data_CL111B _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 N2 O8' _chemical_formula_weight 604.68 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.6543(6) _cell_length_b 12.7816(9) _cell_length_c 29.198(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3229.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3081 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 19.92 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.089 _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 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_% ? _diffrn_reflns_number 26884 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.1045 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6360 _reflns_number_gt 2928 _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, 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^)+(0.0110P)^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 constr _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 0.5(10) _refine_ls_number_reflns 6360 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1333 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.003 _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 0.5064(3) -0.1231(2) 0.09997(10) 0.0614(9) Uani 1 1 d . . . H1A H 0.5891 -0.0984 0.0803 0.074 Uiso 1 1 calc R . . H1B H 0.5257 -0.1963 0.1066 0.074 Uiso 1 1 calc R . . C2 C 0.5095(4) -0.0612(3) 0.14477(13) 0.0901(12) Uani 1 1 d . . . H2A H 0.4224 -0.0827 0.1635 0.108 Uiso 1 1 calc R . . H2B H 0.6031 -0.0788 0.1613 0.108 Uiso 1 1 calc R . . C3 C 0.5033(4) 0.0518(4) 0.13853(14) 0.0980(14) Uani 1 1 d . . . H3 H 0.5827 0.0848 0.1226 0.118 Uiso 1 1 calc R . . C4 C 0.3818(5) 0.1121(4) 0.15572(12) 0.0827(13) Uani 1 1 d . . . H4 H 0.3016 0.0782 0.1709 0.099 Uiso 1 1 calc R . . C5 C 0.3750(5) 0.2226(4) 0.15107(13) 0.1081(14) Uani 1 1 d . . . H5A H 0.2889 0.2405 0.1313 0.130 Uiso 1 1 calc R . . H5B H 0.4689 0.2467 0.1364 0.130 Uiso 1 1 calc R . . C6 C 0.3563(4) 0.2786(3) 0.19597(11) 0.0699(10) Uani 1 1 d . . . H6A H 0.4374 0.2552 0.2165 0.084 Uiso 1 1 calc R . . H6B H 0.3714 0.3528 0.1908 0.084 Uiso 1 1 calc R . . C7 C 0.1521(3) 0.1881(2) 0.25219(9) 0.0382(7) Uani 1 1 d . . . H7 H 0.1549 0.1162 0.2405 0.046 Uiso 1 1 calc R . . C8 C -0.0099(3) 0.2413(2) 0.24452(9) 0.0382(7) Uani 1 1 d . . . C9 C 0.0789(4) 0.3201(3) 0.21457(11) 0.0491(9) Uani 1 1 d . . . C10 C 0.2219(3) 0.1969(2) 0.29931(9) 0.0479(8) Uani 1 1 d . . . H10 H 0.2270 0.2708 0.3081 0.057 Uiso 1 1 calc R . . C11 C 0.3694(4) 0.0621(3) 0.32859(11) 0.0546(9) Uani 1 1 d . . . C12 C 0.1320(4) 0.1363(2) 0.33589(9) 0.0588(9) Uani 1 1 d . . . H12A H 0.0757 0.1834 0.3559 0.071 Uiso 1 1 calc R . . H12B H 0.0599 0.0875 0.3221 0.071 Uiso 1 1 calc R . . C13 C -0.2345(3) 0.2384(3) 0.28833(10) 0.0725(11) Uani 1 1 d . . . H13A H -0.3130 0.2925 0.2889 0.087 Uiso 1 1 calc R . . H13B H -0.2420 0.1971 0.3161 0.087 Uiso 1 1 calc R . . C14 C -0.2510(3) 0.1709(2) 0.24673(9) 0.0558(9) Uani 1 1 d . . . H14 H -0.3387 0.1318 0.2399 0.067 Uiso 1 1 calc R . . C15 C -0.1264(3) 0.1735(2) 0.22100(9) 0.0389(7) Uani 1 1 d . . . C16 C -0.0925(3) 0.1163(2) 0.17804(10) 0.0336(7) Uani 1 1 d . . . C17 C -0.0979(3) 0.1660(2) 0.13616(10) 0.0447(8) Uani 1 1 d . . . H17 H -0.1224 0.2368 0.1348 0.054 Uiso 1 1 calc R . . C18 C -0.0672(3) 0.1119(2) 0.09598(9) 0.0461(9) Uani 1 1 d . . . H18 H -0.0739 0.1464 0.0680 0.055 Uiso 1 1 calc R . . C19 C -0.0265(3) 0.0070(2) 0.09705(9) 0.0336(7) Uani 1 1 d . . . C20 C -0.0162(3) -0.0419(2) 0.13959(9) 0.0454(8) Uani 1 1 d . . . H20 H 0.0141 -0.1116 0.1413 0.054 Uiso 1 1 calc R . . C21 C -0.0507(3) 0.0126(2) 0.17949(10) 0.0435(8) Uani 1 1 d . . . H21 H -0.0454 -0.0216 0.2076 0.052 Uiso 1 1 calc R . . C22 C -0.0007(3) -0.0536(2) 0.05472(9) 0.0405(8) Uani 1 1 d . . . C23 C -0.1020(4) -0.0699(2) 0.02179(10) 0.0556(9) Uani 1 1 d . . . H23 H -0.2020 -0.0434 0.0214 0.067 Uiso 1 1 calc R . . C24 C -0.0338(4) -0.1366(3) -0.01450(10) 0.0691(10) Uani 1 1 d . . . H24A H -0.0892 -0.2024 -0.0169 0.083 Uiso 1 1 calc R . . H24B H -0.0373 -0.1014 -0.0439 0.083 Uiso 1 1 calc R . . C25 C 0.1482(3) -0.1033(2) 0.04181(9) 0.0411(8) Uani 1 1 d . . . C26 C 0.2340(4) -0.1754(3) 0.07665(10) 0.0460(8) Uani 1 1 d . . . C27 C 0.3000(3) -0.0363(2) 0.04307(9) 0.0408(8) Uani 1 1 d . . . H27 H 0.2837 0.0320 0.0575 0.049 Uiso 1 1 calc R . . C28 C 0.3838(3) -0.0273(2) -0.00205(9) 0.0470(8) Uani 1 1 d . . . H28 H 0.4007 -0.0966 -0.0155 0.056 Uiso 1 1 calc R . . C29 C 0.2993(4) 0.0446(2) -0.03600(10) 0.0597(10) Uani 1 1 d . . . H29A H 0.2856 0.0099 -0.0653 0.072 Uiso 1 1 calc R . . H29B H 0.1987 0.0642 -0.0242 0.072 Uiso 1 1 calc R . . C30 C 0.5480(4) 0.1008(3) -0.03029(13) 0.0717(11) Uani 1 1 d . . . C31 C 0.6204(4) 0.0459(3) -0.07223(12) 0.1254(17) Uani 1 1 d . . . H31A H 0.7281 0.0336 -0.0666 0.188 Uiso 1 1 calc R . . H31B H 0.6090 0.0897 -0.0987 0.188 Uiso 1 1 calc R . . H31C H 0.5690 -0.0196 -0.0774 0.188 Uiso 1 1 calc R . . C32 C 0.6362(4) 0.1898(3) -0.01324(14) 0.144(2) Uani 1 1 d . . . H32A H 0.5780 0.2249 0.0101 0.216 Uiso 1 1 calc R . . H32B H 0.6564 0.2374 -0.0380 0.216 Uiso 1 1 calc R . . H32C H 0.7323 0.1656 -0.0007 0.216 Uiso 1 1 calc R . . C34 C 0.5204(3) 0.0516(2) 0.35366(10) 0.0708(10) Uani 1 1 d . . . H34A H 0.5462 0.1171 0.3678 0.106 Uiso 1 1 calc R . . H34B H 0.6002 0.0324 0.3324 0.106 Uiso 1 1 calc R . . H34C H 0.5112 -0.0015 0.3768 0.106 Uiso 1 1 calc R . . C33 C 0.3314(3) -0.0346(2) 0.30013(11) 0.0773(11) Uani 1 1 d . . . H33A H 0.3303 -0.0952 0.3196 0.116 Uiso 1 1 calc R . . H33B H 0.4083 -0.0435 0.2767 0.116 Uiso 1 1 calc R . . H33C H 0.2318 -0.0261 0.2862 0.116 Uiso 1 1 calc R . . N1 N 0.3605(3) -0.11396(19) 0.07555(8) 0.0462(7) Uani 1 1 d . . . N2 N 0.2097(3) 0.26406(19) 0.21841(8) 0.0475(7) Uani 1 1 d . . . O1 O 0.2046(2) -0.25639(17) 0.09642(7) 0.0635(6) Uani 1 1 d . . . O2 O 0.0508(2) 0.40058(17) 0.19439(7) 0.0726(7) Uani 1 1 d . . . O3 O 0.5280(2) 0.02536(16) 0.00509(6) 0.0582(6) Uani 1 1 d . . . O4 O 0.3937(3) 0.13276(17) -0.04082(7) 0.0738(7) Uani 1 1 d . . . O5 O 0.3739(2) 0.15357(16) 0.30010(6) 0.0566(6) Uani 1 1 d . . . O6 O 0.2517(3) 0.08228(17) 0.36030(7) 0.0703(7) Uani 1 1 d . . . O7 O 0.1223(2) -0.15401(16) -0.00058(6) 0.0580(6) Uani 1 1 d . . . O8 O -0.0832(2) 0.28294(14) 0.28355(6) 0.0549(6) 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 0.049(2) 0.067(3) 0.068(2) 0.003(2) -0.008(2) 0.006(2) C2 0.088(3) 0.064(3) 0.118(4) 0.001(3) -0.054(3) -0.001(3) C3 0.063(3) 0.115(4) 0.116(4) -0.024(3) -0.029(3) -0.003(3) C4 0.092(3) 0.088(3) 0.068(3) -0.004(3) -0.005(3) -0.037(3) C5 0.092(3) 0.142(4) 0.091(3) 0.008(3) -0.001(3) -0.003(4) C6 0.059(2) 0.080(3) 0.070(3) 0.008(2) 0.004(2) -0.006(2) C7 0.0396(19) 0.0346(19) 0.0403(19) 0.0030(16) 0.0008(16) -0.0028(16) C8 0.0419(19) 0.0351(18) 0.0375(19) -0.0083(16) 0.0070(16) -0.0009(17) C9 0.048(2) 0.041(2) 0.058(2) -0.0072(19) -0.0086(19) 0.003(2) C10 0.051(2) 0.049(2) 0.044(2) -0.0012(17) -0.0070(18) -0.0058(18) C11 0.058(2) 0.049(2) 0.057(2) 0.005(2) -0.008(2) -0.002(2) C12 0.065(2) 0.060(2) 0.052(2) 0.0048(18) 0.004(2) 0.005(2) C13 0.047(2) 0.101(3) 0.070(3) -0.024(2) 0.019(2) -0.002(2) C14 0.045(2) 0.076(3) 0.046(2) -0.015(2) 0.0068(18) -0.009(2) C15 0.0337(18) 0.0393(19) 0.0437(19) -0.0031(16) 0.0028(17) -0.0020(17) C16 0.0294(17) 0.0359(19) 0.0354(18) -0.0034(16) 0.0001(15) -0.0018(15) C17 0.056(2) 0.0302(18) 0.047(2) 0.0014(18) -0.0010(18) 0.0035(17) C18 0.059(2) 0.051(2) 0.0287(19) 0.0059(17) 0.0000(17) 0.0057(19) C19 0.0329(17) 0.0376(19) 0.0303(18) -0.0016(16) -0.0009(15) -0.0018(16) C20 0.060(2) 0.0358(19) 0.0408(19) 0.0045(17) 0.0029(18) 0.0079(17) C21 0.058(2) 0.0378(19) 0.0348(19) 0.0055(16) 0.0029(16) 0.0037(17) C22 0.042(2) 0.049(2) 0.0309(19) -0.0018(16) 0.0005(16) -0.0034(18) C23 0.047(2) 0.074(2) 0.046(2) -0.0151(19) -0.0051(18) 0.005(2) C24 0.068(3) 0.090(3) 0.049(2) -0.016(2) -0.011(2) -0.006(2) C25 0.048(2) 0.045(2) 0.0307(18) -0.0160(16) 0.0035(17) -0.0025(18) C26 0.054(2) 0.046(2) 0.038(2) -0.0042(18) 0.0139(18) 0.004(2) C27 0.044(2) 0.041(2) 0.0366(18) -0.0018(16) 0.0053(16) 0.0028(17) C28 0.050(2) 0.049(2) 0.043(2) -0.0003(17) 0.0031(18) 0.0012(19) C29 0.063(2) 0.067(3) 0.049(2) 0.004(2) 0.0042(18) -0.011(2) C30 0.058(3) 0.072(3) 0.085(3) 0.028(2) -0.007(2) -0.004(2) C31 0.089(3) 0.199(5) 0.088(3) 0.045(3) 0.037(3) 0.019(4) C32 0.117(4) 0.086(3) 0.229(5) 0.052(3) -0.080(4) -0.054(3) C34 0.075(2) 0.069(2) 0.069(2) 0.001(2) -0.026(2) 0.004(2) C33 0.063(2) 0.057(2) 0.112(3) -0.014(2) -0.023(2) 0.003(2) N1 0.0448(17) 0.0506(18) 0.0431(16) 0.0050(13) -0.0006(15) 0.0018(16) N2 0.0455(16) 0.0515(18) 0.0454(17) 0.0068(15) 0.0037(15) -0.0026(16) O1 0.0701(15) 0.0542(15) 0.0661(15) 0.0095(13) 0.0116(13) -0.0006(14) O2 0.0807(18) 0.0501(16) 0.0869(18) 0.0174(12) 0.0006(14) 0.0094(14) O3 0.0463(13) 0.0673(17) 0.0608(15) 0.0190(12) 0.0043(12) -0.0051(12) O4 0.0705(18) 0.0576(17) 0.0934(17) 0.0207(14) -0.0141(15) -0.0029(15) O5 0.0491(14) 0.0647(15) 0.0560(13) 0.0111(12) -0.0087(12) -0.0027(13) O6 0.0749(16) 0.0838(18) 0.0523(15) 0.0216(13) 0.0028(14) 0.0165(15) O7 0.0647(15) 0.0660(15) 0.0433(13) -0.0215(12) -0.0010(13) -0.0010(13) O8 0.0573(15) 0.0562(14) 0.0514(14) -0.0224(11) 0.0082(12) -0.0009(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 C1 N1 1.455(3) . ? C1 C2 1.529(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.457(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.397(5) . ? C3 H3 0.9300 . ? C4 C5 1.420(4) . ? C4 H4 0.9300 . ? C5 C6 1.502(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N2 1.440(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.471(3) . ? C7 C10 1.507(3) . ? C7 C8 1.574(4) . ? C7 H7 0.9800 . ? C8 O8 1.409(3) . ? C8 C15 1.496(3) . ? C8 C9 1.540(4) . ? C9 O2 1.210(3) . ? C9 N2 1.345(3) . ? C10 O5 1.427(3) . ? C10 C12 1.532(3) . ? C10 H10 0.9800 . ? C11 O6 1.401(3) . ? C11 O5 1.435(3) . ? C11 C34 1.504(3) . ? C11 C33 1.525(4) . ? C12 O6 1.435(3) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 O8 1.435(3) . ? C13 C14 1.497(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.315(3) . ? C14 H14 0.9300 . ? C15 C16 1.481(3) . ? C16 C17 1.379(3) . ? C16 C21 1.376(3) . ? C17 C18 1.388(3) . ? C17 H17 0.9300 . ? C18 C19 1.387(3) . ? C18 H18 0.9300 . ? C19 C20 1.393(3) . ? C19 C22 1.476(3) . ? C20 C21 1.390(3) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.318(3) . ? C22 C25 1.485(3) . ? C23 C24 1.483(3) . ? C23 H23 0.9300 . ? C24 O7 1.428(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 O7 1.415(3) . ? C25 C26 1.560(4) . ? C25 C27 1.568(3) . ? C26 O1 1.213(3) . ? C26 N1 1.347(3) . ? C27 N1 1.469(3) . ? C27 C28 1.508(3) . ? C27 H27 0.9800 . ? C28 O3 1.433(3) . ? C28 C29 1.537(3) . ? C28 H28 0.9800 . ? C29 O4 1.398(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O3 1.423(4) . ? C30 O4 1.430(4) . ? C30 C32 1.458(4) . ? C30 C31 1.544(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? 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 N1 C1 C2 113.2(3) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C1 113.9(3) . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C2 121.9(4) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 123.0(4) . . ? C3 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? C4 C5 C6 113.3(3) . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N2 C6 C5 115.5(3) . . ? N2 C6 H6A 108.4 . . ? C5 C6 H6A 108.4 . . ? N2 C6 H6B 108.4 . . ? C5 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? N2 C7 C10 115.3(2) . . ? N2 C7 C8 85.5(2) . . ? C10 C7 C8 117.0(2) . . ? N2 C7 H7 112.2 . . ? C10 C7 H7 112.2 . . ? C8 C7 H7 112.2 . . ? O8 C8 C15 106.7(2) . . ? O8 C8 C9 115.9(2) . . ? C15 C8 C9 117.0(2) . . ? O8 C8 C7 116.7(2) . . ? C15 C8 C7 114.6(2) . . ? C9 C8 C7 85.4(2) . . ? O2 C9 N2 131.5(3) . . ? O2 C9 C8 137.1(3) . . ? N2 C9 C8 91.4(3) . . ? O5 C10 C7 110.8(2) . . ? O5 C10 C12 105.1(2) . . ? C7 C10 C12 113.3(2) . . ? O5 C10 H10 109.2 . . ? C7 C10 H10 109.2 . . ? C12 C10 H10 109.2 . . ? O6 C11 O5 104.6(2) . . ? O6 C11 C34 109.1(3) . . ? O5 C11 C34 109.3(3) . . ? O6 C11 C33 110.6(3) . . ? O5 C11 C33 110.5(2) . . ? C34 C11 C33 112.3(3) . . ? O6 C12 C10 102.8(2) . . ? O6 C12 H12A 111.2 . . ? C10 C12 H12A 111.2 . . ? O6 C12 H12B 111.2 . . ? C10 C12 H12B 111.2 . . ? H12A C12 H12B 109.1 . . ? O8 C13 C14 103.7(2) . . ? O8 C13 H13A 111.0 . . ? C14 C13 H13A 111.0 . . ? O8 C13 H13B 111.0 . . ? C14 C13 H13B 111.0 . . ? H13A C13 H13B 109.0 . . ? C15 C14 C13 111.8(3) . . ? C15 C14 H14 124.1 . . ? C13 C14 H14 124.1 . . ? C14 C15 C16 129.3(3) . . ? C14 C15 C8 107.8(2) . . ? C16 C15 C8 122.8(2) . . ? C17 C16 C21 118.7(3) . . ? C17 C16 C15 121.1(3) . . ? C21 C16 C15 120.1(3) . . ? C16 C17 C18 120.9(3) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C19 120.8(3) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C18 C19 C20 118.0(3) . . ? C18 C19 C22 121.8(3) . . ? C20 C19 C22 120.1(3) . . ? C21 C20 C19 120.6(3) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C16 C21 C20 120.9(3) . . ? C16 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C19 126.4(3) . . ? C23 C22 C25 108.9(3) . . ? C19 C22 C25 124.6(3) . . ? C22 C23 C24 110.3(3) . . ? C22 C23 H23 124.8 . . ? C24 C23 H23 124.8 . . ? O7 C24 C23 105.2(2) . . ? O7 C24 H24A 110.7 . . ? C23 C24 H24A 110.7 . . ? O7 C24 H24B 110.7 . . ? C23 C24 H24B 110.7 . . ? H24A C24 H24B 108.8 . . ? O7 C25 C22 106.3(2) . . ? O7 C25 C26 112.0(2) . . ? C22 C25 C26 120.0(2) . . ? O7 C25 C27 113.8(2) . . ? C22 C25 C27 119.2(2) . . ? C26 C25 C27 84.7(2) . . ? O1 C26 N1 132.8(3) . . ? O1 C26 C25 135.6(3) . . ? N1 C26 C25 91.6(3) . . ? N1 C27 C28 116.4(2) . . ? N1 C27 C25 86.8(2) . . ? C28 C27 C25 115.1(2) . . ? N1 C27 H27 112.1 . . ? C28 C27 H27 112.1 . . ? C25 C27 H27 112.1 . . ? O3 C28 C27 109.1(2) . . ? O3 C28 C29 103.1(2) . . ? C27 C28 C29 112.4(2) . . ? O3 C28 H28 110.6 . . ? C27 C28 H28 110.6 . . ? C29 C28 H28 110.6 . . ? O4 C29 C28 105.6(2) . . ? O4 C29 H29A 110.6 . . ? C28 C29 H29A 110.6 . . ? O4 C29 H29B 110.6 . . ? C28 C29 H29B 110.6 . . ? H29A C29 H29B 108.8 . . ? O3 C30 O4 103.7(3) . . ? O3 C30 C32 110.1(3) . . ? O4 C30 C32 109.8(3) . . ? O3 C30 C31 108.5(3) . . ? O4 C30 C31 109.8(3) . . ? C32 C30 C31 114.4(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C11 C34 H34A 109.5 . . ? C11 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C11 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C11 C33 H33A 109.5 . . ? C11 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C11 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 N1 C1 130.3(3) . . ? C26 N1 C27 96.9(2) . . ? C1 N1 C27 132.8(3) . . ? C9 N2 C6 129.4(3) . . ? C9 N2 C7 97.1(2) . . ? C6 N2 C7 133.5(3) . . ? C30 O3 C28 108.5(2) . . ? C29 O4 C30 107.1(2) . . ? C10 O5 C11 107.5(2) . . ? C11 O6 C12 106.6(2) . . ? C25 O7 C24 109.1(2) . . ? C8 O8 C13 109.8(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 N1 C1 C2 C3 -66.8(4) . . . . ? C1 C2 C3 C4 118.1(4) . . . . ? C2 C3 C4 C5 178.4(4) . . . . ? C3 C4 C5 C6 -125.0(4) . . . . ? C4 C5 C6 N2 -68.4(5) . . . . ? N2 C7 C8 O8 -122.6(2) . . . . ? C10 C7 C8 O8 -6.5(4) . . . . ? N2 C7 C8 C15 111.7(2) . . . . ? C10 C7 C8 C15 -132.2(3) . . . . ? N2 C7 C8 C9 -5.95(19) . . . . ? C10 C7 C8 C9 110.2(3) . . . . ? O8 C8 C9 O2 -56.5(5) . . . . ? C15 C8 C9 O2 70.7(5) . . . . ? C7 C8 C9 O2 -174.0(4) . . . . ? O8 C8 C9 N2 124.0(2) . . . . ? C15 C8 C9 N2 -108.8(3) . . . . ? C7 C8 C9 N2 6.5(2) . . . . ? N2 C7 C10 O5 -76.5(3) . . . . ? C8 C7 C10 O5 -174.8(2) . . . . ? N2 C7 C10 C12 165.6(2) . . . . ? C8 C7 C10 C12 67.4(3) . . . . ? O5 C10 C12 O6 12.6(3) . . . . ? C7 C10 C12 O6 133.7(2) . . . . ? O8 C13 C14 C15 0.8(4) . . . . ? C13 C14 C15 C16 177.9(3) . . . . ? C13 C14 C15 C8 2.3(4) . . . . ? O8 C8 C15 C14 -4.5(3) . . . . ? C9 C8 C15 C14 -136.2(3) . . . . ? C7 C8 C15 C14 126.2(3) . . . . ? O8 C8 C15 C16 179.5(2) . . . . ? C9 C8 C15 C16 47.9(4) . . . . ? C7 C8 C15 C16 -49.8(4) . . . . ? C14 C15 C16 C17 104.3(4) . . . . ? C8 C15 C16 C17 -80.7(4) . . . . ? C14 C15 C16 C21 -77.5(4) . . . . ? C8 C15 C16 C21 97.5(3) . . . . ? C21 C16 C17 C18 2.3(4) . . . . ? C15 C16 C17 C18 -179.5(3) . . . . ? C16 C17 C18 C19 -1.6(4) . . . . ? C17 C18 C19 C20 -0.6(4) . . . . ? C17 C18 C19 C22 177.0(3) . . . . ? C18 C19 C20 C21 2.1(4) . . . . ? C22 C19 C20 C21 -175.5(3) . . . . ? C17 C16 C21 C20 -0.8(4) . . . . ? C15 C16 C21 C20 -179.0(3) . . . . ? C19 C20 C21 C16 -1.4(4) . . . . ? C18 C19 C22 C23 -59.7(4) . . . . ? C20 C19 C22 C23 117.8(3) . . . . ? C18 C19 C22 C25 118.0(3) . . . . ? C20 C19 C22 C25 -64.5(4) . . . . ? C19 C22 C23 C24 -178.7(3) . . . . ? C25 C22 C23 C24 3.3(4) . . . . ? C22 C23 C24 O7 -2.8(4) . . . . ? C23 C22 C25 O7 -2.6(3) . . . . ? C19 C22 C25 O7 179.3(2) . . . . ? C23 C22 C25 C26 -130.9(3) . . . . ? C19 C22 C25 C26 51.0(4) . . . . ? C23 C22 C25 C27 127.5(3) . . . . ? C19 C22 C25 C27 -50.6(4) . . . . ? O7 C25 C26 O1 -64.8(4) . . . . ? C22 C25 C26 O1 60.9(5) . . . . ? C27 C25 C26 O1 -178.3(4) . . . . ? O7 C25 C26 N1 113.2(2) . . . . ? C22 C25 C26 N1 -121.2(3) . . . . ? C27 C25 C26 N1 -0.4(2) . . . . ? O7 C25 C27 N1 -111.4(2) . . . . ? C22 C25 C27 N1 121.9(3) . . . . ? C26 C25 C27 N1 0.35(19) . . . . ? O7 C25 C27 C28 6.3(4) . . . . ? C22 C25 C27 C28 -120.3(3) . . . . ? C26 C25 C27 C28 118.1(2) . . . . ? N1 C27 C28 O3 -74.0(3) . . . . ? C25 C27 C28 O3 -173.5(2) . . . . ? N1 C27 C28 C29 172.2(2) . . . . ? C25 C27 C28 C29 72.7(3) . . . . ? O3 C28 C29 O4 -5.8(3) . . . . ? C27 C28 C29 O4 111.6(3) . . . . ? O1 C26 N1 C1 -2.7(6) . . . . ? C25 C26 N1 C1 179.2(3) . . . . ? O1 C26 N1 C27 178.5(3) . . . . ? C25 C26 N1 C27 0.4(2) . . . . ? C2 C1 N1 C26 -93.3(4) . . . . ? C2 C1 N1 C27 85.1(4) . . . . ? C28 C27 N1 C26 -116.9(3) . . . . ? C25 C27 N1 C26 -0.4(2) . . . . ? C28 C27 N1 C1 64.3(4) . . . . ? C25 C27 N1 C1 -179.2(3) . . . . ? O2 C9 N2 C6 -5.9(6) . . . . ? C8 C9 N2 C6 173.6(3) . . . . ? O2 C9 N2 C7 173.5(3) . . . . ? C8 C9 N2 C7 -7.0(2) . . . . ? C5 C6 N2 C9 -89.9(4) . . . . ? C5 C6 N2 C7 90.9(4) . . . . ? C10 C7 N2 C9 -111.0(3) . . . . ? C8 C7 N2 C9 6.8(2) . . . . ? C10 C7 N2 C6 68.4(4) . . . . ? C8 C7 N2 C6 -173.8(3) . . . . ? O4 C30 O3 C28 31.5(3) . . . . ? C32 C30 O3 C28 149.0(3) . . . . ? C31 C30 O3 C28 -85.1(3) . . . . ? C27 C28 O3 C30 -135.6(3) . . . . ? C29 C28 O3 C30 -16.0(3) . . . . ? C28 C29 O4 C30 25.3(3) . . . . ? O3 C30 O4 C29 -35.3(3) . . . . ? C32 C30 O4 C29 -152.9(3) . . . . ? C31 C30 O4 C29 80.5(3) . . . . ? C7 C10 O5 C11 -113.1(3) . . . . ? C12 C10 O5 C11 9.6(3) . . . . ? O6 C11 O5 C10 -29.0(3) . . . . ? C34 C11 O5 C10 -145.7(2) . . . . ? C33 C11 O5 C10 90.1(3) . . . . ? O5 C11 O6 C12 37.8(3) . . . . ? C34 C11 O6 C12 154.7(3) . . . . ? C33 C11 O6 C12 -81.2(3) . . . . ? C10 C12 O6 C11 -31.0(3) . . . . ? C22 C25 O7 C24 0.8(3) . . . . ? C26 C25 O7 C24 133.7(3) . . . . ? C27 C25 O7 C24 -132.3(3) . . . . ? C23 C24 O7 C25 1.0(3) . . . . ? C15 C8 O8 C13 5.1(3) . . . . ? C9 C8 O8 C13 137.3(3) . . . . ? C7 C8 O8 C13 -124.4(3) . . . . ? C14 C13 O8 C8 -3.7(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.322 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.039