data_fc1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H19 N O3, C H2 Cl2' _chemical_formula_sum 'C21 H21 Cl2 N O3' _chemical_formula_weight 406.29 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' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6530(10) _cell_length_b 23.257(2) _cell_length_c 10.6200(10) _cell_angle_alpha 90.00 _cell_angle_beta 109.410(10) _cell_angle_gamma 90.00 _cell_volume 2015.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 289(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 11.5 _cell_measurement_theta_max 16.0 _exptl_crystal_description blocks _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 3.069 _exptl_absorpt_correction_type 'empirical, psi scans' _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_T_max 0.544 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 289(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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.6 _diffrn_reflns_number 2810 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 50.44 _reflns_number_total 2109 _reflns_number_gt 1549 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON' _computing_publication_material 'PLATON' _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^)+(0.1511P)^2^+0.5796P] 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_coef 0.0019(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2109 _refine_ls_number_parameters 265 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2175 _refine_ls_wR_factor_gt 0.2024 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.004 _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 N1 N 0.5056(4) 0.93202(16) 0.0976(4) 0.0469(11) Uani 1 1 d . . . H1A H 0.4437 0.9510 0.0300 0.056 Uiso 1 1 calc R . . C2 C 0.6378(6) 0.9604(2) 0.1746(5) 0.0509(13) Uani 1 1 d . . . C3 C 0.7439(6) 0.9320(2) 0.2994(5) 0.0600(15) Uani 1 1 d . . . H3A H 0.7159 0.9471 0.3743 0.072 Uiso 1 1 calc R . . H3B H 0.8572 0.9420 0.3133 0.072 Uiso 1 1 calc R . . C4 C 0.7280(6) 0.8673(2) 0.2977(5) 0.0547(14) Uani 1 1 d . . . H4A H 0.7828 0.8530 0.3872 0.066 Uiso 1 1 calc R . . H4B H 0.7848 0.8517 0.2404 0.066 Uiso 1 1 calc R . . C5 C 0.5502(6) 0.84466(19) 0.2491(5) 0.0474(13) Uani 1 1 d . . . C6 C 0.4509(5) 0.87359(18) 0.1113(5) 0.0432(12) Uani 1 1 d . . . O7 O 0.6724(4) 1.00847(16) 0.1429(4) 0.0765(13) Uani 1 1 d . . . C8 C 0.5563(7) 0.7805(2) 0.2153(6) 0.0600(15) Uani 1 1 d . . . H8A H 0.6566 0.7627 0.2722 0.072 Uiso 1 1 calc R . . H8B H 0.4632 0.7599 0.2247 0.072 Uiso 1 1 calc R . . C9 C 0.5501(6) 0.7816(2) 0.0726(5) 0.0537(14) Uani 1 1 d . . . C10 C 0.4879(5) 0.8337(2) 0.0132(5) 0.0453(13) Uani 1 1 d . . . C11 C 0.5929(7) 0.7384(3) -0.0022(7) 0.0724(17) Uani 1 1 d . . . H11A H 0.6343 0.7033 0.0364 0.087 Uiso 1 1 calc R . . C12 C 0.5716(7) 0.7495(3) -0.1348(7) 0.0768(19) Uani 1 1 d . . . H12A H 0.6017 0.7217 -0.1853 0.092 Uiso 1 1 calc R . . C13 C 0.5068(7) 0.8007(3) -0.1938(6) 0.0707(17) Uani 1 1 d . . . H13A H 0.4908 0.8067 -0.2839 0.085 Uiso 1 1 calc R . . C14 C 0.4655(5) 0.8432(2) -0.1204(5) 0.0542(14) Uani 1 1 d . . . H14A H 0.4229 0.8779 -0.1602 0.065 Uiso 1 1 calc R . . C15 C 0.4746(6) 0.8539(2) 0.3566(5) 0.0560(14) Uani 1 1 d . . . O16 O 0.4417(6) 0.81648(19) 0.4209(5) 0.0951(15) Uani 1 1 d . . . O17 O 0.4492(5) 0.90883(17) 0.3757(4) 0.0696(11) Uani 1 1 d . . . C18 C 0.3678(10) 0.9220(3) 0.4711(7) 0.103(2) Uani 1 1 d . . . H18A H 0.3672 0.9628 0.4836 0.124 Uiso 1 1 calc R . . H18B H 0.4251 0.9038 0.5548 0.124 Uiso 1 1 calc R . . H18C H 0.2571 0.9081 0.4383 0.124 Uiso 1 1 calc R . . C19 C 0.2643(5) 0.8745(2) 0.0865(5) 0.0448(13) Uani 1 1 d . . . C20 C 0.1711(6) 0.8248(2) 0.0459(5) 0.0537(14) Uani 1 1 d . . . H20A H 0.2217 0.7909 0.0342 0.064 Uiso 1 1 calc R . . C21 C 0.0033(6) 0.8253(3) 0.0227(5) 0.0634(16) Uani 1 1 d . . . H21A H -0.0572 0.7917 -0.0027 0.076 Uiso 1 1 calc R . . C22 C -0.0733(6) 0.8752(3) 0.0372(6) 0.0636(16) Uani 1 1 d . . . H22A H -0.1860 0.8757 0.0196 0.076 Uiso 1 1 calc R . . C23 C 0.0154(6) 0.9241(3) 0.0772(6) 0.0652(16) Uani 1 1 d . . . H23A H -0.0370 0.9578 0.0876 0.078 Uiso 1 1 calc R . . C24 C 0.1850(6) 0.9243(2) 0.1031(5) 0.0534(14) Uani 1 1 d . . . H24A H 0.2447 0.9579 0.1314 0.064 Uiso 1 1 calc R . . C25 C 0.9906(9) 0.9135(4) 0.7337(8) 0.114(3) Uani 1 1 d D . . H25A H 1.0573 0.8860 0.7961 0.170 Uiso 0.529(12) 1 d P A 1 H25B H 1.0022 0.9505 0.7828 0.170 Uiso 0.529(12) 1 d P A 1 Cl26 Cl 0.7950(8) 0.8922(10) 0.6830(7) 0.312(9) Uani 0.529(12) 1 d PD A 1 Cl27 Cl 1.0598(7) 0.9228(3) 0.6056(5) 0.105(2) Uani 0.529(12) 1 d PD A 1 H25C H 1.0062 0.8869 0.8065 0.170 Uiso 0.471(12) 1 d P A 2 H25D H 1.0661 0.9458 0.7726 0.170 Uiso 0.471(12) 1 d P A 2 Cl28 Cl 0.7979(11) 0.9400(4) 0.6962(9) 0.206(6) Uani 0.471(12) 1 d PD A 2 Cl29 Cl 1.0476(17) 0.8887(10) 0.6256(13) 0.304(10) Uani 0.471(12) 1 d PD 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 N1 0.028(2) 0.051(2) 0.056(2) 0.0109(19) 0.0062(19) -0.0062(19) C2 0.038(3) 0.049(3) 0.062(3) 0.007(3) 0.012(3) -0.007(3) C3 0.041(3) 0.066(4) 0.064(4) 0.009(3) 0.005(3) -0.014(3) C4 0.038(3) 0.061(3) 0.060(3) 0.012(3) 0.010(2) 0.002(2) C5 0.041(3) 0.045(3) 0.055(3) 0.008(2) 0.015(2) -0.005(2) C6 0.029(3) 0.042(3) 0.058(3) 0.008(2) 0.014(2) -0.006(2) O7 0.058(2) 0.062(3) 0.090(3) 0.020(2) -0.002(2) -0.024(2) C8 0.055(3) 0.051(3) 0.073(4) 0.007(3) 0.020(3) 0.003(3) C9 0.041(3) 0.050(3) 0.070(4) -0.001(3) 0.018(3) 0.001(2) C10 0.025(2) 0.057(3) 0.055(3) 0.000(3) 0.015(2) -0.004(2) C11 0.053(4) 0.067(4) 0.096(5) -0.009(3) 0.024(3) 0.006(3) C12 0.052(4) 0.093(5) 0.091(5) -0.029(4) 0.032(3) -0.004(3) C13 0.051(3) 0.093(5) 0.072(4) -0.014(4) 0.027(3) -0.005(3) C14 0.036(3) 0.064(3) 0.066(4) 0.001(3) 0.022(3) -0.007(2) C15 0.053(3) 0.057(4) 0.059(3) 0.007(3) 0.020(3) -0.011(3) O16 0.130(4) 0.078(3) 0.104(3) 0.016(3) 0.074(3) -0.015(3) O17 0.081(3) 0.070(3) 0.071(3) 0.0004(19) 0.042(2) 0.001(2) C18 0.118(6) 0.116(6) 0.097(5) -0.014(4) 0.065(5) -0.003(5) C19 0.033(3) 0.053(3) 0.050(3) 0.005(2) 0.016(2) -0.004(2) C20 0.039(3) 0.055(3) 0.069(3) 0.000(3) 0.020(3) -0.009(2) C21 0.044(3) 0.076(4) 0.074(4) -0.006(3) 0.024(3) -0.022(3) C22 0.033(3) 0.086(4) 0.075(4) -0.001(3) 0.022(3) -0.010(3) C23 0.043(3) 0.075(4) 0.084(4) -0.005(3) 0.030(3) 0.009(3) C24 0.040(3) 0.051(3) 0.070(4) -0.005(3) 0.021(3) -0.004(2) C25 0.091(5) 0.158(7) 0.088(5) -0.001(5) 0.023(4) -0.007(5) Cl26 0.094(4) 0.73(3) 0.105(4) 0.098(9) 0.017(3) -0.117(8) Cl27 0.105(4) 0.142(4) 0.066(3) -0.016(2) 0.025(2) -0.047(4) Cl28 0.176(8) 0.256(10) 0.138(5) -0.048(6) -0.011(5) 0.131(8) Cl29 0.205(12) 0.42(2) 0.216(11) -0.161(12) -0.031(8) 0.162(12) _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 N1 C2 1.338(6) . ? N1 C6 1.462(6) . ? N1 H1A 0.8600 . ? C2 O7 1.234(6) . ? C2 C3 1.492(7) . ? C3 C4 1.511(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.544(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C15 1.508(7) . ? C5 C8 1.540(7) . ? C5 C6 1.580(7) . ? C6 C10 1.507(7) . ? C6 C19 1.547(6) . ? C8 C9 1.499(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.388(7) . ? C9 C11 1.406(8) . ? C10 C14 1.385(7) . ? C11 C12 1.383(9) . ? C11 H11A 0.9300 . ? C12 C13 1.375(8) . ? C12 H12A 0.9300 . ? C13 C14 1.377(8) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O16 1.197(6) . ? C15 O17 1.324(6) . ? O17 C18 1.445(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C24 1.387(7) . ? C19 C20 1.393(6) . ? C20 C21 1.390(7) . ? C20 H20A 0.9300 . ? C21 C22 1.371(8) . ? C21 H21A 0.9300 . ? C22 C23 1.359(8) . ? C22 H22A 0.9300 . ? C23 C24 1.401(7) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 Cl29 1.506(12) . ? C25 Cl28 1.696(10) . ? C25 Cl26 1.671(9) . ? C25 Cl27 1.672(8) . ? C25 H25A 0.963(8) . ? C25 H25B 0.994(9) . ? C25 H25C 0.965(8) . ? C25 H25D 0.991(8) . ? Cl28 H25B 1.718(10) . ? Cl29 H25A 1.785(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C6 129.5(4) . . ? C2 N1 H1A 115.2 . . ? C6 N1 H1A 115.2 . . ? O7 C2 N1 121.1(4) . . ? O7 C2 C3 120.6(4) . . ? N1 C2 C3 118.3(4) . . ? C2 C3 C4 113.7(4) . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C5 114.9(4) . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? C5 C4 H4B 108.6 . . ? H4A C4 H4B 107.5 . . ? C15 C5 C8 111.8(4) . . ? C15 C5 C4 109.5(4) . . ? C8 C5 C4 107.5(4) . . ? C15 C5 C6 113.7(4) . . ? C8 C5 C6 104.3(4) . . ? C4 C5 C6 109.8(4) . . ? N1 C6 C10 110.7(4) . . ? N1 C6 C19 108.9(4) . . ? C10 C6 C19 109.9(4) . . ? N1 C6 C5 113.2(4) . . ? C10 C6 C5 101.7(4) . . ? C19 C6 C5 112.3(4) . . ? C9 C8 C5 103.0(4) . . ? C9 C8 H8A 111.2 . . ? C5 C8 H8A 111.2 . . ? C9 C8 H8B 111.2 . . ? C5 C8 H8B 111.2 . . ? H8A C8 H8B 109.1 . . ? C10 C9 C11 120.2(5) . . ? C10 C9 C8 110.7(4) . . ? C11 C9 C8 129.1(5) . . ? C9 C10 C14 120.4(5) . . ? C9 C10 C6 111.3(4) . . ? C14 C10 C6 128.4(4) . . ? C12 C11 C9 118.1(6) . . ? C12 C11 H11A 121.0 . . ? C9 C11 H11A 121.0 . . ? C13 C12 C11 121.5(6) . . ? C13 C12 H12A 119.3 . . ? C11 C12 H12A 119.3 . . ? C12 C13 C14 120.4(6) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C13 C14 C10 119.4(5) . . ? C13 C14 H14A 120.3 . . ? C10 C14 H14A 120.3 . . ? O16 C15 O17 122.0(5) . . ? O16 C15 C5 125.0(5) . . ? O17 C15 C5 112.9(4) . . ? C15 O17 C18 117.2(5) . . ? O17 C18 H18A 109.5 . . ? O17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 118.2(4) . . ? C24 C19 C6 121.4(4) . . ? C20 C19 C6 120.3(4) . . ? C21 C20 C19 120.7(5) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C22 C21 C20 120.2(5) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C23 C22 C21 120.0(5) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.7(5) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C19 C24 C23 120.2(5) . . ? C19 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? Cl29 C25 Cl28 120.4(7) . . ? Cl29 C25 Cl26 101.2(8) . . ? Cl28 C25 Cl26 38.8(7) . . ? Cl29 C25 Cl27 29.9(10) . . ? Cl28 C25 Cl27 110.6(6) . . ? Cl26 C25 Cl27 112.0(5) . . ? Cl29 C25 H25A 89.8(9) . . ? Cl28 C25 H25A 136.1(7) . . ? Cl26 C25 H25A 109.6(8) . . ? Cl27 C25 H25A 110.5(6) . . ? Cl29 C25 H25B 136.9(13) . . ? Cl28 C25 H25B 74.3(6) . . ? Cl26 C25 H25B 110.0(10) . . ? Cl27 C25 H25B 108.3(6) . . ? H25A C25 H25B 106.3(7) . . ? Cl29 C25 H25C 111.7(12) . . ? Cl28 C25 H25C 106.6(6) . . ? Cl26 C25 H25C 85.7(6) . . ? Cl27 C25 H25C 137.9(7) . . ? H25A C25 H25C 29.5(3) . . ? H25B C25 H25C 99.9(7) . . ? Cl29 C25 H25D 105.7(11) . . ? Cl28 C25 H25D 106.5(8) . . ? Cl26 C25 H25D 144.7(11) . . ? Cl27 C25 H25D 82.9(5) . . ? H25A C25 H25D 93.1(6) . . ? H25B C25 H25D 35.7(3) . . ? H25C C25 H25D 104.7(7) . . ? C25 Cl28 H25B 33.8(4) . . ? C25 Cl29 H25A 32.7(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 N1 C2 O7 174.6(5) . . . . ? C6 N1 C2 C3 -4.7(7) . . . . ? O7 C2 C3 C4 -156.8(5) . . . . ? N1 C2 C3 C4 22.4(7) . . . . ? C2 C3 C4 C5 -47.0(6) . . . . ? C3 C4 C5 C15 -74.4(6) . . . . ? C3 C4 C5 C8 164.0(4) . . . . ? C3 C4 C5 C6 51.1(6) . . . . ? C2 N1 C6 C10 -103.3(5) . . . . ? C2 N1 C6 C19 135.7(5) . . . . ? C2 N1 C6 C5 10.1(7) . . . . ? C15 C5 C6 N1 91.5(5) . . . . ? C8 C5 C6 N1 -146.5(4) . . . . ? C4 C5 C6 N1 -31.5(5) . . . . ? C15 C5 C6 C10 -149.7(4) . . . . ? C8 C5 C6 C10 -27.8(4) . . . . ? C4 C5 C6 C10 87.2(4) . . . . ? C15 C5 C6 C19 -32.3(5) . . . . ? C8 C5 C6 C19 89.6(4) . . . . ? C4 C5 C6 C19 -155.4(4) . . . . ? C15 C5 C8 C9 152.2(4) . . . . ? C4 C5 C8 C9 -87.6(5) . . . . ? C6 C5 C8 C9 29.0(5) . . . . ? C5 C8 C9 C10 -19.9(5) . . . . ? C5 C8 C9 C11 162.0(5) . . . . ? C11 C9 C10 C14 0.9(7) . . . . ? C8 C9 C10 C14 -177.5(4) . . . . ? C11 C9 C10 C6 -179.9(4) . . . . ? C8 C9 C10 C6 1.8(5) . . . . ? N1 C6 C10 C9 137.1(4) . . . . ? C19 C6 C10 C9 -102.6(4) . . . . ? C5 C6 C10 C9 16.6(5) . . . . ? N1 C6 C10 C14 -43.8(6) . . . . ? C19 C6 C10 C14 76.6(5) . . . . ? C5 C6 C10 C14 -164.3(4) . . . . ? C10 C9 C11 C12 0.2(8) . . . . ? C8 C9 C11 C12 178.2(5) . . . . ? C9 C11 C12 C13 -1.6(8) . . . . ? C11 C12 C13 C14 1.9(8) . . . . ? C12 C13 C14 C10 -0.8(7) . . . . ? C9 C10 C14 C13 -0.6(7) . . . . ? C6 C10 C14 C13 -179.7(4) . . . . ? C8 C5 C15 O16 9.0(7) . . . . ? C4 C5 C15 O16 -110.1(6) . . . . ? C6 C5 C15 O16 126.7(6) . . . . ? C8 C5 C15 O17 -172.1(4) . . . . ? C4 C5 C15 O17 68.9(5) . . . . ? C6 C5 C15 O17 -54.3(5) . . . . ? O16 C15 O17 C18 -4.7(8) . . . . ? C5 C15 O17 C18 176.3(5) . . . . ? N1 C6 C19 C24 -23.0(6) . . . . ? C10 C6 C19 C24 -144.4(4) . . . . ? C5 C6 C19 C24 103.2(5) . . . . ? N1 C6 C19 C20 156.7(4) . . . . ? C10 C6 C19 C20 35.2(6) . . . . ? C5 C6 C19 C20 -77.2(5) . . . . ? C24 C19 C20 C21 0.0(7) . . . . ? C6 C19 C20 C21 -179.7(4) . . . . ? C19 C20 C21 C22 1.2(8) . . . . ? C20 C21 C22 C23 -1.5(8) . . . . ? C21 C22 C23 C24 0.5(9) . . . . ? C20 C19 C24 C23 -1.0(7) . . . . ? C6 C19 C24 C23 178.7(5) . . . . ? C22 C23 C24 C19 0.8(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 50.44 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.588 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.059