# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_method SHELXL-97 _publ_contact_author_name 'Prof Kay Severin' _publ_contact_author_address ; ISIC EPFL Lausanne 1015 SWITZERLAND ; _publ_contact_author_email kay.severin@epfl.ch _publ_contact_author_fax '+41 21 693 9305' _publ_contact_author_phone '+41 21 693 9302' _publ_section_title ; A new method for the synthesis of boronate macrocycles ; loop_ _publ_author_name N.Christinat R.Scopelliti K.Severin data_1 _database_code_depnum_ccdc_archive 'CCDC 233235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 B4 N4 O8' _chemical_formula_sum 'C44 H32 B4 N4 O8' _chemical_formula_weight 787.98 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' B B 0.0013 0.0007 '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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 16.7128(8) _cell_length_b 16.7128(8) _cell_length_c 13.9916(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3908.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 4771 _cell_measurement_theta_min 3.058 _cell_measurement_theta_max 26.81185 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.555 _exptl_absorpt_correction_T_max 0.863 _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction KM4/Sapphire CCD' _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 11750 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1729 _reflns_number_gt 1445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction CrysAlis RED' _computing_data_reduction 'Oxford Diffraction CrysAlis RED' _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^)+(0.0553P)^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 SHELXL _refine_ls_extinction_coef 0.0004(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1729 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 O1 O 0.38001(6) -0.23523(6) 0.08966(7) 0.0175(3) Uani 1 1 d . . . O2 O 0.34729(6) -0.10489(6) 0.14639(7) 0.0190(3) Uani 1 1 d . . . N1 N 0.37030(7) -0.30133(7) 0.23745(8) 0.0170(3) Uani 1 1 d . . . C1 C 0.36622(8) -0.23555(8) 0.18279(10) 0.0158(3) Uani 1 1 d . . . C2 C 0.34634(8) -0.15913(8) 0.21845(10) 0.0169(3) Uani 1 1 d . . . C3 C 0.32879(9) -0.14964(9) 0.31337(11) 0.0206(4) Uani 1 1 d . . . H3 H 0.3154 -0.0988 0.3393 0.025 Uiso 1 1 calc R . . C4 C 0.33151(9) -0.21901(9) 0.37080(10) 0.0227(4) Uani 1 1 d . . . H4 H 0.3189 -0.2151 0.4368 0.027 Uiso 1 1 calc R . . C5 C 0.35192(9) -0.29155(9) 0.33349(10) 0.0202(4) Uani 1 1 d . . . H5 H 0.3536 -0.3368 0.3745 0.024 Uiso 1 1 calc R . . C6 C 0.29263(8) -0.14383(9) -0.01929(10) 0.0177(4) Uani 1 1 d . . . C7 C 0.27489(9) -0.20499(9) -0.08481(11) 0.0230(4) Uani 1 1 d . . . H7 H 0.3094 -0.2501 -0.0889 0.028 Uiso 1 1 calc R . . C8 C 0.20794(10) -0.20106(10) -0.14382(11) 0.0271(4) Uani 1 1 d . . . H8 H 0.1972 -0.2433 -0.1874 0.033 Uiso 1 1 calc R . . C9 C 0.15682(10) -0.13565(10) -0.13920(11) 0.0281(4) Uani 1 1 d . . . H9 H 0.1110 -0.1331 -0.1792 0.034 Uiso 1 1 calc R . . C10 C 0.17320(9) -0.07397(10) -0.07567(12) 0.0255(4) Uani 1 1 d . . . H10 H 0.1388 -0.0288 -0.0726 0.031 Uiso 1 1 calc R . . C11 C 0.24029(9) -0.07826(9) -0.01629(11) 0.0213(4) Uani 1 1 d . . . H11 H 0.2507 -0.0358 0.0271 0.026 Uiso 1 1 calc R . . B1 B 0.36505(10) -0.14949(10) 0.05611(12) 0.0181(4) 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 O1 0.0205(6) 0.0176(6) 0.0144(6) 0.0007(4) 0.0003(4) 0.0022(4) O2 0.0207(6) 0.0182(6) 0.0182(6) 0.0003(4) 0.0006(4) 0.0028(4) N1 0.0159(7) 0.0193(7) 0.0159(6) 0.0004(5) 0.0000(5) -0.0025(5) C1 0.0122(7) 0.0204(8) 0.0148(7) 0.0000(6) -0.0003(6) -0.0015(6) C2 0.0131(8) 0.0182(8) 0.0195(8) 0.0011(6) -0.0012(6) -0.0012(6) C3 0.0184(8) 0.0217(8) 0.0216(8) -0.0057(6) 0.0005(6) -0.0007(6) C4 0.0236(9) 0.0291(9) 0.0153(8) -0.0020(6) 0.0030(6) -0.0023(7) C5 0.0195(8) 0.0244(8) 0.0166(8) 0.0025(6) 0.0013(6) -0.0029(6) C6 0.0175(8) 0.0188(8) 0.0168(8) 0.0025(6) 0.0028(6) -0.0020(6) C7 0.0243(9) 0.0215(8) 0.0232(8) 0.0011(7) -0.0001(7) 0.0037(6) C8 0.0288(9) 0.0288(9) 0.0238(9) -0.0028(7) -0.0032(7) -0.0041(7) C9 0.0210(9) 0.0362(10) 0.0272(9) 0.0046(8) -0.0071(7) -0.0011(7) C10 0.0203(8) 0.0256(9) 0.0307(9) 0.0059(7) -0.0003(7) 0.0045(7) C11 0.0206(8) 0.0201(8) 0.0232(8) 0.0015(6) 0.0010(7) -0.0009(6) B1 0.0209(9) 0.0158(9) 0.0175(8) 0.0001(7) 0.0007(7) 0.0021(7) _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 O1 C1 1.3233(16) . ? O1 B1 1.5285(19) . ? O2 C2 1.3559(17) . ? O2 B1 1.4964(19) . ? N1 C1 1.3409(18) . ? N1 C5 1.3880(18) . ? N1 B1 1.601(2) 12_656 ? C1 C2 1.4108(19) . ? C2 C3 1.369(2) . ? C3 C4 1.411(2) . ? C3 H3 0.9500 . ? C4 C5 1.363(2) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C11 1.403(2) . ? C6 C7 1.405(2) . ? C6 B1 1.608(2) . ? C7 C8 1.392(2) . ? C7 H7 0.9500 . ? C8 C9 1.389(2) . ? C8 H8 0.9500 . ? C9 C10 1.388(2) . ? C9 H9 0.9500 . ? C10 C11 1.397(2) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? B1 N1 1.601(2) 15_655 ? 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 C1 O1 B1 106.12(11) . . ? C2 O2 B1 107.28(11) . . ? C1 N1 C5 116.38(12) . . ? C1 N1 B1 120.93(12) . 12_656 ? C5 N1 B1 122.61(12) . 12_656 ? O1 C1 N1 123.79(13) . . ? O1 C1 C2 112.68(12) . . ? N1 C1 C2 123.54(13) . . ? O2 C2 C3 130.26(13) . . ? O2 C2 C1 109.85(12) . . ? C3 C2 C1 119.89(13) . . ? C2 C3 C4 116.75(14) . . ? C2 C3 H3 121.6 . . ? C4 C3 H3 121.6 . . ? C5 C4 C3 121.37(14) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 N1 122.06(14) . . ? C4 C5 H5 119.0 . . ? N1 C5 H5 119.0 . . ? C11 C6 C7 117.15(14) . . ? C11 C6 B1 119.71(13) . . ? C7 C6 B1 122.97(14) . . ? C8 C7 C6 121.50(15) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C9 C8 C7 120.25(15) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 119.54(14) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.05(15) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C6 121.52(14) . . ? C10 C11 H11 119.2 . . ? C6 C11 H11 119.2 . . ? O2 B1 O1 103.90(11) . . ? O2 B1 N1 110.05(12) . 15_655 ? O1 B1 N1 105.07(11) . 15_655 ? O2 B1 C6 112.03(12) . . ? O1 B1 C6 112.31(12) . . ? N1 B1 C6 112.91(12) 15_655 . ? 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 B1 O1 C1 N1 177.46(13) . . . . ? B1 O1 C1 C2 -2.27(15) . . . . ? C5 N1 C1 O1 -178.30(13) . . . . ? B1 N1 C1 O1 4.9(2) 12_656 . . . ? C5 N1 C1 C2 1.4(2) . . . . ? B1 N1 C1 C2 -175.44(13) 12_656 . . . ? B1 O2 C2 C3 -176.07(15) . . . . ? B1 O2 C2 C1 2.96(16) . . . . ? O1 C1 C2 O2 -0.41(17) . . . . ? N1 C1 C2 O2 179.86(12) . . . . ? O1 C1 C2 C3 178.73(12) . . . . ? N1 C1 C2 C3 -1.0(2) . . . . ? O2 C2 C3 C4 178.69(14) . . . . ? C1 C2 C3 C4 -0.3(2) . . . . ? C2 C3 C4 C5 1.0(2) . . . . ? C3 C4 C5 N1 -0.6(2) . . . . ? C1 N1 C5 C4 -0.6(2) . . . . ? B1 N1 C5 C4 176.19(13) 12_656 . . . ? C11 C6 C7 C8 -0.4(2) . . . . ? B1 C6 C7 C8 174.73(14) . . . . ? C6 C7 C8 C9 0.2(2) . . . . ? C7 C8 C9 C10 0.4(2) . . . . ? C8 C9 C10 C11 -0.6(2) . . . . ? C9 C10 C11 C6 0.3(2) . . . . ? C7 C6 C11 C10 0.2(2) . . . . ? B1 C6 C11 C10 -175.14(13) . . . . ? C2 O2 B1 O1 -4.10(14) . . . . ? C2 O2 B1 N1 -116.14(12) . . . 15_655 ? C2 O2 B1 C6 117.37(13) . . . . ? C1 O1 B1 O2 3.83(14) . . . . ? C1 O1 B1 N1 119.45(11) . . . 15_655 ? C1 O1 B1 C6 -117.45(13) . . . . ? C11 C6 B1 O2 25.96(19) . . . . ? C7 C6 B1 O2 -149.10(13) . . . . ? C11 C6 B1 O1 142.45(13) . . . . ? C7 C6 B1 O1 -32.61(19) . . . . ? C11 C6 B1 N1 -98.97(15) . . . 15_655 ? C7 C6 B1 N1 85.97(17) . . . 15_655 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.350 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.046 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 233236' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H68 B4 N8 O12, 2(C6 H6), 0.5(C5 H12)' _chemical_formula_sum 'C78.50 H86 B4 N8 O12' _chemical_formula_weight 1376.79 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' B B 0.0013 0.0007 '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 Iba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1, y+1, z+1/2' _cell_length_a 26.3143(18) _cell_length_b 28.029(2) _cell_length_c 20.2248(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14917.2(17) _cell_formula_units_Z 8 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 5679 _cell_measurement_theta_min 2.0582 _cell_measurement_theta_max 19.29685 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5832 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9438 _exptl_absorpt_correction_T_max 1.0157 _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Oxford Diffraction KM4/Sapphire CCD' _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 44532 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.03 _reflns_number_total 12697 _reflns_number_gt 7698 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction CrysAlis RED' _computing_data_reduction 'Oxford Diffraction CrysAlis RED' _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^)+(0.0714P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.9(11) _refine_ls_number_reflns 12697 _refine_ls_number_parameters 998 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.002 _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 O1 O 0.16759(10) 0.17117(9) 0.40568(14) 0.0328(7) Uani 1 1 d . . . O2 O 0.20978(10) 0.14764(10) 0.30809(14) 0.0343(7) Uani 1 1 d . . . O3 O 0.43772(15) 0.25139(14) 0.1846(2) 0.0791(13) Uani 1 1 d . . . O4 O 0.19081(9) 0.19541(9) 0.54209(14) 0.0338(7) Uani 1 1 d . . . O5 O 0.14301(10) 0.25459(9) 0.48659(15) 0.0371(7) Uani 1 1 d . . . O6 O -0.1040(2) 0.3018(2) 0.5648(3) 0.133(2) Uani 1 1 d . . . O7 O 0.19649(9) 0.09199(9) 0.54961(13) 0.0291(6) Uani 1 1 d . . . O8 O 0.19065(10) 0.12988(10) 0.65408(14) 0.0350(7) Uani 1 1 d . . . O10 O 0.24972(9) 0.09928(9) 0.42491(13) 0.0311(7) Uani 1 1 d . . . O11 O 0.25936(9) 0.02373(9) 0.47526(13) 0.0305(7) Uani 1 1 d . . . O12 O 0.11224(13) -0.17709(11) 0.38899(18) 0.0556(9) Uani 1 1 d . . . N1 N 0.22623(11) 0.22915(11) 0.43831(17) 0.0305(8) Uani 1 1 d . . . N2 N 0.35674(15) 0.20962(16) 0.2535(2) 0.0572(12) Uani 1 1 d . . . N3 N 0.12348(12) 0.14561(11) 0.56986(16) 0.0292(8) Uani 1 1 d . . . N4 N -0.02164(13) 0.25461(12) 0.50544(19) 0.0399(9) Uani 1 1 d . . . N5 N 0.28483(11) 0.09585(11) 0.53909(17) 0.0310(8) Uani 1 1 d . . . N7 N 0.16940(12) 0.08467(11) 0.37780(17) 0.0302(8) Uani 1 1 d . . . N8 N 0.14738(13) -0.08898(12) 0.43958(19) 0.0380(9) Uani 1 1 d . . . C1 C 0.20939(15) 0.19584(14) 0.3958(2) 0.0319(10) Uani 1 1 d . . . C2 C 0.23506(14) 0.18227(14) 0.3391(2) 0.0308(10) Uani 1 1 d . . . C3 C 0.28019(16) 0.20297(16) 0.3215(2) 0.0377(11) Uani 1 1 d . . . C4 C 0.29806(16) 0.23868(16) 0.3656(2) 0.0394(11) Uani 1 1 d . . . H4 H 0.3292 0.2544 0.3562 0.047 Uiso 1 1 calc R . . C5 C 0.27159(15) 0.25099(15) 0.4215(2) 0.0359(10) Uani 1 1 d . . . H5 H 0.2848 0.2752 0.4495 0.043 Uiso 1 1 calc R . . C6 C 0.30898(18) 0.1850(2) 0.2623(3) 0.0624(15) Uani 1 1 d . . . H6A H 0.3156 0.1504 0.2677 0.075 Uiso 1 1 calc R . . H6B H 0.2879 0.1892 0.2222 0.075 Uiso 1 1 calc R . . C7 C 0.3930(2) 0.1794(2) 0.2147(3) 0.0709(16) Uani 1 1 d . . . H7A H 0.3809 0.1751 0.1687 0.085 Uiso 1 1 calc R . . H7B H 0.3970 0.1476 0.2354 0.085 Uiso 1 1 calc R . . C8 C 0.4429(2) 0.2068(2) 0.2160(4) 0.0829(19) Uani 1 1 d . . . H8A H 0.4537 0.2116 0.2625 0.099 Uiso 1 1 calc R . . H8B H 0.4696 0.1879 0.1934 0.099 Uiso 1 1 calc R . . C9 C 0.40112(19) 0.27876(19) 0.2157(3) 0.0624(15) Uani 1 1 d . . . H9A H 0.3963 0.3090 0.1912 0.075 Uiso 1 1 calc R . . H9B H 0.4124 0.2866 0.2611 0.075 Uiso 1 1 calc R . . C10 C 0.3517(2) 0.2520(2) 0.2185(3) 0.0739(18) Uani 1 1 d . . . H10A H 0.3257 0.2722 0.2400 0.089 Uiso 1 1 calc R . . H10B H 0.3401 0.2450 0.1730 0.089 Uiso 1 1 calc R . . C11 C 0.14224(14) 0.18453(14) 0.5422(2) 0.0311(10) Uani 1 1 d . . . C12 C 0.11286(14) 0.21919(14) 0.5112(2) 0.0315(10) Uani 1 1 d . . . C13 C 0.06115(15) 0.21533(15) 0.5075(2) 0.0370(10) Uani 1 1 d . . . C14 C 0.04133(15) 0.17352(15) 0.5364(2) 0.0382(11) Uani 1 1 d . . . H14 H 0.0057 0.1683 0.5351 0.046 Uiso 1 1 calc R . . C15 C 0.07097(15) 0.14084(15) 0.5659(2) 0.0354(10) Uani 1 1 d . . . H15 H 0.0555 0.1134 0.5847 0.042 Uiso 1 1 calc R . . C16 C 0.02757(17) 0.25174(17) 0.4741(3) 0.0555(14) Uani 1 1 d . . . H16A H 0.0442 0.2834 0.4758 0.067 Uiso 1 1 calc R . . H16B H 0.0231 0.2429 0.4270 0.067 Uiso 1 1 calc R . . C17 C -0.05698(18) 0.28294(18) 0.4660(3) 0.0568(14) Uani 1 1 d . . . H17A H -0.0610 0.2685 0.4217 0.068 Uiso 1 1 calc R . . H17B H -0.0437 0.3157 0.4605 0.068 Uiso 1 1 calc R . . C18 C -0.1073(2) 0.2844(2) 0.5009(4) 0.080(2) Uani 1 1 d . . . H18A H -0.1310 0.3046 0.4753 0.096 Uiso 1 1 calc R . . H18B H -0.1217 0.2517 0.5022 0.096 Uiso 1 1 calc R . . C19 C -0.0704(3) 0.2736(3) 0.6027(3) 0.128(4) Uani 1 1 d . . . H19A H -0.0830 0.2403 0.6048 0.154 Uiso 1 1 calc R . . H19B H -0.0683 0.2862 0.6484 0.154 Uiso 1 1 calc R . . C20 C -0.0189(2) 0.2747(2) 0.5710(3) 0.087(2) Uani 1 1 d . . . H20A H -0.0066 0.3080 0.5685 0.105 Uiso 1 1 calc R . . H20B H 0.0055 0.2562 0.5981 0.105 Uiso 1 1 calc R . . C21 C 0.24177(15) 0.10406(13) 0.5727(2) 0.0279(9) Uani 1 1 d . . . C22 C 0.23935(15) 0.12587(14) 0.6339(2) 0.0331(10) Uani 1 1 d . . . C23 C 0.28252(16) 0.13865(15) 0.6668(2) 0.0384(11) Uani 1 1 d . B . C24 C 0.32813(16) 0.12954(16) 0.6319(2) 0.0409(11) Uani 1 1 d . . . H24 H 0.3595 0.1378 0.6522 0.049 Uiso 1 1 calc R . . C25 C 0.32917(17) 0.11004(15) 0.5721(2) 0.0422(11) Uani 1 1 d . . . H25 H 0.3610 0.1056 0.5509 0.051 Uiso 1 1 calc R . . C26 C 0.2820(2) 0.1624(2) 0.7334(3) 0.0708(17) Uani 1 1 d DU . . H26A H 0.2847 0.1974 0.7275 0.085 Uiso 1 1 calc R A 1 H26B H 0.2494 0.1555 0.7558 0.085 Uiso 1 1 calc R A 1 N6A N 0.3247(4) 0.1455(3) 0.7754(5) 0.060(3) Uani 0.647(6) 1 d PDU B 1 C27A C 0.3314(5) 0.1788(5) 0.8301(6) 0.099(5) Uani 0.647(6) 1 d PDU B 1 H27A H 0.3007 0.1795 0.8584 0.119 Uiso 0.647(6) 1 calc PR B 1 H27B H 0.3379 0.2114 0.8133 0.119 Uiso 0.647(6) 1 calc PR B 1 C28A C 0.3796(5) 0.1594(5) 0.8710(5) 0.108(4) Uani 0.647(6) 1 d PDU B 1 H28A H 0.4106 0.1596 0.8432 0.130 Uiso 0.647(6) 1 calc PR B 1 H28B H 0.3857 0.1793 0.9107 0.130 Uiso 0.647(6) 1 calc PR B 1 O9A O 0.3657(4) 0.1092(4) 0.8905(5) 0.162(5) Uani 0.647(6) 1 d PDU B 1 C29A C 0.3566(6) 0.0800(5) 0.8354(6) 0.162(7) Uani 0.647(6) 1 d PDU B 1 H29A H 0.3492 0.0472 0.8505 0.195 Uiso 0.647(6) 1 calc PR B 1 H29B H 0.3875 0.0789 0.8075 0.195 Uiso 0.647(6) 1 calc PR B 1 C30A C 0.3136(4) 0.0978(4) 0.7958(5) 0.094(3) Uani 0.647(6) 1 d PDU B 1 H30A H 0.3085 0.0772 0.7566 0.113 Uiso 0.647(6) 1 calc PR B 1 H30B H 0.2821 0.0973 0.8225 0.113 Uiso 0.647(6) 1 calc PR B 1 N6B N 0.3306(6) 0.1632(5) 0.7640(11) 0.053(4) Uani 0.353(6) 1 d PDU B 2 C27B C 0.3396(7) 0.2133(6) 0.7697(17) 0.136(10) Uani 0.353(6) 1 d PDU B 2 H27C H 0.3214 0.2260 0.8088 0.163 Uiso 0.353(6) 1 calc PR B 2 H27D H 0.3265 0.2298 0.7300 0.163 Uiso 0.353(6) 1 calc PR B 2 C28B C 0.3951(7) 0.2224(9) 0.7767(10) 0.116(7) Uani 0.353(6) 1 d PDU B 2 H28C H 0.4163 0.1990 0.7526 0.139 Uiso 0.353(6) 1 calc PR B 2 H28D H 0.4049 0.2554 0.7645 0.139 Uiso 0.353(6) 1 calc PR B 2 O9B O 0.3943(5) 0.2149(6) 0.8441(8) 0.118(5) Uani 0.353(6) 1 d PDU B 2 C29B C 0.3950(14) 0.1629(9) 0.854(2) 0.23(2) Uani 0.353(6) 1 d PDU B 2 H29C H 0.4022 0.1531 0.9001 0.279 Uiso 0.353(6) 1 calc PR B 2 H29D H 0.4170 0.1456 0.8224 0.279 Uiso 0.353(6) 1 calc PR B 2 C30B C 0.3369(12) 0.1616(10) 0.8356(12) 0.094(3) Uani 0.35 1 d PDU B 2 H30C H 0.3213 0.1320 0.8532 0.113 Uiso 0.353(6) 1 calc PR B 2 H30D H 0.3193 0.1892 0.8559 0.113 Uiso 0.353(6) 1 calc PR B 2 C31 C 0.21026(14) 0.07139(13) 0.41323(19) 0.0259(9) Uani 1 1 d . . . C32 C 0.21575(14) 0.02661(14) 0.4424(2) 0.0309(9) Uani 1 1 d . . . C33 C 0.17802(14) -0.00740(14) 0.4361(2) 0.0310(9) Uani 1 1 d . . . C34 C 0.13569(15) 0.00698(14) 0.3983(2) 0.0333(10) Uani 1 1 d . . . H34 H 0.1086 -0.0149 0.3918 0.040 Uiso 1 1 calc R . . C35 C 0.13253(16) 0.05043(15) 0.3712(2) 0.0382(11) Uani 1 1 d . . . H35 H 0.1031 0.0580 0.3461 0.046 Uiso 1 1 calc R . . C36 C 0.18149(17) -0.05465(15) 0.4701(2) 0.0432(12) Uani 1 1 d . . . H36A H 0.2168 -0.0666 0.4676 0.052 Uiso 1 1 calc R . . H36B H 0.1725 -0.0508 0.5173 0.052 Uiso 1 1 calc R . . C37 C 0.16843(17) -0.10936(16) 0.3797(2) 0.0442(12) Uani 1 1 d . . . H37A H 0.1986 -0.1289 0.3905 0.053 Uiso 1 1 calc R . . H37B H 0.1791 -0.0835 0.3493 0.053 Uiso 1 1 calc R . . C38 C 0.1287(2) -0.14004(17) 0.3467(3) 0.0586(14) Uani 1 1 d . . . H38A H 0.0992 -0.1200 0.3342 0.070 Uiso 1 1 calc R . . H38B H 0.1430 -0.1540 0.3058 0.070 Uiso 1 1 calc R . . C39 C 0.09191(17) -0.15686(16) 0.4471(3) 0.0511(13) Uani 1 1 d . . . H39A H 0.0795 -0.1826 0.4764 0.061 Uiso 1 1 calc R . . H39B H 0.0626 -0.1364 0.4355 0.061 Uiso 1 1 calc R . . C40 C 0.13109(19) -0.12751(16) 0.4834(3) 0.0498(13) Uani 1 1 d . . . H40A H 0.1162 -0.1141 0.5243 0.060 Uiso 1 1 calc R . . H40B H 0.1605 -0.1477 0.4955 0.060 Uiso 1 1 calc R . . C41 C 0.11298(16) 0.14387(14) 0.3075(2) 0.0374(11) Uani 1 1 d . . . C42 C 0.06774(17) 0.15924(18) 0.3385(3) 0.0527(13) Uani 1 1 d . . . H42 H 0.0674 0.1643 0.3849 0.063 Uiso 1 1 calc R . . C43 C 0.0238(2) 0.1671(2) 0.3021(3) 0.0732(18) Uani 1 1 d . . . H43 H -0.0063 0.1774 0.3238 0.088 Uiso 1 1 calc R . . C44 C 0.0238(2) 0.16007(19) 0.2345(3) 0.0614(15) Uani 1 1 d . . . H44 H -0.0062 0.1659 0.2096 0.074 Uiso 1 1 calc R . . C45 C 0.0665(2) 0.1449(2) 0.2039(3) 0.0583(14) Uani 1 1 d . . . H45 H 0.0665 0.1402 0.1574 0.070 Uiso 1 1 calc R . . C46 C 0.10992(18) 0.13620(18) 0.2393(2) 0.0482(13) Uani 1 1 d . . . H46 H 0.1390 0.1245 0.2167 0.058 Uiso 1 1 calc R . . C47 C 0.22423(15) 0.28216(15) 0.5464(2) 0.0345(10) Uani 1 1 d . . . C48 C 0.20773(17) 0.32883(16) 0.5446(3) 0.0463(12) Uani 1 1 d . . . H48 H 0.1795 0.3370 0.5175 0.056 Uiso 1 1 calc R . . C49 C 0.2319(2) 0.36440(18) 0.5819(3) 0.0528(13) Uani 1 1 d . . . H49 H 0.2201 0.3964 0.5795 0.063 Uiso 1 1 calc R . . C50 C 0.2719(2) 0.35364(17) 0.6214(2) 0.0489(13) Uani 1 1 d . . . H50 H 0.2879 0.3777 0.6470 0.059 Uiso 1 1 calc R . . C51 C 0.28889(18) 0.30751(18) 0.6238(2) 0.0492(13) Uani 1 1 d . . . H51 H 0.3168 0.2996 0.6515 0.059 Uiso 1 1 calc R . . C52 C 0.26582(17) 0.27203(16) 0.5863(2) 0.0424(11) Uani 1 1 d . . . H52 H 0.2787 0.2404 0.5880 0.051 Uiso 1 1 calc R . . C53 C 0.12708(14) 0.06313(15) 0.6300(2) 0.0310(10) Uani 1 1 d . . . C54 C 0.11626(18) 0.0598(2) 0.6970(2) 0.0541(14) Uani 1 1 d . . . H54 H 0.1269 0.0848 0.7256 0.065 Uiso 1 1 calc R . . C55 C 0.0904(2) 0.0212(2) 0.7235(3) 0.0653(16) Uani 1 1 d . . . H55 H 0.0842 0.0198 0.7697 0.078 Uiso 1 1 calc R . . C56 C 0.0739(2) -0.0149(2) 0.6833(3) 0.0652(16) Uani 1 1 d . . . H56 H 0.0554 -0.0410 0.7011 0.078 Uiso 1 1 calc R . . C57 C 0.08448(19) -0.01285(18) 0.6166(3) 0.0547(14) Uani 1 1 d . . . H57 H 0.0738 -0.0379 0.5881 0.066 Uiso 1 1 calc R . . C58 C 0.11080(17) 0.02589(16) 0.5912(2) 0.0447(12) Uani 1 1 d . . . H58 H 0.1179 0.0267 0.5451 0.054 Uiso 1 1 calc R . . C59 C 0.34144(15) 0.06666(15) 0.4389(2) 0.0359(10) Uani 1 1 d . . . C60 C 0.36932(18) 0.02610(19) 0.4471(3) 0.0623(15) Uani 1 1 d . . . H60 H 0.3554 0.0002 0.4714 0.075 Uiso 1 1 calc R . . C61 C 0.41817(19) 0.0221(2) 0.4204(4) 0.085(2) Uani 1 1 d . . . H61 H 0.4372 -0.0064 0.4270 0.102 Uiso 1 1 calc R . . C62 C 0.4385(2) 0.0585(3) 0.3852(3) 0.082(2) Uani 1 1 d . . . H62 H 0.4717 0.0558 0.3673 0.099 Uiso 1 1 calc R . . C63 C 0.4106(2) 0.0996(2) 0.3758(3) 0.0649(16) Uani 1 1 d . . . H63 H 0.4245 0.1254 0.3513 0.078 Uiso 1 1 calc R . . C64 C 0.36269(17) 0.10314(18) 0.4018(2) 0.0453(12) Uani 1 1 d . . . H64 H 0.3435 0.1313 0.3942 0.054 Uiso 1 1 calc R . . B1 B 0.16416(19) 0.13714(16) 0.3473(2) 0.0324(12) Uani 1 1 d . . . B2 B 0.19625(18) 0.24215(18) 0.5041(3) 0.0359(12) Uani 1 1 d . . . B3 B 0.15889(17) 0.10677(17) 0.6031(2) 0.0305(11) Uani 1 1 d . . . B4 B 0.28544(17) 0.07080(16) 0.4694(2) 0.0317(11) Uani 1 1 d . . . C65 C 0.2848(4) -0.00640(16) 0.6405(2) 0.110(3) Uani 1 1 d G . . H65 H 0.2842 0.0014 0.5948 0.132 Uiso 1 1 calc R . . C66 C 0.2395(2) -0.01054(18) 0.6755(4) 0.112(3) Uani 1 1 d G . . H66 H 0.2080 -0.0055 0.6537 0.134 Uiso 1 1 calc R . . C67 C 0.2404(2) -0.0220(2) 0.7424(4) 0.135(4) Uani 1 1 d G . . H67 H 0.2095 -0.0248 0.7663 0.162 Uiso 1 1 calc R . . C68 C 0.2866(3) -0.0293(3) 0.7742(2) 0.157(4) Uani 1 1 d G . . H68 H 0.2872 -0.0371 0.8199 0.188 Uiso 1 1 calc R . . C69 C 0.33181(19) -0.0252(2) 0.7393(4) 0.132(3) Uani 1 1 d G . . H69 H 0.3633 -0.0302 0.7610 0.158 Uiso 1 1 calc R . . C70 C 0.3309(2) -0.01372(19) 0.6724(4) 0.114(3) Uani 1 1 d G . . H70 H 0.3618 -0.0109 0.6485 0.137 Uiso 1 1 calc R . . C71 C 0.0056(2) 0.0485(2) 0.4178(5) 0.085(2) Uani 1 1 d . . . H71 H 0.0093 0.0822 0.4185 0.102 Uiso 1 1 calc R . . C72 C 0.0028(2) 0.0243(3) 0.3597(4) 0.085(2) Uani 1 1 d . . . H72 H 0.0047 0.0411 0.3190 0.102 Uiso 1 1 calc R . . C73 C 0.0031(3) 0.0235(3) 0.4737(4) 0.093(2) Uani 1 1 d . . . H73 H 0.0059 0.0397 0.5148 0.112 Uiso 1 1 calc R . . C74 C 0.4846(9) 0.0740(8) 1.1549(8) 0.29(2) Uani 0.50 1 d PGDU C 3 H74 H 0.4885 0.0693 1.2011 0.080 Uiso 0.50 1 calc PR C 3 C75 C 0.4367(7) 0.0823(6) 1.1285(12) 0.32(2) Uani 0.50 1 d PGDU C 3 H75 H 0.4078 0.0833 1.1566 0.080 Uiso 0.50 1 calc PR C 3 C76 C 0.4310(4) 0.0892(8) 1.0608(13) 0.38(3) Uani 0.50 1 d PGDU C 3 H76 H 0.3982 0.0949 1.0427 0.080 Uiso 0.50 1 calc PR C 3 C77 C 0.4732(7) 0.0877(8) 1.0196(8) 0.195(12) Uani 0.50 1 d PGDU C 3 H77 H 0.4693 0.0924 0.9733 0.080 Uiso 0.50 1 calc PR C 3 C78 C 0.5212(5) 0.0794(6) 1.0460(9) 0.141(7) Uani 0.50 1 d PGDU C 3 H78 H 0.5500 0.0784 1.0178 0.080 Uiso 0.50 1 calc PR C 3 C79 C 0.5269(6) 0.0725(8) 1.1137(10) 0.178(13) Uani 0.50 1 d PGU C 3 H79 H 0.5596 0.0668 1.1317 0.080 Uiso 0.50 1 calc PR C 3 C80 C 0.5364(8) 0.0663(11) 1.2127(11) 0.211(12) Uani 0.50 1 d PDU D 4 H80A H 0.5714 0.0590 1.2256 0.080 Uiso 0.50 1 calc PR D 4 H80B H 0.5140 0.0401 1.2263 0.080 Uiso 0.50 1 calc PR D 4 H80C H 0.5255 0.0958 1.2345 0.080 Uiso 0.50 1 calc PR D 4 C81 C 0.5336(7) 0.0725(11) 1.1387(12) 0.186(11) Uani 0.50 1 d PDU D 4 H81A H 0.5534 0.1007 1.1248 0.080 Uiso 0.50 1 calc PR D 4 H81B H 0.5474 0.0440 1.1161 0.080 Uiso 0.50 1 calc PR D 4 C82 C 0.4800(7) 0.0788(9) 1.1223(11) 0.142(6) Uani 0.50 1 d PDU D 4 H82A H 0.4594 0.0533 1.1429 0.080 Uiso 0.50 1 calc PR D 4 H82B H 0.4677 0.1100 1.1389 0.080 Uiso 0.50 1 calc PR D 4 C83 C 0.4753(9) 0.0768(11) 1.0506(11) 0.186(11) Uani 0.50 1 d PDU D 4 H83A H 0.4815 0.0438 1.0351 0.080 Uiso 0.50 1 calc PR D 4 H83B H 0.5011 0.0978 1.0300 0.080 Uiso 0.50 1 calc PR D 4 C84 C 0.4225(8) 0.0926(7) 1.0301(10) 0.144(7) Uani 0.50 1 d PDU D 4 H84A H 0.4197 0.0916 0.9818 0.080 Uiso 0.50 1 calc PR D 4 H84B H 0.4166 0.1253 1.0456 0.080 Uiso 0.50 1 calc PR D 4 H84C H 0.3972 0.0713 1.0498 0.080 Uiso 0.50 1 calc PR D 4 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 O1 0.0323(16) 0.0237(15) 0.0423(17) 0.0005(14) 0.0019(13) -0.0083(12) O2 0.0331(16) 0.0338(16) 0.0359(16) 0.0036(14) 0.0024(14) -0.0088(13) O3 0.086(3) 0.063(3) 0.088(3) -0.009(2) 0.060(2) -0.026(2) O4 0.0277(15) 0.0300(15) 0.0437(17) 0.0041(15) 0.0069(14) 0.0002(12) O5 0.0324(16) 0.0212(15) 0.058(2) 0.0075(14) 0.0026(14) -0.0021(12) O6 0.137(5) 0.160(5) 0.101(4) -0.034(4) -0.018(3) 0.115(4) O7 0.0232(14) 0.0313(15) 0.0327(16) -0.0018(13) -0.0002(12) -0.0004(11) O8 0.0314(16) 0.0387(17) 0.0350(16) -0.0068(15) 0.0006(13) 0.0009(13) O10 0.0285(14) 0.0278(15) 0.0371(17) -0.0008(13) -0.0053(13) -0.0070(12) O11 0.0253(15) 0.0280(15) 0.0381(17) -0.0005(13) -0.0032(13) -0.0016(12) O12 0.063(2) 0.0324(18) 0.072(2) -0.0046(19) 0.0013(19) -0.0066(15) N1 0.0322(18) 0.0216(17) 0.038(2) 0.0019(17) -0.0029(17) -0.0004(14) N2 0.049(3) 0.073(3) 0.049(3) -0.006(3) 0.017(2) -0.018(2) N3 0.0269(19) 0.0253(18) 0.035(2) 0.0002(16) 0.0028(16) 0.0008(14) N4 0.040(2) 0.028(2) 0.052(2) -0.0014(19) -0.0099(19) 0.0074(16) N5 0.0277(19) 0.0282(18) 0.037(2) 0.0010(17) 0.0007(17) -0.0018(14) N7 0.0248(18) 0.0282(18) 0.038(2) 0.0045(16) -0.0034(17) -0.0056(14) N8 0.039(2) 0.031(2) 0.044(2) 0.0054(19) 0.0026(18) -0.0068(16) C1 0.033(2) 0.021(2) 0.042(3) 0.007(2) -0.002(2) -0.0006(18) C2 0.027(2) 0.027(2) 0.039(3) 0.010(2) -0.008(2) -0.0029(18) C3 0.036(2) 0.044(3) 0.032(3) 0.003(2) 0.001(2) -0.004(2) C4 0.032(2) 0.045(3) 0.041(3) 0.004(2) -0.003(2) -0.009(2) C5 0.030(2) 0.036(2) 0.042(3) 0.006(2) 0.001(2) -0.0055(18) C6 0.041(3) 0.090(4) 0.056(3) -0.010(3) 0.003(3) -0.024(3) C7 0.060(3) 0.067(4) 0.086(4) 0.009(3) 0.015(3) -0.011(3) C8 0.048(3) 0.090(5) 0.111(5) 0.029(4) 0.017(3) 0.006(3) C9 0.050(3) 0.055(3) 0.082(4) 0.008(3) 0.018(3) -0.009(3) C10 0.048(3) 0.070(4) 0.104(5) 0.006(4) -0.018(3) -0.015(3) C11 0.023(2) 0.026(2) 0.044(3) -0.001(2) 0.005(2) -0.0008(17) C12 0.031(2) 0.026(2) 0.037(3) 0.001(2) 0.004(2) 0.0008(18) C13 0.032(2) 0.031(2) 0.047(3) 0.003(2) -0.002(2) -0.0013(19) C14 0.032(2) 0.036(3) 0.047(3) 0.000(2) 0.000(2) -0.004(2) C15 0.032(2) 0.030(2) 0.044(3) 0.007(2) 0.000(2) -0.0006(18) C16 0.042(3) 0.041(3) 0.084(4) 0.018(3) 0.002(3) 0.001(2) C17 0.055(3) 0.044(3) 0.072(4) 0.003(3) -0.025(3) 0.005(2) C18 0.049(3) 0.071(4) 0.121(6) -0.010(4) -0.026(4) 0.031(3) C19 0.133(7) 0.179(9) 0.073(5) -0.030(5) -0.002(5) 0.107(7) C20 0.093(5) 0.078(4) 0.091(5) -0.045(4) -0.050(4) 0.049(3) C21 0.030(2) 0.023(2) 0.031(2) 0.0051(19) 0.0003(19) 0.0001(17) C22 0.034(3) 0.028(2) 0.038(3) -0.004(2) 0.002(2) 0.0046(18) C23 0.035(3) 0.039(3) 0.041(3) -0.006(2) -0.005(2) 0.000(2) C24 0.036(3) 0.044(3) 0.043(3) -0.013(2) -0.010(2) -0.009(2) C25 0.033(2) 0.038(3) 0.055(3) -0.005(2) -0.006(2) -0.008(2) C26 0.051(3) 0.080(4) 0.081(4) -0.038(3) -0.015(3) 0.010(3) N6A 0.065(5) 0.083(6) 0.032(5) -0.031(5) 0.001(3) -0.014(5) C27A 0.064(6) 0.133(10) 0.100(9) -0.095(8) -0.035(6) 0.051(7) C28A 0.123(11) 0.172(9) 0.030(6) -0.065(7) -0.025(5) 0.066(9) O9A 0.215(11) 0.161(8) 0.111(7) -0.044(6) -0.080(7) 0.070(8) C29A 0.265(18) 0.146(10) 0.077(8) -0.042(7) -0.069(10) 0.107(11) C30A 0.131(8) 0.075(5) 0.076(6) -0.001(5) -0.011(5) 0.009(5) N6B 0.035(8) 0.047(7) 0.078(8) -0.006(9) -0.018(8) 0.033(6) C27B 0.101(12) 0.050(8) 0.26(3) 0.064(13) -0.070(16) -0.020(9) C28B 0.111(12) 0.116(16) 0.120(11) -0.045(12) 0.012(14) -0.030(12) O9B 0.084(10) 0.149(13) 0.121(10) -0.006(12) 0.011(8) -0.006(8) C29B 0.21(2) 0.189(19) 0.30(5) 0.09(3) -0.20(3) -0.02(3) C30B 0.131(8) 0.075(5) 0.076(6) -0.001(5) -0.011(5) 0.009(5) C31 0.027(2) 0.022(2) 0.029(2) -0.0073(19) -0.0005(19) -0.0032(16) C32 0.033(2) 0.030(2) 0.030(2) -0.001(2) 0.000(2) 0.0013(18) C33 0.034(2) 0.025(2) 0.035(2) 0.001(2) 0.003(2) -0.0018(18) C34 0.028(2) 0.030(2) 0.041(3) 0.007(2) -0.005(2) -0.0053(18) C35 0.028(2) 0.038(3) 0.048(3) 0.003(2) -0.003(2) -0.0038(19) C36 0.051(3) 0.036(3) 0.042(3) 0.005(2) -0.004(2) -0.009(2) C37 0.051(3) 0.031(2) 0.050(3) 0.002(2) 0.011(2) -0.001(2) C38 0.081(4) 0.034(3) 0.060(3) -0.001(3) 0.000(3) -0.009(3) C39 0.037(3) 0.028(2) 0.089(4) 0.009(3) 0.005(3) -0.002(2) C40 0.058(3) 0.034(3) 0.057(3) 0.004(2) 0.018(3) -0.002(2) C41 0.037(3) 0.023(2) 0.052(3) 0.005(2) 0.000(2) -0.0122(19) C42 0.037(3) 0.067(4) 0.054(3) -0.004(3) 0.003(3) 0.004(2) C43 0.040(3) 0.081(4) 0.098(5) -0.010(4) -0.014(3) 0.019(3) C44 0.052(3) 0.050(3) 0.082(4) 0.000(3) -0.027(3) 0.009(2) C45 0.055(3) 0.067(4) 0.053(3) 0.008(3) -0.010(3) 0.004(3) C46 0.046(3) 0.053(3) 0.047(3) 0.004(3) 0.000(2) -0.002(2) C47 0.029(2) 0.036(2) 0.039(3) 0.000(2) 0.011(2) -0.0038(18) C48 0.049(3) 0.035(3) 0.055(3) 0.000(3) 0.007(3) -0.008(2) C49 0.059(3) 0.039(3) 0.060(3) -0.009(3) 0.010(3) -0.009(2) C50 0.063(3) 0.040(3) 0.043(3) -0.008(2) 0.005(3) -0.016(2) C51 0.047(3) 0.054(3) 0.046(3) 0.010(3) -0.003(2) -0.009(2) C52 0.041(3) 0.037(3) 0.049(3) 0.007(2) -0.003(2) -0.005(2) C53 0.029(2) 0.035(2) 0.029(2) -0.004(2) -0.0005(19) 0.0055(18) C54 0.052(3) 0.067(4) 0.044(3) 0.003(3) 0.007(3) -0.009(3) C55 0.079(4) 0.072(4) 0.044(3) 0.020(3) 0.010(3) -0.016(3) C56 0.056(3) 0.049(4) 0.090(5) 0.032(3) 0.009(3) -0.011(3) C57 0.058(3) 0.042(3) 0.064(4) -0.002(3) 0.006(3) -0.017(2) C58 0.052(3) 0.043(3) 0.038(3) -0.001(2) 0.014(2) -0.002(2) C59 0.035(2) 0.036(3) 0.037(2) -0.009(2) -0.004(2) 0.0041(19) C60 0.044(3) 0.055(3) 0.088(4) 0.001(3) 0.017(3) 0.008(2) C61 0.034(3) 0.078(4) 0.142(6) 0.008(5) 0.022(4) 0.015(3) C62 0.045(3) 0.110(5) 0.091(5) -0.007(4) 0.022(3) 0.004(4) C63 0.047(3) 0.087(4) 0.060(4) 0.008(3) -0.003(3) -0.009(3) C64 0.034(3) 0.059(3) 0.042(3) -0.003(3) 0.004(2) -0.010(2) B1 0.042(3) 0.019(2) 0.035(3) 0.006(2) 0.001(2) 0.000(2) B2 0.032(3) 0.033(3) 0.042(3) 0.002(3) -0.003(2) 0.002(2) B3 0.035(3) 0.027(3) 0.029(3) 0.006(2) 0.002(2) 0.003(2) B4 0.028(3) 0.027(3) 0.040(3) -0.002(2) -0.003(2) -0.001(2) C65 0.236(10) 0.035(4) 0.060(4) 0.005(3) -0.001(7) -0.008(6) C66 0.116(7) 0.056(5) 0.164(9) -0.007(6) -0.085(7) 0.022(4) C67 0.093(7) 0.172(10) 0.140(9) 0.034(7) 0.024(6) -0.025(6) C68 0.127(8) 0.250(13) 0.094(6) 0.065(8) 0.010(7) 0.008(8) C69 0.084(6) 0.166(9) 0.146(9) 0.015(8) -0.036(6) -0.005(6) C70 0.103(6) 0.087(6) 0.152(9) -0.015(6) 0.074(6) -0.027(5) C71 0.040(3) 0.067(4) 0.147(7) 0.000(5) 0.008(5) 0.006(3) C72 0.026(3) 0.143(7) 0.087(4) 0.049(4) -0.003(3) -0.005(4) C73 0.071(4) 0.111(6) 0.098(5) -0.027(5) 0.017(4) -0.022(5) C74 0.38(4) 0.19(4) 0.31(2) -0.05(3) 0.19(2) -0.20(4) C75 0.23(3) 0.17(2) 0.58(5) -0.25(3) 0.31(3) -0.12(2) C76 0.086(11) 0.46(6) 0.60(6) -0.38(5) 0.02(2) -0.08(2) C77 0.133(15) 0.14(2) 0.31(2) -0.09(2) -0.045(19) -0.039(17) C78 0.107(10) 0.102(14) 0.216(18) -0.032(18) 0.038(13) 0.009(12) C79 0.17(2) 0.17(4) 0.201(19) -0.09(2) 0.009(16) -0.06(2) C80 0.112(15) 0.21(3) 0.31(2) 0.03(3) 0.056(16) 0.037(19) C81 0.110(10) 0.15(3) 0.30(2) -0.03(3) 0.116(15) -0.062(16) C82 0.154(13) 0.056(11) 0.215(14) -0.014(15) 0.067(14) -0.003(14) C83 0.26(3) 0.086(16) 0.212(15) -0.037(19) 0.116(17) 0.06(2) C84 0.25(2) 0.056(10) 0.121(12) -0.034(11) 0.078(13) -0.014(13) _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 O1 C1 1.314(5) . ? O1 B1 1.521(6) . ? O2 C2 1.333(5) . ? O2 B1 1.469(5) . ? O3 C9 1.382(6) . ? O3 C8 1.410(7) . ? O4 C11 1.314(4) . ? O4 B2 1.525(6) . ? O5 C12 1.364(5) . ? O5 B2 1.487(5) . ? O6 C18 1.383(8) . ? O6 C19 1.414(8) . ? O7 C21 1.324(4) . ? O7 B3 1.523(5) . ? O8 C22 1.350(5) . ? O8 B3 1.477(6) . ? O10 C31 1.321(4) . ? O10 B4 1.527(5) . ? O11 C32 1.329(4) . ? O11 B4 1.492(5) . ? O12 C39 1.410(6) . ? O12 C38 1.413(6) . ? N1 C1 1.344(5) . ? N1 C5 1.384(5) . ? N1 B2 1.589(6) . ? N2 C10 1.390(7) . ? N2 C6 1.445(6) . ? N2 C7 1.499(7) . ? N3 C11 1.322(5) . ? N3 C15 1.391(5) . ? N3 B3 1.583(6) . ? N4 C20 1.443(7) . ? N4 C16 1.444(6) . ? N4 C17 1.460(6) . ? N5 C21 1.342(5) . ? N5 C25 1.402(5) . ? N5 B4 1.574(6) . ? N7 C31 1.345(5) . ? N7 C35 1.371(5) . ? N7 B1 1.601(5) . ? N8 C37 1.450(6) . ? N8 C36 1.453(5) . ? N8 C40 1.461(5) . ? C1 C2 1.384(6) . ? C2 C3 1.369(6) . ? C3 C4 1.421(6) . ? C3 C6 1.504(7) . ? C4 C5 1.371(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.522(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.501(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.391(5) . ? C12 C13 1.367(5) . ? C13 C14 1.410(6) . ? C13 C16 1.510(6) . ? C14 C15 1.342(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.501(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.501(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.382(6) . ? C22 C23 1.364(6) . ? C23 C24 1.416(6) . ? C23 C26 1.502(7) . ? C24 C25 1.328(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 N6B 1.420(14) . ? C26 N6A 1.486(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N6A C30A 1.429(11) . ? N6A C27A 1.458(11) . ? C27A C28A 1.610(13) . ? C27A H27A 0.9900 . ? C27A H27B 0.9900 . ? C28A O9A 1.507(14) . ? C28A H28A 0.9900 . ? C28A H28B 0.9900 . ? O9A C29A 1.401(11) . ? C29A C30A 1.473(12) . ? C29A H29A 0.9900 . ? C29A H29B 0.9900 . ? C30A H30A 0.9900 . ? C30A H30B 0.9900 . ? N6B C27B 1.429(16) . ? N6B C30B 1.457(18) . ? C27B C28B 1.488(16) . ? C27B C30B 1.97(3) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B O9B 1.380(17) . ? C28B H28C 0.9900 . ? C28B H28D 0.9900 . ? O9B C29B 1.471(19) . ? C29B C30B 1.574(19) . ? C29B H29C 0.9900 . ? C29B H29D 0.9900 . ? C30B H30C 0.9900 . ? C30B H30D 0.9900 . ? C31 C32 1.394(5) . ? C32 C33 1.382(5) . ? C33 C34 1.410(5) . ? C33 C36 1.495(6) . ? C34 C35 1.338(6) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.509(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.509(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.397(6) . ? C41 C42 1.413(6) . ? C41 B1 1.581(6) . ? C42 C43 1.387(7) . ? C42 H42 0.9500 . ? C43 C44 1.382(8) . ? C43 H43 0.9500 . ? C44 C45 1.353(7) . ? C44 H44 0.9500 . ? C45 C46 1.369(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.379(6) . ? C47 C52 1.389(6) . ? C47 B2 1.591(6) . ? C48 C49 1.403(7) . ? C48 H48 0.9500 . ? C49 C50 1.356(7) . ? C49 H49 0.9500 . ? C50 C51 1.369(7) . ? C50 H50 0.9500 . ? C51 C52 1.390(6) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C58 1.375(6) . ? C53 C54 1.387(6) . ? C53 B3 1.579(6) . ? C54 C55 1.385(7) . ? C54 H54 0.9500 . ? C55 C56 1.370(8) . ? C55 H55 0.9500 . ? C56 C57 1.378(7) . ? C56 H56 0.9500 . ? C57 C58 1.387(6) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.363(6) . ? C59 C64 1.386(6) . ? C59 B4 1.602(6) . ? C60 C61 1.399(7) . ? C60 H60 0.9500 . ? C61 C62 1.356(8) . ? C61 H61 0.9500 . ? C62 C63 1.379(8) . ? C62 H62 0.9500 . ? C63 C64 1.369(7) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C65 H65 0.9500 . ? C66 C67 1.3900 . ? C66 H66 0.9500 . ? C67 C68 1.3900 . ? C67 H67 0.9500 . ? C68 C69 1.3900 . ? C68 H68 0.9500 . ? C69 C70 1.3900 . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C73 1.333(9) . ? C71 C72 1.358(9) . ? C71 H71 0.9500 . ? C72 C72 1.371(14) 2 ? C72 H72 0.9500 . ? C73 C73 1.325(14) 2 ? C73 H73 0.9500 . ? C74 C75 1.3900 . ? C74 C79 1.3900 . ? C74 H74 0.9500 . ? C75 C76 1.3900 . ? C75 H75 0.9500 . ? C76 C77 1.3900 . ? C76 H76 0.9500 . ? C77 C78 1.3900 . ? C77 H77 0.9500 . ? C78 C79 1.3900 . ? C78 H78 0.9500 . ? C79 H79 0.9500 . ? C80 C81 1.509(18) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.460(17) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.457(18) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C83 C84 1.516(17) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 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 C1 O1 B1 105.2(3) . . ? C2 O2 B1 107.4(3) . . ? C9 O3 C8 110.8(4) . . ? C11 O4 B2 107.0(3) . . ? C12 O5 B2 106.9(3) . . ? C18 O6 C19 110.4(5) . . ? C21 O7 B3 105.3(3) . . ? C22 O8 B3 106.8(3) . . ? C31 O10 B4 106.2(3) . . ? C32 O11 B4 107.7(3) . . ? C39 O12 C38 109.0(3) . . ? C1 N1 C5 115.7(4) . . ? C1 N1 B2 122.1(3) . . ? C5 N1 B2 122.2(3) . . ? C10 N2 C6 112.9(5) . . ? C10 N2 C7 106.1(4) . . ? C6 N2 C7 110.4(4) . . ? C11 N3 C15 115.2(3) . . ? C11 N3 B3 121.8(3) . . ? C15 N3 B3 122.9(3) . . ? C20 N4 C16 112.3(4) . . ? C20 N4 C17 108.8(4) . . ? C16 N4 C17 111.2(4) . . ? C21 N5 C25 114.4(4) . . ? C21 N5 B4 122.6(3) . . ? C25 N5 B4 123.0(3) . . ? C31 N7 C35 115.1(3) . . ? C31 N7 B1 121.9(3) . . ? C35 N7 B1 123.0(3) . . ? C37 N8 C36 112.3(3) . . ? C37 N8 C40 109.1(3) . . ? C36 N8 C40 114.4(4) . . ? O1 C1 N1 123.0(4) . . ? O1 C1 C2 112.9(4) . . ? N1 C1 C2 124.0(4) . . ? O2 C2 C3 128.3(4) . . ? O2 C2 C1 110.3(3) . . ? C3 C2 C1 121.5(4) . . ? C2 C3 C4 115.0(4) . . ? C2 C3 C6 120.1(4) . . ? C4 C3 C6 124.7(4) . . ? C5 C4 C3 121.8(4) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 N1 122.0(4) . . ? C4 C5 H5 119.0 . . ? N1 C5 H5 119.0 . . ? N2 C6 C3 112.1(4) . . ? N2 C6 H6A 109.2 . . ? C3 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C3 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 104.8(5) . . ? N2 C7 H7A 110.8 . . ? C8 C7 H7A 110.8 . . ? N2 C7 H7B 110.8 . . ? C8 C7 H7B 110.8 . . ? H7A C7 H7B 108.9 . . ? O3 C8 C7 110.8(5) . . ? O3 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O3 C9 C10 110.1(5) . . ? O3 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? O3 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? N2 C10 C9 111.4(5) . . ? N2 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? N2 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? O4 C11 N3 123.8(4) . . ? O4 C11 C12 112.2(3) . . ? N3 C11 C12 124.0(3) . . ? O5 C12 C13 128.0(4) . . ? O5 C12 C11 110.4(3) . . ? C13 C12 C11 121.5(4) . . ? C12 C13 C14 114.3(4) . . ? C12 C13 C16 123.6(4) . . ? C14 C13 C16 122.1(4) . . ? C15 C14 C13 122.4(4) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 N3 122.5(4) . . ? C14 C15 H15 118.7 . . ? N3 C15 H15 118.7 . . ? N4 C16 C13 111.4(4) . . ? N4 C16 H16A 109.3 . . ? C13 C16 H16A 109.3 . . ? N4 C16 H16B 109.3 . . ? C13 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? N4 C17 C18 108.7(4) . . ? N4 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? N4 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.3 . . ? O6 C18 C17 113.1(5) . . ? O6 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? O6 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? O6 C19 C20 108.8(7) . . ? O6 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O6 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? N4 C20 C19 109.8(5) . . ? N4 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? N4 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? O7 C21 N5 122.5(4) . . ? O7 C21 C22 112.8(4) . . ? N5 C21 C22 124.7(4) . . ? O8 C22 C23 128.4(4) . . ? O8 C22 C21 110.6(4) . . ? C23 C22 C21 121.0(4) . . ? C22 C23 C24 114.5(4) . . ? C22 C23 C26 123.1(4) . . ? C24 C23 C26 122.3(4) . . ? C25 C24 C23 123.1(4) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C24 C25 N5 122.2(4) . . ? C24 C25 H25 118.9 . . ? N5 C25 H25 118.9 . . ? N6B C26 N6A 22.4(8) . . ? N6B C26 C23 112.9(10) . . ? N6A C26 C23 111.3(6) . . ? N6B C26 H26A 88.5 . . ? N6A C26 H26A 109.4 . . ? C23 C26 H26A 109.4 . . ? N6B C26 H26B 125.7 . . ? N6A C26 H26B 109.4 . . ? C23 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C30A N6A C27A 113.9(10) . . ? C30A N6A C26 108.1(8) . . ? C27A N6A C26 108.7(9) . . ? N6A C27A C28A 105.7(8) . . ? N6A C27A H27A 110.6 . . ? C28A C27A H27A 110.6 . . ? N6A C27A H27B 110.6 . . ? C28A C27A H27B 110.6 . . ? H27A C27A H27B 108.7 . . ? O9A C28A C27A 105.0(11) . . ? O9A C28A H28A 110.7 . . ? C27A C28A H28A 110.7 . . ? O9A C28A H28B 110.7 . . ? C27A C28A H28B 110.7 . . ? H28A C28A H28B 108.8 . . ? C29A O9A C28A 112.2(11) . . ? O9A C29A C30A 111.6(9) . . ? O9A C29A H29A 109.3 . . ? C30A C29A H29A 109.3 . . ? O9A C29A H29B 109.3 . . ? C30A C29A H29B 109.3 . . ? H29A C29A H29B 108.0 . . ? N6A C30A C29A 108.5(11) . . ? N6A C30A H30A 110.0 . . ? C29A C30A H30A 110.0 . . ? N6A C30A H30B 110.0 . . ? C29A C30A H30B 110.0 . . ? H30A C30A H30B 108.4 . . ? C26 N6B C27B 101.5(11) . . ? C26 N6B C30B 122(2) . . ? C27B N6B C30B 86.1(19) . . ? N6B C27B C28B 109.8(16) . . ? N6B C27B C30B 47.5(11) . . ? C28B C27B C30B 95.6(16) . . ? N6B C27B H27C 109.7 . . ? C28B C27B H27C 109.7 . . ? C30B C27B H27C 73.0 . . ? N6B C27B H27D 109.7 . . ? C28B C27B H27D 109.7 . . ? C30B C27B H27D 151.8 . . ? H27C C27B H27D 108.2 . . ? O9B C28B C27B 93.0(18) . . ? O9B C28B H28C 113.1 . . ? C27B C28B H28C 113.1 . . ? O9B C28B H28D 113.1 . . ? C27B C28B H28D 113.1 . . ? H28C C28B H28D 110.5 . . ? C28B O9B C29B 107(3) . . ? O9B C29B C30B 88.8(19) . . ? O9B C29B H29C 113.8 . . ? C30B C29B H29C 113.8 . . ? O9B C29B H29D 113.8 . . ? C30B C29B H29D 113.8 . . ? H29C C29B H29D 111.1 . . ? N6B C30B C29B 110(2) . . ? N6B C30B C27B 46.4(11) . . ? C29B C30B C27B 96.2(19) . . ? N6B C30B H30C 109.6 . . ? C29B C30B H30C 109.6 . . ? C27B C30B H30C 150.9 . . ? N6B C30B H30D 109.6 . . ? C29B C30B H30D 109.6 . . ? C27B C30B H30D 73.9 . . ? H30C C30B H30D 108.1 . . ? O10 C31 N7 124.0(3) . . ? O10 C31 C32 112.1(3) . . ? N7 C31 C32 123.9(3) . . ? O11 C32 C33 128.6(4) . . ? O11 C32 C31 110.8(3) . . ? C33 C32 C31 120.5(4) . . ? C32 C33 C34 114.8(4) . . ? C32 C33 C36 121.7(4) . . ? C34 C33 C36 123.4(3) . . ? C35 C34 C33 122.1(4) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C34 C35 N7 123.6(4) . . ? C34 C35 H35 118.2 . . ? N7 C35 H35 118.2 . . ? N8 C36 C33 110.7(4) . . ? N8 C36 H36A 109.5 . . ? C33 C36 H36A 109.5 . . ? N8 C36 H36B 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? N8 C37 C38 109.2(4) . . ? N8 C37 H37A 109.8 . . ? C38 C37 H37A 109.8 . . ? N8 C37 H37B 109.8 . . ? C38 C37 H37B 109.8 . . ? H37A C37 H37B 108.3 . . ? O12 C38 C37 111.3(4) . . ? O12 C38 H38A 109.4 . . ? C37 C38 H38A 109.4 . . ? O12 C38 H38B 109.4 . . ? C37 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? O12 C39 C40 111.4(4) . . ? O12 C39 H39A 109.3 . . ? C40 C39 H39A 109.3 . . ? O12 C39 H39B 109.3 . . ? C40 C39 H39B 109.3 . . ? H39A C39 H39B 108.0 . . ? N8 C40 C39 108.0(4) . . ? N8 C40 H40A 110.1 . . ? C39 C40 H40A 110.1 . . ? N8 C40 H40B 110.1 . . ? C39 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? C46 C41 C42 115.9(4) . . ? C46 C41 B1 122.2(4) . . ? C42 C41 B1 121.9(4) . . ? C43 C42 C41 121.0(5) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C44 C43 C42 120.2(6) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 119.8(5) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 120.7(5) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C45 C46 C41 122.5(5) . . ? C45 C46 H46 118.8 . . ? C41 C46 H46 118.8 . . ? C48 C47 C52 117.2(4) . . ? C48 C47 B2 120.6(4) . . ? C52 C47 B2 122.2(4) . . ? C47 C48 C49 121.1(5) . . ? C47 C48 H48 119.4 . . ? C49 C48 H48 119.4 . . ? C50 C49 C48 120.7(5) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C49 C50 C51 119.0(5) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C50 C51 C52 120.9(5) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C47 C52 C51 121.0(4) . . ? C47 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C58 C53 C54 116.3(4) . . ? C58 C53 B3 123.8(4) . . ? C54 C53 B3 119.9(4) . . ? C55 C54 C53 122.1(5) . . ? C55 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? C56 C55 C54 120.2(5) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C57 119.1(5) . . ? C55 C56 H56 120.4 . . ? C57 C56 H56 120.4 . . ? C56 C57 C58 119.7(5) . . ? C56 C57 H57 120.1 . . ? C58 C57 H57 120.1 . . ? C53 C58 C57 122.6(4) . . ? C53 C58 H58 118.7 . . ? C57 C58 H58 118.7 . . ? C60 C59 C64 117.7(4) . . ? C60 C59 B4 120.5(4) . . ? C64 C59 B4 121.8(4) . . ? C59 C60 C61 121.0(5) . . ? C59 C60 H60 119.5 . . ? C61 C60 H60 119.5 . . ? C62 C61 C60 120.3(5) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C61 C62 C63 119.5(5) . . ? C61 C62 H62 120.3 . . ? C63 C62 H62 120.3 . . ? C64 C63 C62 119.8(5) . . ? C64 C63 H63 120.1 . . ? C62 C63 H63 120.1 . . ? C63 C64 C59 121.8(5) . . ? C63 C64 H64 119.1 . . ? C59 C64 H64 119.1 . . ? O2 B1 O1 104.2(3) . . ? O2 B1 C41 113.4(4) . . ? O1 B1 C41 111.8(4) . . ? O2 B1 N7 108.8(3) . . ? O1 B1 N7 105.8(3) . . ? C41 B1 N7 112.3(3) . . ? O5 B2 O4 103.5(3) . . ? O5 B2 N1 108.8(4) . . ? O4 B2 N1 105.7(3) . . ? O5 B2 C47 113.5(4) . . ? O4 B2 C47 112.2(4) . . ? N1 B2 C47 112.4(3) . . ? O8 B3 O7 104.3(3) . . ? O8 B3 C53 113.5(3) . . ? O7 B3 C53 112.2(3) . . ? O8 B3 N3 109.1(3) . . ? O7 B3 N3 105.5(3) . . ? C53 B3 N3 111.6(3) . . ? O11 B4 O10 103.1(3) . . ? O11 B4 N5 108.6(3) . . ? O10 B4 N5 106.8(3) . . ? O11 B4 C59 112.9(3) . . ? O10 B4 C59 112.1(3) . . ? N5 B4 C59 112.7(3) . . ? C66 C65 C70 120.0 . . ? C66 C65 H65 120.0 . . ? C70 C65 H65 120.0 . . ? C67 C66 C65 120.0 . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 C68 120.0 . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C69 C68 C67 120.0 . . ? C69 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C68 C69 C70 120.0 . . ? C68 C69 H69 120.0 . . ? C70 C69 H69 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 H70 120.0 . . ? C65 C70 H70 120.0 . . ? C73 C71 C72 117.9(6) . . ? C73 C71 H71 121.1 . . ? C72 C71 H71 121.1 . . ? C71 C72 C72 120.2(4) . 2 ? C71 C72 H72 119.9 . . ? C72 C72 H72 119.9 2 . ? C73 C73 C71 121.9(4) 2 . ? C73 C73 H73 119.0 2 . ? C71 C73 H73 119.0 . . ? C75 C74 C79 120.0 . . ? C75 C74 H74 120.0 . . ? C79 C74 H74 120.0 . . ? C76 C75 C74 120.0 . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C75 C76 C77 120.0 . . ? C75 C76 H76 120.0 . . ? C77 C76 H76 120.0 . . ? C78 C77 C76 120.0 . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C77 C78 C79 120.0 . . ? C77 C78 H78 120.0 . . ? C79 C78 H78 120.0 . . ? C78 C79 C74 120.0 . . ? C78 C79 H79 120.0 . . ? C74 C79 H79 120.0 . . ? C81 C80 H80A 109.5 . . ? C81 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C81 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C82 C81 C80 106.7(19) . . ? C82 C81 H81A 110.4 . . ? C80 C81 H81A 110.4 . . ? C82 C81 H81B 110.4 . . ? C80 C81 H81B 110.4 . . ? H81A C81 H81B 108.6 . . ? C83 C82 C81 108(2) . . ? C83 C82 H82A 110.2 . . ? C81 C82 H82A 110.2 . . ? C83 C82 H82B 110.2 . . ? C81 C82 H82B 110.2 . . ? H82A C82 H82B 108.5 . . ? C82 C83 C84 109.7(17) . . ? C82 C83 H83A 109.7 . . ? C84 C83 H83A 109.7 . . ? C82 C83 H83B 109.7 . . ? C84 C83 H83B 109.7 . . ? H83A C83 H83B 108.2 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 O1 C1 N1 -178.3(4) . . . . ? B1 O1 C1 C2 -1.1(4) . . . . ? C5 N1 C1 O1 178.3(4) . . . . ? B2 N1 C1 O1 -1.0(6) . . . . ? C5 N1 C1 C2 1.5(5) . . . . ? B2 N1 C1 C2 -177.8(4) . . . . ? B1 O2 C2 C3 178.7(4) . . . . ? B1 O2 C2 C1 -0.5(4) . . . . ? O1 C1 C2 O2 1.1(5) . . . . ? N1 C1 C2 O2 178.2(3) . . . . ? O1 C1 C2 C3 -178.2(4) . . . . ? N1 C1 C2 C3 -1.0(6) . . . . ? O2 C2 C3 C4 -178.9(4) . . . . ? C1 C2 C3 C4 0.2(6) . . . . ? O2 C2 C3 C6 -3.6(7) . . . . ? C1 C2 C3 C6 175.6(4) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C6 C3 C4 C5 -175.1(5) . . . . ? C3 C4 C5 N1 0.5(6) . . . . ? C1 N1 C5 C4 -1.2(6) . . . . ? B2 N1 C5 C4 178.1(4) . . . . ? C10 N2 C6 C3 -84.9(6) . . . . ? C7 N2 C6 C3 156.5(5) . . . . ? C2 C3 C6 N2 -177.2(4) . . . . ? C4 C3 C6 N2 -2.3(7) . . . . ? C10 N2 C7 C8 63.7(6) . . . . ? C6 N2 C7 C8 -173.6(5) . . . . ? C9 O3 C8 C7 59.8(7) . . . . ? N2 C7 C8 O3 -62.4(6) . . . . ? C8 O3 C9 C10 -55.5(6) . . . . ? C6 N2 C10 C9 174.8(5) . . . . ? C7 N2 C10 C9 -64.1(6) . . . . ? O3 C9 C10 N2 60.2(7) . . . . ? B2 O4 C11 N3 178.8(4) . . . . ? B2 O4 C11 C12 -2.6(5) . . . . ? C15 N3 C11 O4 178.8(4) . . . . ? B3 N3 C11 O4 -2.9(6) . . . . ? C15 N3 C11 C12 0.4(6) . . . . ? B3 N3 C11 C12 178.6(4) . . . . ? B2 O5 C12 C13 179.7(4) . . . . ? B2 O5 C12 C11 -1.0(5) . . . . ? O4 C11 C12 O5 2.4(5) . . . . ? N3 C11 C12 O5 -179.0(4) . . . . ? O4 C11 C12 C13 -178.3(4) . . . . ? N3 C11 C12 C13 0.3(7) . . . . ? O5 C12 C13 C14 178.3(4) . . . . ? C11 C12 C13 C14 -1.0(6) . . . . ? O5 C12 C13 C16 -0.3(7) . . . . ? C11 C12 C13 C16 -179.6(4) . . . . ? C12 C13 C14 C15 0.9(7) . . . . ? C16 C13 C14 C15 179.6(5) . . . . ? C13 C14 C15 N3 -0.3(7) . . . . ? C11 N3 C15 C14 -0.4(6) . . . . ? B3 N3 C15 C14 -178.6(4) . . . . ? C20 N4 C16 C13 68.4(5) . . . . ? C17 N4 C16 C13 -169.4(4) . . . . ? C12 C13 C16 N4 -148.6(4) . . . . ? C14 C13 C16 N4 32.9(6) . . . . ? C20 N4 C17 C18 -56.1(6) . . . . ? C16 N4 C17 C18 179.7(4) . . . . ? C19 O6 C18 C17 -58.6(9) . . . . ? N4 C17 C18 O6 56.3(6) . . . . ? C18 O6 C19 C20 59.7(9) . . . . ? C16 N4 C20 C19 -176.0(5) . . . . ? C17 N4 C20 C19 60.4(6) . . . . ? O6 C19 C20 N4 -61.8(8) . . . . ? B3 O7 C21 N5 179.1(4) . . . . ? B3 O7 C21 C22 -1.3(4) . . . . ? C25 N5 C21 O7 -178.5(3) . . . . ? B4 N5 C21 O7 -0.5(5) . . . . ? C25 N5 C21 C22 1.9(5) . . . . ? B4 N5 C21 C22 180.0(4) . . . . ? B3 O8 C22 C23 -174.7(4) . . . . ? B3 O8 C22 C21 2.7(4) . . . . ? O7 C21 C22 O8 -0.9(5) . . . . ? N5 C21 C22 O8 178.7(4) . . . . ? O7 C21 C22 C23 176.8(4) . . . . ? N5 C21 C22 C23 -3.7(6) . . . . ? O8 C22 C23 C24 179.8(4) . . . . ? C21 C22 C23 C24 2.6(6) . . . . ? O8 C22 C23 C26 -2.8(7) . . . . ? C21 C22 C23 C26 -180.0(4) . . . . ? C22 C23 C24 C25 -0.2(7) . . . . ? C26 C23 C24 C25 -177.7(5) . . . . ? C23 C24 C25 N5 -1.4(7) . . . . ? C21 N5 C25 C24 0.6(6) . . . . ? B4 N5 C25 C24 -177.5(4) . . . . ? C22 C23 C26 N6B 167.4(8) . . . . ? C24 C23 C26 N6B -15.3(10) . . . . ? C22 C23 C26 N6A 143.3(6) . . . . ? C24 C23 C26 N6A -39.5(8) . . . . ? N6B C26 N6A C30A -171(4) . . . . ? C23 C26 N6A C30A -72.5(10) . . . . ? N6B C26 N6A C27A 65(3) . . . . ? C23 C26 N6A C27A 163.5(9) . . . . ? C30A N6A C27A C28A 62.0(14) . . . . ? C26 N6A C27A C28A -177.5(10) . . . . ? N6A C27A C28A O9A -57.5(13) . . . . ? C27A C28A O9A C29A 60.1(12) . . . . ? C28A O9A C29A C30A -61.5(16) . . . . ? C27A N6A C30A C29A -61.2(13) . . . . ? C26 N6A C30A C29A 177.9(9) . . . . ? O9A C29A C30A N6A 58.1(16) . . . . ? N6A C26 N6B C27B -151(4) . . . . ? C23 C26 N6B C27B 118.4(17) . . . . ? N6A C26 N6B C30B -58(3) . . . . ? C23 C26 N6B C30B -149.0(16) . . . . ? C26 N6B C27B C28B -159(2) . . . . ? C30B N6B C27B C28B 79(2) . . . . ? C26 N6B C27B C30B 122(2) . . . . ? N6B C27B C28B O9B -84(3) . . . . ? C30B C27B C28B O9B -37.7(19) . . . . ? C27B C28B O9B C29B 80(2) . . . . ? C28B O9B C29B C30B -77(3) . . . . ? C26 N6B C30B C29B 180.0(16) . . . . ? C27B N6B C30B C29B -79(2) . . . . ? C26 N6B C30B C27B -101.1(17) . . . . ? O9B C29B C30B N6B 80(3) . . . . ? O9B C29B C30B C27B 35(3) . . . . ? C28B C27B C30B N6B -112(2) . . . . ? N6B C27B C30B C29B 112(2) . . . . ? C28B C27B C30B C29B 0(3) . . . . ? B4 O10 C31 N7 177.2(4) . . . . ? B4 O10 C31 C32 -2.3(4) . . . . ? C35 N7 C31 O10 179.8(4) . . . . ? B1 N7 C31 O10 -1.5(6) . . . . ? C35 N7 C31 C32 -0.6(6) . . . . ? B1 N7 C31 C32 178.0(4) . . . . ? B4 O11 C32 C33 -177.2(4) . . . . ? B4 O11 C32 C31 1.3(4) . . . . ? O10 C31 C32 O11 0.7(5) . . . . ? N7 C31 C32 O11 -178.9(3) . . . . ? O10 C31 C32 C33 179.4(4) . . . . ? N7 C31 C32 C33 -0.2(6) . . . . ? O11 C32 C33 C34 179.2(4) . . . . ? C31 C32 C33 C34 0.7(6) . . . . ? O11 C32 C33 C36 2.1(7) . . . . ? C31 C32 C33 C36 -176.3(4) . . . . ? C32 C33 C34 C35 -0.5(6) . . . . ? C36 C33 C34 C35 176.5(4) . . . . ? C33 C34 C35 N7 -0.3(7) . . . . ? C31 N7 C35 C34 0.9(6) . . . . ? B1 N7 C35 C34 -177.7(4) . . . . ? C37 N8 C36 C33 80.3(4) . . . . ? C40 N8 C36 C33 -154.6(4) . . . . ? C32 C33 C36 N8 -161.2(4) . . . . ? C34 C33 C36 N8 22.0(6) . . . . ? C36 N8 C37 C38 -173.4(4) . . . . ? C40 N8 C37 C38 58.6(5) . . . . ? C39 O12 C38 C37 59.1(5) . . . . ? N8 C37 C38 O12 -59.0(5) . . . . ? C38 O12 C39 C40 -60.5(5) . . . . ? C37 N8 C40 C39 -59.1(5) . . . . ? C36 N8 C40 C39 174.1(4) . . . . ? O12 C39 C40 N8 60.8(5) . . . . ? C46 C41 C42 C43 -1.5(7) . . . . ? B1 C41 C42 C43 176.9(5) . . . . ? C41 C42 C43 C44 -0.1(9) . . . . ? C42 C43 C44 C45 0.8(9) . . . . ? C43 C44 C45 C46 0.3(9) . . . . ? C44 C45 C46 C41 -2.1(8) . . . . ? C42 C41 C46 C45 2.6(7) . . . . ? B1 C41 C46 C45 -175.8(4) . . . . ? C52 C47 C48 C49 -0.4(6) . . . . ? B2 C47 C48 C49 179.6(4) . . . . ? C47 C48 C49 C50 -0.7(7) . . . . ? C48 C49 C50 C51 0.7(7) . . . . ? C49 C50 C51 C52 0.3(7) . . . . ? C48 C47 C52 C51 1.4(6) . . . . ? B2 C47 C52 C51 -178.6(4) . . . . ? C50 C51 C52 C47 -1.4(7) . . . . ? C58 C53 C54 C55 -0.1(7) . . . . ? B3 C53 C54 C55 -177.1(5) . . . . ? C53 C54 C55 C56 -1.1(8) . . . . ? C54 C55 C56 C57 1.7(8) . . . . ? C55 C56 C57 C58 -1.1(8) . . . . ? C54 C53 C58 C57 0.7(7) . . . . ? B3 C53 C58 C57 177.6(4) . . . . ? C56 C57 C58 C53 -0.1(8) . . . . ? C64 C59 C60 C61 1.6(8) . . . . ? B4 C59 C60 C61 179.7(5) . . . . ? C59 C60 C61 C62 -0.5(10) . . . . ? C60 C61 C62 C63 -0.3(10) . . . . ? C61 C62 C63 C64 -0.1(9) . . . . ? C62 C63 C64 C59 1.3(8) . . . . ? C60 C59 C64 C63 -2.0(7) . . . . ? B4 C59 C64 C63 179.9(4) . . . . ? C2 O2 B1 O1 -0.2(4) . . . . ? C2 O2 B1 C41 121.6(4) . . . . ? C2 O2 B1 N7 -112.6(3) . . . . ? C1 O1 B1 O2 0.8(4) . . . . ? C1 O1 B1 C41 -122.1(4) . . . . ? C1 O1 B1 N7 115.4(3) . . . . ? C46 C41 B1 O2 30.8(6) . . . . ? C42 C41 B1 O2 -147.5(4) . . . . ? C46 C41 B1 O1 148.2(4) . . . . ? C42 C41 B1 O1 -30.1(5) . . . . ? C46 C41 B1 N7 -93.0(5) . . . . ? C42 C41 B1 N7 88.6(5) . . . . ? C31 N7 B1 O2 53.3(5) . . . . ? C35 N7 B1 O2 -128.2(4) . . . . ? C31 N7 B1 O1 -58.1(5) . . . . ? C35 N7 B1 O1 120.4(4) . . . . ? C31 N7 B1 C41 179.7(4) . . . . ? C35 N7 B1 C41 -1.8(6) . . . . ? C12 O5 B2 O4 -0.5(4) . . . . ? C12 O5 B2 N1 111.6(4) . . . . ? C12 O5 B2 C47 -122.4(4) . . . . ? C11 O4 B2 O5 1.8(4) . . . . ? C11 O4 B2 N1 -112.5(3) . . . . ? C11 O4 B2 C47 124.6(4) . . . . ? C1 N1 B2 O5 -54.0(5) . . . . ? C5 N1 B2 O5 126.7(4) . . . . ? C1 N1 B2 O4 56.6(4) . . . . ? C5 N1 B2 O4 -122.7(4) . . . . ? C1 N1 B2 C47 179.3(3) . . . . ? C5 N1 B2 C47 0.1(5) . . . . ? C48 C47 B2 O5 -22.6(6) . . . . ? C52 C47 B2 O5 157.4(4) . . . . ? C48 C47 B2 O4 -139.5(4) . . . . ? C52 C47 B2 O4 40.5(5) . . . . ? C48 C47 B2 N1 101.4(4) . . . . ? C52 C47 B2 N1 -78.6(5) . . . . ? C22 O8 B3 O7 -3.3(4) . . . . ? C22 O8 B3 C53 119.1(4) . . . . ? C22 O8 B3 N3 -115.8(4) . . . . ? C21 O7 B3 O8 2.8(4) . . . . ? C21 O7 B3 C53 -120.5(3) . . . . ? C21 O7 B3 N3 117.8(3) . . . . ? C58 C53 B3 O8 -154.3(4) . . . . ? C54 C53 B3 O8 22.5(6) . . . . ? C58 C53 B3 O7 -36.3(5) . . . . ? C54 C53 B3 O7 140.5(4) . . . . ? C58 C53 B3 N3 82.0(5) . . . . ? C54 C53 B3 N3 -101.2(5) . . . . ? C11 N3 B3 O8 55.8(5) . . . . ? C15 N3 B3 O8 -126.0(4) . . . . ? C11 N3 B3 O7 -55.8(5) . . . . ? C15 N3 B3 O7 122.3(4) . . . . ? C11 N3 B3 C53 -178.0(4) . . . . ? C15 N3 B3 C53 0.2(5) . . . . ? C32 O11 B4 O10 -2.5(4) . . . . ? C32 O11 B4 N5 110.4(3) . . . . ? C32 O11 B4 C59 -123.7(4) . . . . ? C31 O10 B4 O11 2.9(4) . . . . ? C31 O10 B4 N5 -111.4(3) . . . . ? C31 O10 B4 C59 124.7(3) . . . . ? C21 N5 B4 O11 -55.8(5) . . . . ? C25 N5 B4 O11 122.1(4) . . . . ? C21 N5 B4 O10 54.7(4) . . . . ? C25 N5 B4 O10 -127.4(4) . . . . ? C21 N5 B4 C59 178.3(3) . . . . ? C25 N5 B4 C59 -3.8(5) . . . . ? C60 C59 B4 O11 -28.4(6) . . . . ? C64 C59 B4 O11 149.6(4) . . . . ? C60 C59 B4 O10 -144.3(4) . . . . ? C64 C59 B4 O10 33.7(5) . . . . ? C60 C59 B4 N5 95.2(5) . . . . ? C64 C59 B4 N5 -86.8(5) . . . . ? C70 C65 C66 C67 0.0 . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C70 0.0 . . . . ? C68 C69 C70 C65 0.0 . . . . ? C66 C65 C70 C69 0.0 . . . . ? C73 C71 C72 C72 0.4(11) . . . 2 ? C72 C71 C73 C73 -1.6(12) . . . 2 ? C79 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C77 0.0 . . . . ? C75 C76 C77 C78 0.0 . . . . ? C76 C77 C78 C79 0.0 . . . . ? C77 C78 C79 C74 0.0 . . . . ? C75 C74 C79 C78 0.0 . . . . ? C80 C81 C82 C83 -171(3) . . . . ? C81 C82 C83 C84 -169.1(19) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.442 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.046 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 233237' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H20 B4 F12 N4 O8, 2(C6 H6)' _chemical_formula_sum 'C56 H32 B4 F12 N4 O8' _chemical_formula_weight 1160.10 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.538(4) _cell_length_b 13.595(10) _cell_length_c 13.813(12) _cell_angle_alpha 80.64(7) _cell_angle_beta 85.41(4) _cell_angle_gamma 80.58(4) _cell_volume 2471(3) _cell_formula_units_Z 2 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 636 _cell_measurement_theta_min 1.4998 _cell_measurement_theta_max 12.65335 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8806 _exptl_absorpt_correction_T_max 1.2427 _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch mar345 IPDS' _diffrn_measurement_method '60 images with deltaphi = 3 deg. and exp. time = 180 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16104 _diffrn_reflns_av_R_equivalents 0.1172 _diffrn_reflns_av_sigmaI/netI 0.1989 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8192 _reflns_number_gt 2338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'marresearch mar345' _computing_cell_refinement 'Oxford Diffraction CrysAlis RED' _computing_data_reduction 'Oxford Diffraction CrysAlis RED' _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^)+(0.0961P)^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 SHELXL _refine_ls_extinction_coef 0.0003(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8192 _refine_ls_number_parameters 798 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.2037 _refine_ls_R_factor_gt 0.0774 _refine_ls_wR_factor_ref 0.2432 _refine_ls_wR_factor_gt 0.1810 _refine_ls_goodness_of_fit_ref 0.814 _refine_ls_restrained_S_all 0.817 _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 F1 F -0.0636(3) 0.4581(3) 0.3320(3) 0.0837(14) Uani 1 1 d . . . F2A F -0.0770(4) 0.6188(4) 0.4210(5) 0.085(2) Uani 0.759(10) 1 d PD A 1 F2B F 0.2782(11) 0.5984(15) 0.3847(15) 0.102(9) Uani 0.241(10) 1 d PD A 2 F3 F 0.2859(3) 0.4398(3) 0.2992(3) 0.0790(13) Uani 1 1 d . . . F4 F 0.2521(3) 0.2564(4) -0.1444(4) 0.0831(13) Uani 1 1 d . . . F5A F 0.2796(6) 0.2465(7) -0.3364(7) 0.109(4) Uani 0.614(12) 1 d PD B 1 F5B F 0.2940(10) 0.5911(12) -0.4039(10) 0.134(8) Uani 0.386(12) 1 d PD B 2 F6 F 0.2704(3) 0.6030(4) -0.2127(3) 0.0812(13) Uani 1 1 d . . . F7 F 0.7043(3) 0.2539(4) 0.0517(4) 0.0883(14) Uani 1 1 d . . . F8A F 0.6520(4) 0.0255(5) 0.3979(4) 0.083(3) Uani 0.735(11) 1 d PD C 1 F8B F 0.8672(10) 0.1630(18) 0.1636(17) 0.136(10) Uani 0.265(11) 1 d PD C 2 F9 F 0.4922(3) 0.1183(4) 0.3062(3) 0.0994(16) Uani 1 1 d . . . F10 F 0.2971(3) -0.1519(3) 0.1566(3) 0.0734(12) Uani 1 1 d . . . F11A F 0.1723(5) -0.2816(5) 0.1611(6) 0.075(3) Uani 0.530(10) 1 d PD D 1 F11B F -0.0958(5) -0.0169(7) 0.1070(8) 0.086(4) Uani 0.470(10) 1 d PD D 2 F12 F 0.0296(3) 0.1155(3) 0.1084(4) 0.0872(14) Uani 1 1 d . . . O1 O 0.1837(3) 0.3766(3) 0.1518(3) 0.0576(12) Uani 1 1 d . . . O2 O 0.0312(3) 0.3260(3) 0.2195(4) 0.0602(12) Uani 1 1 d . . . O3 O 0.3318(3) 0.3482(3) -0.0036(3) 0.0556(12) Uani 1 1 d . . . O4 O 0.2664(3) 0.5196(3) -0.0161(3) 0.0558(12) Uani 1 1 d . . . O5 O 0.4086(3) 0.1772(3) 0.1358(3) 0.0534(12) Uani 1 1 d . . . O6 O 0.5248(3) 0.2147(3) 0.0022(3) 0.0579(12) Uani 1 1 d . . . O7 O 0.1987(3) 0.1643(3) 0.1700(4) 0.0581(12) Uani 1 1 d . . . O8 O 0.3023(3) 0.0179(3) 0.2401(3) 0.0595(12) Uani 1 1 d . . . N1 N 0.1447(3) 0.3989(4) -0.0144(4) 0.0530(14) Uani 1 1 d . . . N2 N 0.4569(3) 0.3482(4) 0.1045(4) 0.0497(14) Uani 1 1 d . . . N3 N 0.3246(4) 0.0754(4) 0.0590(4) 0.0536(14) Uani 1 1 d . . . N4 N 0.1868(4) 0.2501(4) 0.3038(4) 0.0579(15) Uani 1 1 d . . . C1 C 0.1230(4) 0.3737(5) 0.0820(6) 0.0537(18) Uani 1 1 d . . . C2 C 0.0310(5) 0.3472(5) 0.1211(6) 0.0604(19) Uani 1 1 d . . . C3 C -0.0422(5) 0.3499(5) 0.0586(6) 0.062(2) Uani 1 1 d . . . H3 H -0.1059 0.3326 0.0823 0.074 Uiso 1 1 calc R . . C4 C -0.0208(5) 0.3793(5) -0.0426(6) 0.0624(19) Uani 1 1 d . . . H4 H -0.0712 0.3833 -0.0877 0.075 Uiso 1 1 calc R . . C5 C 0.0696(4) 0.4015(5) -0.0759(5) 0.0540(18) Uani 1 1 d . . . H5 H 0.0822 0.4198 -0.1446 0.065 Uiso 1 1 calc R . . C6 C 0.3800(4) 0.3940(5) 0.0509(5) 0.0497(17) Uani 1 1 d . . . C7 C 0.3432(5) 0.4959(6) 0.0439(5) 0.0558(18) Uani 1 1 d . . . C8 C 0.3857(5) 0.5563(6) 0.0933(5) 0.064(2) Uani 1 1 d . . . H8 H 0.3617 0.6264 0.0898 0.076 Uiso 1 1 calc R . . C9 C 0.4668(5) 0.5085(6) 0.1494(5) 0.0609(19) Uani 1 1 d . . . H9 H 0.4998 0.5475 0.1839 0.073 Uiso 1 1 calc R . . C10 C 0.4993(5) 0.4085(5) 0.1556(5) 0.0542(17) Uani 1 1 d . . . H10 H 0.5529 0.3787 0.1964 0.065 Uiso 1 1 calc R . . C11 C 0.3948(5) 0.1326(5) 0.0592(5) 0.0541(18) Uani 1 1 d . . . C12 C 0.4633(4) 0.1542(5) -0.0208(5) 0.0564(18) Uani 1 1 d . . . C13 C 0.4607(5) 0.1131(5) -0.1011(6) 0.0614(19) Uani 1 1 d . . . H13 H 0.5080 0.1239 -0.1550 0.074 Uiso 1 1 calc R . . C14 C 0.3849(5) 0.0522(5) -0.1042(5) 0.0608(19) Uani 1 1 d . . . H14 H 0.3797 0.0230 -0.1612 0.073 Uiso 1 1 calc R . . C15 C 0.3213(5) 0.0367(5) -0.0259(5) 0.0611(19) Uani 1 1 d . . . H15 H 0.2709 -0.0035 -0.0296 0.073 Uiso 1 1 calc R . . C16 C 0.2191(5) 0.1717(5) 0.2585(6) 0.0556(18) Uani 1 1 d . . . C17 C 0.2783(5) 0.0836(6) 0.3042(6) 0.0597(19) Uani 1 1 d . . . C18 C 0.2989(5) 0.0747(6) 0.4004(6) 0.063(2) Uani 1 1 d . . . H18 H 0.3362 0.0150 0.4332 0.076 Uiso 1 1 calc R . . C19 C 0.2626(5) 0.1577(6) 0.4491(5) 0.066(2) Uani 1 1 d . . . H19 H 0.2759 0.1544 0.5162 0.079 Uiso 1 1 calc R . . C20 C 0.2092(5) 0.2418(6) 0.4016(5) 0.0630(19) Uani 1 1 d . . . H20 H 0.1862 0.2970 0.4360 0.076 Uiso 1 1 calc R . . C21 C 0.1120(5) 0.4417(5) 0.3095(5) 0.0570(18) Uani 1 1 d . . . C22 C 0.0223(5) 0.4920(6) 0.3425(6) 0.066(2) Uani 1 1 d . A . C23 C 0.0152(5) 0.5758(6) 0.3888(6) 0.073(2) Uani 1 1 d D . . C24 C 0.0980(7) 0.6152(6) 0.4034(6) 0.081(2) Uani 1 1 d . A . H24 H 0.0920 0.6733 0.4347 0.098 Uiso 1 1 calc R . . C25 C 0.1902(7) 0.5694(7) 0.3721(6) 0.081(2) Uani 1 1 d D . . C26 C 0.1929(5) 0.4868(6) 0.3256(6) 0.068(2) Uani 1 1 d . A . C27 C 0.2657(5) 0.4297(6) -0.1695(5) 0.0603(19) Uani 1 1 d . . . C28 C 0.2677(6) 0.3414(7) -0.2096(7) 0.079(2) Uani 1 1 d . B . C29 C 0.2809(7) 0.3374(9) -0.3096(8) 0.104(4) Uani 1 1 d D . . C30 C 0.2926(6) 0.4218(11) -0.3751(7) 0.096(4) Uani 1 1 d . B . H30 H 0.3026 0.4198 -0.4437 0.115 Uiso 1 1 calc R . . C31 C 0.2893(6) 0.5080(9) -0.3381(7) 0.086(3) Uani 1 1 d D . . C32 C 0.2767(5) 0.5123(7) -0.2409(6) 0.066(2) Uani 1 1 d . B . C33 C 0.5888(5) 0.1930(5) 0.1720(5) 0.0584(18) Uani 1 1 d . . . C34 C 0.6864(5) 0.1974(6) 0.1389(7) 0.066(2) Uani 1 1 d . C . C35 C 0.7713(7) 0.1517(6) 0.1875(8) 0.085(3) Uani 1 1 d D . . C36 C 0.7589(5) 0.0911(6) 0.2765(7) 0.080(2) Uani 1 1 d . C . H36 H 0.8148 0.0550 0.3111 0.096 Uiso 1 1 calc R . . C37 C 0.6651(6) 0.0853(6) 0.3118(5) 0.080(2) Uani 1 1 d D . . C38 C 0.5818(5) 0.1342(7) 0.2631(6) 0.076(2) Uani 1 1 d . C . C39 C 0.1698(5) -0.0127(5) 0.1350(5) 0.0561(18) Uani 1 1 d . . . C40 C 0.1998(5) -0.1155(6) 0.1458(6) 0.0610(19) Uani 1 1 d . D . C41 C 0.1356(6) -0.1830(6) 0.1449(6) 0.073(2) Uani 1 1 d D . . C42 C 0.0362(6) -0.1513(6) 0.1359(6) 0.075(2) Uani 1 1 d . D . H42 H -0.0087 -0.1988 0.1398 0.090 Uiso 1 1 calc R . . C43 C 0.0012(5) -0.0505(7) 0.1213(6) 0.075(2) Uani 1 1 d D . . C44 C 0.0693(5) 0.0169(5) 0.1216(6) 0.0632(19) Uani 1 1 d . D . B1 B 0.1268(6) 0.3495(7) 0.2472(6) 0.061(2) Uani 1 1 d . . . B2 B 0.2521(6) 0.4273(6) -0.0525(6) 0.058(2) Uani 1 1 d . . . B3 B 0.4963(6) 0.2336(6) 0.1062(6) 0.058(2) Uani 1 1 d . . . B4 B 0.2467(6) 0.0607(6) 0.1500(6) 0.058(2) Uani 1 1 d . . . C45 C 0.2064(7) 0.7993(6) 0.5061(7) 0.080(2) Uani 1 1 d . . . H45 H 0.2738 0.7693 0.5172 0.096 Uiso 1 1 calc R . . C46 C 0.1810(7) 0.8570(7) 0.4167(7) 0.086(3) Uani 1 1 d . . . H46 H 0.2317 0.8690 0.3665 0.103 Uiso 1 1 calc R . . C47 C 0.0814(8) 0.8971(7) 0.4005(7) 0.091(3) Uani 1 1 d . . . H47 H 0.0635 0.9333 0.3380 0.109 Uiso 1 1 calc R . . C48 C 0.0106(7) 0.8847(8) 0.4733(8) 0.097(3) Uani 1 1 d . . . H48 H -0.0566 0.9153 0.4622 0.117 Uiso 1 1 calc R . . C49 C 0.0320(7) 0.8300(8) 0.5619(8) 0.093(3) Uani 1 1 d . . . H49 H -0.0199 0.8214 0.6116 0.112 Uiso 1 1 calc R . . C50 C 0.1299(9) 0.7866(7) 0.5799(6) 0.092(3) Uani 1 1 d . . . H50 H 0.1453 0.7482 0.6422 0.111 Uiso 1 1 calc R . . C51 C 0.5345(7) 0.1793(9) -0.3741(8) 0.097(3) Uani 1 1 d . . . H51 H 0.5411 0.1192 -0.3276 0.116 Uiso 1 1 calc R . . C52 C 0.5003(7) 0.1803(8) -0.4657(8) 0.097(3) Uani 1 1 d . . . H52 H 0.4858 0.1196 -0.4831 0.117 Uiso 1 1 calc R . . C53 C 0.4865(7) 0.2705(10) -0.5344(8) 0.109(3) Uani 1 1 d . . . H53 H 0.4614 0.2719 -0.5970 0.130 Uiso 1 1 calc R . . C54 C 0.5112(8) 0.3562(9) -0.5063(12) 0.118(4) Uani 1 1 d . . . H54 H 0.5011 0.4175 -0.5510 0.141 Uiso 1 1 calc R . . C55 C 0.5501(7) 0.3574(11) -0.4156(12) 0.127(4) Uani 1 1 d . . . H55 H 0.5693 0.4165 -0.3992 0.153 Uiso 1 1 calc R . . C56 C 0.5590(7) 0.2673(10) -0.3512(9) 0.112(3) Uani 1 1 d . . . H56 H 0.5831 0.2659 -0.2881 0.134 Uiso 1 1 calc R . . 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 F1 0.069(3) 0.090(3) 0.098(4) -0.041(3) -0.002(2) -0.001(2) F2A 0.078(4) 0.077(4) 0.104(5) -0.045(4) -0.009(3) 0.009(3) F2B 0.103(16) 0.081(15) 0.13(2) -0.005(13) 0.026(12) -0.060(12) F3 0.068(3) 0.092(3) 0.082(3) -0.026(3) 0.003(2) -0.019(2) F4 0.098(3) 0.071(3) 0.083(3) -0.027(3) -0.025(2) 0.006(2) F5A 0.102(6) 0.128(9) 0.101(7) -0.061(6) -0.022(5) 0.024(5) F5B 0.112(11) 0.22(2) 0.071(11) 0.028(11) 0.003(7) -0.068(11) F6 0.075(3) 0.087(4) 0.079(3) 0.009(3) -0.014(2) -0.021(2) F7 0.073(3) 0.093(4) 0.093(4) 0.017(3) -0.014(2) -0.020(2) F8A 0.092(4) 0.093(5) 0.062(5) 0.013(4) -0.026(3) -0.017(3) F8B 0.15(2) 0.13(2) 0.13(2) 0.008(15) -0.022(15) -0.036(16) F9 0.082(3) 0.145(5) 0.066(3) 0.001(3) -0.007(2) -0.019(3) F10 0.066(2) 0.057(3) 0.097(3) -0.019(2) -0.008(2) -0.001(2) F11A 0.083(5) 0.056(6) 0.085(6) -0.004(4) -0.010(4) -0.009(4) F11B 0.067(6) 0.081(7) 0.121(9) -0.038(6) -0.017(5) -0.009(5) F12 0.078(3) 0.063(3) 0.126(4) -0.026(3) -0.030(3) -0.003(2) O1 0.055(3) 0.058(3) 0.061(3) -0.010(2) -0.009(2) -0.008(2) O2 0.069(3) 0.059(3) 0.053(3) -0.014(3) -0.002(2) -0.006(2) O3 0.052(2) 0.055(3) 0.059(3) -0.010(2) -0.009(2) 0.000(2) O4 0.065(3) 0.048(3) 0.055(3) -0.007(2) -0.008(2) -0.010(2) O5 0.057(2) 0.048(3) 0.056(3) -0.005(2) -0.013(2) -0.007(2) O6 0.052(2) 0.062(3) 0.056(3) -0.005(2) -0.006(2) -0.003(2) O7 0.068(3) 0.051(3) 0.056(3) -0.013(2) -0.004(2) -0.005(2) O8 0.069(3) 0.051(3) 0.055(3) -0.004(3) -0.003(2) -0.004(2) N1 0.045(3) 0.057(4) 0.053(4) -0.005(3) -0.004(3) 0.001(2) N2 0.036(3) 0.058(4) 0.050(4) -0.003(3) -0.003(2) 0.003(2) N3 0.062(3) 0.046(3) 0.053(4) -0.007(3) -0.006(3) -0.006(3) N4 0.060(3) 0.060(4) 0.055(4) -0.015(3) 0.003(3) -0.008(3) C1 0.042(4) 0.048(4) 0.073(6) -0.019(4) -0.008(4) -0.002(3) C2 0.054(4) 0.052(5) 0.078(6) -0.013(4) -0.007(4) -0.011(3) C3 0.044(4) 0.052(5) 0.090(6) -0.018(4) 0.006(4) -0.007(3) C4 0.059(4) 0.063(5) 0.067(6) -0.009(4) -0.013(4) -0.012(3) C5 0.049(4) 0.052(4) 0.062(5) -0.007(4) -0.014(3) -0.004(3) C6 0.052(4) 0.041(4) 0.058(5) -0.012(4) 0.008(3) -0.013(3) C7 0.054(4) 0.067(5) 0.049(5) -0.011(4) 0.000(3) -0.015(4) C8 0.056(4) 0.063(5) 0.068(5) -0.006(4) 0.008(4) -0.008(4) C9 0.055(4) 0.058(5) 0.072(5) -0.021(4) -0.010(4) -0.003(3) C10 0.053(4) 0.058(5) 0.052(4) -0.008(4) -0.007(3) -0.009(3) C11 0.055(4) 0.047(4) 0.057(5) -0.009(4) -0.017(3) 0.010(3) C12 0.045(4) 0.061(5) 0.060(5) -0.011(4) -0.009(3) 0.007(3) C13 0.064(4) 0.057(5) 0.057(5) -0.011(4) 0.003(3) 0.004(4) C14 0.067(4) 0.061(5) 0.053(5) -0.014(4) -0.001(4) -0.002(4) C15 0.066(4) 0.060(5) 0.055(5) -0.003(4) -0.012(4) -0.004(3) C16 0.054(4) 0.052(5) 0.060(5) -0.007(4) 0.001(3) -0.009(3) C17 0.059(4) 0.064(5) 0.058(5) -0.015(4) 0.001(4) -0.008(4) C18 0.057(4) 0.065(5) 0.065(6) -0.008(4) -0.001(4) -0.007(4) C19 0.080(5) 0.064(5) 0.046(5) 0.004(4) -0.001(4) -0.003(4) C20 0.070(4) 0.068(5) 0.053(5) -0.013(4) 0.002(4) -0.014(4) C21 0.061(4) 0.055(5) 0.054(5) -0.006(4) -0.005(3) -0.007(3) C22 0.055(4) 0.066(5) 0.076(6) -0.016(4) -0.001(4) -0.003(4) C23 0.080(5) 0.073(6) 0.060(5) -0.017(4) 0.000(4) 0.011(5) C24 0.113(7) 0.060(5) 0.081(7) -0.026(5) -0.006(5) -0.027(5) C25 0.099(6) 0.076(6) 0.067(6) -0.014(5) 0.002(5) -0.012(5) C26 0.067(5) 0.062(5) 0.069(5) -0.008(4) 0.011(4) -0.001(4) C27 0.056(4) 0.071(5) 0.053(5) -0.014(4) -0.009(3) 0.002(4) C28 0.066(5) 0.091(7) 0.079(7) -0.011(6) -0.009(4) -0.007(4) C29 0.091(6) 0.144(11) 0.078(8) -0.067(8) -0.028(5) 0.038(6) C30 0.058(5) 0.172(12) 0.043(6) -0.011(7) 0.001(4) 0.015(6) C31 0.060(5) 0.127(9) 0.069(7) -0.023(7) 0.006(4) -0.004(5) C32 0.058(4) 0.078(6) 0.061(6) -0.011(5) -0.005(4) -0.007(4) C33 0.059(4) 0.059(5) 0.055(5) 0.000(4) -0.010(3) -0.006(3) C34 0.052(4) 0.053(5) 0.094(6) -0.011(4) -0.015(4) -0.008(3) C35 0.074(6) 0.055(5) 0.122(9) -0.007(5) -0.025(5) 0.001(4) C36 0.055(5) 0.071(6) 0.111(8) -0.001(5) -0.026(5) -0.005(4) C37 0.088(6) 0.085(6) 0.068(6) -0.010(5) -0.022(5) -0.007(5) C38 0.049(4) 0.092(6) 0.083(6) -0.013(5) -0.011(4) -0.002(4) C39 0.053(4) 0.055(5) 0.057(5) -0.003(4) 0.002(3) -0.004(3) C40 0.057(4) 0.056(5) 0.072(5) -0.017(4) -0.007(4) -0.005(4) C41 0.081(5) 0.059(6) 0.077(6) -0.013(4) -0.007(4) -0.005(4) C42 0.081(5) 0.056(5) 0.093(7) -0.023(5) -0.002(4) -0.017(4) C43 0.070(5) 0.085(7) 0.073(6) -0.011(5) -0.010(4) -0.016(5) C44 0.069(4) 0.047(5) 0.074(5) -0.011(4) -0.015(4) -0.003(4) B1 0.056(5) 0.077(6) 0.051(5) -0.016(5) -0.002(4) -0.007(4) B2 0.056(4) 0.053(5) 0.061(6) -0.002(4) -0.008(4) 0.002(4) B3 0.055(5) 0.050(5) 0.064(6) -0.008(4) 0.004(4) -0.001(4) B4 0.058(5) 0.056(5) 0.060(6) -0.012(4) -0.011(4) -0.003(4) C45 0.099(6) 0.069(6) 0.071(6) -0.007(5) -0.007(5) -0.012(5) C46 0.097(6) 0.072(6) 0.093(8) -0.014(5) 0.004(5) -0.027(5) C47 0.114(7) 0.078(6) 0.074(7) -0.001(5) 0.006(6) -0.012(5) C48 0.090(6) 0.111(8) 0.081(7) -0.006(6) 0.006(6) 0.000(5) C49 0.086(6) 0.091(7) 0.111(9) -0.040(7) 0.022(6) -0.031(5) C50 0.159(9) 0.079(6) 0.048(5) -0.020(5) 0.018(6) -0.048(6) C51 0.098(7) 0.099(8) 0.086(8) 0.000(6) -0.006(6) -0.004(6) C52 0.099(7) 0.087(8) 0.090(8) 0.011(6) 0.017(6) -0.005(5) C53 0.080(6) 0.123(10) 0.112(9) -0.022(8) 0.006(5) 0.013(6) C54 0.090(7) 0.086(9) 0.163(13) -0.005(8) 0.017(7) -0.001(6) C55 0.081(7) 0.135(12) 0.163(13) -0.022(11) 0.001(7) -0.011(7) C56 0.095(7) 0.107(9) 0.130(10) -0.013(9) -0.001(6) -0.016(6) _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 F1 C22 1.345(8) . ? F2A C23 1.361(6) . ? F2B C25 1.347(7) . ? F3 C26 1.365(7) . ? F4 C28 1.378(10) . ? F5A C29 1.350(7) . ? F5B C31 1.336(7) . ? F6 C32 1.340(9) . ? F7 C34 1.346(9) . ? F8A C37 1.343(6) . ? F8B C35 1.341(7) . ? F9 C38 1.342(8) . ? F10 C40 1.339(7) . ? F11A C41 1.339(6) . ? F11B C43 1.337(6) . ? F12 C44 1.350(8) . ? O1 C1 1.326(8) . ? O1 B1 1.496(9) . ? O2 C2 1.342(9) . ? O2 B1 1.476(9) . ? O3 C6 1.321(7) . ? O3 B2 1.508(9) . ? O4 C7 1.347(8) . ? O4 B2 1.472(9) . ? O5 C11 1.341(8) . ? O5 B3 1.511(9) . ? O6 C12 1.350(8) . ? O6 B3 1.509(9) . ? O7 C16 1.298(8) . ? O7 B4 1.510(9) . ? O8 C17 1.343(8) . ? O8 B4 1.492(9) . ? N1 C1 1.340(9) . ? N1 C5 1.368(8) . ? N1 B2 1.592(9) . ? N2 C6 1.334(8) . ? N2 C10 1.381(8) . ? N2 B3 1.559(10) . ? N3 C11 1.324(8) . ? N3 C15 1.368(9) . ? N3 B4 1.583(10) . ? N4 C16 1.319(8) . ? N4 C20 1.390(9) . ? N4 B1 1.581(10) . ? C1 C2 1.396(9) . ? C2 C3 1.358(9) . ? C3 C4 1.410(10) . ? C3 H3 0.9500 . ? C4 C5 1.337(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.385(9) . ? C7 C8 1.367(9) . ? C8 C9 1.403(9) . ? C8 H8 0.9500 . ? C9 C10 1.349(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.410(9) . ? C12 C13 1.325(9) . ? C13 C14 1.427(9) . ? C13 H13 0.9500 . ? C14 C15 1.339(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.413(9) . ? C17 C18 1.361(10) . ? C18 C19 1.407(10) . ? C18 H18 0.9500 . ? C19 C20 1.350(9) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.375(9) . ? C21 C26 1.390(10) . ? C21 B1 1.609(11) . ? C22 C23 1.381(10) . ? C23 C24 1.361(10) . ? C24 C25 1.370(11) . ? C24 H24 0.9500 . ? C25 C26 1.376(11) . ? C27 C32 1.389(10) . ? C27 C28 1.396(11) . ? C27 B2 1.608(11) . ? C28 C29 1.387(13) . ? C29 C30 1.364(13) . ? C30 C31 1.345(13) . ? C30 H30 0.9500 . ? C31 C32 1.349(12) . ? C33 C34 1.370(9) . ? C33 C38 1.383(10) . ? C33 B3 1.578(10) . ? C34 C35 1.382(10) . ? C35 C36 1.379(12) . ? C36 C37 1.333(10) . ? C36 H36 0.9500 . ? C37 C38 1.377(10) . ? C39 C44 1.372(9) . ? C39 C40 1.378(9) . ? C39 B4 1.601(10) . ? C40 C41 1.367(10) . ? C41 C42 1.352(10) . ? C42 C43 1.362(10) . ? C42 H42 0.9500 . ? C43 C44 1.403(10) . ? C45 C46 1.387(11) . ? C45 C50 1.405(11) . ? C45 H45 0.9500 . ? C46 C47 1.391(11) . ? C46 H46 0.9500 . ? C47 C48 1.342(11) . ? C47 H47 0.9500 . ? C48 C49 1.351(13) . ? C48 H48 0.9500 . ? C49 C50 1.383(12) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.380(13) . ? C51 C56 1.382(13) . ? C51 H51 0.9500 . ? C52 C53 1.418(13) . ? C52 H52 0.9500 . ? C53 C54 1.384(14) . ? C53 H53 0.9500 . ? C54 C55 1.401(16) . ? C54 H54 0.9500 . ? C55 C56 1.386(15) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? 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 C1 O1 B1 106.0(5) . . ? C2 O2 B1 106.5(5) . . ? C6 O3 B2 106.8(5) . . ? C7 O4 B2 108.1(5) . . ? C11 O5 B3 106.6(5) . . ? C12 O6 B3 107.8(5) . . ? C16 O7 B4 107.2(5) . . ? C17 O8 B4 107.3(5) . . ? C1 N1 C5 116.6(5) . . ? C1 N1 B2 120.4(6) . . ? C5 N1 B2 122.9(6) . . ? C6 N2 C10 116.1(6) . . ? C6 N2 B3 120.8(6) . . ? C10 N2 B3 123.0(5) . . ? C11 N3 C15 115.6(6) . . ? C11 N3 B4 120.5(6) . . ? C15 N3 B4 123.8(6) . . ? C16 N4 C20 117.4(7) . . ? C16 N4 B1 120.4(6) . . ? C20 N4 B1 122.1(6) . . ? O1 C1 N1 124.2(6) . . ? O1 C1 C2 111.8(7) . . ? N1 C1 C2 123.9(7) . . ? O2 C2 C3 131.1(6) . . ? O2 C2 C1 110.5(6) . . ? C3 C2 C1 118.4(8) . . ? C2 C3 C4 118.0(7) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 120.8(7) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 N1 122.3(7) . . ? C4 C5 H5 118.9 . . ? N1 C5 H5 118.9 . . ? O3 C6 N2 124.2(6) . . ? O3 C6 C7 112.0(6) . . ? N2 C6 C7 123.8(6) . . ? O4 C7 C8 129.8(7) . . ? O4 C7 C6 109.8(6) . . ? C8 C7 C6 120.4(7) . . ? C7 C8 C9 115.9(7) . . ? C7 C8 H8 122.0 . . ? C9 C8 H8 122.0 . . ? C10 C9 C8 121.8(7) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 N2 121.9(6) . . ? C9 C10 H10 119.0 . . ? N2 C10 H10 119.0 . . ? N3 C11 O5 123.7(6) . . ? N3 C11 C12 124.1(7) . . ? O5 C11 C12 112.2(6) . . ? C13 C12 O6 131.0(7) . . ? C13 C12 C11 119.2(7) . . ? O6 C12 C11 109.8(6) . . ? C12 C13 C14 118.0(7) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? C15 C14 C13 119.3(7) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 N3 123.8(7) . . ? C14 C15 H15 118.1 . . ? N3 C15 H15 118.1 . . ? O7 C16 N4 125.2(7) . . ? O7 C16 C17 112.3(6) . . ? N4 C16 C17 122.5(7) . . ? O8 C17 C18 130.4(7) . . ? O8 C17 C16 109.4(7) . . ? C18 C17 C16 120.1(7) . . ? C17 C18 C19 117.2(7) . . ? C17 C18 H18 121.4 . . ? C19 C18 H18 121.4 . . ? C20 C19 C18 120.7(7) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 N4 122.0(7) . . ? C19 C20 H20 119.0 . . ? N4 C20 H20 119.0 . . ? C22 C21 C26 112.1(7) . . ? C22 C21 B1 126.6(6) . . ? C26 C21 B1 120.9(6) . . ? F1 C22 C21 119.6(7) . . ? F1 C22 C23 117.1(6) . . ? C21 C22 C23 123.2(7) . . ? F2A C23 C24 119.8(8) . . ? F2A C23 C22 118.8(7) . . ? C24 C23 C22 121.4(6) . . ? C23 C24 C25 118.8(8) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? F2B C25 C24 124.9(12) . . ? F2B C25 C26 117.7(11) . . ? C24 C25 C26 117.4(8) . . ? F3 C26 C25 116.3(7) . . ? F3 C26 C21 116.5(7) . . ? C25 C26 C21 127.0(7) . . ? C32 C27 C28 112.5(8) . . ? C32 C27 B2 127.5(7) . . ? C28 C27 B2 120.1(7) . . ? F4 C28 C29 120.3(9) . . ? F4 C28 C27 116.5(8) . . ? C29 C28 C27 123.2(9) . . ? F5A C29 C30 123.3(11) . . ? F5A C29 C28 115.8(11) . . ? C30 C29 C28 120.8(9) . . ? C31 C30 C29 116.9(9) . . ? C31 C30 H30 121.6 . . ? C29 C30 H30 121.6 . . ? F5B C31 C30 116.0(12) . . ? F5B C31 C32 121.4(12) . . ? C30 C31 C32 122.6(10) . . ? F6 C32 C31 117.5(9) . . ? F6 C32 C27 118.5(7) . . ? C31 C32 C27 124.0(9) . . ? C34 C33 C38 112.1(7) . . ? C34 C33 B3 123.7(7) . . ? C38 C33 B3 123.3(6) . . ? F7 C34 C33 118.5(6) . . ? F7 C34 C35 114.8(7) . . ? C33 C34 C35 126.7(9) . . ? F8B C35 C36 113.0(12) . . ? F8B C35 C34 128.8(14) . . ? C36 C35 C34 118.1(9) . . ? C37 C36 C35 117.2(8) . . ? C37 C36 H36 121.4 . . ? C35 C36 H36 121.4 . . ? C36 C37 F8A 117.8(8) . . ? C36 C37 C38 123.5(8) . . ? F8A C37 C38 118.7(8) . . ? F9 C38 C37 116.8(8) . . ? F9 C38 C33 120.8(7) . . ? C37 C38 C33 122.4(7) . . ? C44 C39 C40 114.2(6) . . ? C44 C39 B4 125.1(6) . . ? C40 C39 B4 120.4(6) . . ? F10 C40 C41 117.8(7) . . ? F10 C40 C39 118.8(6) . . ? C41 C40 C39 123.4(6) . . ? F11A C41 C42 120.9(8) . . ? F11A C41 C40 118.2(7) . . ? C42 C41 C40 120.7(7) . . ? C41 C42 C43 119.3(7) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? F11B C43 C42 120.6(8) . . ? F11B C43 C44 121.0(8) . . ? C42 C43 C44 118.4(6) . . ? F12 C44 C39 120.7(6) . . ? F12 C44 C43 115.4(6) . . ? C39 C44 C43 123.8(7) . . ? O2 B1 O1 105.0(6) . . ? O2 B1 N4 108.4(6) . . ? O1 B1 N4 107.9(5) . . ? O2 B1 C21 113.1(6) . . ? O1 B1 C21 110.0(6) . . ? N4 B1 C21 112.1(6) . . ? O4 B2 O3 103.3(6) . . ? O4 B2 N1 109.7(6) . . ? O3 B2 N1 108.9(6) . . ? O4 B2 C27 116.1(7) . . ? O3 B2 C27 109.2(6) . . ? N1 B2 C27 109.4(6) . . ? O6 B3 O5 103.6(6) . . ? O6 B3 N2 108.7(6) . . ? O5 B3 N2 107.7(5) . . ? O6 B3 C33 109.5(5) . . ? O5 B3 C33 113.2(6) . . ? N2 B3 C33 113.7(6) . . ? O8 B4 O7 103.3(6) . . ? O8 B4 N3 109.2(5) . . ? O7 B4 N3 107.5(6) . . ? O8 B4 C39 109.1(6) . . ? O7 B4 C39 115.1(6) . . ? N3 B4 C39 112.2(6) . . ? C46 C45 C50 118.2(9) . . ? C46 C45 H45 120.9 . . ? C50 C45 H45 120.9 . . ? C45 C46 C47 120.0(8) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 119.9(9) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C47 C48 C49 122.0(9) . . ? C47 C48 H48 119.0 . . ? C49 C48 H48 119.0 . . ? C48 C49 C50 119.7(9) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C45 120.0(9) . . ? C49 C50 H50 120.0 . . ? C45 C50 H50 120.0 . . ? C52 C51 C56 118.8(11) . . ? C52 C51 H51 120.6 . . ? C56 C51 H51 120.6 . . ? C51 C52 C53 121.1(11) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C54 C53 C52 117.1(11) . . ? C54 C53 H53 121.4 . . ? C52 C53 H53 121.4 . . ? C53 C54 C55 123.5(13) . . ? C53 C54 H54 118.2 . . ? C55 C54 H54 118.2 . . ? C56 C55 C54 116.1(13) . . ? C56 C55 H55 121.9 . . ? C54 C55 H55 121.9 . . ? C51 C56 C55 123.2(13) . . ? C51 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? 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 B1 O1 C1 N1 176.2(6) . . . . ? B1 O1 C1 C2 0.0(7) . . . . ? C5 N1 C1 O1 -173.4(6) . . . . ? B2 N1 C1 O1 4.7(9) . . . . ? C5 N1 C1 C2 2.3(9) . . . . ? B2 N1 C1 C2 -179.6(6) . . . . ? B1 O2 C2 C3 -171.9(8) . . . . ? B1 O2 C2 C1 5.6(7) . . . . ? O1 C1 C2 O2 -3.6(8) . . . . ? N1 C1 C2 O2 -179.9(6) . . . . ? O1 C1 C2 C3 174.2(6) . . . . ? N1 C1 C2 C3 -2.1(10) . . . . ? O2 C2 C3 C4 177.4(7) . . . . ? C1 C2 C3 C4 0.1(10) . . . . ? C2 C3 C4 C5 1.4(10) . . . . ? C3 C4 C5 N1 -1.2(11) . . . . ? C1 N1 C5 C4 -0.7(9) . . . . ? B2 N1 C5 C4 -178.7(6) . . . . ? B2 O3 C6 N2 -179.1(6) . . . . ? B2 O3 C6 C7 -0.9(7) . . . . ? C10 N2 C6 O3 178.9(6) . . . . ? B3 N2 C6 O3 0.0(9) . . . . ? C10 N2 C6 C7 0.8(9) . . . . ? B3 N2 C6 C7 -178.0(6) . . . . ? B2 O4 C7 C8 178.4(7) . . . . ? B2 O4 C7 C6 -0.8(7) . . . . ? O3 C6 C7 O4 1.1(8) . . . . ? N2 C6 C7 O4 179.3(6) . . . . ? O3 C6 C7 C8 -178.2(6) . . . . ? N2 C6 C7 C8 0.1(10) . . . . ? O4 C7 C8 C9 -178.9(6) . . . . ? C6 C7 C8 C9 0.2(10) . . . . ? C7 C8 C9 C10 -1.4(10) . . . . ? C8 C9 C10 N2 2.4(10) . . . . ? C6 N2 C10 C9 -2.0(9) . . . . ? B3 N2 C10 C9 176.8(6) . . . . ? C15 N3 C11 O5 179.6(5) . . . . ? B4 N3 C11 O5 3.4(9) . . . . ? C15 N3 C11 C12 -0.1(9) . . . . ? B4 N3 C11 C12 -176.3(6) . . . . ? B3 O5 C11 N3 179.3(6) . . . . ? B3 O5 C11 C12 -1.0(7) . . . . ? B3 O6 C12 C13 -176.9(7) . . . . ? B3 O6 C12 C11 1.0(7) . . . . ? N3 C11 C12 C13 -2.1(10) . . . . ? O5 C11 C12 C13 178.2(6) . . . . ? N3 C11 C12 O6 179.7(6) . . . . ? O5 C11 C12 O6 0.0(7) . . . . ? O6 C12 C13 C14 -179.4(6) . . . . ? C11 C12 C13 C14 2.9(10) . . . . ? C12 C13 C14 C15 -1.7(10) . . . . ? C13 C14 C15 N3 -0.6(10) . . . . ? C11 N3 C15 C14 1.4(9) . . . . ? B4 N3 C15 C14 177.5(6) . . . . ? B4 O7 C16 N4 -177.3(6) . . . . ? B4 O7 C16 C17 0.7(7) . . . . ? C20 N4 C16 O7 174.8(6) . . . . ? B1 N4 C16 O7 -6.2(10) . . . . ? C20 N4 C16 C17 -3.0(9) . . . . ? B1 N4 C16 C17 176.0(6) . . . . ? B4 O8 C17 C18 171.0(7) . . . . ? B4 O8 C17 C16 -6.1(7) . . . . ? O7 C16 C17 O8 3.6(8) . . . . ? N4 C16 C17 O8 -178.3(6) . . . . ? O7 C16 C17 C18 -173.9(6) . . . . ? N4 C16 C17 C18 4.2(10) . . . . ? O8 C17 C18 C19 -179.6(7) . . . . ? C16 C17 C18 C19 -2.7(10) . . . . ? C17 C18 C19 C20 0.4(10) . . . . ? C18 C19 C20 N4 0.7(10) . . . . ? C16 N4 C20 C19 0.6(9) . . . . ? B1 N4 C20 C19 -178.3(6) . . . . ? C26 C21 C22 F1 179.8(7) . . . . ? B1 C21 C22 F1 6.9(12) . . . . ? C26 C21 C22 C23 -1.8(11) . . . . ? B1 C21 C22 C23 -174.6(8) . . . . ? F1 C22 C23 F2A 0.1(11) . . . . ? C21 C22 C23 F2A -178.4(7) . . . . ? F1 C22 C23 C24 179.5(7) . . . . ? C21 C22 C23 C24 1.0(13) . . . . ? F2A C23 C24 C25 178.7(8) . . . . ? C22 C23 C24 C25 -0.7(13) . . . . ? C23 C24 C25 F2B -177.7(13) . . . . ? C23 C24 C25 C26 1.3(13) . . . . ? F2B C25 C26 F3 2.0(14) . . . . ? C24 C25 C26 F3 -177.1(7) . . . . ? F2B C25 C26 C21 176.7(12) . . . . ? C24 C25 C26 C21 -2.4(13) . . . . ? C22 C21 C26 F3 177.3(6) . . . . ? B1 C21 C26 F3 -9.5(10) . . . . ? C22 C21 C26 C25 2.5(12) . . . . ? B1 C21 C26 C25 175.8(8) . . . . ? C32 C27 C28 F4 -176.8(6) . . . . ? B2 C27 C28 F4 3.3(9) . . . . ? C32 C27 C28 C29 1.1(10) . . . . ? B2 C27 C28 C29 -178.8(7) . . . . ? F4 C28 C29 F5A -1.3(12) . . . . ? C27 C28 C29 F5A -179.1(7) . . . . ? F4 C28 C29 C30 177.5(8) . . . . ? C27 C28 C29 C30 -0.3(13) . . . . ? F5A C29 C30 C31 178.0(8) . . . . ? C28 C29 C30 C31 -0.8(13) . . . . ? C29 C30 C31 F5B -175.6(10) . . . . ? C29 C30 C31 C32 1.0(12) . . . . ? F5B C31 C32 F6 -0.9(13) . . . . ? C30 C31 C32 F6 -177.3(7) . . . . ? F5B C31 C32 C27 176.3(10) . . . . ? C30 C31 C32 C27 -0.1(12) . . . . ? C28 C27 C32 F6 176.3(6) . . . . ? B2 C27 C32 F6 -3.8(11) . . . . ? C28 C27 C32 C31 -0.9(10) . . . . ? B2 C27 C32 C31 179.0(7) . . . . ? C38 C33 C34 F7 -178.7(7) . . . . ? B3 C33 C34 F7 11.7(11) . . . . ? C38 C33 C34 C35 -1.0(12) . . . . ? B3 C33 C34 C35 -170.6(8) . . . . ? F7 C34 C35 F8B 6.2(19) . . . . ? C33 C34 C35 F8B -171.5(16) . . . . ? F7 C34 C35 C36 -178.9(7) . . . . ? C33 C34 C35 C36 3.4(13) . . . . ? F8B C35 C36 C37 172.2(14) . . . . ? C34 C35 C36 C37 -3.5(13) . . . . ? C35 C36 C37 F8A 179.2(8) . . . . ? C35 C36 C37 C38 1.7(14) . . . . ? C36 C37 C38 F9 177.7(8) . . . . ? F8A C37 C38 F9 0.2(12) . . . . ? C36 C37 C38 C33 0.7(14) . . . . ? F8A C37 C38 C33 -176.7(8) . . . . ? C34 C33 C38 F9 -177.9(7) . . . . ? B3 C33 C38 F9 -8.2(12) . . . . ? C34 C33 C38 C37 -1.1(12) . . . . ? B3 C33 C38 C37 168.6(8) . . . . ? C44 C39 C40 F10 178.2(6) . . . . ? B4 C39 C40 F10 -8.5(10) . . . . ? C44 C39 C40 C41 -0.9(11) . . . . ? B4 C39 C40 C41 172.4(7) . . . . ? F10 C40 C41 F11A 4.2(11) . . . . ? C39 C40 C41 F11A -176.7(8) . . . . ? F10 C40 C41 C42 178.9(7) . . . . ? C39 C40 C41 C42 -2.0(13) . . . . ? F11A C41 C42 C43 178.8(8) . . . . ? C40 C41 C42 C43 4.2(13) . . . . ? C41 C42 C43 F11B 176.4(9) . . . . ? C41 C42 C43 C44 -3.5(12) . . . . ? C40 C39 C44 F12 -178.9(7) . . . . ? B4 C39 C44 F12 8.1(11) . . . . ? C40 C39 C44 C43 1.6(11) . . . . ? B4 C39 C44 C43 -171.4(7) . . . . ? F11B C43 C44 F12 1.1(12) . . . . ? C42 C43 C44 F12 -179.0(7) . . . . ? F11B C43 C44 C39 -179.4(8) . . . . ? C42 C43 C44 C39 0.6(12) . . . . ? C2 O2 B1 O1 -5.4(7) . . . . ? C2 O2 B1 N4 -120.5(6) . . . . ? C2 O2 B1 C21 114.6(7) . . . . ? C1 O1 B1 O2 3.3(7) . . . . ? C1 O1 B1 N4 118.7(6) . . . . ? C1 O1 B1 C21 -118.7(6) . . . . ? C16 N4 B1 O2 64.7(8) . . . . ? C20 N4 B1 O2 -116.4(6) . . . . ? C16 N4 B1 O1 -48.5(8) . . . . ? C20 N4 B1 O1 130.4(6) . . . . ? C16 N4 B1 C21 -169.7(6) . . . . ? C20 N4 B1 C21 9.2(9) . . . . ? C22 C21 B1 O2 4.7(11) . . . . ? C26 C21 B1 O2 -167.6(7) . . . . ? C22 C21 B1 O1 121.7(8) . . . . ? C26 C21 B1 O1 -50.6(9) . . . . ? C22 C21 B1 N4 -118.3(8) . . . . ? C26 C21 B1 N4 69.5(9) . . . . ? C7 O4 B2 O3 0.2(7) . . . . ? C7 O4 B2 N1 116.2(6) . . . . ? C7 O4 B2 C27 -119.2(6) . . . . ? C6 O3 B2 O4 0.4(7) . . . . ? C6 O3 B2 N1 -116.1(6) . . . . ? C6 O3 B2 C27 124.5(6) . . . . ? C1 N1 B2 O4 -64.2(8) . . . . ? C5 N1 B2 O4 113.8(7) . . . . ? C1 N1 B2 O3 48.1(8) . . . . ? C5 N1 B2 O3 -133.9(6) . . . . ? C1 N1 B2 C27 167.4(6) . . . . ? C5 N1 B2 C27 -14.6(9) . . . . ? C32 C27 B2 O4 -9.0(10) . . . . ? C28 C27 B2 O4 170.9(6) . . . . ? C32 C27 B2 O3 -125.1(7) . . . . ? C28 C27 B2 O3 54.8(8) . . . . ? C32 C27 B2 N1 115.8(8) . . . . ? C28 C27 B2 N1 -64.3(8) . . . . ? C12 O6 B3 O5 -1.6(6) . . . . ? C12 O6 B3 N2 -115.8(6) . . . . ? C12 O6 B3 C33 119.4(6) . . . . ? C11 O5 B3 O6 1.5(6) . . . . ? C11 O5 B3 N2 116.6(6) . . . . ? C11 O5 B3 C33 -116.9(6) . . . . ? C6 N2 B3 O6 56.7(7) . . . . ? C10 N2 B3 O6 -122.0(6) . . . . ? C6 N2 B3 O5 -54.9(8) . . . . ? C10 N2 B3 O5 126.4(6) . . . . ? C6 N2 B3 C33 178.9(6) . . . . ? C10 N2 B3 C33 0.2(9) . . . . ? C34 C33 B3 O6 35.5(10) . . . . ? C38 C33 B3 O6 -132.9(8) . . . . ? C34 C33 B3 O5 150.5(7) . . . . ? C38 C33 B3 O5 -17.9(10) . . . . ? C34 C33 B3 N2 -86.2(8) . . . . ? C38 C33 B3 N2 105.3(8) . . . . ? C17 O8 B4 O7 6.3(7) . . . . ? C17 O8 B4 N3 120.4(6) . . . . ? C17 O8 B4 C39 -116.6(6) . . . . ? C16 O7 B4 O8 -4.2(7) . . . . ? C16 O7 B4 N3 -119.6(6) . . . . ? C16 O7 B4 C39 114.7(7) . . . . ? C11 N3 B4 O8 -57.9(8) . . . . ? C15 N3 B4 O8 126.2(6) . . . . ? C11 N3 B4 O7 53.5(8) . . . . ? C15 N3 B4 O7 -122.4(6) . . . . ? C11 N3 B4 C39 -179.0(6) . . . . ? C15 N3 B4 C39 5.1(9) . . . . ? C44 C39 B4 O8 127.8(7) . . . . ? C40 C39 B4 O8 -44.8(9) . . . . ? C44 C39 B4 O7 12.2(11) . . . . ? C40 C39 B4 O7 -160.4(6) . . . . ? C44 C39 B4 N3 -111.1(8) . . . . ? C40 C39 B4 N3 76.3(8) . . . . ? C50 C45 C46 C47 -2.5(13) . . . . ? C45 C46 C47 C48 3.7(14) . . . . ? C46 C47 C48 C49 -3.0(16) . . . . ? C47 C48 C49 C50 1.3(16) . . . . ? C48 C49 C50 C45 -0.2(14) . . . . ? C46 C45 C50 C49 0.8(12) . . . . ? C56 C51 C52 C53 -2.5(14) . . . . ? C51 C52 C53 C54 1.6(13) . . . . ? C52 C53 C54 C55 1.2(15) . . . . ? C53 C54 C55 C56 -2.9(16) . . . . ? C52 C51 C56 C55 0.6(15) . . . . ? C54 C55 C56 C51 2.0(16) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.333 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.073 #===END