Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 X-Sun-Data-Type: default X-Sun-Data-Description: default X-Sun-Data-Name: 182_1874.cif X-Sun-Charset: us-ascii X-Sun-Content-Lines: 605 _journal_coden_Cambridge 182 _journal_page_first 207 _journal_year 2001 loop_ _publ_author_name 'D.Seebach' 'M.Brenner' 'M.Rueping' 'B.Schweizer' 'B.Jaun' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 160.5 _chemical_formula_moiety ? _chemical_formula_sum 'C46 H80 N4 O7' _chemical_formula_weight 801.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.462(2) _cell_length_b 20.472(6) _cell_length_c 13.866(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.14(2) _cell_angle_gamma 90.00 _cell_volume 2580.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 20.0 _cell_measurement_theta_max 21.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8540 _exptl_absorpt_correction_T_max 0.9892 _exptl_absorpt_process_details ? _exptl_special_details ; extremly thin crystal, 75% of intensities weak ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method \o/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 10000s _diffrn_standards_decay_% ? _diffrn_reflns_number 4479 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.4192 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 66.23 _reflns_number_total 4479 _reflns_number_gt 1140 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction 'MolEN (Enraf-Nonius, 1990)' _computing_structure_solution 'SIR97 (Altomare, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLUTO, ORTEP (Johnson, 1976)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ > 3sigma(F^2^). 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^. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _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 1.0(14) _refine_ls_number_reflns 1140 _refine_ls_number_parameters 243 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.3955 _refine_ls_R_factor_gt 0.0898 _refine_ls_wR_factor_ref 0.2829 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 1.525 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.432 _refine_ls_shift/su_mean 0.018 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 0.138(3) 0.4398(13) 0.414(2) 0.068(8) Uiso 1 1 d . . . C2 C 0.135(2) 0.4051(11) 0.5051(16) 0.053(7) Uiso 1 1 d . . . H2 H 0.2007 0.3675 0.5099 0.063 Uiso 1 1 calc R . . C3 C 0.202(2) 0.4471(10) 0.5968(13) 0.033(6) Uiso 1 1 d . . . H3 H 0.3033 0.4577 0.5970 0.040 Uiso 1 1 calc R . . C4 C 0.208(2) 0.4153(11) 0.6961(14) 0.042(7) Uiso 1 1 d . . . H4 H 0.1067 0.4081 0.6994 0.051 Uiso 1 1 calc R . . C5 C 0.287(2) 0.3493(11) 0.7053(17) 0.069(8) Uiso 1 1 d . . . H5A H 0.2976 0.3316 0.7711 0.104 Uiso 1 1 calc R . . H5B H 0.3821 0.3553 0.6949 0.104 Uiso 1 1 calc R . . H5C H 0.2301 0.3198 0.6557 0.104 Uiso 1 1 calc R . . N6 N 0.2838(17) 0.4541(8) 0.7802(11) 0.029(5) Uiso 1 1 d . . . H6 H 0.3776 0.4579 0.7925 0.035 Uiso 1 1 calc R . . C7 C 0.222(3) 0.4825(11) 0.8365(16) 0.044(7) Uiso 1 1 d . . . C8 C 0.314(2) 0.5133(10) 0.9387(14) 0.035(6) Uiso 1 1 d . . . H8 H 0.4180 0.5095 0.9400 0.042 Uiso 1 1 calc R . . C9 C 0.284(2) 0.5854(10) 0.9468(15) 0.042(6) Uiso 1 1 d . . . H9 H 0.1818 0.5887 0.9493 0.050 Uiso 1 1 calc R . . C10 C 0.294(2) 0.6249(11) 0.8606(17) 0.053(7) Uiso 1 1 d . . . H10 H 0.2291 0.6040 0.8010 0.063 Uiso 1 1 calc R . . N11 N 0.4489(17) 0.6219(8) 0.8480(13) 0.044(5) Uiso 1 1 d . . . H11 H 0.5205 0.6123 0.8996 0.053 Uiso 1 1 calc R . . C12 C 0.478(2) 0.6328(11) 0.7642(17) 0.047(7) Uiso 1 1 d . . . C13 C 0.645(2) 0.6387(10) 0.7670(15) 0.038(6) Uiso 1 1 d . . . H13 H 0.7078 0.6294 0.8346 0.045 Uiso 1 1 calc R . . C14 C 0.677(2) 0.5924(11) 0.6927(17) 0.052(7) Uiso 1 1 d . . . H14 H 0.6102 0.6029 0.6268 0.062 Uiso 1 1 calc R . . C15 C 0.649(2) 0.5202(11) 0.7159(16) 0.051(7) Uiso 1 1 d . . . H15 H 0.5528 0.5183 0.7293 0.061 Uiso 1 1 calc R . . N16 N 0.7564(17) 0.4948(8) 0.8039(11) 0.034(5) Uiso 1 1 d . . . H16 H 0.8445 0.5102 0.8198 0.041 Uiso 1 1 calc R . . C17 C 0.724(2) 0.4501(11) 0.8586(15) 0.035(6) Uiso 1 1 d . . . C18 C 0.850(2) 0.4163(10) 0.9379(14) 0.028(6) Uiso 1 1 d . . . H18 H 0.9296 0.4482 0.9609 0.033 Uiso 1 1 calc R . . C19 C 0.812(2) 0.3914(10) 1.0271(15) 0.036(6) Uiso 1 1 d . . . H19 H 0.7381 0.3572 1.0024 0.043 Uiso 1 1 calc R . . C20 C 0.741(2) 0.4395(9) 1.0806(14) 0.030(6) Uiso 1 1 d . . . H20 H 0.6624 0.4610 1.0293 0.036 Uiso 1 1 calc R . . N21 N 0.8445(18) 0.4912(9) 1.1302(12) 0.050(6) Uiso 1 1 d . . . H21 H 0.9183 0.4796 1.1791 0.060 Uiso 1 1 calc R . . C22 C 0.834(3) 0.5521(13) 1.1069(18) 0.055(7) Uiso 1 1 d . . . O23 O 0.9267(17) 0.5913(8) 1.1732(12) 0.069(5) Uiso 1 1 d . . . C24 C 0.942(3) 0.6602(13) 1.1545(19) 0.069(8) Uiso 1 1 d . . . C25 C 0.986(2) 0.6709(13) 1.0630(17) 0.076(8) Uiso 1 1 d . . . H25A H 1.0634 0.6408 1.0609 0.114 Uiso 1 1 calc R . . H25B H 1.0217 0.7149 1.0624 0.114 Uiso 1 1 calc R . . H25C H 0.9036 0.6642 1.0055 0.114 Uiso 1 1 calc R . . C26 C 1.068(3) 0.6787(14) 1.2477(19) 0.103(10) Uiso 1 1 d . . . H26A H 1.1562 0.6563 1.2454 0.154 Uiso 1 1 calc R . . H26B H 1.0423 0.6662 1.3073 0.154 Uiso 1 1 calc R . . H26C H 1.0841 0.7250 1.2482 0.154 Uiso 1 1 calc R . . C27 C 0.801(3) 0.6934(15) 1.154(2) 0.123(12) Uiso 1 1 d . . . H27A H 0.8180 0.7393 1.1658 0.184 Uiso 1 1 calc R . . H27B H 0.7637 0.6753 1.2063 0.184 Uiso 1 1 calc R . . H27C H 0.7297 0.6869 1.0904 0.184 Uiso 1 1 calc R . . O28 O 0.0285(17) 0.4495(8) 0.3396(12) 0.071(5) Uiso 1 1 d . . . O29 O 0.2657(16) 0.4647(8) 0.4125(11) 0.067(5) Uiso 1 1 d . . . C30 C 0.278(3) 0.5069(12) 0.3297(19) 0.073(8) Uiso 1 1 d . . . H30A H 0.1946 0.5362 0.3115 0.087 Uiso 1 1 calc R . . H30B H 0.2763 0.4801 0.2716 0.087 Uiso 1 1 calc R . . C31 C 0.415(3) 0.5456(14) 0.3569(19) 0.072(8) Uiso 1 1 d . . . C32 C 0.529(4) 0.5205(17) 0.338(2) 0.126(12) Uiso 1 1 d . . . H32 H 0.5170 0.4803 0.3051 0.151 Uiso 1 1 calc R . . C33 C 0.674(4) 0.550(2) 0.362(3) 0.167(16) Uiso 1 1 d . . . H33 H 0.7614 0.5301 0.3584 0.200 Uiso 1 1 calc R . . C34 C 0.659(4) 0.616(2) 0.394(3) 0.147(14) Uiso 1 1 d . . . H34 H 0.7388 0.6435 0.3978 0.177 Uiso 1 1 calc R . . C35 C 0.549(4) 0.6413(19) 0.418(2) 0.139(13) Uiso 1 1 d . . . H35 H 0.5556 0.6830 0.4459 0.167 Uiso 1 1 calc R . . C36 C 0.417(3) 0.6042(15) 0.402(2) 0.101(11) Uiso 1 1 d . . . H36 H 0.3369 0.6196 0.4212 0.121 Uiso 1 1 calc R . . C37 C -0.017(2) 0.3771(11) 0.4980(18) 0.052(7) Uiso 1 1 d . . . H37A H -0.0879 0.4121 0.4777 0.063 Uiso 1 1 calc R . . H37B H -0.0179 0.3635 0.5648 0.063 Uiso 1 1 calc R . . C38 C -0.069(3) 0.3194(15) 0.427(2) 0.093(10) Uiso 1 1 d . . . H38 H -0.0710 0.3324 0.3582 0.112 Uiso 1 1 calc R . . C39 C 0.028(3) 0.2588(15) 0.457(2) 0.129(12) Uiso 1 1 d . . . H39A H 0.0192 0.2423 0.5195 0.194 Uiso 1 1 calc R . . H39B H 0.1292 0.2702 0.4636 0.194 Uiso 1 1 calc R . . H39C H -0.0022 0.2258 0.4059 0.194 Uiso 1 1 calc R . . C40 C -0.223(3) 0.3015(17) 0.430(2) 0.135(12) Uiso 1 1 d . . . H40A H -0.2638 0.2693 0.3796 0.202 Uiso 1 1 calc R . . H40B H -0.2843 0.3398 0.4180 0.202 Uiso 1 1 calc R . . H40C H -0.2195 0.2840 0.4951 0.202 Uiso 1 1 calc R . . C41 C 0.293(3) 0.4700(12) 1.0241(17) 0.072(8) Uiso 1 1 d . . . H41A H 0.3663 0.4807 1.0853 0.108 Uiso 1 1 calc R . . H41B H 0.3027 0.4250 1.0079 0.108 Uiso 1 1 calc R . . H41C H 0.1969 0.4774 1.0324 0.108 Uiso 1 1 calc R . . C42 C 0.116(2) 0.5108(11) 0.5868(16) 0.058(7) Uiso 1 1 d . . . H42A H 0.1160 0.5319 0.5250 0.088 Uiso 1 1 calc R . . H42B H 0.1608 0.5389 0.6422 0.088 Uiso 1 1 calc R . . H42C H 0.0164 0.5016 0.5868 0.088 Uiso 1 1 calc R . . C43 C 0.379(2) 0.6119(10) 1.0481(15) 0.053(7) Uiso 1 1 d . . . H43A H 0.3327 0.6023 1.0997 0.079 Uiso 1 1 calc R . . H43B H 0.3905 0.6583 1.0434 0.079 Uiso 1 1 calc R . . H43C H 0.4745 0.5915 1.0643 0.079 Uiso 1 1 calc R . . C44 C 0.244(3) 0.6967(12) 0.858(2) 0.091(10) Uiso 1 1 d . . . H44A H 0.3124 0.7208 0.9096 0.137 Uiso 1 1 calc R . . H44B H 0.1479 0.6988 0.8682 0.137 Uiso 1 1 calc R . . H44C H 0.2405 0.7153 0.7935 0.137 Uiso 1 1 calc R . . C45 C 0.670(3) 0.7108(11) 0.7353(18) 0.065(8) Uiso 1 1 d . . . H45A H 0.7753 0.7175 0.7495 0.078 Uiso 1 1 calc R . . H45B H 0.6290 0.7140 0.6632 0.078 Uiso 1 1 calc R . . C46 C 0.610(3) 0.7648(13) 0.7814(19) 0.076(9) Uiso 1 1 d . . . H46 H 0.5035 0.7587 0.7662 0.091 Uiso 1 1 calc R . . C47 C 0.672(3) 0.7674(14) 0.8930(19) 0.106(11) Uiso 1 1 d . . . H47A H 0.6488 0.7277 0.9220 0.160 Uiso 1 1 calc R . . H47B H 0.6300 0.8038 0.9191 0.160 Uiso 1 1 calc R . . H47C H 0.7769 0.7726 0.9096 0.160 Uiso 1 1 calc R . . C48 C 0.639(3) 0.8303(15) 0.733(2) 0.112(11) Uiso 1 1 d . . . H48A H 0.7405 0.8327 0.7341 0.169 Uiso 1 1 calc R . . H48B H 0.6156 0.8662 0.7707 0.169 Uiso 1 1 calc R . . H48C H 0.5782 0.8324 0.6651 0.169 Uiso 1 1 calc R . . C49 C 0.841(2) 0.6021(13) 0.6858(18) 0.087(9) Uiso 1 1 d . . . H49A H 0.9070 0.6054 0.7522 0.130 Uiso 1 1 calc R . . H49B H 0.8467 0.6413 0.6490 0.130 Uiso 1 1 calc R . . H49C H 0.8688 0.5653 0.6519 0.130 Uiso 1 1 calc R . . O50 O 0.0823(15) 0.4909(7) 0.8211(9) 0.049(4) Uiso 1 1 d . . . O51 O 0.3851(15) 0.6416(7) 0.6820(11) 0.053(4) Uiso 1 1 d . . . O52 O 0.5950(14) 0.4275(7) 0.8516(9) 0.043(4) Uiso 1 1 d . . . C53 C 0.905(2) 0.3631(11) 0.8830(16) 0.067(8) Uiso 1 1 d . . . H53A H 0.8283 0.3318 0.8577 0.101 Uiso 1 1 calc R . . H53B H 0.9880 0.3418 0.9281 0.101 Uiso 1 1 calc R . . H53C H 0.9347 0.3817 0.8280 0.101 Uiso 1 1 calc R . . C54 C 0.643(2) 0.4739(11) 0.6280(15) 0.059(8) Uiso 1 1 d . . . H54A H 0.7366 0.4746 0.6129 0.088 Uiso 1 1 calc R . . H54B H 0.5676 0.4879 0.5701 0.088 Uiso 1 1 calc R . . H54C H 0.6228 0.4304 0.6458 0.088 Uiso 1 1 calc R . . C55 C 0.944(2) 0.3569(11) 1.1042(16) 0.061(8) Uiso 1 1 d . . . H55A H 1.0199 0.3885 1.1314 0.091 Uiso 1 1 calc R . . H55B H 0.9828 0.3231 1.0707 0.091 Uiso 1 1 calc R . . H55C H 0.9111 0.3382 1.1575 0.091 Uiso 1 1 calc R . . C56 C 0.670(2) 0.4102(6) 1.1588(13) 0.067(8) Uiso 1 1 d . . . H56A H 0.7436 0.4043 1.2215 0.101 Uiso 1 1 calc R . . H56B H 0.6259 0.3689 1.1351 0.101 Uiso 1 1 calc R . . H56C H 0.5954 0.4395 1.1682 0.101 Uiso 1 1 calc R . . O57 O 0.7390(15) 0.5770(6) 1.0297(10) 0.057(5) Uiso 1 1 d R . . _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 O28 1.26(2) . ? C1 O29 1.32(2) . ? C1 C2 1.45(3) . ? C2 C3 1.52(2) . ? C2 C37 1.52(3) . ? C3 C4 1.51(2) . ? C3 C42 1.52(2) . ? C4 N6 1.43(2) . ? C4 C5 1.53(3) . ? N6 C7 1.24(2) . ? C7 O50 1.29(2) . ? C7 C8 1.57(3) . ? C8 C9 1.51(3) . ? C8 C41 1.54(3) . ? C9 C10 1.47(3) . ? C9 C43 1.54(2) . ? C10 N11 1.53(2) . ? C10 C44 1.54(3) . ? N11 C12 1.29(2) . ? C12 O51 1.24(2) . ? C12 C13 1.57(3) . ? C13 C14 1.49(2) . ? C13 C45 1.58(3) . ? C14 C15 1.55(3) . ? C14 C49 1.60(3) . ? C15 N16 1.45(2) . ? C15 C54 1.53(3) . ? N16 C17 1.28(2) . ? C17 O52 1.28(2) . ? C17 C18 1.55(2) . ? C18 C19 1.47(2) . ? C18 C53 1.50(2) . ? C19 C20 1.50(2) . ? C19 C55 1.57(3) . ? C20 N21 1.47(2) . ? C20 C56 1.55(2) . ? N21 C22 1.28(3) . ? C22 O57 1.30(2) . ? C22 O23 1.35(2) . ? O23 C24 1.45(3) . ? C24 C25 1.46(3) . ? C24 C27 1.50(3) . ? C24 C26 1.54(3) . ? O29 C30 1.47(2) . ? C30 C31 1.47(3) . ? C31 C32 1.29(3) . ? C31 C36 1.35(3) . ? C32 C33 1.45(4) . ? C33 C34 1.45(5) . ? C34 C35 1.29(4) . ? C35 C36 1.42(4) . ? C37 C38 1.53(3) . ? C38 C40 1.52(3) . ? C38 C39 1.53(3) . ? C45 C46 1.47(3) . ? C46 C47 1.50(3) . ? C46 C48 1.56(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 O28 C1 O29 118(2) . . ? O28 C1 C2 125(2) . . ? O29 C1 C2 117(2) . . ? C1 C2 C3 110(2) . . ? C1 C2 C37 112(2) . . ? C3 C2 C37 115.7(18) . . ? C4 C3 C2 114.8(18) . . ? C4 C3 C42 109.5(16) . . ? C2 C3 C42 108.6(16) . . ? N6 C4 C3 112.7(17) . . ? N6 C4 C5 107.3(17) . . ? C3 C4 C5 110.4(17) . . ? C7 N6 C4 123.9(18) . . ? N6 C7 O50 127(2) . . ? N6 C7 C8 121(2) . . ? O50 C7 C8 112(2) . . ? C9 C8 C41 115.9(18) . . ? C9 C8 C7 112.9(17) . . ? C41 C8 C7 107.8(17) . . ? C10 C9 C8 114.9(19) . . ? C10 C9 C43 113.3(19) . . ? C8 C9 C43 109.6(17) . . ? C9 C10 N11 110.5(18) . . ? C9 C10 C44 117(2) . . ? N11 C10 C44 109.5(19) . . ? C12 N11 C10 123.4(18) . . ? O51 C12 N11 125(2) . . ? O51 C12 C13 117(2) . . ? N11 C12 C13 117(2) . . ? C14 C13 C12 109.3(17) . . ? C14 C13 C45 109.0(18) . . ? C12 C13 C45 107.1(17) . . ? C13 C14 C15 112.6(18) . . ? C13 C14 C49 110.6(18) . . ? C15 C14 C49 111(2) . . ? N16 C15 C54 108.0(17) . . ? N16 C15 C14 113.3(18) . . ? C54 C15 C14 113.2(18) . . ? C17 N16 C15 121.7(19) . . ? O52 C17 N16 127(2) . . ? O52 C17 C18 115(2) . . ? N16 C17 C18 118.3(19) . . ? C19 C18 C53 112.1(18) . . ? C19 C18 C17 115.4(17) . . ? C53 C18 C17 105.9(16) . . ? C18 C19 C20 115.9(17) . . ? C18 C19 C55 112.9(18) . . ? C20 C19 C55 109.8(17) . . ? N21 C20 C19 112.1(16) . . ? N21 C20 C56 108.2(16) . . ? C19 C20 C56 115.7(15) . . ? C22 N21 C20 126(2) . . ? N21 C22 O57 125(2) . . ? N21 C22 O23 115(2) . . ? O57 C22 O23 120(2) . . ? C22 O23 C24 122(2) . . ? O23 C24 C25 112(2) . . ? O23 C24 C27 108(2) . . ? C25 C24 C27 114(2) . . ? O23 C24 C26 100(2) . . ? C25 C24 C26 110(2) . . ? C27 C24 C26 112(2) . . ? C1 O29 C30 121.2(19) . . ? O29 C30 C31 112(2) . . ? C32 C31 C36 123(3) . . ? C32 C31 C30 117(3) . . ? C36 C31 C30 120(3) . . ? C31 C32 C33 126(4) . . ? C34 C33 C32 107(4) . . ? C35 C34 C33 128(4) . . ? C34 C35 C36 119(4) . . ? C31 C36 C35 117(3) . . ? C2 C37 C38 117.4(19) . . ? C40 C38 C37 108(2) . . ? C40 C38 C39 108(3) . . ? C37 C38 C39 113(2) . . ? C46 C45 C13 118(2) . . ? C45 C46 C47 113(2) . . ? C45 C46 C48 109(2) . . ? C47 C46 C48 110(2) . . ? 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 O28 C1 C2 C3 -127(2) . . . . ? O29 C1 C2 C3 51(3) . . . . ? O28 C1 C2 C37 4(3) . . . . ? O29 C1 C2 C37 -179(2) . . . . ? C1 C2 C3 C4 -178.8(19) . . . . ? C37 C2 C3 C4 53(2) . . . . ? C1 C2 C3 C42 58(2) . . . . ? C37 C2 C3 C42 -70(2) . . . . ? C2 C3 C4 N6 174.5(17) . . . . ? C42 C3 C4 N6 -63(2) . . . . ? C2 C3 C4 C5 55(2) . . . . ? C42 C3 C4 C5 176.9(17) . . . . ? C3 C4 N6 C7 109(2) . . . . ? C5 C4 N6 C7 -129(2) . . . . ? C4 N6 C7 O50 -12(3) . . . . ? C4 N6 C7 C8 168.4(18) . . . . ? N6 C7 C8 C9 123(2) . . . . ? O50 C7 C8 C9 -56(2) . . . . ? N6 C7 C8 C41 -107(2) . . . . ? O50 C7 C8 C41 73(2) . . . . ? C41 C8 C9 C10 -175.4(18) . . . . ? C7 C8 C9 C10 -50(3) . . . . ? C41 C8 C9 C43 56(2) . . . . ? C7 C8 C9 C43 -179.3(18) . . . . ? C8 C9 C10 N11 -62(2) . . . . ? C43 C9 C10 N11 65(2) . . . . ? C8 C9 C10 C44 172(2) . . . . ? C43 C9 C10 C44 -61(3) . . . . ? C9 C10 N11 C12 156(2) . . . . ? C44 C10 N11 C12 -73(3) . . . . ? C10 N11 C12 O51 -6(4) . . . . ? C10 N11 C12 C13 170.6(17) . . . . ? O51 C12 C13 C14 -56(3) . . . . ? N11 C12 C13 C14 126(2) . . . . ? O51 C12 C13 C45 62(2) . . . . ? N11 C12 C13 C45 -116(2) . . . . ? C12 C13 C14 C15 -61(2) . . . . ? C45 C13 C14 C15 -177.8(19) . . . . ? C12 C13 C14 C49 174.4(18) . . . . ? C45 C13 C14 C49 58(2) . . . . ? C13 C14 C15 N16 -71(2) . . . . ? C49 C14 C15 N16 53(2) . . . . ? C13 C14 C15 C54 165.5(18) . . . . ? C49 C14 C15 C54 -70(2) . . . . ? C54 C15 N16 C17 -83(2) . . . . ? C14 C15 N16 C17 150.3(19) . . . . ? C15 N16 C17 O52 -8(3) . . . . ? C15 N16 C17 C18 168.1(17) . . . . ? O52 C17 C18 C19 -32(2) . . . . ? N16 C17 C18 C19 151.4(18) . . . . ? O52 C17 C18 C53 93(2) . . . . ? N16 C17 C18 C53 -84(2) . . . . ? C53 C18 C19 C20 -174.0(17) . . . . ? C17 C18 C19 C20 -53(2) . . . . ? C53 C18 C19 C55 58(2) . . . . ? C17 C18 C19 C55 179.4(17) . . . . ? C18 C19 C20 N21 -68(2) . . . . ? C55 C19 C20 N21 61(2) . . . . ? C18 C19 C20 C56 166.9(18) . . . . ? C55 C19 C20 C56 -64(2) . . . . ? C19 C20 N21 C22 114(2) . . . . ? C56 C20 N21 C22 -117(2) . . . . ? C20 N21 C22 O57 -7(3) . . . . ? C20 N21 C22 O23 169.4(17) . . . . ? N21 C22 O23 C24 173.2(19) . . . . ? O57 C22 O23 C24 -10(3) . . . . ? C22 O23 C24 C25 -58(3) . . . . ? C22 O23 C24 C27 67(3) . . . . ? C22 O23 C24 C26 -175.4(19) . . . . ? O28 C1 O29 C30 5(3) . . . . ? C2 C1 O29 C30 -173.1(19) . . . . ? C1 O29 C30 C31 162(2) . . . . ? O29 C30 C31 C32 91(3) . . . . ? O29 C30 C31 C36 -88(3) . . . . ? C36 C31 C32 C33 1(5) . . . . ? C30 C31 C32 C33 -177(3) . . . . ? C31 C32 C33 C34 -10(5) . . . . ? C32 C33 C34 C35 14(6) . . . . ? C33 C34 C35 C36 -8(6) . . . . ? C32 C31 C36 C35 6(4) . . . . ? C30 C31 C36 C35 -175(2) . . . . ? C34 C35 C36 C31 -3(5) . . . . ? C1 C2 C37 C38 71(3) . . . . ? C3 C2 C37 C38 -162(2) . . . . ? C2 C37 C38 C40 -178(2) . . . . ? C2 C37 C38 C39 63(3) . . . . ? C14 C13 C45 C46 165(2) . . . . ? C12 C13 C45 C46 47(3) . . . . ? C13 C45 C46 C47 61(3) . . . . ? C13 C45 C46 C48 -176(2) . . . . ? _diffrn_measured_fraction_theta_max 0.245 _diffrn_reflns_theta_full 66.23 _diffrn_measured_fraction_theta_full 0.245 _refine_diff_density_max 0.242 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.054 ----------