# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2007 data_dbr30 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H32 N2 O4' _chemical_formula_weight 568.65 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)/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 12.027(2) _cell_length_b 10.945(2) _cell_length_c 24.151(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.89(3) _cell_angle_gamma 90.00 _cell_volume 3057.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9670 _exptl_absorpt_correction_T_max 0.9904 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 28453 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5330 _reflns_number_gt 4371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0590P)^2^+1.4139P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'constr' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5330 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.1602 _refine_ls_wR_factor_gt 0.1515 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.001 _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 C4 C 0.65093(19) 0.6745(2) 0.62425(11) 0.0417(6) Uani 1 1 d . . . H4 H 0.6718 0.7365 0.6546 0.050 Uiso 1 1 calc R . . C5 C 0.76701(19) 0.6309(2) 0.61224(10) 0.0373(5) Uani 1 1 d . . . C6 C 0.83075(19) 0.7447(2) 0.59707(10) 0.0356(5) Uani 1 1 d . . . H6 H 0.8386 0.8029 0.6287 0.043 Uiso 1 1 calc R . . C8 C 0.9520(2) 0.7170(2) 0.59363(10) 0.0379(6) Uani 1 1 d . . . C9 C 1.0461(2) 0.7546(3) 0.63720(12) 0.0538(7) Uani 1 1 d . . . H9 H 1.0342 0.7978 0.6682 0.065 Uiso 1 1 calc R . . C10 C 1.1574(2) 0.7293(3) 0.63558(14) 0.0711(9) Uani 1 1 d . . . H10 H 1.2195 0.7552 0.6655 0.085 Uiso 1 1 calc R . . C11 C 1.1774(3) 0.6665(3) 0.59040(16) 0.0713(10) Uani 1 1 d . . . H11 H 1.2525 0.6486 0.5896 0.086 Uiso 1 1 calc R . . C12 C 1.0854(3) 0.6303(3) 0.54652(15) 0.0684(9) Uani 1 1 d . . . H12 H 1.0981 0.5879 0.5155 0.082 Uiso 1 1 calc R . . C13 C 0.9735(2) 0.6561(3) 0.54765(13) 0.0554(7) Uani 1 1 d . . . H13 H 0.9120 0.6320 0.5170 0.067 Uiso 1 1 calc R . . C14 C 1.0393(3) 1.0708(3) 0.57625(13) 0.0613(8) Uani 1 1 d . . . H14 H 0.9994 0.9998 0.5618 0.074 Uiso 1 1 calc R . . C15 C 0.9784(2) 1.1763(2) 0.57867(11) 0.0507(7) Uani 1 1 d . . . C16 C 1.0393(3) 1.2799(3) 0.60009(12) 0.0585(7) Uani 1 1 d . . . H16 H 0.9998 1.3520 0.6024 0.070 Uiso 1 1 calc R . . C17 C 1.1581(3) 1.2785(3) 0.61820(14) 0.0666(8) Uani 1 1 d . . . H17 H 1.1985 1.3495 0.6322 0.080 Uiso 1 1 calc R . . C18 C 1.2167(3) 1.1727(3) 0.61558(14) 0.0672(8) Uani 1 1 d . . . H18 H 1.2971 1.1716 0.6280 0.081 Uiso 1 1 calc R . . C19 C 1.1573(3) 1.0688(3) 0.59479(14) 0.0677(9) Uani 1 1 d . . . H19 H 1.1971 0.9965 0.5932 0.081 Uiso 1 1 calc R . . C22 C 0.6872(2) 1.0695(2) 0.56419(12) 0.0554(7) Uani 1 1 d . . . C23 C 0.8493(3) 1.1810(3) 0.55630(15) 0.0709(9) Uani 1 1 d . . . H23A H 0.8206 1.2572 0.5676 0.085 Uiso 1 1 calc R . . H23B H 0.8267 1.1765 0.5146 0.085 Uiso 1 1 calc R . . C24 C 0.5906(2) 0.5729(2) 0.64700(12) 0.0482(6) Uani 1 1 d . . . C25 C 0.5218(3) 0.4874(3) 0.61159(16) 0.0732(9) Uani 1 1 d . . . H25 H 0.5085 0.4939 0.5719 0.088 Uiso 1 1 calc R . . C26 C 0.4728(3) 0.3931(4) 0.6340(2) 0.0934(12) Uani 1 1 d . . . H26 H 0.4275 0.3362 0.6092 0.112 Uiso 1 1 calc R . . C27 C 0.4891(3) 0.3813(4) 0.6913(2) 0.0951(13) Uani 1 1 d . . . H27 H 0.4555 0.3167 0.7059 0.114 Uiso 1 1 calc R . . C28 C 0.5557(3) 0.4656(4) 0.72787(18) 0.0870(12) Uani 1 1 d . . . H28 H 0.5672 0.4587 0.7674 0.104 Uiso 1 1 calc R . . C29 C 0.6060(3) 0.5614(3) 0.70541(14) 0.0637(8) Uani 1 1 d . . . H29 H 0.6508 0.6186 0.7303 0.076 Uiso 1 1 calc R . . C31 C 0.9389(2) 0.5728(3) 0.76339(11) 0.0545(7) Uani 1 1 d . . . H31A H 0.9154 0.4880 0.7638 0.065 Uiso 1 1 calc R . . H31B H 0.9243 0.6132 0.7965 0.065 Uiso 1 1 calc R . . C32 C 1.0657(2) 0.5786(2) 0.76778(10) 0.0476(6) Uani 1 1 d . . . C33 C 1.1231(3) 0.4836(3) 0.75055(13) 0.0645(8) Uani 1 1 d . . . H33 H 1.0839 0.4118 0.7368 0.077 Uiso 1 1 calc R . . C34 C 1.2392(3) 0.4950(4) 0.75367(15) 0.0808(11) Uani 1 1 d . . . H34 H 1.2777 0.4307 0.7418 0.097 Uiso 1 1 calc R . . C35 C 1.2980(3) 0.6004(4) 0.77416(15) 0.0826(11) Uani 1 1 d . . . H35 H 1.3758 0.6082 0.7757 0.099 Uiso 1 1 calc R . . C36 C 1.2414(3) 0.6932(3) 0.79218(14) 0.0727(9) Uani 1 1 d . . . H36 H 1.2811 0.7643 0.8066 0.087 Uiso 1 1 calc R . . C37 C 1.1262(3) 0.6830(3) 0.78925(12) 0.0582(7) Uani 1 1 d . . . H37 H 1.0887 0.7472 0.8019 0.070 Uiso 1 1 calc R . . C38 C 0.8416(2) 0.5616(2) 0.66384(10) 0.0382(5) Uani 1 1 d . . . C39 C 0.5757(2) 0.7384(2) 0.57053(11) 0.0480(6) Uani 1 1 d . . . H39 H 0.5531 0.6792 0.5396 0.058 Uiso 1 1 calc R . . H39A H 0.5059 0.7681 0.5787 0.058 Uiso 1 1 calc R . . C40 C 0.6363(2) 0.8451(2) 0.55045(11) 0.0460(6) Uani 1 1 d . . . H40 H 0.5882 0.8696 0.5124 0.055 Uiso 1 1 calc R . . C41 C 0.6479(2) 0.9576(2) 0.59048(11) 0.0476(6) Uani 1 1 d . . . H41 H 0.7056 0.9392 0.6269 0.057 Uiso 1 1 calc R . . C42 C 0.7537(2) 0.8060(2) 0.54324(10) 0.0434(6) Uani 1 1 d . . . H42 H 0.7932 0.8773 0.5341 0.052 Uiso 1 1 calc R . . H42A H 0.7414 0.7498 0.5111 0.052 Uiso 1 1 calc R . . C43 C 0.7391(2) 0.5437(2) 0.56348(12) 0.0446(6) Uani 1 1 d . . . C44 C 0.5375(3) 0.9853(3) 0.60281(14) 0.0645(8) Uani 1 1 d . . . N3 N 0.4533(3) 1.0050(3) 0.61321(16) 0.1040(11) Uani 1 1 d . . . N4 N 0.7146(2) 0.4816(2) 0.52427(11) 0.0655(7) Uani 1 1 d . . . O1 O 0.86987(14) 0.63196(16) 0.71011(7) 0.0446(4) Uani 1 1 d . . . O3 O 0.62504(19) 1.1386(2) 0.53330(13) 0.1112(11) Uani 1 1 d . . . O4 O 0.80107(15) 1.07851(16) 0.58001(8) 0.0536(5) Uani 1 1 d . . . O6 O 0.86953(17) 0.45753(16) 0.66236(8) 0.0597(5) 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 C4 0.0299(12) 0.0456(14) 0.0503(15) -0.0004(12) 0.0122(11) 0.0021(10) C5 0.0305(12) 0.0419(13) 0.0389(13) 0.0036(11) 0.0084(10) 0.0038(10) C6 0.0381(12) 0.0346(13) 0.0350(12) 0.0006(10) 0.0114(10) 0.0020(10) C8 0.0413(13) 0.0333(13) 0.0422(14) 0.0084(11) 0.0167(11) 0.0036(10) C9 0.0416(15) 0.0687(19) 0.0522(16) 0.0026(14) 0.0148(12) 0.0028(13) C10 0.0395(16) 0.100(3) 0.071(2) 0.0150(19) 0.0112(15) 0.0023(16) C11 0.0482(18) 0.082(2) 0.096(3) 0.028(2) 0.0397(18) 0.0191(16) C12 0.069(2) 0.066(2) 0.089(2) -0.0006(18) 0.0515(19) 0.0068(16) C13 0.0539(16) 0.0579(17) 0.0622(18) -0.0035(14) 0.0288(14) -0.0044(14) C14 0.065(2) 0.0498(17) 0.0687(19) -0.0036(15) 0.0180(15) -0.0089(15) C15 0.0541(16) 0.0500(16) 0.0491(16) 0.0079(13) 0.0161(13) -0.0022(13) C16 0.0628(19) 0.0513(17) 0.0661(19) -0.0039(15) 0.0254(15) -0.0027(14) C17 0.0612(19) 0.064(2) 0.078(2) -0.0140(17) 0.0243(16) -0.0175(16) C18 0.0482(17) 0.075(2) 0.084(2) -0.0006(18) 0.0275(16) -0.0066(16) C19 0.062(2) 0.062(2) 0.088(2) -0.0004(17) 0.0360(17) 0.0098(16) C22 0.0413(15) 0.0470(16) 0.0667(18) 0.0056(14) -0.0040(13) 0.0078(13) C23 0.0598(19) 0.0579(19) 0.086(2) 0.0230(17) 0.0054(16) -0.0019(15) C24 0.0332(13) 0.0508(16) 0.0651(18) 0.0068(14) 0.0212(12) 0.0059(12) C25 0.0547(18) 0.078(2) 0.088(2) 0.0057(19) 0.0221(17) -0.0214(17) C26 0.066(2) 0.087(3) 0.133(4) 0.007(3) 0.038(2) -0.032(2) C27 0.068(2) 0.086(3) 0.149(4) 0.037(3) 0.060(3) -0.004(2) C28 0.074(2) 0.107(3) 0.098(3) 0.040(2) 0.053(2) 0.021(2) C29 0.0551(17) 0.074(2) 0.072(2) 0.0123(17) 0.0340(15) 0.0070(15) C31 0.0568(17) 0.0662(18) 0.0386(14) 0.0097(13) 0.0101(12) 0.0050(14) C32 0.0509(15) 0.0529(16) 0.0344(13) 0.0067(12) 0.0038(11) 0.0072(13) C33 0.0604(19) 0.0584(19) 0.0639(19) -0.0072(15) -0.0014(15) 0.0122(15) C34 0.065(2) 0.096(3) 0.075(2) -0.007(2) 0.0090(18) 0.033(2) C35 0.0501(19) 0.119(3) 0.073(2) 0.011(2) 0.0068(16) 0.009(2) C36 0.059(2) 0.082(2) 0.070(2) 0.0060(18) 0.0045(16) -0.0090(18) C37 0.0632(19) 0.0558(18) 0.0500(17) 0.0013(14) 0.0063(14) 0.0038(14) C38 0.0352(12) 0.0353(14) 0.0475(14) 0.0025(11) 0.0169(11) -0.0011(10) C39 0.0320(13) 0.0515(16) 0.0557(16) 0.0044(13) 0.0040(11) 0.0042(11) C40 0.0376(13) 0.0498(15) 0.0425(14) 0.0079(12) -0.0029(11) 0.0043(11) C41 0.0333(13) 0.0496(15) 0.0545(16) 0.0062(13) 0.0027(11) 0.0106(11) C42 0.0483(15) 0.0426(14) 0.0387(13) 0.0061(11) 0.0109(11) 0.0026(11) C43 0.0400(14) 0.0446(15) 0.0488(16) 0.0010(13) 0.0116(12) -0.0027(11) C44 0.0438(17) 0.066(2) 0.080(2) -0.0064(16) 0.0121(15) 0.0110(14) N3 0.0541(18) 0.120(3) 0.141(3) -0.024(2) 0.0326(19) 0.0183(18) N4 0.0666(16) 0.0651(17) 0.0625(16) -0.0195(14) 0.0138(13) -0.0065(13) O1 0.0445(10) 0.0486(10) 0.0395(10) 0.0019(8) 0.0095(7) 0.0071(8) O3 0.0573(14) 0.0792(16) 0.163(3) 0.0645(18) -0.0278(15) -0.0012(12) O4 0.0418(10) 0.0515(11) 0.0636(12) 0.0130(9) 0.0078(9) 0.0047(8) O6 0.0696(13) 0.0379(11) 0.0659(13) 0.0043(9) 0.0091(10) 0.0130(9) _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 C4 C24 1.511(3) . ? C4 C39 1.532(3) . ? C4 C5 1.575(3) . ? C4 H4 0.9800 . ? C5 C43 1.481(4) . ? C5 C38 1.524(3) . ? C5 C6 1.558(3) . ? C6 C8 1.514(3) . ? C6 C42 1.529(3) . ? C6 H6 0.9800 . ? C8 C9 1.380(4) . ? C8 C13 1.379(3) . ? C9 C10 1.378(4) . ? C9 H9 0.9300 . ? C10 C11 1.366(5) . ? C10 H10 0.9300 . ? C11 C12 1.365(5) . ? C11 H11 0.9300 . ? C12 C13 1.382(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.366(4) . ? C14 C15 1.377(4) . ? C14 H14 0.9300 . ? C15 C16 1.372(4) . ? C15 C23 1.499(4) . ? C16 C17 1.375(4) . ? C16 H16 0.9300 . ? C17 C18 1.366(4) . ? C17 H17 0.9300 . ? C18 C19 1.364(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C22 O3 1.176(3) . ? C22 O4 1.321(3) . ? C22 C41 1.513(4) . ? C23 O4 1.451(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C29 1.377(4) . ? C24 C25 1.380(4) . ? C25 C26 1.371(5) . ? C25 H25 0.9300 . ? C26 C27 1.350(6) . ? C26 H26 0.9300 . ? C27 C28 1.373(6) . ? C27 H27 0.9300 . ? C28 C29 1.393(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C31 O1 1.476(3) . ? C31 C32 1.501(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.373(4) . ? C32 C37 1.378(4) . ? C33 C34 1.384(5) . ? C33 H33 0.9300 . ? C34 C35 1.373(5) . ? C34 H34 0.9300 . ? C35 C36 1.359(5) . ? C35 H35 0.9300 . ? C36 C37 1.372(4) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 O6 1.190(3) . ? C38 O1 1.323(3) . ? C39 C40 1.525(4) . ? C39 H39 0.9700 . ? C39 H39A 0.9700 . ? C40 C42 1.530(3) . ? C40 C41 1.548(4) . ? C40 H40 0.9800 . ? C41 C44 1.470(4) . ? C41 H41 0.9800 . ? C42 H42 0.9700 . ? C42 H42A 0.9700 . ? C43 N4 1.137(3) . ? C44 N3 1.130(4) . ? 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 C24 C4 C39 114.4(2) . . ? C24 C4 C5 112.47(19) . . ? C39 C4 C5 109.3(2) . . ? C24 C4 H4 106.8 . . ? C39 C4 H4 106.8 . . ? C5 C4 H4 106.8 . . ? C43 C5 C38 106.5(2) . . ? C43 C5 C6 110.33(19) . . ? C38 C5 C6 111.90(18) . . ? C43 C5 C4 108.76(19) . . ? C38 C5 C4 110.70(19) . . ? C6 C5 C4 108.63(18) . . ? C8 C6 C42 114.19(19) . . ? C8 C6 C5 113.35(18) . . ? C42 C6 C5 109.15(19) . . ? C8 C6 H6 106.5 . . ? C42 C6 H6 106.5 . . ? C5 C6 H6 106.5 . . ? C9 C8 C13 117.6(2) . . ? C9 C8 C6 120.0(2) . . ? C13 C8 C6 122.5(2) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 120.6(3) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 118.9(3) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 120.8(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C8 C13 C12 120.8(3) . . ? C8 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C19 C14 C15 121.1(3) . . ? C19 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 118.3(3) . . ? C16 C15 C23 120.1(3) . . ? C14 C15 C23 121.6(3) . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 119.9(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 119.9(3) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? O3 C22 O4 124.4(3) . . ? O3 C22 C41 124.7(3) . . ? O4 C22 C41 110.9(2) . . ? O4 C23 C15 108.6(2) . . ? O4 C23 H23A 110.0 . . ? C15 C23 H23A 110.0 . . ? O4 C23 H23B 110.0 . . ? C15 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? C29 C24 C25 117.6(3) . . ? C29 C24 C4 119.7(3) . . ? C25 C24 C4 122.7(3) . . ? C26 C25 C24 121.0(3) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C27 C26 C25 121.3(4) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 119.4(3) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C27 C28 C29 119.6(4) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C24 C29 C28 121.1(3) . . ? C24 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? O1 C31 C32 111.2(2) . . ? O1 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? O1 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C33 C32 C37 119.0(3) . . ? C33 C32 C31 122.1(3) . . ? C37 C32 C31 118.9(3) . . ? C32 C33 C34 119.9(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.5(3) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C35 C34 119.3(3) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 120.7(3) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C32 120.6(3) . . ? C36 C37 H37 119.7 . . ? C32 C37 H37 119.7 . . ? O6 C38 O1 125.0(2) . . ? O6 C38 C5 124.0(2) . . ? O1 C38 C5 111.0(2) . . ? C40 C39 C4 113.3(2) . . ? C40 C39 H39 108.9 . . ? C4 C39 H39 108.9 . . ? C40 C39 H39A 108.9 . . ? C4 C39 H39A 108.9 . . ? H39 C39 H39A 107.7 . . ? C39 C40 C42 111.0(2) . . ? C39 C40 C41 112.3(2) . . ? C42 C40 C41 111.4(2) . . ? C39 C40 H40 107.3 . . ? C42 C40 H40 107.3 . . ? C41 C40 H40 107.3 . . ? C44 C41 C22 108.8(2) . . ? C44 C41 C40 111.0(2) . . ? C22 C41 C40 111.5(2) . . ? C44 C41 H41 108.5 . . ? C22 C41 H41 108.5 . . ? C40 C41 H41 108.5 . . ? C40 C42 C6 112.9(2) . . ? C40 C42 H42 109.0 . . ? C6 C42 H42 109.0 . . ? C40 C42 H42A 109.0 . . ? C6 C42 H42A 109.0 . . ? H42 C42 H42A 107.8 . . ? N4 C43 C5 176.4(3) . . ? N3 C44 C41 178.6(4) . . ? C38 O1 C31 115.7(2) . . ? C22 O4 C23 116.0(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.233 _refine_diff_density_min -0.158 _refine_diff_density_rms 0.038