# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- KDS_CC.cif' _publ_contact_author_name 'Professor Ken D. Shimizu' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina 29208 USA ; _publ_contact_author_phone '1 803 777 6523' _publ_contact_author_fax '1 803 777 9521' _publ_contact_author_email shimizu@mail.chem.sc.edu loop_ _publ_author_name _publ_author_address Y.S.Chong ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; W.G.Burns ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; B.E.Dial ; Department of Chemistry and Biochemistry University of South Carolina Columbia, South Carolina, 29208 USA ; K.D.Shimizu ; Department of Chemistry University of Cincinnati Cincinnati, OH, 45221 USA ; ###================================================== ### CRYSTAL DATA ###================================================== data_sqz2new _database_code_depnum_ccdc_archive 'CCDC 846375' #TrackingRef '- KDS_CC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H34 N2 O6' _chemical_formula_sum 'C36 H34 N2 O6' _chemical_formula_weight 590.65 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 trigonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 31.419(5) _cell_length_b 31.419(5) _cell_length_c 9.403(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 8039(5) _cell_formula_units_Z 9 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2117 _cell_measurement_theta_min 2.246 _cell_measurement_theta_max 21.926 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 0.075 _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 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11935 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 22.54 _reflns_number_total 2353 _reflns_number_gt 1259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Columns of diffuse solvent along [001]. Columns located at (x,y) = (0,0); (1/3,2/3); (2/3,1/3). SQUEEZE used. 1665.6 e/A-3 total solvent-accessible volume per cell, corresponding to 484 e/cell. 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^)+(0.0909P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2353 _refine_ls_number_parameters 206 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1973 _refine_ls_wR_factor_gt 0.1779 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _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 0.55458(17) 0.94778(16) 0.6216(5) 0.0672(12) Uani 1 1 d . . . C2 C 0.54738(15) 0.98219(14) 0.5327(4) 0.0605(11) Uani 1 1 d . . . C3 C 0.50366(14) 0.98370(13) 0.5427(4) 0.0552(10) Uani 1 1 d . . . C4 C 0.46605(15) 0.95320(15) 0.6400(4) 0.0629(11) Uani 1 1 d . . . C5 C 0.47248(18) 0.91845(16) 0.7285(5) 0.0732(13) Uani 1 1 d . . . C6 C 0.58278(15) 1.01195(15) 0.4382(5) 0.0719(13) Uani 1 1 d . . . H6 H 0.6116 1.0106 0.4312 0.086 Uiso 1 1 calc R . . C7 C 0.57642(15) 1.04433(16) 0.3523(5) 0.0750(13) Uani 1 1 d . . . H7 H 0.6011 1.0645 0.2890 0.090 Uiso 1 1 calc R . . C8 C 0.52293(17) 0.88444(18) 0.8051(6) 0.0751(13) Uani 1 1 d . . . C9 C 0.50574(19) 0.8377(2) 0.7579(6) 0.0853(14) Uani 1 1 d . . . C10 C 0.5090(2) 0.80407(19) 0.8457(7) 0.1056(18) Uani 1 1 d . . . H10 H 0.4960 0.7715 0.8181 0.127 Uiso 1 1 calc R . . C11 C 0.5321(2) 0.8205(2) 0.9760(7) 0.1106(19) Uani 1 1 d . . . H11 H 0.5348 0.7980 1.0341 0.133 Uiso 1 1 calc R . . C12 C 0.5512(2) 0.8674(2) 1.0248(6) 0.0968(16) Uani 1 1 d . . . C13 C 0.54552(18) 0.89913(18) 0.9353(5) 0.0864(15) Uani 1 1 d . . . H13 H 0.5573 0.9314 0.9642 0.104 Uiso 1 1 calc R . . C14 C 0.5753(3) 0.8827(3) 1.1724(6) 0.121(2) Uani 1 1 d . . . C15 C 0.5376(3) 0.8643(4) 1.2803(8) 0.213(4) Uani 1 1 d . . . H15A H 0.5216 0.8287 1.2796 0.256 Uiso 1 1 calc R . . H15B H 0.5536 0.8753 1.3720 0.256 Uiso 1 1 calc R . . C16 C 0.5011(3) 0.8773(4) 1.2710(8) 0.221(5) Uani 1 1 d . . . H16A H 0.5097 0.9017 1.1983 0.332 Uiso 1 1 calc R . . H16B H 0.4982 0.8903 1.3606 0.332 Uiso 1 1 calc R . . H16C H 0.4703 0.8488 1.2476 0.332 Uiso 1 1 calc R . . C17 C 0.6082(3) 0.8583(3) 1.2049(7) 0.166(3) Uani 1 1 d . . . H17A H 0.6246 0.8701 1.2945 0.249 Uiso 1 1 calc R . . H17B H 0.6322 0.8668 1.1309 0.249 Uiso 1 1 calc R . . H17C H 0.5877 0.8232 1.2089 0.249 Uiso 1 1 calc R . . C18 C 0.6093(3) 0.9386(3) 1.1848(7) 0.143(2) Uani 1 1 d . . . H18A H 0.5905 0.9547 1.1699 0.214 Uiso 1 1 calc R . . H18B H 0.6347 0.9495 1.1145 0.214 Uiso 1 1 calc R . . H18C H 0.6237 0.9465 1.2779 0.214 Uiso 1 1 calc R . . N1 N 0.51722(13) 0.91904(13) 0.7178(4) 0.0728(11) Uani 1 1 d . . . O1 O 0.59086(11) 0.94415(11) 0.6160(3) 0.0880(11) Uani 1 1 d . . . O2 O 0.44100(12) 0.88980(13) 0.8082(4) 0.1027(12) Uani 1 1 d . . . O3 O 0.48367(17) 0.82559(15) 0.6272(5) 0.1260(14) Uani 1 1 d D . . H3 H 0.475(2) 0.7951(11) 0.597(6) 0.16(3) Uiso 1 1 d 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 0.058(3) 0.081(3) 0.072(3) 0.010(3) 0.001(3) 0.042(3) C2 0.053(3) 0.065(3) 0.071(3) 0.011(2) 0.007(2) 0.035(2) C3 0.053(2) 0.050(3) 0.055(3) 0.008(2) 0.007(2) 0.020(2) C4 0.064(3) 0.067(3) 0.060(3) 0.012(2) 0.005(2) 0.034(2) C5 0.078(3) 0.074(3) 0.072(3) 0.022(3) 0.015(3) 0.040(3) C6 0.060(3) 0.084(3) 0.087(3) 0.024(3) 0.017(3) 0.047(3) C7 0.059(3) 0.085(3) 0.084(3) 0.021(3) 0.016(2) 0.039(3) C8 0.090(3) 0.078(4) 0.073(4) 0.019(3) 0.002(3) 0.053(3) C9 0.104(4) 0.084(4) 0.073(4) 0.013(3) -0.002(3) 0.051(3) C10 0.135(5) 0.082(4) 0.120(5) 0.025(4) 0.008(4) 0.069(4) C11 0.155(5) 0.106(5) 0.098(5) 0.034(4) 0.001(4) 0.086(4) C12 0.136(5) 0.103(4) 0.079(4) 0.023(4) 0.008(3) 0.080(4) C13 0.112(4) 0.095(4) 0.072(4) 0.014(3) 0.003(3) 0.067(3) C14 0.153(6) 0.158(6) 0.071(4) 0.020(4) 0.002(4) 0.092(5) C15 0.165(8) 0.379(14) 0.107(6) 0.035(7) 0.017(6) 0.145(9) C16 0.194(8) 0.413(15) 0.133(7) -0.007(8) -0.010(6) 0.209(10) C17 0.190(7) 0.234(8) 0.132(6) 0.025(5) -0.018(5) 0.149(7) C18 0.160(6) 0.152(6) 0.116(5) -0.016(4) -0.042(5) 0.078(5) N1 0.074(3) 0.083(3) 0.076(3) 0.021(2) 0.009(2) 0.050(2) O1 0.075(2) 0.098(2) 0.110(3) 0.0287(19) 0.0088(19) 0.0570(19) O2 0.094(2) 0.109(3) 0.114(3) 0.060(2) 0.039(2) 0.058(2) O3 0.172(4) 0.095(3) 0.110(3) -0.007(3) -0.028(3) 0.066(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 C1 O1 1.202(4) . ? C1 N1 1.397(5) . ? C1 C2 1.471(5) . ? C2 C6 1.364(5) . ? C2 C3 1.401(5) . ? C3 C3 1.407(7) 10_676 ? C3 C4 1.422(5) . ? C4 C7 1.377(5) 10_676 ? C4 C5 1.465(6) . ? C5 O2 1.208(4) . ? C5 N1 1.400(5) . ? C6 C7 1.390(5) . ? C6 H6 0.9300 . ? C7 C4 1.377(5) 10_676 ? C7 H7 0.9300 . ? C8 C9 1.362(6) . ? C8 C13 1.374(6) . ? C8 N1 1.443(5) . ? C9 O3 1.368(6) . ? C9 C10 1.383(6) . ? C10 C11 1.387(7) . ? C10 H10 0.9300 . ? C11 C12 1.362(7) . ? C11 H11 0.9300 . ? C12 C13 1.384(6) . ? C12 C14 1.538(7) . ? C13 H13 0.9300 . ? C14 C15 1.442(9) . ? C14 C18 1.537(8) . ? C14 C17 1.597(8) . ? C15 C16 1.399(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? O3 H3 0.90(2) . ? 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 O1 C1 N1 119.8(4) . . ? O1 C1 C2 123.1(4) . . ? N1 C1 C2 117.1(4) . . ? C6 C2 C3 119.8(4) . . ? C6 C2 C1 120.1(4) . . ? C3 C2 C1 120.0(4) . . ? C2 C3 C3 120.4(4) . 10_676 ? C2 C3 C4 121.2(3) . . ? C3 C3 C4 118.3(4) 10_676 . ? C7 C4 C3 119.9(4) 10_676 . ? C7 C4 C5 120.7(4) 10_676 . ? C3 C4 C5 119.4(4) . . ? O2 C5 N1 119.8(4) . . ? O2 C5 C4 122.7(4) . . ? N1 C5 C4 117.5(4) . . ? C2 C6 C7 120.9(4) . . ? C2 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C4 C7 C6 120.6(4) 10_676 . ? C4 C7 H7 119.7 10_676 . ? C6 C7 H7 119.7 . . ? C9 C8 C13 120.8(4) . . ? C9 C8 N1 119.7(5) . . ? C13 C8 N1 119.4(4) . . ? C8 C9 O3 117.7(5) . . ? C8 C9 C10 119.2(5) . . ? O3 C9 C10 123.0(5) . . ? C9 C10 C11 117.9(5) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C12 C11 C10 124.5(5) . . ? C12 C11 H11 117.8 . . ? C10 C11 H11 117.8 . . ? C11 C12 C13 115.4(5) . . ? C11 C12 C14 121.6(5) . . ? C13 C12 C14 122.9(6) . . ? C8 C13 C12 122.1(5) . . ? C8 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C15 C14 C18 111.5(7) . . ? C15 C14 C12 109.5(6) . . ? C18 C14 C12 112.2(5) . . ? C15 C14 C17 105.8(6) . . ? C18 C14 C17 106.7(6) . . ? C12 C14 C17 110.9(5) . . ? C16 C15 C14 117.9(8) . . ? C16 C15 H15A 107.8 . . ? C14 C15 H15A 107.8 . . ? C16 C15 H15B 107.8 . . ? C14 C15 H15B 107.8 . . ? H15A C15 H15B 107.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C1 N1 C5 124.6(4) . . ? C1 N1 C8 118.3(3) . . ? C5 N1 C8 116.8(4) . . ? C9 O3 H3 115(4) . . ? 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 O1 C1 C2 C6 0.0(7) . . . . ? N1 C1 C2 C6 178.9(4) . . . . ? O1 C1 C2 C3 178.6(4) . . . . ? N1 C1 C2 C3 -2.5(6) . . . . ? C6 C2 C3 C3 -1.0(7) . . . 10_676 ? C1 C2 C3 C3 -179.6(4) . . . 10_676 ? C6 C2 C3 C4 -180.0(4) . . . . ? C1 C2 C3 C4 1.4(6) . . . . ? C2 C3 C4 C7 179.7(4) . . . 10_676 ? C3 C3 C4 C7 0.8(7) 10_676 . . 10_676 ? C2 C3 C4 C5 -1.9(6) . . . . ? C3 C3 C4 C5 179.1(4) 10_676 . . . ? C7 C4 C5 O2 2.1(7) 10_676 . . . ? C3 C4 C5 O2 -176.2(4) . . . . ? C7 C4 C5 N1 -178.2(4) 10_676 . . . ? C3 C4 C5 N1 3.4(6) . . . . ? C3 C2 C6 C7 0.7(6) . . . . ? C1 C2 C6 C7 179.3(4) . . . . ? C2 C6 C7 C4 -0.5(7) . . . 10_676 ? C13 C8 C9 O3 -180.0(5) . . . . ? N1 C8 C9 O3 0.3(7) . . . . ? C13 C8 C9 C10 3.2(7) . . . . ? N1 C8 C9 C10 -176.5(4) . . . . ? C8 C9 C10 C11 -3.3(8) . . . . ? O3 C9 C10 C11 -179.9(5) . . . . ? C9 C10 C11 C12 1.1(9) . . . . ? C10 C11 C12 C13 1.1(9) . . . . ? C10 C11 C12 C14 178.4(6) . . . . ? C9 C8 C13 C12 -0.9(7) . . . . ? N1 C8 C13 C12 178.8(4) . . . . ? C11 C12 C13 C8 -1.2(7) . . . . ? C14 C12 C13 C8 -178.5(5) . . . . ? C11 C12 C14 C15 -75.5(8) . . . . ? C13 C12 C14 C15 101.6(8) . . . . ? C11 C12 C14 C18 160.1(6) . . . . ? C13 C12 C14 C18 -22.8(8) . . . . ? C11 C12 C14 C17 40.8(8) . . . . ? C13 C12 C14 C17 -142.0(6) . . . . ? C18 C14 C15 C16 68.8(10) . . . . ? C12 C14 C15 C16 -56.0(11) . . . . ? C17 C14 C15 C16 -175.5(8) . . . . ? O1 C1 N1 C5 -176.6(4) . . . . ? C2 C1 N1 C5 4.4(6) . . . . ? O1 C1 N1 C8 -1.9(6) . . . . ? C2 C1 N1 C8 179.1(4) . . . . ? O2 C5 N1 C1 174.8(4) . . . . ? C4 C5 N1 C1 -4.9(6) . . . . ? O2 C5 N1 C8 0.0(6) . . . . ? C4 C5 N1 C8 -179.7(4) . . . . ? C9 C8 N1 C1 -90.2(5) . . . . ? C13 C8 N1 C1 90.0(5) . . . . ? C9 C8 N1 C5 84.9(5) . . . . ? C13 C8 N1 C5 -94.8(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.54 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.246 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.041 _vrf_THETM01_sqz2new ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: No diffraction observed at higher angles due to extensive disorder. Dataset truncated at 2-theta ca. 45 degrees ; _vrf_PLAT023_sqz2new ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 22.54 Deg. RESPONSE: No diffraction observed at higher angles due to extensive disorder. Dataset truncated at 2-theta ca. 45 degrees ; _vrf_PLAT601_sqz2new ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 500 A**3 RESPONSE: Voids contain heavily disordered sovlent species which could not be identified or modeled. The congtribution of these species was removed from the structure factor calculations with Squeeze: 1665.6 e/A-3 total solvent-accessible volume per cell, corresponding to 484 e/cell. ; #===END data_gbbbm _database_code_depnum_ccdc_archive 'CCDC 846376' #TrackingRef '- KDS_CC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H46 N2 O6' _chemical_formula_sum 'C50 H46 N2 O6' _chemical_formula_weight 770.89 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2972(8) _cell_length_b 13.2286(9) _cell_length_c 14.8485(10) _cell_angle_alpha 89.1900(10) _cell_angle_beta 70.0700(10) _cell_angle_gamma 76.7010(10) _cell_volume 2025.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 5304 _cell_measurement_theta_min 2.217 _cell_measurement_theta_max 24.102 _exptl_crystal_description wedge _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.083 _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 150(1) _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 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12391 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 23.26 _reflns_number_total 5790 _reflns_number_gt 4121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART NT V5.625 (Bruker, 1998)' _computing_cell_refinement 'SAINT+ NT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT+ NT V6.22' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V6.1 (Sheldrick, 2000)' _computing_publication_material 'SHELXTL V6.1' _refine_special_details ; 17 restraints used to model -(C Me2 Et) group disorder 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^)+(0.0943P)^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_number_reflns 5790 _refine_ls_number_parameters 571 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1657 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.017 _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 C1 C 0.3962(3) 0.2979(2) 0.5226(2) 0.0355(7) Uani 1 1 d . . . C2 C 0.4178(3) 0.3955(2) 0.5535(2) 0.0324(7) Uani 1 1 d . . . C3 C 0.4920(3) 0.4523(2) 0.48540(19) 0.0287(6) Uani 1 1 d . . . C4 C 0.5529(3) 0.4152(2) 0.38715(19) 0.0311(7) Uani 1 1 d . . . C5 C 0.5380(3) 0.3152(2) 0.3555(2) 0.0329(7) Uani 1 1 d . . . C6 C 0.3627(3) 0.4321(2) 0.6484(2) 0.0402(8) Uani 1 1 d . . . H6 H 0.3150 0.3923 0.6944 0.048 Uiso 1 1 calc R . . C7 C 0.6237(3) 0.4726(2) 0.3221(2) 0.0386(8) Uani 1 1 d . . . H7 H 0.6638 0.4474 0.2566 0.046 Uiso 1 1 calc R . . C8 C 0.4352(3) 0.1692(2) 0.39424(19) 0.0322(7) Uani 1 1 d . . . C9 C 0.5284(3) 0.0790(2) 0.38735(19) 0.0325(7) Uani 1 1 d . . . C10 C 0.5090(3) -0.0139(2) 0.35965(19) 0.0325(7) Uani 1 1 d . . . H10 H 0.5712 -0.0775 0.3548 0.039 Uiso 1 1 calc R . . C11 C 0.3983(3) -0.0125(2) 0.3393(2) 0.0362(7) Uani 1 1 d . A . H11 H 0.3866 -0.0765 0.3199 0.043 Uiso 1 1 calc R . . C12 C 0.3034(3) 0.0773(2) 0.3456(2) 0.0375(7) Uani 1 1 d D . . C13 C 0.3256(3) 0.1685(2) 0.3749(2) 0.0352(7) Uani 1 1 d . A . H13 H 0.2627 0.2322 0.3815 0.042 Uiso 1 1 calc R . . C14 C 0.7339(3) -0.0013(2) 0.4013(2) 0.0380(7) Uani 1 1 d . . . H14A H 0.6956 -0.0607 0.4259 0.046 Uiso 1 1 calc R . . H14B H 0.7855 0.0103 0.4407 0.046 Uiso 1 1 calc R . . C15 C 0.8226(3) -0.0287(2) 0.2989(2) 0.0351(7) Uani 1 1 d . . . C16 C 0.8515(3) 0.0482(3) 0.2361(2) 0.0437(8) Uani 1 1 d . . . H16 H 0.8089 0.1191 0.2559 0.052 Uiso 1 1 calc R . . C17 C 0.9423(3) 0.0216(3) 0.1448(2) 0.0512(9) Uani 1 1 d . . . H17 H 0.9618 0.0746 0.1022 0.061 Uiso 1 1 calc R . . C18 C 1.0045(3) -0.0805(3) 0.1153(2) 0.0557(9) Uani 1 1 d . . . H18 H 1.0688 -0.0982 0.0532 0.067 Uiso 1 1 calc R . . C19 C 0.9729(3) -0.1569(3) 0.1761(3) 0.0609(10) Uani 1 1 d . . . H19 H 1.0137 -0.2280 0.1556 0.073 Uiso 1 1 calc R . . C20 C 0.8817(3) -0.1304(3) 0.2673(2) 0.0501(9) Uani 1 1 d . . . H20 H 0.8598 -0.1838 0.3086 0.060 Uiso 1 1 calc R . . C21A C 0.1739(4) 0.0770(8) 0.3320(4) 0.0376(19) Uani 0.702(7) 1 d PD A 1 C22A C 0.0629(4) 0.0982(5) 0.4297(4) 0.0612(17) Uani 0.702(7) 1 d PD A 1 H22A H 0.0655 0.1605 0.4632 0.092 Uiso 0.702(7) 1 calc PR A 1 H22B H 0.0729 0.0384 0.4685 0.092 Uiso 0.702(7) 1 calc PR A 1 H22C H -0.0204 0.1093 0.4197 0.092 Uiso 0.702(7) 1 calc PR A 1 C23A C 0.1767(8) -0.0238(6) 0.2849(8) 0.052(2) Uani 0.702(7) 1 d PD A 1 H23A H 0.0936 -0.0191 0.2760 0.079 Uiso 0.702(7) 1 calc PR A 1 H23B H 0.1916 -0.0808 0.3257 0.079 Uiso 0.702(7) 1 calc PR A 1 H23C H 0.2467 -0.0374 0.2223 0.079 Uiso 0.702(7) 1 calc PR A 1 C24A C 0.1397(4) 0.1683(4) 0.2706(3) 0.0483(16) Uani 0.702(7) 1 d PD A 1 H24A H 0.0551 0.1683 0.2646 0.058 Uiso 0.702(7) 1 calc PR A 1 H24B H 0.1296 0.2348 0.3053 0.058 Uiso 0.702(7) 1 calc PR A 1 C25A C 0.2381(7) 0.1642(7) 0.1713(5) 0.073(2) Uani 0.702(7) 1 d PD A 1 H25A H 0.3249 0.1317 0.1722 0.110 Uiso 0.702(7) 1 calc PR A 1 H25B H 0.2359 0.2351 0.1506 0.110 Uiso 0.702(7) 1 calc PR A 1 H25C H 0.2177 0.1233 0.1266 0.110 Uiso 0.702(7) 1 calc PR A 1 C21B C 0.1940(9) 0.084(2) 0.3035(11) 0.0376(19) Uani 0.298(7) 1 d PD A 2 C22B C 0.0702(10) 0.1532(10) 0.3763(9) 0.047(3) Uiso 0.298(7) 1 d PD A 2 H22D H 0.0830 0.1608 0.4376 0.070 Uiso 0.298(7) 1 calc PR A 2 H22E H -0.0025 0.1208 0.3857 0.070 Uiso 0.298(7) 1 calc PR A 2 H22F H 0.0511 0.2220 0.3518 0.070 Uiso 0.298(7) 1 calc PR A 2 C23B C 0.160(3) -0.030(2) 0.3203(18) 0.070(10) Uiso 0.298(7) 1 d PD A 2 H23D H 0.1374 -0.0424 0.3886 0.105 Uiso 0.298(7) 1 calc PR A 2 H23E H 0.2359 -0.0837 0.2827 0.105 Uiso 0.298(7) 1 calc PR A 2 H23F H 0.0868 -0.0310 0.2997 0.105 Uiso 0.298(7) 1 calc PR A 2 C24B C 0.2160(13) 0.1116(10) 0.2081(10) 0.048(4) Uiso 0.298(7) 1 d PD A 2 H24C H 0.1345 0.1181 0.1948 0.058 Uiso 0.298(7) 1 calc PR A 2 H24D H 0.2817 0.0535 0.1648 0.058 Uiso 0.298(7) 1 calc PR A 2 C25B C 0.262(2) 0.2130(16) 0.1819(16) 0.073(2) Uani 0.298(7) 1 d PD A 2 H25D H 0.2159 0.2661 0.2353 0.110 Uiso 0.298(7) 1 calc PR A 2 H25E H 0.2441 0.2380 0.1243 0.110 Uiso 0.298(7) 1 calc PR A 2 H25F H 0.3555 0.1992 0.1694 0.110 Uiso 0.298(7) 1 calc PR A 2 N1 N 0.4542(2) 0.26590(16) 0.42496(16) 0.0318(6) Uani 1 1 d . . . O1 O 0.59123(19) 0.27652(15) 0.27382(14) 0.0422(5) Uani 1 1 d . . . O2 O 0.3295(2) 0.24751(16) 0.57748(15) 0.0494(6) Uani 1 1 d . . . O3 O 0.63164(17) 0.08967(14) 0.41216(14) 0.0380(5) Uani 1 1 d . . . C26 C 0.3916(3) 0.8004(2) 0.0331(2) 0.0386(8) Uani 1 1 d . . . C27 C 0.4117(3) 0.8995(2) -0.0078(2) 0.0347(7) Uani 1 1 d . . . C28 C 0.4916(3) 0.9521(2) 0.01951(19) 0.0324(7) Uani 1 1 d . . . C29 C 0.5559(3) 0.9108(2) 0.0833(2) 0.0346(7) Uani 1 1 d . . . C30 C 0.5375(3) 0.8107(2) 0.1249(2) 0.0382(7) Uani 1 1 d . . . C31 C 0.3527(3) 0.9405(2) -0.0712(2) 0.0403(8) Uani 1 1 d . . . H31 H 0.3016 0.9034 -0.0903 0.048 Uiso 1 1 calc R . . C32 C 0.6329(3) 0.9630(2) 0.1084(2) 0.0403(8) Uani 1 1 d . . . H32 H 0.6764 0.9340 0.1508 0.048 Uiso 1 1 calc R . . C33 C 0.4324(3) 0.6667(2) 0.1400(2) 0.0380(7) Uani 1 1 d . . . C34 C 0.5230(3) 0.5759(2) 0.0982(2) 0.0363(7) Uani 1 1 d . . . C35 C 0.5006(3) 0.4829(2) 0.1369(2) 0.0395(8) Uani 1 1 d . . . H35 H 0.5605 0.4188 0.1090 0.047 Uiso 1 1 calc R . . C36 C 0.3914(3) 0.4837(2) 0.2159(2) 0.0385(7) Uani 1 1 d . B . H36 H 0.3780 0.4192 0.2412 0.046 Uiso 1 1 calc R . . C37 C 0.3001(3) 0.5747(2) 0.2600(2) 0.0400(8) Uani 1 1 d D . . C38 C 0.3235(3) 0.6667(2) 0.2181(2) 0.0398(8) Uani 1 1 d . B . H38 H 0.2626 0.7308 0.2443 0.048 Uiso 1 1 calc R . . C39 C 0.7316(3) 0.4963(2) -0.0166(2) 0.0454(8) Uani 1 1 d . . . H39A H 0.7892 0.5097 -0.0804 0.055 Uiso 1 1 calc R . . H39B H 0.6966 0.4365 -0.0254 0.055 Uiso 1 1 calc R . . C40 C 0.8098(3) 0.4680(2) 0.0482(2) 0.0422(8) Uani 1 1 d . . . C41 C 0.8402(3) 0.5447(3) 0.0924(2) 0.0474(8) Uani 1 1 d . . . H41 H 0.8085 0.6158 0.0838 0.057 Uiso 1 1 calc R . . C42 C 0.9155(3) 0.5190(3) 0.1484(2) 0.0547(9) Uani 1 1 d . . . H42 H 0.9369 0.5725 0.1774 0.066 Uiso 1 1 calc R . . C43 C 0.9606(3) 0.4167(3) 0.1630(3) 0.0610(10) Uani 1 1 d . . . H43 H 1.0111 0.3996 0.2032 0.073 Uiso 1 1 calc R . . C44 C 0.9321(4) 0.3392(3) 0.1191(3) 0.0649(10) Uani 1 1 d . . . H44 H 0.9651 0.2682 0.1274 0.078 Uiso 1 1 calc R . . C45 C 0.8557(3) 0.3647(3) 0.0631(3) 0.0533(9) Uani 1 1 d . . . H45 H 0.8342 0.3110 0.0343 0.064 Uiso 1 1 calc R . . C46A C 0.174(8) 0.576(13) 0.343(6) 0.045(12) Uani 0.476(9) 1 d PD B 3 C47A C 0.1891(16) 0.4742(19) 0.3940(13) 0.062(4) Uani 0.476(9) 1 d PD B 3 H47A H 0.2556 0.4703 0.4233 0.093 Uiso 0.476(9) 1 calc PR B 3 H47B H 0.2150 0.4147 0.3471 0.093 Uiso 0.476(9) 1 calc PR B 3 H47C H 0.1063 0.4728 0.4440 0.093 Uiso 0.476(9) 1 calc PR B 3 C48A C 0.0596(7) 0.5841(8) 0.3083(6) 0.061(3) Uani 0.476(9) 1 d PD B 3 H48A H -0.0213 0.5967 0.3636 0.091 Uiso 0.476(9) 1 calc PR B 3 H48B H 0.0706 0.5190 0.2724 0.091 Uiso 0.476(9) 1 calc PR B 3 H48C H 0.0562 0.6419 0.2664 0.091 Uiso 0.476(9) 1 calc PR B 3 C49A C 0.1381(8) 0.6697(7) 0.4153(6) 0.059(3) Uani 0.476(9) 1 d PD B 3 H49A H 0.1336 0.7345 0.3812 0.071 Uiso 0.476(9) 1 calc PR B 3 H49B H 0.0513 0.6734 0.4639 0.071 Uiso 0.476(9) 1 calc PR B 3 C50A C 0.2317(12) 0.6624(11) 0.4634(10) 0.091(2) Uiso 0.476(9) 1 d PD B 3 H50A H 0.2086 0.6215 0.5195 0.136 Uiso 0.476(9) 1 calc PR B 3 H50B H 0.2316 0.7325 0.4841 0.136 Uiso 0.476(9) 1 calc PR B 3 H50C H 0.3183 0.6284 0.4190 0.136 Uiso 0.476(9) 1 calc PR B 3 C46B C 0.187(7) 0.577(12) 0.354(5) 0.045(12) Uani 0.524(9) 1 d PD B 4 C47B C 0.1534(19) 0.4674(19) 0.3650(18) 0.137(10) Uani 0.524(9) 1 d PD B 4 H47D H 0.0885 0.4664 0.4285 0.206 Uiso 0.524(9) 1 calc PR B 4 H47E H 0.2321 0.4132 0.3580 0.206 Uiso 0.524(9) 1 calc PR B 4 H47F H 0.1188 0.4543 0.3153 0.206 Uiso 0.524(9) 1 calc PR B 4 C48B C 0.0634(6) 0.6506(7) 0.3462(6) 0.061(3) Uani 0.524(9) 1 d PD B 4 H48D H 0.0580 0.7220 0.3670 0.092 Uiso 0.524(9) 1 calc PR B 4 H48E H -0.0132 0.6282 0.3872 0.092 Uiso 0.524(9) 1 calc PR B 4 H48F H 0.0669 0.6480 0.2794 0.092 Uiso 0.524(9) 1 calc PR B 4 C49B C 0.2085(9) 0.6096(9) 0.4362(6) 0.081(3) Uani 0.524(9) 1 d PD B 4 H49C H 0.2737 0.5518 0.4479 0.097 Uiso 0.524(9) 1 calc PR B 4 H49D H 0.1267 0.6150 0.4910 0.097 Uiso 0.524(9) 1 calc PR B 4 C50B C 0.2516(10) 0.7074(8) 0.4431(7) 0.091(2) Uiso 0.524(9) 1 d PD B 4 H50D H 0.3415 0.6988 0.4000 0.136 Uiso 0.524(9) 1 calc PR B 4 H50E H 0.2456 0.7216 0.5092 0.136 Uiso 0.524(9) 1 calc PR B 4 H50F H 0.1957 0.7657 0.4243 0.136 Uiso 0.524(9) 1 calc PR B 4 N2 N 0.4528(2) 0.76378(17) 0.09939(17) 0.0359(6) Uani 1 1 d . . . O4 O 0.5899(2) 0.77039(16) 0.18032(15) 0.0472(6) Uani 1 1 d . . . O5 O 0.3242(2) 0.75187(16) 0.01279(16) 0.0495(6) Uani 1 1 d . . . O6 O 0.62603(19) 0.58636(15) 0.02039(14) 0.0435(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 0.0375(17) 0.0289(17) 0.0403(19) 0.0018(14) -0.0113(15) -0.0116(14) C2 0.0341(16) 0.0272(16) 0.0353(17) -0.0004(13) -0.0093(14) -0.0103(13) C3 0.0284(14) 0.0275(15) 0.0314(16) 0.0017(12) -0.0119(13) -0.0066(12) C4 0.0321(15) 0.0266(16) 0.0344(17) 0.0009(13) -0.0104(13) -0.0082(13) C5 0.0373(16) 0.0275(16) 0.0339(18) -0.0007(14) -0.0128(14) -0.0068(13) C6 0.0438(18) 0.0358(18) 0.0378(18) 0.0024(14) -0.0055(15) -0.0167(14) C7 0.0442(18) 0.0355(18) 0.0336(17) -0.0035(14) -0.0080(14) -0.0127(14) C8 0.0363(16) 0.0252(16) 0.0347(17) -0.0013(13) -0.0110(14) -0.0083(13) C9 0.0300(16) 0.0366(18) 0.0297(16) 0.0019(13) -0.0070(13) -0.0108(14) C10 0.0331(16) 0.0244(16) 0.0377(17) -0.0003(13) -0.0096(14) -0.0062(13) C11 0.0391(17) 0.0242(16) 0.0431(18) -0.0040(13) -0.0105(15) -0.0089(14) C12 0.0374(17) 0.0341(18) 0.0405(18) -0.0034(14) -0.0134(14) -0.0073(14) C13 0.0323(16) 0.0258(16) 0.0447(18) -0.0034(13) -0.0136(14) -0.0011(13) C14 0.0306(16) 0.0422(18) 0.0421(18) 0.0036(14) -0.0158(14) -0.0055(14) C15 0.0277(15) 0.0404(19) 0.0409(18) 0.0087(15) -0.0160(14) -0.0095(14) C16 0.0391(18) 0.045(2) 0.050(2) 0.0109(16) -0.0191(16) -0.0112(15) C17 0.052(2) 0.064(2) 0.044(2) 0.0198(18) -0.0192(18) -0.0237(18) C18 0.052(2) 0.067(3) 0.041(2) 0.0036(19) -0.0075(17) -0.0133(19) C19 0.061(2) 0.048(2) 0.055(2) 0.0034(19) -0.0021(19) -0.0050(18) C20 0.0472(19) 0.042(2) 0.052(2) 0.0098(16) -0.0063(17) -0.0099(16) C21A 0.036(2) 0.037(2) 0.042(4) 0.004(4) -0.015(3) -0.010(2) C22A 0.036(3) 0.091(4) 0.063(4) 0.016(3) -0.021(3) -0.021(3) C23A 0.048(4) 0.041(4) 0.086(8) -0.003(4) -0.042(5) -0.014(3) C24A 0.042(3) 0.052(3) 0.054(3) -0.005(3) -0.022(3) -0.006(2) C25A 0.046(4) 0.107(8) 0.063(4) 0.010(5) -0.021(3) -0.008(4) C21B 0.036(2) 0.037(2) 0.042(4) 0.004(4) -0.015(3) -0.010(2) C25B 0.046(4) 0.107(8) 0.063(4) 0.010(5) -0.021(3) -0.008(4) N1 0.0371(13) 0.0245(13) 0.0351(14) -0.0016(11) -0.0107(11) -0.0122(11) O1 0.0538(13) 0.0330(12) 0.0383(13) -0.0038(10) -0.0118(11) -0.0135(10) O2 0.0612(14) 0.0398(13) 0.0444(13) -0.0010(10) -0.0038(11) -0.0286(11) O3 0.0321(11) 0.0352(12) 0.0504(13) 0.0017(9) -0.0182(10) -0.0090(9) C26 0.0375(17) 0.0286(17) 0.0435(19) 0.0002(14) -0.0055(15) -0.0090(14) C27 0.0335(16) 0.0298(17) 0.0346(17) 0.0045(14) -0.0052(14) -0.0059(13) C28 0.0308(15) 0.0286(15) 0.0297(16) -0.0005(13) -0.0022(13) -0.0042(13) C29 0.0348(16) 0.0307(17) 0.0334(17) 0.0034(13) -0.0068(14) -0.0058(13) C30 0.0426(18) 0.0322(18) 0.0333(17) 0.0033(14) -0.0077(15) -0.0050(14) C31 0.0408(17) 0.0398(19) 0.0432(18) 0.0078(15) -0.0137(15) -0.0168(14) C32 0.0456(18) 0.0352(18) 0.0423(19) 0.0084(15) -0.0177(15) -0.0105(15) C33 0.0421(18) 0.0299(17) 0.0401(18) 0.0091(14) -0.0128(15) -0.0077(14) C34 0.0377(17) 0.0349(18) 0.0347(17) 0.0050(14) -0.0103(14) -0.0090(14) C35 0.0404(18) 0.0292(17) 0.0459(19) 0.0010(14) -0.0148(16) -0.0028(14) C36 0.0393(17) 0.0310(17) 0.0432(19) 0.0072(14) -0.0110(15) -0.0099(14) C37 0.0420(18) 0.0319(18) 0.0433(19) 0.0082(15) -0.0116(15) -0.0084(15) C38 0.0412(18) 0.0275(17) 0.0425(19) 0.0026(14) -0.0063(15) -0.0052(14) C39 0.0392(18) 0.0403(19) 0.0449(19) -0.0027(15) -0.0030(15) -0.0041(15) C40 0.0320(16) 0.042(2) 0.0425(19) 0.0006(15) -0.0018(15) -0.0062(14) C41 0.0444(19) 0.044(2) 0.047(2) 0.0018(16) -0.0059(17) -0.0117(16) C42 0.047(2) 0.060(2) 0.057(2) 0.0010(18) -0.0153(18) -0.0165(18) C43 0.050(2) 0.063(3) 0.075(3) 0.016(2) -0.027(2) -0.0138(19) C44 0.059(2) 0.045(2) 0.094(3) 0.013(2) -0.034(2) -0.0099(18) C45 0.048(2) 0.043(2) 0.064(2) -0.0029(17) -0.0151(18) -0.0083(16) C46A 0.041(11) 0.040(3) 0.049(13) 0.008(13) -0.009(12) -0.008(12) C47A 0.031(6) 0.064(10) 0.068(7) 0.036(7) 0.010(5) -0.009(5) C48A 0.052(5) 0.062(6) 0.056(5) 0.001(4) -0.005(4) -0.014(4) C49A 0.050(5) 0.059(6) 0.057(5) 0.003(4) -0.014(4) 0.000(4) C46B 0.041(11) 0.040(3) 0.049(13) 0.008(13) -0.009(12) -0.008(12) C47B 0.098(15) 0.060(8) 0.18(2) 0.011(13) 0.046(12) -0.031(11) C48B 0.039(4) 0.078(6) 0.060(5) -0.004(4) -0.011(4) -0.008(4) C49B 0.058(5) 0.096(8) 0.067(6) -0.012(5) -0.024(4) 0.028(5) N2 0.0418(14) 0.0282(14) 0.0381(14) 0.0091(11) -0.0129(12) -0.0107(11) O4 0.0623(14) 0.0365(13) 0.0481(14) 0.0135(10) -0.0261(12) -0.0117(11) O5 0.0570(14) 0.0374(13) 0.0621(15) 0.0117(11) -0.0245(12) -0.0212(11) O6 0.0409(12) 0.0370(12) 0.0426(13) 0.0047(10) -0.0039(10) -0.0064(10) _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 O2 1.214(3) . ? C1 N1 1.397(3) . ? C1 C2 1.474(4) . ? C2 C6 1.376(4) . ? C2 C3 1.407(4) . ? C3 C3 1.410(5) 2_666 ? C3 C4 1.422(4) . ? C4 C7 1.371(4) . ? C4 C5 1.475(4) . ? C5 O1 1.213(3) . ? C5 N1 1.409(4) . ? C6 C7 1.398(4) 2_666 ? C6 H6 0.9500 . ? C7 C6 1.398(4) 2_666 ? C7 H7 0.9500 . ? C8 C13 1.366(4) . ? C8 C9 1.376(4) . ? C8 N1 1.449(3) . ? C9 O3 1.374(3) . ? C9 C10 1.387(4) . ? C10 C11 1.380(4) . ? C10 H10 0.9500 . ? C11 C12 1.385(4) . ? C11 H11 0.9500 . ? C12 C13 1.392(4) . ? C12 C21A 1.544(5) . ? C12 C21B 1.548(9) . ? C13 H13 0.9500 . ? C14 O3 1.431(3) . ? C14 C15 1.502(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.366(4) . ? C15 C16 1.389(4) . ? C16 C17 1.383(4) . ? C16 H16 0.9500 . ? C17 C18 1.372(5) . ? C17 H17 0.9500 . ? C18 C19 1.373(5) . ? C18 H18 0.9500 . ? C19 C20 1.384(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21A C23A 1.503(11) . ? C21A C22A 1.538(6) . ? C21A C24A 1.560(10) . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C24A C25A 1.506(9) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C21B C24B 1.41(2) . ? C21B C22B 1.538(7) . ? C21B C23B 1.63(4) . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24B C25B 1.55(2) . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C26 O5 1.213(3) . ? C26 N2 1.407(4) . ? C26 C27 1.470(4) . ? C27 C31 1.368(4) . ? C27 C28 1.417(4) . ? C28 C29 1.412(4) . ? C28 C28 1.413(5) 2_675 ? C29 C32 1.371(4) . ? C29 C30 1.481(4) . ? C30 O4 1.219(3) . ? C30 N2 1.403(4) . ? C31 C32 1.406(4) 2_675 ? C31 H31 0.9500 . ? C32 C31 1.406(4) 2_675 ? C32 H32 0.9500 . ? C33 C38 1.373(4) . ? C33 C34 1.378(4) . ? C33 N2 1.444(4) . ? C34 O6 1.364(3) . ? C34 C35 1.390(4) . ? C35 C36 1.381(4) . ? C35 H35 0.9500 . ? C36 C37 1.391(4) . ? C36 H36 0.9500 . ? C37 C38 1.397(4) . ? C37 C46B 1.533(12) . ? C37 C46A 1.533(13) . ? C38 H38 0.9500 . ? C39 O6 1.436(3) . ? C39 C40 1.505(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.382(4) . ? C40 C45 1.389(4) . ? C41 C42 1.368(4) . ? C41 H41 0.9500 . ? C42 C43 1.375(5) . ? C42 H42 0.9500 . ? C43 C44 1.376(5) . ? C43 H43 0.9500 . ? C44 C45 1.378(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46A C48A 1.53(13) . ? C46A C49A 1.54(15) . ? C46A C47A 1.54(15) . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C49A C50A 1.450(15) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C50A H50A 0.9800 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? C46B C49B 1.41(12) . ? C46B C48B 1.55(12) . ? C46B C47B 1.58(15) . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C49B C50B 1.499(15) . ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? 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 O2 C1 N1 120.3(2) . . ? O2 C1 C2 122.9(3) . . ? N1 C1 C2 116.8(2) . . ? C6 C2 C3 120.2(2) . . ? C6 C2 C1 119.9(3) . . ? C3 C2 C1 119.9(2) . . ? C2 C3 C3 119.7(3) . 2_666 ? C2 C3 C4 121.5(2) . . ? C3 C3 C4 118.8(3) 2_666 . ? C7 C4 C3 120.3(2) . . ? C7 C4 C5 120.2(2) . . ? C3 C4 C5 119.5(2) . . ? O1 C5 N1 120.2(2) . . ? O1 C5 C4 123.3(3) . . ? N1 C5 C4 116.5(2) . . ? C2 C6 C7 120.5(3) . 2_666 ? C2 C6 H6 119.7 . . ? C7 C6 H6 119.7 2_666 . ? C4 C7 C6 120.5(3) . 2_666 ? C4 C7 H7 119.7 . . ? C6 C7 H7 119.7 2_666 . ? C13 C8 C9 121.5(2) . . ? C13 C8 N1 120.1(2) . . ? C9 C8 N1 118.4(2) . . ? O3 C9 C8 115.7(2) . . ? O3 C9 C10 125.8(3) . . ? C8 C9 C10 118.4(3) . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 123.5(3) . . ? C10 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 115.6(3) . . ? C11 C12 C21A 123.2(4) . . ? C13 C12 C21A 120.9(4) . . ? C11 C12 C21B 123.9(9) . . ? C13 C12 C21B 119.2(10) . . ? C8 C13 C12 121.9(3) . . ? C8 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? O3 C14 C15 113.0(2) . . ? O3 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? O3 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C20 C15 C16 118.7(3) . . ? C20 C15 C14 120.1(3) . . ? C16 C15 C14 121.1(3) . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.4(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 120.0(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C15 C20 C19 121.2(3) . . ? C15 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C23A C21A C22A 109.2(7) . . ? C23A C21A C12 112.8(5) . . ? C22A C21A C12 109.9(4) . . ? C23A C21A C24A 109.2(5) . . ? C22A C21A C24A 105.8(5) . . ? C12 C21A C24A 109.8(6) . . ? C21A C22A H22A 109.5 . . ? C21A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C21A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C21A C23A H23A 109.5 . . ? C21A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C21A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? C25A C24A C21A 114.9(5) . . ? C25A C24A H24A 108.6 . . ? C21A C24A H24A 108.6 . . ? C25A C24A H24B 108.6 . . ? C21A C24A H24B 108.6 . . ? H24A C24A H24B 107.5 . . ? C24A C25A H25A 109.5 . . ? C24A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C24A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C24B C21B C22B 113.4(16) . . ? C24B C21B C12 118.9(14) . . ? C22B C21B C12 106.8(8) . . ? C24B C21B C23B 112.2(14) . . ? C22B C21B C23B 100.1(16) . . ? C12 C21B C23B 103.4(17) . . ? C21B C22B H22D 109.5 . . ? C21B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C21B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C21B C23B H23D 109.5 . . ? C21B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C21B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C21B C24B C25B 116.4(15) . . ? C21B C24B H24C 108.2 . . ? C25B C24B H24C 108.2 . . ? C21B C24B H24D 108.2 . . ? C25B C24B H24D 108.2 . . ? H24C C24B H24D 107.3 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C1 N1 C5 125.4(2) . . ? C1 N1 C8 117.1(2) . . ? C5 N1 C8 117.2(2) . . ? C9 O3 C14 117.5(2) . . ? O5 C26 N2 120.4(3) . . ? O5 C26 C27 122.6(3) . . ? N2 C26 C27 117.0(3) . . ? C31 C27 C28 120.6(3) . . ? C31 C27 C26 119.9(3) . . ? C28 C27 C26 119.5(3) . . ? C29 C28 C28 119.3(3) . 2_675 ? C29 C28 C27 122.0(3) . . ? C28 C28 C27 118.7(3) 2_675 . ? C32 C29 C28 120.9(3) . . ? C32 C29 C30 119.7(3) . . ? C28 C29 C30 119.4(3) . . ? O4 C30 N2 120.3(3) . . ? O4 C30 C29 123.0(3) . . ? N2 C30 C29 116.7(3) . . ? C27 C31 C32 120.7(3) . 2_675 ? C27 C31 H31 119.7 . . ? C32 C31 H31 119.7 2_675 . ? C29 C32 C31 119.8(3) . 2_675 ? C29 C32 H32 120.1 . . ? C31 C32 H32 120.1 2_675 . ? C38 C33 C34 121.7(3) . . ? C38 C33 N2 119.7(2) . . ? C34 C33 N2 118.6(3) . . ? O6 C34 C33 116.0(3) . . ? O6 C34 C35 126.1(3) . . ? C33 C34 C35 117.9(3) . . ? C36 C35 C34 120.0(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 122.8(3) . . ? C35 C36 H36 118.6 . . ? C37 C36 H36 118.6 . . ? C36 C37 C38 115.9(3) . . ? C36 C37 C46B 123(6) . . ? C38 C37 C46B 121(6) . . ? C36 C37 C46A 123(6) . . ? C38 C37 C46A 121(6) . . ? C33 C38 C37 121.7(3) . . ? C33 C38 H38 119.2 . . ? C37 C38 H38 119.2 . . ? O6 C39 C40 112.8(2) . . ? O6 C39 H39A 109.0 . . ? C40 C39 H39A 109.0 . . ? O6 C39 H39B 109.0 . . ? C40 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C41 C40 C45 118.6(3) . . ? C41 C40 C39 120.4(3) . . ? C45 C40 C39 121.0(3) . . ? C42 C41 C40 120.6(3) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 120.6(3) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 119.7(4) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C45 119.9(3) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C44 C45 C40 120.6(3) . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? C48A C46A C37 112(6) . . ? C48A C46A C49A 107(8) . . ? C37 C46A C49A 111(9) . . ? C48A C46A C47A 107(8) . . ? C37 C46A C47A 110(8) . . ? C49A C46A C47A 110(6) . . ? C46A C47A H47A 109.5 . . ? C46A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C46A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C46A C48A H48A 109.5 . . ? C46A C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? C46A C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C50A C49A C46A 112(5) . . ? C50A C49A H49A 109.3 . . ? C46A C49A H49A 109.3 . . ? C50A C49A H49B 109.3 . . ? C46A C49A H49B 109.3 . . ? H49A C49A H49B 107.9 . . ? C49A C50A H50A 109.5 . . ? C49A C50A H50B 109.5 . . ? H50A C50A H50B 109.5 . . ? C49A C50A H50C 109.5 . . ? H50A C50A H50C 109.5 . . ? H50B C50A H50C 109.5 . . ? C49B C46B C37 114(6) . . ? C49B C46B C48B 109(8) . . ? C37 C46B C48B 109(6) . . ? C49B C46B C47B 111(7) . . ? C37 C46B C47B 109(8) . . ? C48B C46B C47B 104(6) . . ? C46B C47B H47D 109.5 . . ? C46B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C46B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C46B C48B H48D 109.5 . . ? C46B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C46B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C46B C49B C50B 123(5) . . ? C46B C49B H49C 106.6 . . ? C50B C49B H49C 106.6 . . ? C46B C49B H49D 106.6 . . ? C50B C49B H49D 106.6 . . ? H49C C49B H49D 106.6 . . ? C49B C50B H50D 109.5 . . ? C49B C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? C49B C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? C30 N2 C26 125.3(2) . . ? C30 N2 C33 117.6(2) . . ? C26 N2 C33 116.9(2) . . ? C34 O6 C39 117.6(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 O2 C1 C2 C6 1.0(5) . . . . ? N1 C1 C2 C6 179.5(3) . . . . ? O2 C1 C2 C3 -177.5(3) . . . . ? N1 C1 C2 C3 1.0(4) . . . . ? C6 C2 C3 C3 -1.1(5) . . . 2_666 ? C1 C2 C3 C3 177.4(3) . . . 2_666 ? C6 C2 C3 C4 178.4(3) . . . . ? C1 C2 C3 C4 -3.1(4) . . . . ? C2 C3 C4 C7 179.4(3) . . . . ? C3 C3 C4 C7 -1.2(5) 2_666 . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C3 C4 C5 179.6(3) 2_666 . . . ? C7 C4 C5 O1 3.8(4) . . . . ? C3 C4 C5 O1 -176.9(3) . . . . ? C7 C4 C5 N1 -174.4(3) . . . . ? C3 C4 C5 N1 4.9(4) . . . . ? C3 C2 C6 C7 2.0(4) . . . 2_666 ? C1 C2 C6 C7 -176.4(3) . . . 2_666 ? C3 C4 C7 C6 0.2(4) . . . 2_666 ? C5 C4 C7 C6 179.5(3) . . . 2_666 ? C13 C8 C9 O3 -177.7(2) . . . . ? N1 C8 C9 O3 0.9(4) . . . . ? C13 C8 C9 C10 0.2(4) . . . . ? N1 C8 C9 C10 178.8(2) . . . . ? O3 C9 C10 C11 178.3(2) . . . . ? C8 C9 C10 C11 0.6(4) . . . . ? C9 C10 C11 C12 -0.5(4) . . . . ? C10 C11 C12 C13 -0.4(4) . . . . ? C10 C11 C12 C21A -174.0(3) . . . . ? C10 C11 C12 C21B 166.8(11) . . . . ? C9 C8 C13 C12 -1.2(4) . . . . ? N1 C8 C13 C12 -179.7(3) . . . . ? C11 C12 C13 C8 1.2(4) . . . . ? C21A C12 C13 C8 175.0(4) . . . . ? C21B C12 C13 C8 -166.6(8) . . . . ? O3 C14 C15 C20 -148.7(3) . . . . ? O3 C14 C15 C16 34.8(4) . . . . ? C20 C15 C16 C17 -2.4(4) . . . . ? C14 C15 C16 C17 174.1(3) . . . . ? C15 C16 C17 C18 0.0(5) . . . . ? C16 C17 C18 C19 2.1(5) . . . . ? C17 C18 C19 C20 -1.8(5) . . . . ? C16 C15 C20 C19 2.7(5) . . . . ? C14 C15 C20 C19 -173.9(3) . . . . ? C18 C19 C20 C15 -0.7(5) . . . . ? C11 C12 C21A C23A -16.1(8) . . . . ? C13 C12 C21A C23A 170.5(6) . . . . ? C21B C12 C21A C23A 82(4) . . . . ? C11 C12 C21A C22A 105.9(6) . . . . ? C13 C12 C21A C22A -67.4(7) . . . . ? C21B C12 C21A C22A -156(5) . . . . ? C11 C12 C21A C24A -138.1(4) . . . . ? C13 C12 C21A C24A 48.5(5) . . . . ? C21B C12 C21A C24A -40(4) . . . . ? C23A C21A C24A C25A -63.8(7) . . . . ? C22A C21A C24A C25A 178.8(5) . . . . ? C12 C21A C24A C25A 60.3(6) . . . . ? O2 C1 N1 C5 -176.9(3) . . . . ? C2 C1 N1 C5 4.5(4) . . . . ? O2 C1 N1 C8 -2.4(4) . . . . ? C2 C1 N1 C8 179.0(2) . . . . ? O1 C5 N1 C1 174.3(3) . . . . ? C4 C5 N1 C1 -7.4(4) . . . . ? O1 C5 N1 C8 -0.2(4) . . . . ? C4 C5 N1 C8 178.1(2) . . . . ? C13 C8 N1 C1 83.8(3) . . . . ? C9 C8 N1 C1 -94.8(3) . . . . ? C13 C8 N1 C5 -101.2(3) . . . . ? C9 C8 N1 C5 80.2(3) . . . . ? C8 C9 O3 C14 -176.8(2) . . . . ? C10 C9 O3 C14 5.4(4) . . . . ? C15 C14 O3 C9 77.5(3) . . . . ? O5 C26 C27 C31 0.3(4) . . . . ? N2 C26 C27 C31 -178.7(2) . . . . ? O5 C26 C27 C28 179.8(3) . . . . ? N2 C26 C27 C28 0.9(4) . . . . ? C31 C27 C28 C29 -178.7(3) . . . . ? C26 C27 C28 C29 1.8(4) . . . . ? C31 C27 C28 C28 0.4(4) . . . 2_675 ? C26 C27 C28 C28 -179.1(3) . . . 2_675 ? C28 C28 C29 C32 0.7(5) 2_675 . . . ? C27 C28 C29 C32 179.8(3) . . . . ? C28 C28 C29 C30 179.5(3) 2_675 . . . ? C27 C28 C29 C30 -1.4(4) . . . . ? C32 C29 C30 O4 -1.2(4) . . . . ? C28 C29 C30 O4 180.0(3) . . . . ? C32 C29 C30 N2 177.2(2) . . . . ? C28 C29 C30 N2 -1.6(4) . . . . ? C28 C27 C31 C32 -1.8(4) . . . 2_675 ? C26 C27 C31 C32 177.7(3) . . . 2_675 ? C28 C29 C32 C31 0.7(4) . . . 2_675 ? C30 C29 C32 C31 -178.1(3) . . . 2_675 ? C38 C33 C34 O6 179.3(3) . . . . ? N2 C33 C34 O6 0.0(4) . . . . ? C38 C33 C34 C35 0.6(4) . . . . ? N2 C33 C34 C35 -178.7(3) . . . . ? O6 C34 C35 C36 -179.6(3) . . . . ? C33 C34 C35 C36 -1.1(4) . . . . ? C34 C35 C36 C37 0.0(5) . . . . ? C35 C36 C37 C38 1.5(4) . . . . ? C35 C36 C37 C46B -173(5) . . . . ? C35 C36 C37 C46A 176(6) . . . . ? C34 C33 C38 C37 1.0(5) . . . . ? N2 C33 C38 C37 -179.7(3) . . . . ? C36 C37 C38 C33 -2.0(4) . . . . ? C46B C37 C38 C33 173(5) . . . . ? C46A C37 C38 C33 -176(6) . . . . ? O6 C39 C40 C41 -41.5(4) . . . . ? O6 C39 C40 C45 140.1(3) . . . . ? C45 C40 C41 C42 1.0(5) . . . . ? C39 C40 C41 C42 -177.5(3) . . . . ? C40 C41 C42 C43 -1.1(5) . . . . ? C41 C42 C43 C44 1.5(5) . . . . ? C42 C43 C44 C45 -1.9(5) . . . . ? C43 C44 C45 C40 1.8(5) . . . . ? C41 C40 C45 C44 -1.3(5) . . . . ? C39 C40 C45 C44 177.1(3) . . . . ? O4 C30 N2 C26 -177.0(3) . . . . ? C29 C30 N2 C26 4.5(4) . . . . ? O4 C30 N2 C33 -0.8(4) . . . . ? C29 C30 N2 C33 -179.3(2) . . . . ? O5 C26 N2 C30 176.9(3) . . . . ? C27 C26 N2 C30 -4.2(4) . . . . ? O5 C26 N2 C33 0.7(4) . . . . ? C27 C26 N2 C33 179.6(2) . . . . ? C38 C33 N2 C30 99.4(3) . . . . ? C34 C33 N2 C30 -81.3(3) . . . . ? C38 C33 N2 C26 -84.1(3) . . . . ? C34 C33 N2 C26 95.2(3) . . . . ? C33 C34 O6 C39 171.1(3) . . . . ? C35 C34 O6 C39 -10.3(4) . . . . ? C40 C39 O6 C34 -71.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.930 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.047 #===END