2) 0.027(2) 0.029(3) -0.001(2) 0.0038(19) 0.0009(18) C40 0.038(2) 0.033(3) 0.041(4) -0.002(2) 0.004(2) -0.0003(19) C41 0.047(2) 0.025(2) 0.041(4) -0.005(2) 0.012(2) -0.0045(18) C42 0.042(2) 0.022(2) 0.045(4) -0.002(2) 0.008(2) 0.0017(18) C43 0.036(2) 0.032(3) 0.030(3) -0.002(2) 0.0024(19) 0.0047(18) C44 0.044(3) 0.043(3) 0.044(4) 0.008(3) 0.009(2) 0.009(2) C45 0.037(2) 0.061(3) 0.064(5) 0.006(3) 0.010(2) 0.010(2) N1 0.041(2) 0.028(2) 0.046(3) -0.0041(18) 0.0096(18) -0.0116(15) N2 0.0392(19) 0.030(2) 0.031(3) -0.0017(17) 0.0082(17) -0.0049(15) N3 0.0346(18) 0.024(2) 0.040(3) -0.0013(17) 0.0034(16) 0.0003(14) N4 0.0366(18) 0.031(2) 0.032(3) 0.0037(18) 0.0064(16) -0.0023(15) N5 0.0386(19) 0.0220(19) 0.048(3) -0.0046(18) 0.0082(17) -0.0059(14) N6 0.0357(18) 0.0209(19) 0.039(3) 0.0001(17) 0.0043(16) -0.0053(14) N7 0.0334(18) 0.0213(19) 0.061(3) 0.0020(18) 0.0020(18) -0.0019(14) N8 0.0302(17) 0.028(2) 0.043(3) -0.0016(18) 0.0096(16) -0.0028(15) N9 0.0304(17) 0.0198(19) 0.056(3) 0.0021(18) 0.0031(17) 0.0010(13) N10 0.0314(17) 0.0237(19) 0.040(3) 0.0011(17) 0.0099(16) 0.0023(14) N11 0.0341(18) 0.0211(19) 0.041(3) 0.0014(17) 0.0092(16) 0.0048(14) N12 0.0358(18) 0.027(2) 0.036(3) 0.0037(17) 0.0089(16) 0.0039(15) N13 0.0330(18) 0.024(2) 0.050(3) -0.0045(18) 0.0048(17) 0.0002(14) N14 0.0350(18) 0.026(2) 0.038(3) -0.0059(17) 0.0034(16) 0.0033(14) N15 0.0368(18) 0.026(2) 0.050(3) -0.0033(18) 0.0046(17) 0.0032(14) O1 0.0563(19) 0.033(2) 0.065(3) -0.0024(18) 0.0033(17) -0.0172(15) O2 0.0422(17) 0.0344(18) 0.059(3) 0.0007(16) 0.0021(15) 0.0031(14) O3 0.0386(18) 0.053(2) 0.122(4) -0.019(2) -0.013(2) -0.0073(16) O4 0.0410(17) 0.032(2) 0.126(4) 0.006(2) 0.0069(19) -0.0076(14) O5 0.0408(17) 0.0265(18) 0.101(3) 0.0046(18) -0.0003(17) -0.0013(14) O6 0.0314(15) 0.0273(17) 0.088(3) -0.0067(18) -0.0025(16) -0.0026(12) O7 0.0400(16) 0.0200(17) 0.096(3) -0.0042(17) -0.0028(17) -0.0025(13) O8 0.0435(16) 0.0272(18) 0.061(3) -0.0034(16) 0.0048(15) 0.0102(13) O9 0.0374(17) 0.047(2) 0.088(3) -0.001(2) -0.0058(18) 0.0134(15) O10 0.0379(16) 0.043(2) 0.072(3) -0.0062(18) -0.0043(16) -0.0020(15) O11 0.0528(19) 0.040(2) 0.097(4) -0.021(2) 0.0136(19) 0.0108(16) O12 0.057(2) 0.052(2) 0.053(3) 0.009(2) 0.0022(17) -0.0019(16) C46 0.072(3) 0.045(3) 0.058(5) 0.003(3) 0.019(3) -0.005(2) O13 0.071(2) 0.040(2) 0.077(4) 0.002(2) 0.011(2) 0.0065(17) O14 0.056(2) 0.080(3) 0.065(3) 0.003(2) -0.001(2) 0.0011(18) C47 0.049(3) 0.102(5) 0.072(5) 0.020(4) 0.001(3) 0.004(3) C48 0.069(4) 0.058(4) 0.098(6) 0.012(4) 0.014(4) 0.017(3) O15 0.151(16) 0.095(13) 0.069(8) 0.011(6) 0.006(8) 0.052(10) O15' 0.098(14) 0.015(6) 0.098(10) -0.003(7) 0.042(10) -0.005(7) C49 0.070(4) 0.094(5) 0.086(6) 0.019(4) 0.019(4) 0.015(3) O16 0.077(4) 0.077(4) 0.061(7) -0.024(4) 0.008(4) 0.008(3) O16' 0.051(8) 0.069(8) 0.083(17) -0.001(7) 0.006(8) 0.014(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.496(6) . ? C2 O1 1.228(5) . ? C2 N1 1.357(5) . ? C3 N2 1.334(5) . ? C3 C4 1.385(6) . ? C3 N1 1.398(5) . ? C4 C5 1.359(6) . ? C5 C6 1.379(6) . ? C6 C7 1.381(5) . ? C7 N2 1.340(5) . ? C7 N3 1.398(5) . ? C8 O2 1.221(5) . ? C8 N3 1.356(5) . ? C8 C9 1.502(6) . ? C9 N4 1.345(5) . ? C9 C10 1.372(6) . ? C10 C11 1.401(6) . ? C11 O3 1.351(5) . ? C11 C12 1.375(6) . ? C12 C13 1.364(6) . ? C13 N4 1.349(5) . ? C13 C14 1.496(6) . ? C14 O4 1.215(5) . ? C14 N5 1.354(5) . ? C15 N6 1.334(5) . ? C15 N5 1.389(5) . ? C15 C16 1.409(6) . ? C16 C17 1.349(5) . ? C17 C18 1.382(5) . ? C18 C19 1.395(5) . ? C19 N6 1.328(5) . ? C19 N7 1.397(5) . ? C20 O5 1.227(5) . ? C20 N7 1.347(5) . ? C20 C21 1.494(6) . ? C21 N8 1.363(5) . ? C21 C22 1.375(5) . ? C22 C23 1.399(5) . ? C23 O6 1.338(5) . ? C23 C24 1.386(6) . ? C24 C25 1.365(5) . ? C25 N8 1.327(5) . ? C25 C26 1.526(5) . ? C26 O7 1.212(5) . ? C26 N9 1.353(5) . ? C27 N10 1.334(5) . ? C27 C28 1.393(6) . ? C27 N9 1.408(5) . ? C28 C29 1.374(6) . ? C29 C30 1.377(6) . ? C30 C31 1.372(5) . ? C31 N10 1.342(5) . ? C31 N11 1.411(5) . ? C32 O8 1.222(5) . ? C32 N11 1.360(5) . ? C32 C33 1.498(6) . ? C33 N12 1.350(5) . ? C33 C34 1.374(5) . ? C34 C35 1.379(6) . ? C35 O9 1.331(5) . ? C35 C36 1.406(6) . ? C36 C37 1.374(5) . ? C37 N12 1.345(5) . ? C37 C38 1.507(6) . ? C38 O10 1.215(5) . ? C38 N13 1.358(5) . ? C39 N14 1.333(5) . ? C39 C40 1.379(5) . ? C39 N13 1.397(5) . ? C40 C41 1.374(6) . ? C41 C42 1.372(5) . ? C42 C43 1.385(6) . ? C43 N14 1.338(5) . ? C43 N15 1.393(5) . ? C44 O11 1.224(5) . ? C44 N15 1.373(5) . ? C44 C45 1.491(6) . ? O12 C46 1.427(6) . ? O14 C47 1.420(6) . ? C48 O15' 1.393(12) . ? C48 O15 1.422(12) . ? C49 O16 1.374(7) . ? C49 O16' 1.478(12) . ? 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 C2 N1 123.1(4) . . ? O1 C2 C1 122.8(4) . . ? N1 C2 C1 114.1(4) . . ? N2 C3 C4 122.4(4) . . ? N2 C3 N1 112.9(4) . . ? C4 C3 N1 124.6(4) . . ? C5 C4 C3 117.7(4) . . ? C4 C5 C6 121.8(4) . . ? C5 C6 C7 116.5(4) . . ? N2 C7 C6 123.3(4) . . ? N2 C7 N3 112.9(3) . . ? C6 C7 N3 123.9(4) . . ? O2 C8 N3 125.1(4) . . ? O2 C8 C9 121.7(4) . . ? N3 C8 C9 113.2(3) . . ? N4 C9 C10 123.6(4) . . ? N4 C9 C8 116.8(3) . . ? C10 C9 C8 119.6(4) . . ? C9 C10 C11 118.8(4) . . ? O3 C11 C12 119.8(4) . . ? O3 C11 C10 122.5(4) . . ? C12 C11 C10 117.7(4) . . ? C13 C12 C11 119.9(4) . . ? N4 C13 C12 123.5(4) . . ? N4 C13 C14 116.9(3) . . ? C12 C13 C14 119.6(4) . . ? O4 C14 N5 123.9(4) . . ? O4 C14 C13 120.8(4) . . ? N5 C14 C13 115.3(4) . . ? N6 C15 N5 114.0(3) . . ? N6 C15 C16 122.0(3) . . ? N5 C15 C16 124.0(3) . . ? C17 C16 C15 117.3(4) . . ? C16 C17 C18 122.6(4) . . ? C17 C18 C19 115.7(4) . . ? N6 C19 C18 123.7(3) . . ? N6 C19 N7 113.4(3) . . ? C18 C19 N7 122.9(4) . . ? O5 C20 N7 124.1(4) . . ? O5 C20 C21 121.9(4) . . ? N7 C20 C21 114.0(3) . . ? N8 C21 C22 123.8(4) . . ? N8 C21 C20 116.0(3) . . ? C22 C21 C20 120.1(4) . . ? C21 C22 C23 118.2(4) . . ? O6 C23 C24 122.9(4) . . ? O6 C23 C22 119.0(4) . . ? C24 C23 C22 118.1(4) . . ? C25 C24 C23 119.1(4) . . ? N8 C25 C24 124.6(4) . . ? N8 C25 C26 118.6(3) . . ? C24 C25 C26 116.8(3) . . ? O7 C26 N9 126.1(4) . . ? O7 C26 C25 118.7(4) . . ? N9 C26 C25 115.2(3) . . ? N10 C27 C28 123.5(4) . . ? N10 C27 N9 113.9(3) . . ? C28 C27 N9 122.6(4) . . ? C29 C28 C27 117.6(4) . . ? C28 C29 C30 120.5(4) . . ? C31 C30 C29 117.4(4) . . ? N10 C31 C30 124.4(4) . . ? N10 C31 N11 112.6(3) . . ? C30 C31 N11 123.0(4) . . ? O8 C32 N11 124.3(4) . . ? O8 C32 C33 120.1(3) . . ? N11 C32 C33 115.5(4) . . ? N12 C33 C34 123.6(4) . . ? N12 C33 C32 118.5(3) . . ? C34 C33 C32 117.9(4) . . ? C33 C34 C35 120.0(4) . . ? O9 C35 C34 118.5(4) . . ? O9 C35 C36 124.2(4) . . ? C34 C35 C36 117.3(4) . . ? C37 C36 C35 118.8(4) . . ? N12 C37 C36 124.4(4) . . ? N12 C37 C38 117.5(3) . . ? C36 C37 C38 118.1(4) . . ? O10 C38 N13 125.0(4) . . ? O10 C38 C37 121.7(4) . . ? N13 C38 C37 113.2(3) . . ? N14 C39 C40 123.8(4) . . ? N14 C39 N13 112.8(3) . . ? C40 C39 N13 123.4(3) . . ? C41 C40 C39 116.8(4) . . ? C42 C41 C40 121.2(4) . . ? C41 C42 C43 117.5(4) . . ? N14 C43 C42 122.6(3) . . ? N14 C43 N15 112.6(3) . . ? C42 C43 N15 124.8(4) . . ? O11 C44 N15 122.8(4) . . ? O11 C44 C45 123.3(4) . . ? N15 C44 C45 113.9(4) . . ? C2 N1 C3 128.9(4) . . ? C3 N2 C7 118.2(3) . . ? C8 N3 C7 129.4(3) . . ? C9 N4 C13 116.5(3) . . ? C14 N5 C15 128.6(4) . . ? C19 N6 C15 118.7(3) . . ? C20 N7 C19 130.8(4) . . ? C25 N8 C21 116.0(3) . . ? C26 N9 C27 125.9(3) . . ? C27 N10 C31 116.7(3) . . ? C32 N11 C31 127.3(3) . . ? C37 N12 C33 115.9(3) . . ? C38 N13 C39 128.8(3) . . ? C39 N14 C43 117.9(3) . . ? C44 N15 C43 127.9(4) . . ? O15' C48 O15 20.0(15) . . ? O16 C49 O16' 48.6(7) . . ? _diffrn_measured_fraction_theta_max 0.844 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.844 _refine_diff_density_max 0.325 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.054 #===END