data_ys628 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 N2 O7' _chemical_formula_weight 536.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.8185(16) _cell_length_b 8.3688(17) _cell_length_c 22.032(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.00(3) _cell_angle_gamma 90.00 _cell_volume 1436.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3439 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 27.53 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9800 _exptl_absorpt_correction_T_max 0.9895 _exptl_absorpt_process_details 'SADABS (Sheldricks, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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_% 1 _diffrn_reflns_number 10610 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0593 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4999 _reflns_number_gt 3787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.1500P)^2^+0.6700P] 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 1(2) _refine_ls_number_reflns 4999 _refine_ls_number_parameters 328 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2190 _refine_ls_wR_factor_gt 0.1988 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.011 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.0760(5) 0.4503(4) 0.49065(16) 0.0571(10) Uani 1 1 d . . . O2 O 0.4110(4) 0.5951(4) 0.69970(17) 0.0533(9) Uani 1 1 d . . . O3 O 0.5868(5) 0.8040(4) 0.7076(2) 0.0657(12) Uani 1 1 d . . . O4 O 0.8636(4) 0.6324(4) 0.71012(17) 0.0492(9) Uani 1 1 d . A . H4 H 0.9064 0.6473 0.7450 0.059 Uiso 1 1 calc R . . O5 O 0.7126(6) 0.5636(4) 0.82136(17) 0.0657(11) Uani 1 1 d . . . O6 O 0.9597(5) -0.0191(4) 0.68146(18) 0.0619(10) Uani 1 1 d . . . O7 O 1.1138(6) -0.0140(7) 0.7979(3) 0.0954(16) Uani 1 1 d . . . H7 H 1.0778 -0.0391 0.7632 0.115 Uiso 1 1 calc R . . N1 N 0.6347(5) 0.4883(4) 0.59980(17) 0.0408(9) Uani 1 1 d . . . N2 N 0.7696(4) 0.1160(4) 0.73641(17) 0.0379(9) Uani 1 1 d . A . C1 C 0.2882(5) 0.2213(5) 0.6189(2) 0.0370(10) Uani 1 1 d . . . H1 H 0.2687 0.1366 0.6447 0.044 Uiso 1 1 calc R . . C2 C 0.1597(6) 0.2706(6) 0.5748(2) 0.0430(11) Uani 1 1 d . . . H2 H 0.0539 0.2190 0.5711 0.052 Uiso 1 1 calc R . . C3 C 0.1913(6) 0.3972(5) 0.5366(2) 0.0405(11) Uani 1 1 d . . . C4 C 0.3468(6) 0.4787(5) 0.54224(19) 0.0400(10) Uani 1 1 d . . . H4A H 0.3660 0.5649 0.5170 0.048 Uiso 1 1 calc R . . C5 C 0.4717(6) 0.4288(5) 0.58594(19) 0.0359(10) Uani 1 1 d . . . C6 C 0.4419(6) 0.2981(5) 0.62382(19) 0.0340(10) Uani 1 1 d . . . C7 C 0.6099(5) 0.2638(5) 0.6616(2) 0.0325(9) Uani 1 1 d . . . C8 C 0.7094(5) 0.4247(5) 0.6578(2) 0.0339(10) Uani 1 1 d . A . H8 H 0.8293 0.3979 0.6526 0.041 Uiso 1 1 calc R . . C9 C 0.7103(5) 0.5419(5) 0.7118(2) 0.0356(10) Uani 1 1 d . . . C10 C 0.7234(6) 0.4525(5) 0.7731(2) 0.0415(11) Uani 1 1 d . A . H10 H 0.8409 0.4107 0.7782 0.050 Uiso 1 1 calc R . . C11 C 0.6068(6) 0.3080(6) 0.7832(2) 0.0415(11) Uani 1 1 d . . . C12 C 0.6064(5) 0.2015(5) 0.7269(2) 0.0353(10) Uani 1 1 d . A . H12 H 0.5126 0.1240 0.7278 0.042 Uiso 1 1 calc R . . C13 C 0.7129(6) 0.1271(5) 0.6334(2) 0.0386(10) Uani 1 1 d . . . H13A H 0.6364 0.0431 0.6172 0.046 Uiso 1 1 calc R . . H13B H 0.7766 0.1677 0.6008 0.046 Uiso 1 1 calc R . . C14 C 0.8323(6) 0.0659(5) 0.6850(2) 0.0405(11) Uani 1 1 d . . . C15 C 0.8187(7) 0.0852(6) 0.8003(2) 0.0529(13) Uani 1 1 d . . . H15 H 0.7875 -0.0251 0.8094 0.063 Uiso 1 1 calc R A . C16 C 0.6992(7) 0.1988(7) 0.8320(2) 0.0560(14) Uani 1 1 d . A . H16A H 0.6158 0.1376 0.8524 0.067 Uiso 1 1 calc R . . H16B H 0.7657 0.2628 0.8623 0.067 Uiso 1 1 calc R . . C17 C -0.0775(7) 0.3619(7) 0.4762(3) 0.0607(15) Uani 1 1 d . . . H17A H -0.0495 0.2520 0.4695 0.073 Uiso 1 1 calc R . . H17B H -0.1376 0.4049 0.4400 0.073 Uiso 1 1 calc R . . H17C H -0.1491 0.3691 0.5094 0.073 Uiso 1 1 calc R . . C18 C 0.6925(7) 0.6344(6) 0.5726(2) 0.0524(13) Uani 1 1 d . . . H18A H 0.6666 0.6301 0.5292 0.063 Uiso 1 1 calc R . . H18B H 0.8142 0.6456 0.5818 0.063 Uiso 1 1 calc R . . H18C H 0.6349 0.7242 0.5887 0.063 Uiso 1 1 calc R . . C19 C 0.5640(6) 0.6639(5) 0.7064(2) 0.0385(10) Uani 1 1 d . A . C20 C 0.2638(6) 0.7019(8) 0.6934(4) 0.0741(18) Uani 1 1 d . . . H20A H 0.2603 0.7640 0.7299 0.089 Uiso 1 1 calc R . . H20B H 0.1604 0.6403 0.6868 0.089 Uiso 1 1 calc R . . H20C H 0.2737 0.7720 0.6594 0.089 Uiso 1 1 calc R . . C21 C 0.8952(16) 0.6110(15) 0.8474(5) 0.065(3) Uiso 0.604(14) 1 d P A 1 H21A H 0.9605 0.5164 0.8602 0.078 Uiso 0.604(14) 1 calc PR A 1 H21B H 0.9546 0.6657 0.8166 0.078 Uiso 0.604(14) 1 calc PR A 1 C22 C 0.8785(12) 0.7185(10) 0.9005(3) 0.061(3) Uiso 0.604(14) 1 d PG A 1 C23 C 1.0232(10) 0.7972(12) 0.9267(4) 0.090(4) Uiso 0.604(14) 1 d PG A 1 H23 H 1.1287 0.7828 0.9110 0.108 Uiso 0.604(14) 1 calc PR A 1 C24 C 1.0102(14) 0.8975(13) 0.9763(5) 0.121(6) Uiso 0.604(14) 1 d PG A 1 H24 H 1.1069 0.9502 0.9938 0.145 Uiso 0.604(14) 1 calc PR A 1 C25 C 0.8525(17) 0.9191(16) 0.9999(5) 0.151(9) Uiso 0.604(14) 1 d PG A 1 H25 H 0.8438 0.9863 1.0331 0.181 Uiso 0.604(14) 1 calc PR A 1 C26 C 0.7078(14) 0.8404(18) 0.9737(5) 0.176(10) Uiso 0.604(14) 1 d PG A 1 H26 H 0.6023 0.8548 0.9894 0.211 Uiso 0.604(14) 1 calc PR A 1 C27 C 0.7208(11) 0.7401(14) 0.9240(5) 0.097(5) Uiso 0.604(14) 1 d PG A 1 H27 H 0.6240 0.6874 0.9065 0.116 Uiso 0.604(14) 1 calc PR A 1 C21' C 0.827(3) 0.616(3) 0.8606(9) 0.076(5) Uiso 0.396(14) 1 d P A 2 H21C H 0.9216 0.6532 0.8387 0.091 Uiso 0.396(14) 1 calc PR A 2 H21D H 0.8686 0.5264 0.8853 0.091 Uiso 0.396(14) 1 calc PR A 2 C22' C 0.787(2) 0.7447(17) 0.9025(6) 0.082(5) Uiso 0.396(14) 1 d PG A 2 C23' C 0.919(2) 0.814(2) 0.9399(9) 0.124(9) Uiso 0.396(14) 1 d PG A 2 H23' H 1.0317 0.7831 0.9369 0.149 Uiso 0.396(14) 1 calc PR A 2 C24' C 0.881(3) 0.931(2) 0.9816(8) 0.155(13) Uiso 0.396(14) 1 d PG A 2 H24' H 0.9696 0.9780 1.0066 0.186 Uiso 0.396(14) 1 calc PR A 2 C25' C 0.712(3) 0.978(2) 0.9860(8) 0.126(9) Uiso 0.396(14) 1 d PG A 2 H25' H 0.6876 1.0564 1.0139 0.151 Uiso 0.396(14) 1 calc PR A 2 C26' C 0.581(2) 0.908(2) 0.9487(9) 0.165(13) Uiso 0.396(14) 1 d PG A 2 H26' H 0.4676 0.9399 0.9516 0.198 Uiso 0.396(14) 1 calc PR A 2 C27' C 0.618(2) 0.792(2) 0.9069(7) 0.096(7) Uiso 0.396(14) 1 d PG A 2 H27' H 0.5296 0.7449 0.8820 0.115 Uiso 0.396(14) 1 calc PR A 2 C28 C 0.4169(7) 0.3397(8) 0.7971(3) 0.0618(15) Uani 1 1 d . A . H28A H 0.3624 0.4025 0.7638 0.074 Uiso 1 1 calc R . . H28B H 0.3581 0.2376 0.7967 0.074 Uiso 1 1 calc R . . C29 C 0.3876(11) 0.4219(16) 0.8548(4) 0.144(5) Uani 1 1 d . . . H29A H 0.4560 0.3722 0.8879 0.173 Uiso 1 1 calc R A . H29B H 0.2684 0.4144 0.8619 0.173 Uiso 1 1 calc R . . H29C H 0.4194 0.5323 0.8522 0.173 Uiso 1 1 calc R . . C30 C 1.0083(8) 0.1082(8) 0.8194(3) 0.0747(18) Uani 1 1 d . A . H30A H 1.0445 0.2104 0.8042 0.090 Uiso 1 1 calc R . . H30B H 1.0249 0.1115 0.8635 0.090 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.066(2) 0.042(2) 0.059(2) 0.0012(17) -0.0173(18) -0.0024(17) O2 0.0295(16) 0.040(2) 0.090(3) -0.0091(19) 0.0052(15) 0.0030(14) O3 0.054(2) 0.0199(19) 0.124(4) -0.0038(19) 0.008(2) 0.0040(15) O4 0.0380(16) 0.0342(18) 0.074(2) -0.0069(18) -0.0002(16) -0.0075(15) O5 0.098(3) 0.045(2) 0.052(2) -0.0149(18) -0.008(2) 0.006(2) O6 0.057(2) 0.046(2) 0.085(3) -0.002(2) 0.0155(19) 0.0177(19) O7 0.078(3) 0.083(4) 0.120(4) -0.004(3) -0.019(3) 0.035(3) N1 0.043(2) 0.0283(19) 0.052(2) 0.0076(18) 0.0090(17) -0.0086(17) N2 0.0414(19) 0.0184(17) 0.053(2) 0.0045(17) 0.0010(17) -0.0008(16) C1 0.045(2) 0.022(2) 0.046(3) 0.0036(19) 0.012(2) -0.0084(19) C2 0.039(2) 0.040(3) 0.051(3) -0.002(2) 0.009(2) -0.004(2) C3 0.048(3) 0.029(2) 0.044(3) -0.008(2) 0.001(2) 0.006(2) C4 0.056(3) 0.028(2) 0.036(2) 0.0044(19) 0.005(2) 0.002(2) C5 0.050(3) 0.025(2) 0.034(2) 0.0036(18) 0.0115(19) 0.0000(19) C6 0.046(2) 0.021(2) 0.036(2) -0.0043(17) 0.0069(18) 0.0009(18) C7 0.031(2) 0.023(2) 0.044(2) -0.0008(18) 0.0082(18) -0.0019(17) C8 0.030(2) 0.024(2) 0.050(3) 0.0039(19) 0.0108(18) -0.0019(17) C9 0.032(2) 0.022(2) 0.053(3) -0.0004(19) 0.0062(19) 0.0004(17) C10 0.044(2) 0.026(2) 0.053(3) -0.006(2) -0.001(2) 0.0113(19) C11 0.044(3) 0.037(2) 0.044(3) -0.003(2) 0.004(2) 0.001(2) C12 0.036(2) 0.024(2) 0.046(3) 0.0041(19) 0.0034(19) -0.0011(18) C13 0.045(2) 0.024(2) 0.048(3) -0.002(2) 0.011(2) -0.002(2) C14 0.041(2) 0.016(2) 0.065(3) -0.002(2) 0.008(2) 0.0003(18) C15 0.064(3) 0.033(3) 0.062(3) 0.013(2) 0.002(2) 0.000(2) C16 0.069(3) 0.051(3) 0.048(3) 0.012(3) 0.004(3) -0.005(3) C17 0.063(4) 0.050(3) 0.066(4) -0.005(3) -0.012(3) 0.010(3) C18 0.066(3) 0.038(3) 0.054(3) 0.011(2) 0.011(3) -0.015(2) C19 0.043(2) 0.028(3) 0.044(3) -0.0015(19) 0.003(2) 0.0006(19) C20 0.032(3) 0.067(4) 0.124(5) -0.002(4) 0.010(3) 0.011(3) C28 0.054(3) 0.069(4) 0.065(4) -0.002(3) 0.023(3) -0.001(3) C29 0.088(6) 0.217(13) 0.133(8) -0.093(9) 0.044(5) -0.008(7) C30 0.071(4) 0.070(4) 0.079(4) 0.005(4) -0.013(3) 0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C3 1.370(6) . ? O1 C17 1.423(6) . ? O2 C19 1.324(5) . ? O2 C20 1.454(6) . ? O3 C19 1.187(6) . ? O4 C9 1.421(5) . ? O5 C21' 1.27(2) . ? O5 C10 1.420(6) . ? O5 C21 1.544(12) . ? O6 C14 1.231(5) . ? O7 C30 1.421(8) . ? N1 C5 1.377(6) . ? N1 C18 1.451(6) . ? N1 C8 1.458(6) . ? N2 C14 1.340(6) . ? N2 C15 1.450(6) . ? N2 C12 1.462(5) . ? C1 C6 1.358(6) . ? C1 C2 1.397(7) . ? C2 C3 1.389(7) . ? C3 C4 1.390(6) . ? C4 C5 1.375(6) . ? C5 C6 1.408(6) . ? C6 C7 1.520(6) . ? C7 C12 1.533(6) . ? C7 C13 1.559(6) . ? C7 C8 1.561(5) . ? C8 C9 1.542(6) . ? C9 C19 1.530(6) . ? C9 C10 1.540(6) . ? C10 C11 1.542(7) . ? C11 C12 1.527(6) . ? C11 C16 1.543(7) . ? C11 C28 1.564(7) . ? C13 C14 1.498(7) . ? C15 C30 1.518(8) . ? C15 C16 1.542(7) . ? C21 C22 1.490(14) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C21' C22' 1.47(2) . ? C22' C23' 1.3900 . ? C22' C27' 1.3900 . ? C23' C24' 1.3900 . ? C24' C25' 1.3900 . ? C25' C26' 1.3900 . ? C26' C27' 1.3900 . ? C28 C29 1.482(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 O1 C17 119.0(4) . . ? C19 O2 C20 116.3(4) . . ? C21' O5 C10 130.9(11) . . ? C21' O5 C21 23.5(9) . . ? C10 O5 C21 109.5(6) . . ? C5 N1 C18 121.9(4) . . ? C5 N1 C8 110.8(3) . . ? C18 N1 C8 123.7(4) . . ? C14 N2 C15 132.8(4) . . ? C14 N2 C12 114.3(4) . . ? C15 N2 C12 112.3(4) . . ? C6 C1 C2 119.6(4) . . ? C3 C2 C1 119.4(4) . . ? O1 C3 C4 114.9(4) . . ? O1 C3 C2 123.7(4) . . ? C4 C3 C2 121.4(4) . . ? C5 C4 C3 118.4(4) . . ? C4 C5 N1 129.2(4) . . ? C4 C5 C6 120.5(4) . . ? N1 C5 C6 110.3(4) . . ? C1 C6 C5 120.7(4) . . ? C1 C6 C7 132.1(4) . . ? C5 C6 C7 107.0(4) . . ? C6 C7 C12 119.5(3) . . ? C6 C7 C13 111.8(4) . . ? C12 C7 C13 100.2(3) . . ? C6 C7 C8 102.6(3) . . ? C12 C7 C8 113.2(4) . . ? C13 C7 C8 109.5(3) . . ? N1 C8 C9 114.7(3) . . ? N1 C8 C7 101.5(3) . . ? C9 C8 C7 118.4(3) . . ? O4 C9 C19 105.6(3) . . ? O4 C9 C10 106.8(4) . . ? C19 C9 C10 112.6(3) . . ? O4 C9 C8 105.5(3) . . ? C19 C9 C8 114.3(4) . . ? C10 C9 C8 111.3(3) . . ? O5 C10 C9 109.6(4) . . ? O5 C10 C11 109.3(4) . . ? C9 C10 C11 120.8(4) . . ? C12 C11 C16 100.8(4) . . ? C12 C11 C10 107.5(4) . . ? C16 C11 C10 108.5(4) . . ? C12 C11 C28 108.8(4) . . ? C16 C11 C28 111.1(4) . . ? C10 C11 C28 118.6(4) . . ? N2 C12 C11 103.3(3) . . ? N2 C12 C7 102.3(3) . . ? C11 C12 C7 124.4(4) . . ? C14 C13 C7 104.9(4) . . ? O6 C14 N2 126.3(5) . . ? O6 C14 C13 127.1(4) . . ? N2 C14 C13 106.6(4) . . ? N2 C15 C30 114.6(4) . . ? N2 C15 C16 102.2(4) . . ? C30 C15 C16 114.3(5) . . ? C11 C16 C15 108.3(4) . . ? O3 C19 O2 124.4(4) . . ? O3 C19 C9 123.2(4) . . ? O2 C19 C9 112.4(4) . . ? C22 C21 O5 107.8(8) . . ? C23 C22 C27 120.0 . . ? C23 C22 C21 119.2(7) . . ? C27 C22 C21 120.8(7) . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C22 120.0 . . ? O5 C21' C22' 120.6(17) . . ? C23' C22' C27' 120.0 . . ? C23' C22' C21' 119.5(13) . . ? C27' C22' C21' 120.4(13) . . ? C24' C23' C22' 120.0 . . ? C23' C24' C25' 120.0 . . ? C24' C25' C26' 120.0 . . ? C27' C26' C25' 120.0 . . ? C26' C27' C22' 120.0 . . ? C29 C28 C11 117.8(6) . . ? O7 C30 C15 113.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.1(6) . . . . ? C17 O1 C3 C4 172.0(4) . . . . ? C17 O1 C3 C2 -7.1(7) . . . . ? C1 C2 C3 O1 177.5(4) . . . . ? C1 C2 C3 C4 -1.6(7) . . . . ? O1 C3 C4 C5 -177.7(4) . . . . ? C2 C3 C4 C5 1.4(6) . . . . ? C3 C4 C5 N1 179.3(4) . . . . ? C3 C4 C5 C6 0.1(6) . . . . ? C18 N1 C5 C4 7.9(7) . . . . ? C8 N1 C5 C4 167.0(4) . . . . ? C18 N1 C5 C6 -172.8(4) . . . . ? C8 N1 C5 C6 -13.7(5) . . . . ? C2 C1 C6 C5 1.4(6) . . . . ? C2 C1 C6 C7 -172.9(4) . . . . ? C4 C5 C6 C1 -1.6(6) . . . . ? N1 C5 C6 C1 179.1(4) . . . . ? C4 C5 C6 C7 174.0(4) . . . . ? N1 C5 C6 C7 -5.3(5) . . . . ? C1 C6 C7 C12 -38.6(6) . . . . ? C5 C6 C7 C12 146.5(4) . . . . ? C1 C6 C7 C13 78.0(6) . . . . ? C5 C6 C7 C13 -96.9(4) . . . . ? C1 C6 C7 C8 -164.8(4) . . . . ? C5 C6 C7 C8 20.3(4) . . . . ? C5 N1 C8 C9 -103.3(4) . . . . ? C18 N1 C8 C9 55.4(5) . . . . ? C5 N1 C8 C7 25.6(4) . . . . ? C18 N1 C8 C7 -175.7(4) . . . . ? C6 C7 C8 N1 -26.8(4) . . . . ? C12 C7 C8 N1 -157.0(3) . . . . ? C13 C7 C8 N1 92.0(4) . . . . ? C6 C7 C8 C9 99.7(4) . . . . ? C12 C7 C8 C9 -30.5(5) . . . . ? C13 C7 C8 C9 -141.4(4) . . . . ? N1 C8 C9 O4 -86.4(4) . . . . ? C7 C8 C9 O4 153.7(3) . . . . ? N1 C8 C9 C19 29.1(5) . . . . ? C7 C8 C9 C19 -90.8(5) . . . . ? N1 C8 C9 C10 158.1(3) . . . . ? C7 C8 C9 C10 38.2(5) . . . . ? C21' O5 C10 C9 -106.2(14) . . . . ? C21 O5 C10 C9 -95.1(6) . . . . ? C21' O5 C10 C11 119.3(14) . . . . ? C21 O5 C10 C11 130.4(6) . . . . ? O4 C9 C10 O5 69.1(4) . . . . ? C19 C9 C10 O5 -46.3(5) . . . . ? C8 C9 C10 O5 -176.2(4) . . . . ? O4 C9 C10 C11 -162.5(4) . . . . ? C19 C9 C10 C11 82.0(5) . . . . ? C8 C9 C10 C11 -47.9(5) . . . . ? O5 C10 C11 C12 173.6(4) . . . . ? C9 C10 C11 C12 45.2(5) . . . . ? O5 C10 C11 C16 -78.1(4) . . . . ? C9 C10 C11 C16 153.4(4) . . . . ? O5 C10 C11 C28 49.8(6) . . . . ? C9 C10 C11 C28 -78.7(5) . . . . ? C14 N2 C12 C11 -154.3(4) . . . . ? C15 N2 C12 C11 33.2(4) . . . . ? C14 N2 C12 C7 -24.1(4) . . . . ? C15 N2 C12 C7 163.4(4) . . . . ? C16 C11 C12 N2 -35.0(4) . . . . ? C10 C11 C12 N2 78.5(4) . . . . ? C28 C11 C12 N2 -151.9(4) . . . . ? C16 C11 C12 C7 -150.3(4) . . . . ? C10 C11 C12 C7 -36.8(5) . . . . ? C28 C11 C12 C7 92.8(5) . . . . ? C6 C7 C12 N2 154.5(3) . . . . ? C13 C7 C12 N2 32.1(4) . . . . ? C8 C7 C12 N2 -84.4(4) . . . . ? C6 C7 C12 C11 -89.7(5) . . . . ? C13 C7 C12 C11 147.9(4) . . . . ? C8 C7 C12 C11 31.3(5) . . . . ? C6 C7 C13 C14 -158.9(3) . . . . ? C12 C7 C13 C14 -31.2(4) . . . . ? C8 C7 C13 C14 88.1(4) . . . . ? C15 N2 C14 O6 -3.3(8) . . . . ? C12 N2 C14 O6 -173.8(4) . . . . ? C15 N2 C14 C13 174.2(4) . . . . ? C12 N2 C14 C13 3.6(5) . . . . ? C7 C13 C14 O6 -164.3(4) . . . . ? C7 C13 C14 N2 18.2(4) . . . . ? C14 N2 C15 C30 49.9(7) . . . . ? C12 N2 C15 C30 -139.4(4) . . . . ? C14 N2 C15 C16 174.1(4) . . . . ? C12 N2 C15 C16 -15.2(5) . . . . ? C12 C11 C16 C15 27.3(5) . . . . ? C10 C11 C16 C15 -85.5(5) . . . . ? C28 C11 C16 C15 142.5(4) . . . . ? N2 C15 C16 C11 -8.6(5) . . . . ? C30 C15 C16 C11 115.7(5) . . . . ? C20 O2 C19 O3 0.1(8) . . . . ? C20 O2 C19 C9 -179.2(5) . . . . ? O4 C9 C19 O3 -7.2(6) . . . . ? C10 C9 C19 O3 109.0(6) . . . . ? C8 C9 C19 O3 -122.6(5) . . . . ? O4 C9 C19 O2 172.1(4) . . . . ? C10 C9 C19 O2 -71.6(5) . . . . ? C8 C9 C19 O2 56.7(5) . . . . ? C21' O5 C21 C22 -18(3) . . . . ? C10 O5 C21 C22 -176.1(6) . . . . ? O5 C21 C22 C23 -170.5(6) . . . . ? O5 C21 C22 C27 9.7(11) . . . . ? C27 C22 C23 C24 0.0 . . . . ? C21 C22 C23 C24 -179.8(9) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C22 0.0 . . . . ? C23 C22 C27 C26 0.0 . . . . ? C21 C22 C27 C26 179.8(9) . . . . ? C10 O5 C21' C22' 173.6(10) . . . . ? C21 O5 C21' C22' 146(4) . . . . ? O5 C21' C22' C23' -171.9(14) . . . . ? O5 C21' C22' C27' 11(2) . . . . ? C27' C22' C23' C24' 0.0 . . . . ? C21' C22' C23' C24' -177.3(16) . . . . ? C22' C23' C24' C25' 0.0 . . . . ? C23' C24' C25' C26' 0.0 . . . . ? C24' C25' C26' C27' 0.0 . . . . ? C25' C26' C27' C22' 0.0 . . . . ? C23' C22' C27' C26' 0.0 . . . . ? C21' C22' C27' C26' 177.2(16) . . . . ? C12 C11 C28 C29 171.6(7) . . . . ? C16 C11 C28 C29 61.5(9) . . . . ? C10 C11 C28 C29 -65.2(9) . . . . ? N2 C15 C30 O7 -72.6(7) . . . . ? C16 C15 C30 O7 169.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.326 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.052