# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Kay Severin' 'Nicolas Christinat' 'Rosario Scopelliti' _publ_contact_author_name 'Kay Severin' _publ_contact_author_email KAY.SEVERIN@EPFL.CH _publ_section_title ; Boron-Based Rotaxanes by Multicomponent Self-Assembly ; # Attachment 'compounds1-3.cif' data_rotaxane_1 _database_code_depnum_ccdc_archive 'CCDC 683419' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H44 O10, C40 H24 B2 F12 N2 O4' _chemical_formula_sum 'C76 H68 B2 F12 N2 O14' _chemical_formula_weight 1482.94 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7382(12) _cell_length_b 16.517(3) _cell_length_c 17.832(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.670(13) _cell_angle_gamma 90.00 _cell_volume 3417.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 114 _cell_measurement_theta_min 3.694 _cell_measurement_theta_max 17.818 _exptl_crystal_description prismatic _exptl_crystal_colour amber _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8159 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS V2.10, Sheldrick, G.M., 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX II 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 40239 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5990 _reflns_number_gt 4138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs, 1990-2000)' _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^)+(0.2000P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5990 _refine_ls_number_parameters 498 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.2110 _refine_ls_R_factor_gt 0.1633 _refine_ls_wR_factor_ref 0.5002 _refine_ls_wR_factor_gt 0.4567 _refine_ls_goodness_of_fit_ref 2.105 _refine_ls_restrained_S_all 2.106 _refine_ls_shift/su_max 0.006 _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 -0.5822(7) 0.1243(4) -0.2625(5) 0.068(2) Uani 1 1 d . . . F2 F -0.7144(5) 0.2135(4) -0.2720(4) 0.0546(19) Uani 1 1 d . . . F3 F -0.6102(7) 0.2030(6) -0.3604(4) 0.079(3) Uani 1 1 d . . . F4 F -0.6016(6) 0.4369(4) -0.0928(4) 0.0519(19) Uani 1 1 d . . . F5 F -0.5817(6) 0.5111(3) -0.1892(4) 0.0447(16) Uani 1 1 d . . . F6 F -0.4418(6) 0.4993(4) -0.0961(4) 0.0553(19) Uani 1 1 d . . . O1 O -0.1143(6) 0.3592(4) -0.1813(4) 0.0363(17) Uani 1 1 d . . . O2 O -0.1505(6) 0.2728(6) -0.2864(4) 0.048(2) Uani 1 1 d . . . N1 N -0.1467(6) 0.2131(5) -0.1585(5) 0.0315(19) Uani 1 1 d . . . B1 B -0.1870(10) 0.2920(7) -0.2119(6) 0.033(3) Uani 1 1 d . . . C1 C -0.0283(9) 0.3652(7) -0.2251(6) 0.041(3) Uani 1 1 d . . . C2 C 0.0674(10) 0.4160(9) -0.2123(9) 0.062(4) Uani 1 1 d . . . H2 H 0.0820 0.4507 -0.1695 0.074 Uiso 1 1 calc R . . C3 C 0.1433(11) 0.4118(14) -0.2696(13) 0.102(9) Uani 1 1 d . . . H3 H 0.2100 0.4451 -0.2634 0.123 Uiso 1 1 calc R . . C4 C 0.1245(15) 0.3639(16) -0.3304(12) 0.112(10) Uani 1 1 d . . . H4 H 0.1753 0.3653 -0.3671 0.135 Uiso 1 1 calc R . . C5 C 0.0264(13) 0.3099(11) -0.3402(8) 0.076(5) Uani 1 1 d . . . H5 H 0.0141 0.2725 -0.3811 0.091 Uiso 1 1 calc R . . C6 C -0.0495(10) 0.3148(9) -0.2873(7) 0.053(4) Uani 1 1 d . . . C7 C -0.0990(8) 0.1463(7) -0.1811(7) 0.041(3) Uani 1 1 d . . . H7 H -0.0882 0.1410 -0.2326 0.049 Uiso 1 1 calc R . . C8 C -0.0640(9) 0.0829(7) -0.1295(8) 0.049(3) Uani 1 1 d . . . H8 H -0.0333 0.0344 -0.1469 0.059 Uiso 1 1 calc R . . C9 C -0.0745(9) 0.0914(8) -0.0535(7) 0.047(3) Uani 1 1 d . . . C10 C -0.1245(10) 0.1604(8) -0.0306(7) 0.047(3) Uani 1 1 d . . . H10 H -0.1344 0.1680 0.0208 0.056 Uiso 1 1 calc R . . C11 C -0.1594(10) 0.2172(7) -0.0839(6) 0.043(3) Uani 1 1 d . . . H11 H -0.1960 0.2640 -0.0678 0.052 Uiso 1 1 calc R . . C12 C -0.0335(9) 0.0302(7) 0.0061(7) 0.042(3) Uani 1 1 d . . . H12 H -0.0569 0.0352 0.0547 0.051 Uiso 1 1 calc R . . C13 C -0.3216(8) 0.3061(7) -0.2136(5) 0.034(2) Uani 1 1 d . . . C14 C -0.4025(8) 0.2498(7) -0.2469(5) 0.033(2) Uani 1 1 d . . . H14 H -0.3780 0.2025 -0.2703 0.040 Uiso 1 1 calc R . . C15 C -0.5209(8) 0.2634(6) -0.2456(5) 0.029(2) Uani 1 1 d . . . C16 C -0.5597(8) 0.3313(6) -0.2108(6) 0.033(2) Uani 1 1 d . . . H16 H -0.6398 0.3390 -0.2103 0.039 Uiso 1 1 calc R . . C17 C -0.4810(8) 0.3875(6) -0.1769(5) 0.030(2) Uani 1 1 d . . . C18 C -0.3618(9) 0.3750(6) -0.1782(6) 0.036(2) Uani 1 1 d . . . H18 H -0.3078 0.4136 -0.1548 0.043 Uiso 1 1 calc R . . C19 C -0.6048(9) 0.2017(7) -0.2855(6) 0.036(2) Uani 1 1 d . . . C20 C -0.5243(9) 0.4594(6) -0.1397(6) 0.036(2) Uani 1 1 d . . . O3 O -0.1320(7) -0.3242(6) -0.0362(5) 0.052(2) Uani 1 1 d . . . O4 O -0.2501(6) -0.1905(5) 0.0211(4) 0.0429(19) Uani 1 1 d . . . O5 O -0.3830(7) 0.1618(5) 0.0200(4) 0.048(2) Uani 1 1 d . . . O6 O -0.3039(6) 0.3225(5) 0.0129(4) 0.0424(19) Uani 1 1 d . . . O7A O -0.058(2) 0.429(2) 0.1183(16) 0.084(8) Uani 0.51(3) 1 d PDU . 1 C21A C -0.055(2) -0.399(2) -0.1403(17) 0.083(12) Uani 0.51(3) 1 d PD . 1 H21A H -0.0916 -0.4317 -0.1837 0.100 Uiso 0.51(3) 1 calc PR . 1 H21B H -0.0481 -0.3428 -0.1596 0.100 Uiso 0.51(3) 1 calc PR . 1 O7B O -0.046(3) 0.4521(17) 0.081(2) 0.117(11) Uani 0.49(3) 1 d PDU . 2 C21B C -0.047(4) -0.454(3) -0.052(3) 0.12(2) Uani 0.49(3) 1 d PD . 2 H21C H -0.0264 -0.4437 0.0034 0.148 Uiso 0.49(3) 1 calc PR . 2 H21D H -0.0790 -0.5093 -0.0579 0.148 Uiso 0.49(3) 1 calc PR . 2 C22 C -0.1381(12) -0.3955(10) -0.0831(9) 0.068(4) Uani 1 1 d D . . H22A H -0.2175 -0.4002 -0.1108 0.081 Uiso 1 1 calc R . 1 H22B H -0.1239 -0.4434 -0.0496 0.081 Uiso 1 1 calc R . 1 C23 C -0.2024(11) -0.3298(8) 0.0201(7) 0.049(3) Uani 1 1 d . . . H23A H -0.1792 -0.3771 0.0530 0.059 Uiso 1 1 calc R . . H23B H -0.2836 -0.3374 -0.0035 0.059 Uiso 1 1 calc R . . C24 C -0.1919(10) -0.2548(8) 0.0664(7) 0.051(3) Uani 1 1 d . . . H24A H -0.2273 -0.2628 0.1128 0.062 Uiso 1 1 calc R . . H24B H -0.1096 -0.2409 0.0816 0.062 Uiso 1 1 calc R . . C25 C -0.2583(8) -0.1146(7) 0.0542(6) 0.037(3) Uani 1 1 d . . . C26 C -0.3156(8) -0.0542(8) 0.0051(6) 0.041(3) Uani 1 1 d . . . C27 C -0.3237(8) 0.0255(7) 0.0351(6) 0.038(3) Uani 1 1 d . . . C28 C -0.2789(9) 0.0406(8) 0.1125(6) 0.047(3) Uani 1 1 d . . . H28 H -0.2850 0.0933 0.1327 0.056 Uiso 1 1 calc R . . C29 C -0.2281(9) -0.0182(7) 0.1573(6) 0.042(3) Uani 1 1 d . . . H29 H -0.1992 -0.0068 0.2088 0.050 Uiso 1 1 calc R . . C30 C -0.2168(9) -0.0980(8) 0.1284(6) 0.045(3) Uani 1 1 d . . . H30 H -0.1807 -0.1393 0.1607 0.054 Uiso 1 1 calc R . . C31 C -0.3658(9) -0.0713(8) -0.0718(6) 0.045(3) Uani 1 1 d . . . H31 H -0.3607 -0.1241 -0.0921 0.054 Uiso 1 1 calc R . . C32 C -0.4208(9) -0.0114(9) -0.1152(6) 0.054(3) Uani 1 1 d . . . H32 H -0.4551 -0.0228 -0.1658 0.064 Uiso 1 1 calc R . . C33 C -0.4276(9) 0.0691(9) -0.0857(6) 0.047(3) Uani 1 1 d . . . H33 H -0.4638 0.1109 -0.1172 0.056 Uiso 1 1 calc R . . C34 C -0.3830(9) 0.0852(8) -0.0138(6) 0.044(3) Uani 1 1 d . . . C35 C -0.4430(10) 0.2267(9) -0.0204(8) 0.060(4) Uani 1 1 d . . . H35A H -0.5271 0.2169 -0.0267 0.072 Uiso 1 1 calc R . . H35B H -0.4198 0.2316 -0.0714 0.072 Uiso 1 1 calc R . . C36 C -0.4129(10) 0.3033(9) 0.0247(6) 0.050(3) Uani 1 1 d . . . H36A H -0.4674 0.3473 0.0066 0.060 Uiso 1 1 calc R . . H36B H -0.4153 0.2939 0.0793 0.060 Uiso 1 1 calc R . . C37 C -0.2477(15) 0.3850(7) 0.0621(9) 0.067(4) Uani 1 1 d . . . H37A H -0.2617 0.3759 0.1149 0.080 Uiso 1 1 calc R . . H37B H -0.2789 0.4388 0.0454 0.080 Uiso 1 1 calc R . . C38 C -0.1092(12) 0.3814(8) 0.0581(11) 0.079(6) Uani 1 1 d D . . H38A H -0.0807 0.3250 0.0635 0.095 Uiso 1 1 calc R . 1 H38B H -0.0926 0.4034 0.0093 0.095 Uiso 1 1 calc R . 1 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 0.065(5) 0.041(4) 0.089(6) -0.013(4) -0.018(4) 0.013(3) F2 0.039(4) 0.047(4) 0.083(5) -0.014(4) 0.030(4) -0.011(3) F3 0.064(5) 0.137(8) 0.037(4) -0.010(4) 0.010(3) -0.056(5) F4 0.074(5) 0.027(3) 0.066(5) 0.006(3) 0.047(4) 0.009(3) F5 0.054(4) 0.029(3) 0.051(4) 0.009(3) 0.011(3) 0.013(3) F6 0.054(4) 0.052(4) 0.059(4) -0.019(3) 0.007(3) 0.004(3) O1 0.026(3) 0.043(4) 0.041(4) 0.014(3) 0.011(3) 0.003(3) O2 0.035(4) 0.086(6) 0.025(4) 0.001(4) 0.010(3) 0.030(4) N1 0.022(4) 0.036(5) 0.037(5) 0.005(4) 0.005(3) 0.007(3) B1 0.034(6) 0.039(7) 0.026(6) 0.007(5) 0.007(5) 0.009(5) C1 0.029(5) 0.055(7) 0.042(6) 0.030(6) 0.014(4) 0.008(5) C2 0.033(6) 0.083(10) 0.070(9) 0.036(8) 0.008(6) 0.012(6) C3 0.025(7) 0.157(18) 0.134(17) 0.127(16) 0.042(9) 0.034(9) C4 0.062(11) 0.20(2) 0.088(13) 0.105(16) 0.057(10) 0.080(13) C5 0.063(9) 0.132(14) 0.041(7) 0.041(8) 0.035(7) 0.058(9) C6 0.044(7) 0.082(9) 0.037(6) 0.034(7) 0.016(5) 0.034(6) C7 0.022(5) 0.042(6) 0.057(7) 0.000(5) 0.001(5) 0.004(4) C8 0.035(6) 0.033(6) 0.076(9) -0.005(6) -0.003(5) -0.002(5) C9 0.028(5) 0.068(8) 0.044(7) 0.019(6) 0.001(5) -0.020(5) C10 0.039(6) 0.061(8) 0.041(6) 0.015(6) 0.001(5) 0.001(5) C11 0.039(6) 0.051(7) 0.039(6) 0.010(5) 0.007(5) 0.006(5) C12 0.034(6) 0.041(6) 0.053(7) -0.007(5) 0.006(5) -0.015(4) C13 0.033(5) 0.045(6) 0.026(5) 0.005(4) 0.014(4) 0.009(4) C14 0.031(5) 0.048(6) 0.021(5) 0.002(4) 0.005(4) 0.012(4) C15 0.034(5) 0.028(5) 0.025(5) 0.008(4) 0.007(4) 0.016(4) C16 0.026(5) 0.040(6) 0.034(5) 0.016(4) 0.008(4) 0.003(4) C17 0.028(5) 0.035(5) 0.029(5) 0.006(4) 0.011(4) 0.008(4) C18 0.037(5) 0.040(6) 0.030(5) 0.003(4) 0.007(4) 0.008(4) C19 0.036(5) 0.041(6) 0.029(5) 0.006(4) -0.001(4) 0.013(4) C20 0.037(6) 0.030(5) 0.044(6) 0.009(5) 0.017(5) 0.009(4) O3 0.041(4) 0.072(6) 0.042(5) 0.010(4) 0.006(4) -0.002(4) O4 0.033(4) 0.059(5) 0.036(4) 0.005(4) 0.002(3) -0.008(3) O5 0.051(5) 0.058(5) 0.033(4) 0.007(4) -0.006(3) -0.017(4) O6 0.032(4) 0.047(4) 0.045(4) -0.018(4) -0.001(3) 0.011(3) O7A 0.058(12) 0.13(2) 0.058(16) -0.005(15) 0.002(13) -0.003(13) C21A 0.07(2) 0.09(2) 0.09(2) -0.04(2) 0.023(17) 0.032(17) O7B 0.09(2) 0.20(3) 0.059(18) 0.04(2) 0.006(17) 0.033(19) C21B 0.14(4) 0.12(4) 0.12(4) 0.07(3) 0.08(3) 0.08(3) C22 0.053(8) 0.073(10) 0.079(10) 0.013(8) 0.016(7) 0.011(7) C23 0.051(7) 0.061(8) 0.039(6) 0.008(6) 0.014(5) 0.002(6) C24 0.040(6) 0.076(9) 0.039(6) 0.016(6) 0.009(5) -0.019(6) C25 0.023(5) 0.060(7) 0.031(5) 0.003(5) 0.008(4) -0.012(4) C26 0.026(5) 0.076(8) 0.023(5) 0.004(5) 0.011(4) -0.008(5) C27 0.020(5) 0.065(7) 0.030(5) 0.002(5) 0.007(4) -0.009(5) C28 0.035(6) 0.070(8) 0.036(6) 0.014(6) 0.005(5) -0.016(5) C29 0.036(6) 0.061(8) 0.028(5) -0.004(5) 0.003(4) -0.013(5) C30 0.035(6) 0.067(8) 0.036(6) 0.015(6) 0.012(5) -0.005(5) C31 0.028(5) 0.076(9) 0.032(6) 0.001(6) 0.006(4) -0.005(5) C32 0.026(6) 0.103(11) 0.030(6) 0.007(7) 0.000(4) -0.004(6) C33 0.026(5) 0.085(9) 0.029(6) 0.004(6) -0.001(4) -0.007(5) C34 0.031(5) 0.068(8) 0.034(6) 0.007(6) 0.007(4) -0.014(5) C35 0.030(6) 0.094(11) 0.053(8) 0.033(8) -0.004(5) -0.010(6) C36 0.043(6) 0.079(9) 0.029(6) 0.019(6) 0.011(5) 0.019(6) C37 0.112(12) 0.025(6) 0.059(8) -0.017(6) 0.001(8) 0.002(7) C38 0.049(8) 0.038(7) 0.145(16) -0.055(9) -0.001(8) 0.015(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 C19 1.356(13) . ? F2 C19 1.358(12) . ? F3 C19 1.327(12) . ? F4 C20 1.374(11) . ? F5 C20 1.335(12) . ? F6 C20 1.323(13) . ? O1 C1 1.370(12) . ? O1 B1 1.455(14) . ? O2 C6 1.375(16) . ? O2 B1 1.489(13) . ? N1 C7 1.328(13) . ? N1 C11 1.362(14) . ? N1 B1 1.641(14) . ? B1 C13 1.594(14) . ? C1 C6 1.379(19) . ? C1 C2 1.393(18) . ? C2 C3 1.46(2) . ? C2 H2 0.9500 . ? C3 C4 1.33(3) . ? C3 H3 0.9500 . ? C4 C5 1.45(3) . ? C4 H4 0.9500 . ? C5 C6 1.394(16) . ? C5 H5 0.9500 . ? C7 C8 1.413(17) . ? C7 H7 0.9500 . ? C8 C9 1.386(18) . ? C8 H8 0.9500 . ? C9 C10 1.371(19) . ? C9 C12 1.493(17) . ? C10 C11 1.355(16) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C12 1.31(2) 3 ? C12 H12 0.9500 . ? C13 C14 1.396(15) . ? C13 C18 1.418(14) . ? C14 C15 1.412(14) . ? C14 H14 0.9500 . ? C15 C16 1.391(14) . ? C15 C19 1.518(15) . ? C16 C17 1.383(15) . ? C16 H16 0.9500 . ? C17 C18 1.418(14) . ? C17 C20 1.487(14) . ? C18 H18 0.9500 . ? O3 C23 1.397(14) . ? O3 C22 1.441(18) . ? O4 C25 1.394(14) . ? O4 C24 1.442(15) . ? O5 C34 1.401(15) . ? O5 C35 1.418(15) . ? O6 C36 1.365(14) . ? O6 C37 1.447(15) . ? O7A C38 1.389(17) . ? O7A C21A 1.41(4) 3 ? C21A O7A 1.41(4) 3 ? C21A C22 1.513(18) . ? C21A H21A 0.9900 . ? C21A H21B 0.9900 . ? O7B C21B 1.28(5) 3 ? O7B C38 1.410(19) . ? C21B O7B 1.28(5) 3 ? C21B C22 1.489(18) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.482(18) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.368(15) . ? C25 C26 1.427(16) . ? C26 C27 1.430(17) . ? C26 C31 1.436(15) . ? C27 C34 1.426(17) . ? C27 C28 1.423(16) . ? C28 C29 1.339(17) . ? C28 H28 0.9500 . ? C29 C30 1.427(17) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.358(18) . ? C31 H31 0.9500 . ? C32 C33 1.436(19) . ? C32 H32 0.9500 . ? C33 C34 1.336(15) . ? C33 H33 0.9500 . ? C35 C36 1.51(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.64(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? 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 106.4(9) . . ? C6 O2 B1 105.5(9) . . ? C7 N1 C11 116.8(10) . . ? C7 N1 B1 125.5(9) . . ? C11 N1 B1 117.6(9) . . ? O1 B1 O2 105.4(9) . . ? O1 B1 C13 114.8(9) . . ? O2 B1 C13 115.6(9) . . ? O1 B1 N1 106.7(8) . . ? O2 B1 N1 104.7(8) . . ? C13 B1 N1 109.0(8) . . ? O1 C1 C6 110.8(10) . . ? O1 C1 C2 126.6(12) . . ? C6 C1 C2 122.6(11) . . ? C1 C2 C3 114.9(17) . . ? C1 C2 H2 122.6 . . ? C3 C2 H2 122.6 . . ? C4 C3 C2 123.7(18) . . ? C4 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? C3 C4 C5 119.7(13) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 117.5(17) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? O2 C6 C1 110.2(9) . . ? O2 C6 C5 128.2(15) . . ? C1 C6 C5 121.5(14) . . ? N1 C7 C8 120.9(11) . . ? N1 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 120.1(12) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 118.7(11) . . ? C10 C9 C12 117.2(11) . . ? C8 C9 C12 124.1(12) . . ? C11 C10 C9 117.7(12) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? N1 C11 C10 125.8(11) . . ? N1 C11 H11 117.1 . . ? C10 C11 H11 117.1 . . ? C12 C12 C9 122.2(15) 3 . ? C12 C12 H12 118.9 3 . ? C9 C12 H12 118.9 . . ? C14 C13 C18 118.3(9) . . ? C14 C13 B1 121.3(9) . . ? C18 C13 B1 120.3(10) . . ? C13 C14 C15 119.6(9) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 121.7(9) . . ? C16 C15 C19 121.2(8) . . ? C14 C15 C19 117.1(9) . . ? C17 C16 C15 119.6(9) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 119.4(9) . . ? C16 C17 C20 118.7(9) . . ? C18 C17 C20 121.9(9) . . ? C13 C18 C17 121.3(10) . . ? C13 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? F3 C19 F2 105.9(9) . . ? F3 C19 F1 107.3(10) . . ? F2 C19 F1 103.2(9) . . ? F3 C19 C15 113.0(9) . . ? F2 C19 C15 112.6(8) . . ? F1 C19 C15 114.0(8) . . ? F6 C20 F5 108.8(9) . . ? F6 C20 F4 105.6(9) . . ? F5 C20 F4 105.2(8) . . ? F6 C20 C17 113.0(8) . . ? F5 C20 C17 112.8(9) . . ? F4 C20 C17 110.9(8) . . ? C23 O3 C22 112.3(10) . . ? C25 O4 C24 118.8(8) . . ? C34 O5 C35 119.7(9) . . ? C36 O6 C37 115.1(10) . . ? C38 O7A C21A 107(2) . 3 ? O7A C21A C22 120(3) 3 . ? O7A C21A H21A 107.4 3 . ? C22 C21A H21A 107.4 . . ? O7A C21A H21B 107.4 3 . ? C22 C21A H21B 107.4 . . ? H21A C21A H21B 106.9 . . ? C21B O7B C38 110(4) 3 . ? O7B C21B C22 116(3) 3 . ? O7B C21B H21C 108.3 3 . ? C22 C21B H21C 108.3 . . ? O7B C21B H21D 108.3 3 . ? C22 C21B H21D 108.3 . . ? H21C C21B H21D 107.4 . . ? O3 C22 C21B 110(3) . . ? O3 C22 C21A 115.9(17) . . ? C21B C22 C21A 74(2) . . ? O3 C22 H22A 108.3 . . ? C21B C22 H22A 135.1 . . ? C21A C22 H22A 108.3 . . ? O3 C22 H22B 108.3 . . ? C21B C22 H22B 37.7 . . ? C21A C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? O3 C23 C24 109.6(10) . . ? O3 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? O3 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? O4 C24 C23 108.2(10) . . ? O4 C24 H24A 110.1 . . ? C23 C24 H24A 110.1 . . ? O4 C24 H24B 110.1 . . ? C23 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? C30 C25 O4 123.6(11) . . ? C30 C25 C26 121.3(11) . . ? O4 C25 C26 115.2(9) . . ? C25 C26 C27 117.8(9) . . ? C25 C26 C31 122.4(12) . . ? C27 C26 C31 119.8(11) . . ? C34 C27 C28 123.2(12) . . ? C34 C27 C26 117.5(10) . . ? C28 C27 C26 119.2(11) . . ? C29 C28 C27 121.2(12) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 120.8(10) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C25 C30 C29 119.7(11) . . ? C25 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C26 119.5(13) . . ? C32 C31 H31 120.2 . . ? C26 C31 H31 120.2 . . ? C31 C32 C33 120.8(11) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 120.1(12) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 O5 124.6(12) . . ? C33 C34 C27 122.2(13) . . ? O5 C34 C27 113.1(9) . . ? O5 C35 C36 107.7(10) . . ? O5 C35 H35A 110.2 . . ? C36 C35 H35A 110.2 . . ? O5 C35 H35B 110.2 . . ? C36 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? O6 C36 C35 105.2(9) . . ? O6 C36 H36A 110.7 . . ? C35 C36 H36A 110.7 . . ? O6 C36 H36B 110.7 . . ? C35 C36 H36B 110.7 . . ? H36A C36 H36B 108.8 . . ? O6 C37 C38 108.2(10) . . ? O6 C37 H37A 110.1 . . ? C38 C37 H37A 110.1 . . ? O6 C37 H37B 110.1 . . ? C38 C37 H37B 110.1 . . ? H37A C37 H37B 108.4 . . ? O7A C38 O7B 33.0(12) . . ? O7A C38 C37 105.4(15) . . ? O7B C38 C37 116.0(18) . . ? O7A C38 H38A 110.7 . . ? O7B C38 H38A 126.6 . . ? C37 C38 H38A 110.7 . . ? O7A C38 H38B 110.7 . . ? O7B C38 H38B 77.8 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? 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 C1 O1 B1 O2 -12.4(10) . . . . ? C1 O1 B1 C13 -140.7(9) . . . . ? C1 O1 B1 N1 98.5(8) . . . . ? C6 O2 B1 O1 12.1(10) . . . . ? C6 O2 B1 C13 140.0(9) . . . . ? C6 O2 B1 N1 -100.2(9) . . . . ? C7 N1 B1 O1 -115.2(10) . . . . ? C11 N1 B1 O1 62.5(11) . . . . ? C7 N1 B1 O2 -3.8(13) . . . . ? C11 N1 B1 O2 173.9(9) . . . . ? C7 N1 B1 C13 120.4(10) . . . . ? C11 N1 B1 C13 -62.0(12) . . . . ? B1 O1 C1 C6 8.4(11) . . . . ? B1 O1 C1 C2 -173.4(10) . . . . ? O1 C1 C2 C3 -178.0(10) . . . . ? C6 C1 C2 C3 0.1(16) . . . . ? C1 C2 C3 C4 0(2) . . . . ? C2 C3 C4 C5 -3(2) . . . . ? C3 C4 C5 C6 4(2) . . . . ? B1 O2 C6 C1 -7.4(11) . . . . ? B1 O2 C6 C5 171.7(11) . . . . ? O1 C1 C6 O2 -0.5(12) . . . . ? C2 C1 C6 O2 -178.8(10) . . . . ? O1 C1 C6 C5 -179.7(10) . . . . ? C2 C1 C6 C5 2.0(17) . . . . ? C4 C5 C6 O2 176.8(11) . . . . ? C4 C5 C6 C1 -4.1(17) . . . . ? C11 N1 C7 C8 0.3(14) . . . . ? B1 N1 C7 C8 177.9(9) . . . . ? N1 C7 C8 C9 -3.0(16) . . . . ? C7 C8 C9 C10 3.3(16) . . . . ? C7 C8 C9 C12 -176.1(9) . . . . ? C8 C9 C10 C11 -1.1(16) . . . . ? C12 C9 C10 C11 178.4(10) . . . . ? C7 N1 C11 C10 2.2(17) . . . . ? B1 N1 C11 C10 -175.6(11) . . . . ? C9 C10 C11 N1 -1.8(18) . . . . ? C10 C9 C12 C12 -167.3(13) . . . 3 ? C8 C9 C12 C12 12.2(19) . . . 3 ? O1 B1 C13 C14 174.9(9) . . . . ? O2 B1 C13 C14 51.8(14) . . . . ? N1 B1 C13 C14 -65.6(12) . . . . ? O1 B1 C13 C18 -7.9(13) . . . . ? O2 B1 C13 C18 -130.9(10) . . . . ? N1 B1 C13 C18 111.6(10) . . . . ? C18 C13 C14 C15 1.1(14) . . . . ? B1 C13 C14 C15 178.4(9) . . . . ? C13 C14 C15 C16 -1.0(14) . . . . ? C13 C14 C15 C19 177.5(9) . . . . ? C14 C15 C16 C17 0.5(14) . . . . ? C19 C15 C16 C17 -178.1(9) . . . . ? C15 C16 C17 C18 0.0(14) . . . . ? C15 C16 C17 C20 -179.7(8) . . . . ? C14 C13 C18 C17 -0.7(14) . . . . ? B1 C13 C18 C17 -178.0(9) . . . . ? C16 C17 C18 C13 0.1(14) . . . . ? C20 C17 C18 C13 179.8(9) . . . . ? C16 C15 C19 F3 109.6(11) . . . . ? C14 C15 C19 F3 -69.0(12) . . . . ? C16 C15 C19 F2 -10.4(13) . . . . ? C14 C15 C19 F2 171.0(9) . . . . ? C16 C15 C19 F1 -127.5(10) . . . . ? C14 C15 C19 F1 53.9(12) . . . . ? C16 C17 C20 F6 166.6(9) . . . . ? C18 C17 C20 F6 -13.1(14) . . . . ? C16 C17 C20 F5 -69.5(12) . . . . ? C18 C17 C20 F5 110.8(11) . . . . ? C16 C17 C20 F4 48.2(13) . . . . ? C18 C17 C20 F4 -131.4(10) . . . . ? C23 O3 C22 C21B -92(2) . . . . ? C23 O3 C22 C21A -173.8(17) . . . . ? O7B C21B C22 O3 -97(4) 3 . . . ? O7B C21B C22 C21A 16(4) 3 . . . ? O7A C21A C22 O3 86(3) 3 . . . ? O7A C21A C22 C21B -19(4) 3 . . . ? C22 O3 C23 C24 179.8(10) . . . . ? C25 O4 C24 C23 176.0(8) . . . . ? O3 C23 C24 O4 72.2(12) . . . . ? C24 O4 C25 C30 -2.0(13) . . . . ? C24 O4 C25 C26 179.0(8) . . . . ? C30 C25 C26 C27 2.8(13) . . . . ? O4 C25 C26 C27 -178.2(8) . . . . ? C30 C25 C26 C31 -176.3(9) . . . . ? O4 C25 C26 C31 2.7(13) . . . . ? C25 C26 C27 C34 -178.8(8) . . . . ? C31 C26 C27 C34 0.2(13) . . . . ? C25 C26 C27 C28 -2.3(13) . . . . ? C31 C26 C27 C28 176.8(9) . . . . ? C34 C27 C28 C29 177.1(10) . . . . ? C26 C27 C28 C29 0.8(15) . . . . ? C27 C28 C29 C30 0.4(16) . . . . ? O4 C25 C30 C29 179.4(9) . . . . ? C26 C25 C30 C29 -1.7(14) . . . . ? C28 C29 C30 C25 0.0(15) . . . . ? C25 C26 C31 C32 179.0(9) . . . . ? C27 C26 C31 C32 0.0(14) . . . . ? C26 C31 C32 C33 1.0(16) . . . . ? C31 C32 C33 C34 -2.3(16) . . . . ? C32 C33 C34 O5 178.6(9) . . . . ? C32 C33 C34 C27 2.5(16) . . . . ? C35 O5 C34 C33 6.3(15) . . . . ? C35 O5 C34 C27 -177.2(9) . . . . ? C28 C27 C34 C33 -177.9(10) . . . . ? C26 C27 C34 C33 -1.5(14) . . . . ? C28 C27 C34 O5 5.6(13) . . . . ? C26 C27 C34 O5 -178.0(8) . . . . ? C34 O5 C35 C36 -171.5(9) . . . . ? C37 O6 C36 C35 -168.5(10) . . . . ? O5 C35 C36 O6 75.5(11) . . . . ? C36 O6 C37 C38 163.5(12) . . . . ? C21A O7A C38 O7B -93(4) 3 . . . ? C21A O7A C38 C37 152(2) 3 . . . ? C21B O7B C38 O7A 125(5) 3 . . . ? C21B O7B C38 C37 -157(2) 3 . . . ? O6 C37 C38 O7A -167(2) . . . . ? O6 C37 C38 O7B 160(2) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.720 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.142 #===END data_rotaxane_2 _database_code_depnum_ccdc_archive 'CCDC 683420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H24 B2 F12 N2 O4, C28 H40 O10, 3(C7 H8)' _chemical_formula_sum 'C89 H88 B2 F12 N2 O14' _chemical_formula_weight 1659.23 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 13.4013(9) _cell_length_b 14.5562(10) _cell_length_c 22.3107(17) _cell_angle_alpha 96.487(6) _cell_angle_beta 107.062(6) _cell_angle_gamma 92.798(6) _cell_volume 4118.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 2987 _cell_measurement_theta_min 2.5924 _cell_measurement_theta_max 27.5764 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_T_min 0.80453 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 8.2812 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26573 _diffrn_reflns_av_R_equivalents 0.1597 _diffrn_reflns_av_sigmaI/netI 0.2857 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 22.98 _reflns_number_total 11389 _reflns_number_gt 3936 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _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^)+(0.1917P)^2^+7.1509P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11389 _refine_ls_number_parameters 1141 _refine_ls_number_restraints 804 _refine_ls_R_factor_all 0.3203 _refine_ls_R_factor_gt 0.1543 _refine_ls_wR_factor_ref 0.4318 _refine_ls_wR_factor_gt 0.3282 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.037 _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 -0.2330(9) 0.5310(8) -0.1716(4) 0.131(5) Uani 1 1 d DU . . F2 F -0.1083(8) 0.5247(8) -0.2112(5) 0.111(4) Uani 1 1 d DU . . F3 F -0.2273(7) 0.6110(7) -0.2449(4) 0.089(3) Uani 1 1 d DU . . F4A F -0.1409(17) 0.9429(14) -0.1621(7) 0.092(6) Uani 0.519(12) 1 d PDU A 1 F5A F 0.0090(10) 0.9744(10) -0.0899(9) 0.067(5) Uani 0.519(12) 1 d PDU A 1 F6A F -0.1253(13) 0.9568(11) -0.0644(8) 0.058(5) Uani 0.519(12) 1 d PDU A 1 F4B F -0.1877(11) 0.9199(13) -0.1434(9) 0.068(6) Uani 0.481(12) 1 d PDU A 2 F5B F -0.0410(14) 0.9417(12) -0.1573(9) 0.064(5) Uani 0.481(12) 1 d PDU A 2 F6B F -0.0570(19) 0.9764(15) -0.0640(8) 0.100(6) Uani 0.481(12) 1 d PDU A 2 F7 F 0.5398(9) 0.5631(7) 0.6932(5) 0.107(4) Uani 1 1 d DU . . F8 F 0.5785(9) 0.6816(9) 0.7614(5) 0.123(4) Uani 1 1 d DU . . F9 F 0.4254(8) 0.6564(8) 0.7016(5) 0.101(3) Uani 1 1 d DU . . F10 F 0.6590(10) 0.9957(9) 0.6873(6) 0.157(5) Uani 1 1 d DU . . F11 F 0.4945(9) 0.9886(8) 0.6533(7) 0.147(5) Uani 1 1 d DU . . F12 F 0.5868(11) 1.0081(8) 0.5914(6) 0.140(5) Uani 1 1 d DU . . O1 O 0.1321(6) 0.7572(6) 0.0740(4) 0.030(2) Uani 1 1 d . . . O2 O 0.0327(5) 0.6124(5) 0.0534(4) 0.025(2) Uani 1 1 d . . . O3 O 0.4821(7) 0.5950(7) 0.4555(5) 0.049(3) Uani 1 1 d . . . O4 O 0.5570(7) 0.7362(7) 0.4411(4) 0.059(3) Uani 1 1 d . . . O5 O 0.5190(6) 0.7227(5) 0.1644(4) 0.026(2) Uani 1 1 d . . . O6 O 0.6924(6) 0.3864(6) 0.1676(3) 0.026(2) Uani 1 1 d . . . O7 O 0.7588(6) 0.2248(5) 0.1159(4) 0.025(2) Uani 1 1 d . . . O8 O 0.7168(6) 0.0953(5) 0.0050(4) 0.024(2) Uani 1 1 d . . . O9 O 0.6108(6) 0.1442(6) -0.1163(4) 0.028(2) Uani 1 1 d . . . O10 O 0.9894(7) 0.2868(6) 0.3376(4) 0.037(2) Uani 1 1 d . . . O11 O 0.8237(6) 0.6277(6) 0.3263(4) 0.035(2) Uani 1 1 d . . . O12 O 0.7520(6) 0.7908(6) 0.3748(4) 0.034(2) Uani 1 1 d . . . O13 O 0.7892(6) 0.9078(6) 0.4924(4) 0.031(2) Uani 1 1 d . . . O14 O 0.8901(6) 0.8516(6) 0.6115(4) 0.032(2) Uani 1 1 d . . . N1 N 0.1906(7) 0.6220(6) 0.0164(4) 0.017(2) Uani 1 1 d U . . N2 N 0.6781(7) 0.6196(7) 0.4931(6) 0.035(3) Uani 1 1 d . . . B1 B 0.0932(10) 0.6772(11) 0.0282(7) 0.027(4) Uani 1 1 d . . . B2 B 0.5698(13) 0.6731(12) 0.4858(8) 0.042(5) Uani 1 1 d . . . C1 C 0.0914(8) 0.7464(9) 0.1236(5) 0.022(3) Uani 1 1 d U . . C2 C 0.0992(9) 0.8068(9) 0.1756(5) 0.025(3) Uani 1 1 d U . . H2 H 0.1394 0.8649 0.1834 0.029 Uiso 1 1 calc R . . C3 C 0.0475(10) 0.7821(10) 0.2167(6) 0.038(3) Uani 1 1 d U . . H3 H 0.0522 0.8236 0.2537 0.045 Uiso 1 1 calc R . . C4 C -0.0127(11) 0.6956(11) 0.2051(6) 0.047(3) Uani 1 1 d U . . H4 H -0.0483 0.6798 0.2341 0.057 Uiso 1 1 calc R . . C5 C -0.0203(9) 0.6325(10) 0.1503(6) 0.037(3) Uani 1 1 d U . . H5 H -0.0603 0.5743 0.1418 0.045 Uiso 1 1 calc R . . C6 C 0.0325(9) 0.6590(9) 0.1099(5) 0.023(3) Uani 1 1 d U . . C7 C 0.1902(9) 0.5300(9) 0.0129(6) 0.030(3) Uani 1 1 d U . . H7 H 0.1296 0.4959 0.0154 0.036 Uiso 1 1 calc R . . C8 C 0.2725(9) 0.4817(9) 0.0060(5) 0.025(3) Uani 1 1 d U . . H8 H 0.2679 0.4159 0.0021 0.030 Uiso 1 1 calc R . . C9 C 0.3631(8) 0.5319(8) 0.0048(5) 0.015(2) Uani 1 1 d U . . C10 C 0.3619(9) 0.6257(8) 0.0071(5) 0.020(2) Uani 1 1 d U . . H10 H 0.4217 0.6614 0.0049 0.024 Uiso 1 1 calc R . . C11 C 0.2764(9) 0.6700(8) 0.0125(5) 0.020(3) Uani 1 1 d U . . H11 H 0.2778 0.7355 0.0136 0.025 Uiso 1 1 calc R . . C12 C 0.4542(8) 0.4803(8) 0.0013(5) 0.019(3) Uani 1 1 d U . . H12 H 0.4476 0.4149 0.0007 0.022 Uiso 1 1 calc R . . C13 C 0.0222(9) 0.7047(9) -0.0395(6) 0.025(3) Uani 1 1 d U . . C14 C -0.0388(9) 0.6360(9) -0.0877(6) 0.029(3) Uani 1 1 d U . . H14 H -0.0318 0.5724 -0.0828 0.035 Uiso 1 1 calc R . . C15 C -0.1072(9) 0.6585(10) -0.1409(6) 0.035(3) Uani 1 1 d U . . C16 C -0.1242(10) 0.7503(11) -0.1495(7) 0.042(3) Uani 1 1 d U . . H16 H -0.1747 0.7651 -0.1862 0.050 Uiso 1 1 calc R . . C17 C -0.0653(10) 0.8194(10) -0.1030(7) 0.041(3) Uani 1 1 d U A . C18 C 0.0046(9) 0.7939(9) -0.0502(6) 0.030(3) Uani 1 1 d U . . H18 H 0.0439 0.8422 -0.0186 0.036 Uiso 1 1 calc R . . C19 C -0.1704(12) 0.5839(12) -0.1913(7) 0.068(4) Uani 1 1 d DU . . C20 C -0.0837(10) 0.9190(10) -0.1121(7) 0.061(3) Uani 1 1 d DU . . C21 C 0.4253(12) 0.6318(10) 0.4057(7) 0.044(3) Uani 1 1 d U . . C22 C 0.3206(12) 0.5881(11) 0.3659(7) 0.056(3) Uani 1 1 d U . . H22 H 0.2901 0.5323 0.3739 0.067 Uiso 1 1 calc R . . C23 C 0.2714(13) 0.6348(11) 0.3167(8) 0.059(4) Uani 1 1 d U . . H23 H 0.2078 0.6072 0.2868 0.070 Uiso 1 1 calc R . . C24 C 0.3120(13) 0.7218(11) 0.3092(8) 0.060(4) Uani 1 1 d U . . H24 H 0.2738 0.7541 0.2763 0.072 Uiso 1 1 calc R . . C25 C 0.4079(11) 0.7608(10) 0.3497(7) 0.046(3) Uani 1 1 d U . . H25 H 0.4362 0.8206 0.3466 0.055 Uiso 1 1 calc R . . C26 C 0.4604(13) 0.7077(11) 0.3950(7) 0.051(3) Uani 1 1 d U . . C27 C 0.7659(10) 0.6666(9) 0.4937(6) 0.033(3) Uani 1 1 d U . . H27 H 0.7652 0.7312 0.4908 0.039 Uiso 1 1 calc R . . C28 C 0.8584(9) 0.6255(9) 0.4985(5) 0.027(3) Uani 1 1 d U . . H28 H 0.9202 0.6627 0.5011 0.032 Uiso 1 1 calc R . . C29 C 0.8618(9) 0.5317(9) 0.4996(5) 0.021(2) Uani 1 1 d U . . C30 C 0.7697(9) 0.4823(10) 0.4996(6) 0.032(3) Uani 1 1 d U . . H30 H 0.7678 0.4173 0.5012 0.039 Uiso 1 1 calc R . . C31 C 0.6816(10) 0.5288(10) 0.4974(6) 0.038(3) Uani 1 1 d U . . H31 H 0.6204 0.4946 0.4990 0.045 Uiso 1 1 calc R . . C32 C 0.9552(8) 0.4818(8) 0.5016(5) 0.018(3) Uani 1 1 d U . . H32 H 0.9503 0.4175 0.5055 0.021 Uiso 1 1 calc R . . C33 C 0.5820(13) 0.7149(12) 0.5548(8) 0.060(3) Uani 1 1 d U . . C34 C 0.5557(11) 0.6640(12) 0.5996(7) 0.054(3) Uani 1 1 d U . . H34 H 0.5434 0.5985 0.5893 0.064 Uiso 1 1 calc R . . C35 C 0.5469(13) 0.7013(13) 0.6547(9) 0.071(3) Uani 1 1 d U . . C36 C 0.5632(13) 0.7981(13) 0.6714(9) 0.072(4) Uani 1 1 d U . . H36 H 0.5673 0.8250 0.7130 0.087 Uiso 1 1 calc R . . C37 C 0.5732(14) 0.8536(13) 0.6269(10) 0.081(4) Uani 1 1 d U . . C38 C 0.5837(13) 0.8074(12) 0.5669(8) 0.070(4) Uani 1 1 d U . . H38 H 0.5920 0.8444 0.5359 0.084 Uiso 1 1 calc R . . C39 C 0.5209(12) 0.6542(12) 0.7012(8) 0.078(4) Uani 1 1 d DU . . C40 C 0.5809(14) 0.9605(14) 0.6383(9) 0.110(5) Uani 1 1 d DU . . C41 C 0.4206(8) 0.7288(9) 0.1750(6) 0.027(3) Uani 1 1 d . . . H41A H 0.4228 0.7074 0.2159 0.032 Uiso 1 1 calc R . . H41B H 0.3660 0.6891 0.1409 0.032 Uiso 1 1 calc R . . C42 C 0.5558(9) 0.6363(9) 0.1638(5) 0.022(3) Uani 1 1 d U . . C43 C 0.5049(9) 0.5573(8) 0.1700(5) 0.020(3) Uani 1 1 d U . . H43 H 0.4365 0.5587 0.1743 0.024 Uiso 1 1 calc R . . C44 C 0.5524(9) 0.4724(9) 0.1702(5) 0.026(3) Uani 1 1 d U . . H44 H 0.5157 0.4170 0.1740 0.031 Uiso 1 1 calc R . . C45 C 0.6514(9) 0.4706(9) 0.1648(5) 0.024(3) Uani 1 1 d U . . C46 C 0.7047(9) 0.5517(8) 0.1595(5) 0.023(3) Uani 1 1 d U . . H46 H 0.7743 0.5508 0.1571 0.027 Uiso 1 1 calc R . . C47 C 0.6577(9) 0.6335(9) 0.1575(5) 0.026(3) Uani 1 1 d U . . H47 H 0.6936 0.6882 0.1520 0.031 Uiso 1 1 calc R . . C48 C 0.7971(9) 0.3817(9) 0.1648(6) 0.028(3) Uani 1 1 d U . . H48A H 0.8459 0.4243 0.2001 0.034 Uiso 1 1 calc R . . H48B H 0.8023 0.4004 0.1244 0.034 Uiso 1 1 calc R . . C49 C 0.8252(8) 0.2833(8) 0.1696(6) 0.024(3) Uani 1 1 d U . . H49A H 0.8994 0.2791 0.1712 0.029 Uiso 1 1 calc R . . H49B H 0.8159 0.2635 0.2088 0.029 Uiso 1 1 calc R . . C50 C 0.7856(9) 0.1332(8) 0.1184(6) 0.026(3) Uani 1 1 d U . . H50A H 0.7819 0.1132 0.1587 0.032 Uiso 1 1 calc R . . H50B H 0.8583 0.1295 0.1167 0.032 Uiso 1 1 calc R . . C51 C 0.7120(9) 0.0703(9) 0.0639(6) 0.028(3) Uani 1 1 d U . . H51A H 0.7303 0.0055 0.0669 0.034 Uiso 1 1 calc R . . H51B H 0.6396 0.0734 0.0662 0.034 Uiso 1 1 calc R . . C52 C 0.6578(10) 0.0300(8) -0.0470(5) 0.026(3) Uani 1 1 d U . . H52A H 0.5836 0.0240 -0.0477 0.031 Uiso 1 1 calc R . . H52B H 0.6856 -0.0315 -0.0434 0.031 Uiso 1 1 calc R . . C53 C 0.6662(9) 0.0636(8) -0.1053(5) 0.024(3) Uani 1 1 d U . . H53A H 0.7409 0.0786 -0.1014 0.029 Uiso 1 1 calc R . . H53B H 0.6369 0.0143 -0.1416 0.029 Uiso 1 1 calc R . . C54 C 0.6036(9) 0.1741(9) -0.1758(6) 0.029(3) Uani 1 1 d . . . H54A H 0.5480 0.1347 -0.2095 0.035 Uiso 1 1 calc R . . H54B H 0.6708 0.1675 -0.1853 0.035 Uiso 1 1 calc R . . C55 C 1.0908(10) 0.2748(10) 0.3303(6) 0.035(4) Uani 1 1 d . . . H55A H 1.1450 0.3133 0.3653 0.042 Uiso 1 1 calc R . . H55B H 1.0939 0.2948 0.2899 0.042 Uiso 1 1 calc R . . C56 C 0.9527(9) 0.3754(9) 0.3369(5) 0.025(3) Uani 1 1 d U . . C57 C 1.0092(10) 0.4544(9) 0.3329(5) 0.027(3) Uani 1 1 d U . . H57 H 1.0794 0.4517 0.3320 0.032 Uiso 1 1 calc R . . C58 C 0.9643(9) 0.5376(9) 0.3302(5) 0.024(3) Uani 1 1 d U . . H58 H 1.0047 0.5920 0.3282 0.029 Uiso 1 1 calc R . . C59 C 0.8622(9) 0.5437(9) 0.3303(5) 0.022(3) Uani 1 1 d U . . C60 C 0.8065(9) 0.4624(9) 0.3337(5) 0.026(3) Uani 1 1 d U . . H60 H 0.7362 0.4642 0.3346 0.031 Uiso 1 1 calc R . . C61 C 0.8513(9) 0.3799(9) 0.3356(5) 0.030(3) Uani 1 1 d U . . H61 H 0.8106 0.3249 0.3361 0.036 Uiso 1 1 calc R . . C62 C 0.7195(10) 0.6328(9) 0.3259(6) 0.034(3) Uani 1 1 d U . . H62A H 0.7106 0.6133 0.3652 0.041 Uiso 1 1 calc R . . H62B H 0.6726 0.5908 0.2895 0.041 Uiso 1 1 calc R . . C63 C 0.6915(10) 0.7323(9) 0.3211(6) 0.034(3) Uani 1 1 d U . . H63A H 0.7040 0.7527 0.2829 0.041 Uiso 1 1 calc R . . H63B H 0.6162 0.7357 0.3171 0.041 Uiso 1 1 calc R . . C64 C 0.7101(10) 0.8765(8) 0.3811(6) 0.029(3) Uani 1 1 d U . . H64A H 0.6418 0.8670 0.3891 0.035 Uiso 1 1 calc R . . H64B H 0.6982 0.9040 0.3412 0.035 Uiso 1 1 calc R . . C65 C 0.7829(10) 0.9415(8) 0.4343(5) 0.026(3) Uani 1 1 d U . . H65A H 0.8533 0.9465 0.4285 0.031 Uiso 1 1 calc R . . H65B H 0.7569 1.0040 0.4348 0.031 Uiso 1 1 calc R . . C66 C 0.8578(10) 0.9696(10) 0.5428(5) 0.037(3) Uani 1 1 d U . . H66A H 0.8370 1.0337 0.5404 0.044 Uiso 1 1 calc R . . H66B H 0.9306 0.9686 0.5407 0.044 Uiso 1 1 calc R . . C67 C 0.8505(11) 0.9372(10) 0.6045(6) 0.043(3) Uani 1 1 d U . . H67A H 0.8904 0.9833 0.6408 0.051 Uiso 1 1 calc R . . H67B H 0.7763 0.9327 0.6041 0.051 Uiso 1 1 calc R . . C68 C 0.8898(11) 0.8222(9) 0.6691(7) 0.042(4) Uani 1 1 d . . . H68A H 0.8212 0.8314 0.6761 0.051 Uiso 1 1 calc R . . H68B H 0.9445 0.8602 0.7041 0.051 Uiso 1 1 calc R . . C69 C 0.2813(10) 0.2013(9) -0.0240(6) 0.034(3) Uani 1 1 d U . . C70 C 0.3728(10) 0.1810(8) -0.0387(6) 0.034(3) Uani 1 1 d U . . H70 H 0.3693 0.1567 -0.0807 0.041 Uiso 1 1 calc R . . C71 C 0.4666(11) 0.1960(9) 0.0071(7) 0.037(3) Uani 1 1 d U . . H71 H 0.5287 0.1850 -0.0040 0.045 Uiso 1 1 calc R . . C72 C 0.4744(11) 0.2272(9) 0.0699(7) 0.046(3) Uani 1 1 d U . . H72 H 0.5398 0.2352 0.1023 0.055 Uiso 1 1 calc R . . C73 C 0.3826(12) 0.2455(9) 0.0823(7) 0.045(3) Uani 1 1 d U . . H73 H 0.3847 0.2684 0.1243 0.054 Uiso 1 1 calc R . . C74 C 0.2867(11) 0.2318(9) 0.0356(7) 0.040(3) Uani 1 1 d U . . H74 H 0.2245 0.2443 0.0460 0.048 Uiso 1 1 calc R . . C75 C 0.1779(10) 0.1822(10) -0.0781(7) 0.059(4) Uani 1 1 d U . . H75A H 0.1204 0.1687 -0.0608 0.088 Uiso 1 1 calc R . . H75B H 0.1827 0.1288 -0.1078 0.088 Uiso 1 1 calc R . . H75C H 0.1647 0.2369 -0.1003 0.088 Uiso 1 1 calc R . . C76 C 1.2053(12) 0.7856(10) 0.5155(7) 0.049(3) Uani 1 1 d U . . C77 C 1.1083(11) 0.8046(9) 0.5272(7) 0.044(3) Uani 1 1 d U . . H77 H 1.1035 0.8167 0.5690 0.053 Uiso 1 1 calc R . . C78 C 1.0232(11) 0.8045(9) 0.4755(7) 0.045(3) Uani 1 1 d U . . H78 H 0.9579 0.8152 0.4824 0.054 Uiso 1 1 calc R . . C79 C 1.0255(12) 0.7897(10) 0.4133(7) 0.053(3) Uani 1 1 d U . . H79 H 0.9644 0.7926 0.3789 0.063 Uiso 1 1 calc R . . C80 C 1.1164(12) 0.7713(10) 0.4034(7) 0.052(3) Uani 1 1 d U . . H80 H 1.1196 0.7579 0.3614 0.062 Uiso 1 1 calc R . . C81 C 1.2076(11) 0.7714(9) 0.4549(6) 0.040(3) Uani 1 1 d U . . H81 H 1.2723 0.7613 0.4469 0.048 Uiso 1 1 calc R . . C82 C 1.3037(13) 0.7832(11) 0.5705(8) 0.067(5) Uani 1 1 d U . . H82A H 1.3653 0.7865 0.5554 0.100 Uiso 1 1 calc R . . H82B H 1.3001 0.7254 0.5887 0.100 Uiso 1 1 calc R . . H82C H 1.3091 0.8362 0.6029 0.100 Uiso 1 1 calc R . . C83A C 0.7844(9) 0.0064(10) 0.2624(7) 0.053(3) Uani 0.694(12) 1 d PGU B 1 C84A C 0.7031(12) -0.0475(8) 0.2165(7) 0.049(4) Uani 0.694(12) 1 d PGU B 1 H84A H 0.7105 -0.1108 0.2044 0.059 Uiso 0.694(12) 1 calc PR B 1 C85A C 0.6110(10) -0.0086(10) 0.1883(6) 0.049(4) Uani 0.694(12) 1 d PGU B 1 H85A H 0.5554 -0.0454 0.1569 0.058 Uiso 0.694(12) 1 calc PR B 1 C86A C 0.6002(10) 0.0841(11) 0.2060(7) 0.054(4) Uani 0.694(12) 1 d PGU B 1 H86A H 0.5372 0.1107 0.1867 0.064 Uiso 0.694(12) 1 calc PR B 1 C87A C 0.6815(12) 0.1380(8) 0.2520(7) 0.054(4) Uani 0.694(12) 1 d PGU B 1 H87A H 0.6741 0.2014 0.2641 0.065 Uiso 0.694(12) 1 calc PR B 1 C88A C 0.7736(10) 0.0992(10) 0.2802(6) 0.052(4) Uani 0.694(12) 1 d PGU B 1 H88A H 0.8291 0.1360 0.3116 0.063 Uiso 0.694(12) 1 calc PR B 1 C89A C 0.8846(19) -0.0306(18) 0.2915(12) 0.068(6) Uani 0.694(12) 1 d PU B 1 H89A H 0.8729 -0.0975 0.2919 0.102 Uiso 0.694(12) 1 calc PR B 1 H89B H 0.9148 0.0003 0.3350 0.102 Uiso 0.694(12) 1 calc PR B 1 H89C H 0.9328 -0.0194 0.2670 0.102 Uiso 0.694(12) 1 calc PR B 1 C83B C 0.681(2) 0.039(2) 0.2368(16) 0.052(3) Uani 0.306(12) 1 d PGU B 2 C84B C 0.682(2) -0.053(2) 0.2115(14) 0.051(4) Uani 0.306(12) 1 d PGU B 2 H84B H 0.6212 -0.0832 0.1806 0.061 Uiso 0.306(12) 1 calc PR B 2 C85B C 0.771(3) -0.0995(19) 0.2316(16) 0.053(4) Uani 0.306(12) 1 d PGU B 2 H85B H 0.7715 -0.1621 0.2143 0.064 Uiso 0.306(12) 1 calc PR B 2 C86B C 0.860(2) -0.055(2) 0.2768(17) 0.056(5) Uani 0.306(12) 1 d PGU B 2 H86B H 0.9210 -0.0867 0.2905 0.067 Uiso 0.306(12) 1 calc PR B 2 C87B C 0.860(2) 0.037(2) 0.3021(15) 0.054(4) Uani 0.306(12) 1 d PGU B 2 H87B H 0.9203 0.0677 0.3330 0.065 Uiso 0.306(12) 1 calc PR B 2 C88B C 0.770(3) 0.0840(19) 0.2820(16) 0.053(4) Uani 0.306(12) 1 d PGU B 2 H88B H 0.7700 0.1466 0.2993 0.063 Uiso 0.306(12) 1 calc PR B 2 C89B C 0.585(4) 0.081(4) 0.212(3) 0.058(7) Uani 0.306(12) 1 d PU B 2 H89D H 0.5539 0.0573 0.1672 0.087 Uiso 0.306(12) 1 calc PR B 2 H89E H 0.5999 0.1487 0.2169 0.087 Uiso 0.306(12) 1 calc PR B 2 H89F H 0.5364 0.0661 0.2355 0.087 Uiso 0.306(12) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.162(10) 0.146(10) 0.050(6) -0.004(6) 0.005(7) -0.120(8) F2 0.117(9) 0.107(9) 0.070(7) -0.038(7) -0.012(7) -0.002(7) F3 0.065(6) 0.110(8) 0.062(6) 0.016(6) -0.026(5) -0.022(6) F4A 0.108(12) 0.065(10) 0.098(11) 0.052(9) 0.008(10) 0.010(10) F5A 0.060(9) 0.023(8) 0.132(11) 0.020(8) 0.044(9) 0.027(7) F6A 0.044(10) 0.028(9) 0.118(11) 0.022(8) 0.039(9) 0.020(8) F4B 0.071(11) 0.055(11) 0.092(11) 0.062(9) 0.023(9) 0.028(9) F5B 0.068(10) 0.041(9) 0.107(10) 0.040(8) 0.049(9) 0.027(8) F6B 0.098(13) 0.049(10) 0.132(12) 0.008(10) 0.005(12) 0.012(11) F7 0.169(10) 0.082(8) 0.092(7) 0.016(7) 0.075(7) 0.006(8) F8 0.142(10) 0.154(11) 0.072(7) -0.004(8) 0.043(7) -0.023(9) F9 0.085(7) 0.116(9) 0.126(8) 0.041(7) 0.060(7) 0.014(7) F10 0.162(11) 0.114(10) 0.169(12) -0.075(9) 0.051(10) -0.045(9) F11 0.121(9) 0.077(8) 0.257(13) -0.030(9) 0.094(9) 0.040(7) F12 0.215(12) 0.061(8) 0.149(11) 0.007(8) 0.065(10) 0.018(8) O1 0.038(5) 0.022(5) 0.037(5) 0.001(4) 0.021(5) 0.005(4) O2 0.018(4) 0.025(5) 0.034(5) 0.000(4) 0.014(4) -0.012(4) O3 0.047(6) 0.042(6) 0.067(7) 0.008(6) 0.032(6) -0.006(5) O4 0.047(6) 0.068(8) 0.043(6) 0.024(6) -0.017(5) -0.023(6) O5 0.025(5) 0.015(5) 0.038(5) 0.005(4) 0.009(4) 0.006(4) O6 0.025(5) 0.031(6) 0.022(5) 0.000(4) 0.009(4) 0.006(4) O7 0.034(5) 0.013(5) 0.026(5) -0.003(4) 0.005(4) 0.012(4) O8 0.039(5) 0.011(5) 0.022(5) -0.003(4) 0.014(4) -0.007(4) O9 0.035(5) 0.026(5) 0.027(5) 0.004(4) 0.016(4) 0.008(4) O10 0.039(6) 0.035(6) 0.042(6) 0.008(5) 0.022(5) 0.004(5) O11 0.026(5) 0.035(6) 0.037(6) -0.006(5) 0.005(4) -0.002(5) O12 0.031(5) 0.039(6) 0.017(5) -0.017(4) -0.006(4) -0.009(5) O13 0.040(5) 0.029(5) 0.015(5) -0.001(4) 0.000(4) -0.009(5) O14 0.048(6) 0.023(5) 0.031(5) 0.011(4) 0.018(5) 0.013(5) N1 0.013(5) 0.014(5) 0.027(5) 0.004(4) 0.011(4) -0.008(4) N2 0.015(6) 0.010(6) 0.087(9) 0.015(6) 0.023(6) -0.002(5) B1 0.016(8) 0.033(10) 0.026(9) -0.007(8) 0.002(7) -0.016(7) B2 0.043(11) 0.037(11) 0.058(12) 0.011(10) 0.035(10) -0.008(9) C1 0.013(5) 0.029(6) 0.023(5) 0.005(5) 0.005(5) -0.007(5) C2 0.024(5) 0.038(6) 0.012(5) -0.005(5) 0.008(5) 0.000(5) C3 0.042(6) 0.056(7) 0.016(5) -0.004(5) 0.014(5) 0.010(6) C4 0.047(6) 0.067(7) 0.028(6) 0.005(6) 0.012(5) 0.004(6) C5 0.028(6) 0.056(7) 0.029(6) 0.011(5) 0.010(5) -0.002(6) C6 0.015(5) 0.035(6) 0.020(5) 0.005(5) 0.010(5) -0.003(5) C7 0.022(6) 0.028(7) 0.047(7) 0.011(6) 0.019(6) 0.004(6) C8 0.021(5) 0.021(6) 0.039(6) 0.003(5) 0.017(5) 0.003(5) C9 0.017(5) 0.021(5) 0.013(4) 0.006(4) 0.012(4) 0.006(4) C10 0.028(5) 0.022(5) 0.019(5) 0.004(5) 0.022(4) 0.002(5) C11 0.027(5) 0.016(5) 0.022(5) -0.012(5) 0.019(5) -0.004(5) C12 0.028(5) 0.011(5) 0.022(5) 0.012(4) 0.012(4) 0.001(4) C13 0.020(5) 0.027(6) 0.037(6) 0.007(5) 0.021(5) 0.003(5) C14 0.022(6) 0.028(6) 0.043(6) 0.006(5) 0.019(5) -0.003(5) C15 0.021(5) 0.050(6) 0.040(6) 0.005(5) 0.020(5) 0.001(5) C16 0.032(6) 0.057(7) 0.046(6) 0.023(6) 0.020(5) 0.014(6) C17 0.032(5) 0.050(6) 0.058(6) 0.024(5) 0.031(5) 0.011(5) C18 0.026(5) 0.033(6) 0.047(6) 0.014(5) 0.031(5) 0.011(5) C19 0.054(7) 0.086(8) 0.050(7) 0.006(7) 0.001(6) -0.009(7) C20 0.052(7) 0.053(6) 0.087(7) 0.029(6) 0.029(6) 0.013(6) C21 0.070(7) 0.039(7) 0.039(7) 0.023(6) 0.031(6) 0.023(6) C22 0.069(7) 0.046(7) 0.061(7) 0.012(6) 0.028(6) 0.024(6) C23 0.067(7) 0.046(7) 0.065(7) 0.013(6) 0.019(6) 0.011(6) C24 0.067(7) 0.049(7) 0.068(7) 0.014(6) 0.019(6) 0.020(7) C25 0.056(7) 0.030(7) 0.053(7) 0.018(6) 0.011(6) 0.015(6) C26 0.072(7) 0.040(7) 0.048(7) 0.014(6) 0.023(6) 0.016(6) C27 0.034(7) 0.012(6) 0.050(7) 0.005(6) 0.010(6) 0.001(6) C28 0.030(6) 0.021(6) 0.033(6) 0.005(5) 0.015(5) 0.001(5) C29 0.021(5) 0.027(5) 0.021(5) 0.009(4) 0.013(4) 0.004(4) C30 0.026(6) 0.033(6) 0.039(6) 0.000(5) 0.014(5) -0.006(5) C31 0.026(6) 0.039(8) 0.050(7) -0.002(6) 0.021(6) -0.018(6) C32 0.023(6) 0.017(6) 0.018(6) 0.009(5) 0.010(5) 0.010(5) C33 0.071(7) 0.057(7) 0.074(7) 0.030(7) 0.046(6) 0.030(7) C34 0.052(6) 0.058(7) 0.073(7) 0.037(6) 0.039(6) 0.032(6) C35 0.071(6) 0.071(7) 0.084(7) 0.024(7) 0.035(6) 0.019(6) C36 0.078(7) 0.064(8) 0.083(8) -0.003(7) 0.039(7) 0.013(7) C37 0.090(7) 0.057(7) 0.102(8) -0.002(7) 0.045(7) 0.004(7) C38 0.086(7) 0.058(7) 0.084(8) 0.010(7) 0.053(7) -0.006(7) C39 0.082(8) 0.085(8) 0.086(8) 0.030(7) 0.052(7) -0.005(8) C40 0.120(9) 0.065(8) 0.142(9) -0.024(8) 0.050(8) 0.016(8) C41 0.015(7) 0.033(9) 0.041(8) 0.006(7) 0.020(6) 0.004(6) C42 0.032(6) 0.021(6) 0.017(5) 0.006(5) 0.012(5) -0.003(5) C43 0.028(6) 0.024(6) 0.012(5) -0.004(5) 0.015(5) -0.003(5) C44 0.035(6) 0.033(6) 0.014(5) -0.001(5) 0.017(5) 0.000(5) C45 0.029(6) 0.020(6) 0.020(5) -0.007(5) 0.007(5) -0.003(5) C46 0.023(6) 0.020(6) 0.029(5) -0.002(5) 0.016(5) -0.004(5) C47 0.032(6) 0.020(6) 0.027(5) 0.005(5) 0.013(5) -0.005(5) C48 0.017(6) 0.032(7) 0.036(7) 0.004(6) 0.011(5) 0.010(6) C49 0.009(6) 0.033(7) 0.033(7) 0.008(6) 0.008(5) 0.005(5) C50 0.022(6) 0.023(7) 0.038(7) 0.011(6) 0.011(5) 0.009(5) C51 0.022(6) 0.020(7) 0.047(7) 0.012(6) 0.014(6) 0.000(5) C52 0.036(6) 0.017(6) 0.029(6) -0.003(5) 0.020(6) 0.006(6) C53 0.031(6) 0.022(7) 0.026(6) 0.000(5) 0.018(5) 0.002(6) C54 0.021(7) 0.041(9) 0.031(8) -0.004(7) 0.018(6) 0.015(7) C55 0.039(9) 0.044(10) 0.032(8) 0.017(7) 0.021(7) 0.005(8) C56 0.028(6) 0.022(6) 0.024(5) 0.004(5) 0.006(5) 0.002(5) C57 0.031(6) 0.027(6) 0.020(5) 0.001(5) 0.005(5) -0.002(5) C58 0.030(6) 0.022(6) 0.018(5) 0.005(5) 0.006(5) -0.005(5) C59 0.029(6) 0.019(6) 0.013(5) -0.002(5) 0.001(5) 0.003(5) C60 0.026(6) 0.029(6) 0.017(5) -0.009(5) 0.003(5) 0.001(5) C61 0.030(6) 0.025(6) 0.028(6) -0.004(5) 0.003(5) -0.009(5) C62 0.032(7) 0.041(7) 0.017(6) -0.011(6) -0.004(6) -0.010(6) C63 0.035(7) 0.036(7) 0.019(6) 0.002(6) -0.009(6) -0.008(6) C64 0.043(7) 0.004(6) 0.040(7) 0.004(5) 0.015(6) 0.001(5) C65 0.035(7) 0.011(6) 0.033(7) 0.001(5) 0.013(6) 0.004(5) C66 0.042(7) 0.038(8) 0.022(7) -0.003(6) 0.001(6) -0.007(6) C67 0.041(7) 0.041(8) 0.034(7) -0.012(6) 0.001(6) -0.012(7) C68 0.050(10) 0.033(10) 0.056(10) 0.027(8) 0.024(8) 0.011(8) C69 0.039(6) 0.020(6) 0.042(6) 0.011(5) 0.012(5) -0.004(5) C70 0.047(6) 0.013(6) 0.045(6) 0.007(5) 0.017(5) 0.004(5) C71 0.036(6) 0.018(6) 0.061(7) 0.019(6) 0.016(6) -0.002(5) C72 0.045(6) 0.025(6) 0.059(7) 0.011(6) 0.001(6) -0.011(6) C73 0.066(7) 0.027(6) 0.041(7) 0.004(6) 0.019(6) -0.004(6) C74 0.047(6) 0.034(6) 0.048(6) 0.010(6) 0.028(6) 0.001(6) C75 0.039(8) 0.043(9) 0.083(11) 0.021(8) -0.002(8) -0.004(8) C76 0.053(6) 0.033(6) 0.060(7) -0.001(6) 0.023(6) -0.008(6) C77 0.050(7) 0.028(6) 0.059(7) 0.000(6) 0.028(6) -0.005(6) C78 0.046(6) 0.023(6) 0.062(7) -0.005(6) 0.020(6) -0.015(6) C79 0.053(7) 0.036(7) 0.058(7) -0.015(6) 0.010(6) -0.012(6) C80 0.054(7) 0.046(7) 0.050(7) -0.008(6) 0.014(6) -0.012(6) C81 0.046(6) 0.036(6) 0.045(7) 0.000(6) 0.028(6) -0.006(6) C82 0.083(11) 0.044(10) 0.076(11) 0.004(9) 0.030(9) 0.011(9) C83A 0.059(7) 0.068(7) 0.032(6) 0.004(6) 0.018(5) -0.020(6) C84A 0.057(7) 0.065(8) 0.027(6) 0.001(6) 0.018(6) -0.022(6) C85A 0.056(7) 0.064(8) 0.027(6) 0.000(6) 0.020(6) -0.018(7) C86A 0.057(8) 0.074(8) 0.032(7) -0.001(6) 0.023(6) -0.017(7) C87A 0.058(7) 0.070(8) 0.035(6) -0.008(6) 0.023(6) -0.018(7) C88A 0.057(7) 0.067(8) 0.032(6) -0.002(6) 0.020(5) -0.021(6) C89A 0.069(11) 0.079(12) 0.046(10) 0.009(10) 0.007(9) -0.021(10) C83B 0.058(7) 0.068(7) 0.031(6) 0.000(6) 0.020(5) -0.019(6) C84B 0.057(7) 0.066(8) 0.028(7) 0.001(6) 0.019(6) -0.021(7) C85B 0.060(8) 0.068(9) 0.032(7) 0.001(7) 0.021(7) -0.019(7) C86B 0.061(9) 0.070(9) 0.035(8) 0.004(8) 0.018(7) -0.018(8) C87B 0.059(8) 0.069(9) 0.033(7) 0.002(7) 0.018(7) -0.020(7) C88B 0.058(7) 0.068(8) 0.032(7) -0.001(6) 0.021(6) -0.021(7) C89B 0.058(11) 0.078(12) 0.037(11) -0.002(10) 0.021(10) -0.014(11) _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 C19 1.311(14) . ? F2 C19 1.354(14) . ? F3 C19 1.331(13) . ? F4A C20 1.251(15) . ? F5A C20 1.376(15) . ? F6A C20 1.411(15) . ? F4B C20 1.365(15) . ? F5B C20 1.361(15) . ? F6B C20 1.234(15) . ? F7 C39 1.364(15) . ? F8 C39 1.342(15) . ? F9 C39 1.285(14) . ? F10 C40 1.305(16) . ? F11 C40 1.364(16) . ? F12 C40 1.338(16) . ? O1 C1 1.390(13) . ? O1 B1 1.426(16) . ? O2 C6 1.363(13) . ? O2 B1 1.475(15) . ? O3 C21 1.333(15) . ? O3 B2 1.538(19) . ? O4 C26 1.406(17) . ? O4 B2 1.411(18) . ? O5 C42 1.374(13) . ? O5 C41 1.411(12) . ? O6 C45 1.367(13) . ? O6 C48 1.428(12) . ? O7 C50 1.400(13) . ? O7 C49 1.422(13) . ? O8 C52 1.418(13) . ? O8 C51 1.422(13) . ? O9 C54 1.423(13) . ? O9 C53 1.425(13) . ? O10 C56 1.402(14) . ? O10 C55 1.431(14) . ? O11 C59 1.353(13) . ? O11 C62 1.400(14) . ? O12 C63 1.397(13) . ? O12 C64 1.402(13) . ? O13 C66 1.416(14) . ? O13 C65 1.417(13) . ? O14 C67 1.386(15) . ? O14 C68 1.402(14) . ? N1 C7 1.332(14) . ? N1 C11 1.346(13) . ? N1 B1 1.636(17) . ? N2 C27 1.327(14) . ? N2 C31 1.339(16) . ? N2 B2 1.654(19) . ? B1 C13 1.636(18) . ? B2 C33 1.55(2) . ? C1 C2 1.349(16) . ? C1 C6 1.416(16) . ? C2 C3 1.370(16) . ? C2 H2 0.9500 . ? C3 C4 1.417(19) . ? C3 H3 0.9500 . ? C4 C5 1.419(18) . ? C4 H4 0.9500 . ? C5 C6 1.374(15) . ? C5 H5 0.9500 . ? C7 C8 1.373(15) . ? C7 H7 0.9500 . ? C8 C9 1.395(15) . ? C8 H8 0.9500 . ? C9 C10 1.362(15) . ? C9 C12 1.481(14) . ? C10 C11 1.370(15) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C12 1.35(2) 2_665 ? C12 H12 0.9500 . ? C13 C18 1.366(16) . ? C13 C14 1.410(16) . ? C14 C15 1.354(16) . ? C14 H14 0.9500 . ? C15 C16 1.391(18) . ? C15 C19 1.495(19) . ? C16 C17 1.384(19) . ? C16 H16 0.9500 . ? C17 C18 1.375(17) . ? C17 C20 1.508(19) . ? C18 H18 0.9500 . ? C21 C26 1.255(19) . ? C21 C22 1.49(2) . ? C22 C23 1.375(19) . ? C22 H22 0.9500 . ? C23 C24 1.40(2) . ? C23 H23 0.9500 . ? C24 C25 1.386(19) . ? C24 H24 0.9500 . ? C25 C26 1.388(18) . ? C25 H25 0.9500 . ? C27 C28 1.384(16) . ? C27 H27 0.9500 . ? C28 C29 1.371(16) . ? C28 H28 0.9500 . ? C29 C30 1.398(16) . ? C29 C32 1.470(14) . ? C30 C31 1.380(16) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C32 1.31(2) 2_766 ? C32 H32 0.9500 . ? C33 C38 1.34(2) . ? C33 C34 1.420(19) . ? C34 C35 1.33(2) . ? C34 H34 0.9500 . ? C35 C36 1.40(2) . ? C35 C39 1.42(2) . ? C36 C37 1.38(2) . ? C36 H36 0.9500 . ? C37 C38 1.48(2) . ? C37 C40 1.54(2) . ? C38 H38 0.9500 . ? C41 C54 1.464(16) 2_665 ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.350(15) . ? C42 C47 1.414(15) . ? C43 C44 1.418(16) . ? C43 H43 0.9500 . ? C44 C45 1.368(15) . ? C44 H44 0.9500 . ? C45 C46 1.384(16) . ? C46 C47 1.372(15) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.506(16) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.499(16) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.472(15) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C41 1.464(16) 2_665 ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C68 1.448(17) 2_766 ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C61 1.356(16) . ? C56 C57 1.371(16) . ? C57 C58 1.378(16) . ? C57 H57 0.9500 . ? C58 C59 1.376(16) . ? C58 H58 0.9500 . ? C59 C60 1.388(16) . ? C60 C61 1.368(16) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.521(17) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.494(16) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.532(17) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C55 1.448(17) 2_766 ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C74 1.333(17) . ? C69 C70 1.394(17) . ? C69 C75 1.536(17) . ? C70 C71 1.357(17) . ? C70 H70 0.9500 . ? C71 C72 1.397(19) . ? C71 H71 0.9500 . ? C72 C73 1.370(19) . ? C72 H72 0.9500 . ? C73 C74 1.386(18) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C81 1.354(18) . ? C76 C77 1.432(18) . ? C76 C82 1.52(2) . ? C77 C78 1.363(18) . ? C77 H77 0.9500 . ? C78 C79 1.389(19) . ? C78 H78 0.9500 . ? C79 C80 1.333(19) . ? C79 H79 0.9500 . ? C80 C81 1.411(18) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83A C84A 1.3900 . ? C83A C88A 1.3900 . ? C83A C89A 1.47(2) . ? C84A C85A 1.3900 . ? C84A H84A 0.9500 . ? C85A C86A 1.3900 . ? C85A H85A 0.9500 . ? C86A C87A 1.3900 . ? C86A H86A 0.9500 . ? C87A C88A 1.3900 . ? C87A H87A 0.9500 . ? C88A H88A 0.9500 . ? C89A H89A 0.9800 . ? C89A H89B 0.9800 . ? C89A H89C 0.9800 . ? C83B C84B 1.3900 . ? C83B C88B 1.3900 . ? C83B C89B 1.44(6) . ? C84B C85B 1.3900 . ? C84B H84B 0.9500 . ? C85B C86B 1.3900 . ? C85B H85B 0.9500 . ? C86B C87B 1.3900 . ? C86B H86B 0.9500 . ? C87B C88B 1.3900 . ? C87B H87B 0.9500 . ? C88B H88B 0.9500 . ? C89B H89D 0.9800 . ? C89B H89E 0.9800 . ? C89B H89F 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 106.5(9) . . ? C6 O2 B1 104.1(9) . . ? C21 O3 B2 100.9(12) . . ? C26 O4 B2 106.1(11) . . ? C42 O5 C41 116.2(9) . . ? C45 O6 C48 117.8(9) . . ? C50 O7 C49 109.7(8) . . ? C52 O8 C51 112.4(9) . . ? C54 O9 C53 113.9(8) . . ? C56 O10 C55 119.1(10) . . ? C59 O11 C62 117.0(10) . . ? C63 O12 C64 111.9(9) . . ? C66 O13 C65 109.4(9) . . ? C67 O14 C68 112.1(10) . . ? C7 N1 C11 117.9(10) . . ? C7 N1 B1 122.1(10) . . ? C11 N1 B1 119.9(9) . . ? C27 N2 C31 117.2(11) . . ? C27 N2 B2 120.0(10) . . ? C31 N2 B2 122.8(10) . . ? O1 B1 O2 109.0(10) . . ? O1 B1 N1 110.1(9) . . ? O2 B1 N1 106.3(10) . . ? O1 B1 C13 111.6(11) . . ? O2 B1 C13 111.2(9) . . ? N1 B1 C13 108.5(10) . . ? O4 B2 O3 105.0(12) . . ? O4 B2 C33 116.5(14) . . ? O3 B2 C33 116.7(12) . . ? O4 B2 N2 111.9(11) . . ? O3 B2 N2 103.4(11) . . ? C33 B2 N2 102.7(12) . . ? C2 C1 O1 128.8(11) . . ? C2 C1 C6 123.0(11) . . ? O1 C1 C6 108.2(10) . . ? C1 C2 C3 118.1(12) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C2 C3 C4 121.1(13) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 120.3(13) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 117.4(13) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? O2 C6 C5 127.8(11) . . ? O2 C6 C1 112.0(10) . . ? C5 C6 C1 120.1(12) . . ? N1 C7 C8 123.7(11) . . ? N1 C7 H7 118.2 . . ? C8 C7 H7 118.2 . . ? C7 C8 C9 118.3(11) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C10 C9 C8 117.5(11) . . ? C10 C9 C12 124.3(10) . . ? C8 C9 C12 118.2(10) . . ? C9 C10 C11 121.6(11) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? N1 C11 C10 121.0(11) . . ? N1 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C12 C12 C9 124.5(13) 2_665 . ? C12 C12 H12 117.8 2_665 . ? C9 C12 H12 117.8 . . ? C18 C13 C14 114.9(12) . . ? C18 C13 B1 123.5(12) . . ? C14 C13 B1 120.9(11) . . ? C15 C14 C13 121.5(13) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 121.8(14) . . ? C14 C15 C19 120.2(13) . . ? C16 C15 C19 118.0(13) . . ? C17 C16 C15 118.0(13) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C18 C17 C16 118.5(14) . . ? C18 C17 C20 123.3(14) . . ? C16 C17 C20 118.2(13) . . ? C13 C18 C17 125.3(14) . . ? C13 C18 H18 117.4 . . ? C17 C18 H18 117.4 . . ? F1 C19 F3 107.4(12) . . ? F1 C19 F2 104.5(13) . . ? F3 C19 F2 102.7(12) . . ? F1 C19 C15 113.0(12) . . ? F3 C19 C15 116.7(13) . . ? F2 C19 C15 111.4(12) . . ? F6B C20 F4A 118.3(19) . . ? F6B C20 F5B 112.8(15) . . ? F4A C20 F5B 60.2(12) . . ? F6B C20 F4B 111.1(15) . . ? F4A C20 F4B 40.8(10) . . ? F5B C20 F4B 100.4(12) . . ? F6B C20 F5A 53.9(12) . . ? F4A C20 F5A 110.9(14) . . ? F5B C20 F5A 64.9(11) . . ? F4B C20 F5A 142.7(15) . . ? F6B C20 F6A 41.1(11) . . ? F4A C20 F6A 104.8(14) . . ? F5B C20 F6A 143.2(15) . . ? F4B C20 F6A 76.7(12) . . ? F5A C20 F6A 95.0(12) . . ? F6B C20 C17 116.7(16) . . ? F4A C20 C17 123.6(16) . . ? F5B C20 C17 108.1(12) . . ? F4B C20 C17 106.5(13) . . ? F5A C20 C17 110.6(12) . . ? F6A C20 C17 107.8(12) . . ? C26 C21 O3 117.9(16) . . ? C26 C21 C22 120.2(14) . . ? O3 C21 C22 121.8(13) . . ? C23 C22 C21 114.9(15) . . ? C23 C22 H22 122.5 . . ? C21 C22 H22 122.5 . . ? C22 C23 C24 122.0(17) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C25 C24 C23 120.1(15) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 116.3(15) . . ? C24 C25 H25 121.8 . . ? C26 C25 H25 121.8 . . ? C21 C26 C25 126.0(16) . . ? C21 C26 O4 109.0(13) . . ? C25 C26 O4 124.6(14) . . ? N2 C27 C28 122.8(12) . . ? N2 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C29 C28 C27 120.7(12) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 116.5(11) . . ? C28 C29 C32 124.3(11) . . ? C30 C29 C32 119.2(11) . . ? C31 C30 C29 119.4(12) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? N2 C31 C30 123.3(12) . . ? N2 C31 H31 118.4 . . ? C30 C31 H31 118.4 . . ? C32 C32 C29 125.7(14) 2_766 . ? C32 C32 H32 117.1 2_766 . ? C29 C32 H32 117.1 . . ? C38 C33 C34 115.5(16) . . ? C38 C33 B2 117.2(15) . . ? C34 C33 B2 123.7(16) . . ? C35 C34 C33 124.8(17) . . ? C35 C34 H34 117.6 . . ? C33 C34 H34 117.6 . . ? C34 C35 C36 119.4(18) . . ? C34 C35 C39 127.4(18) . . ? C36 C35 C39 113.2(17) . . ? C37 C36 C35 119.4(18) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 117.6(17) . . ? C36 C37 C40 123.5(18) . . ? C38 C37 C40 118.8(17) . . ? C33 C38 C37 122.0(17) . . ? C33 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? F9 C39 F8 104.9(13) . . ? F9 C39 F7 107.2(13) . . ? F8 C39 F7 101.9(13) . . ? F9 C39 C35 115.3(15) . . ? F8 C39 C35 116.3(15) . . ? F7 C39 C35 110.1(14) . . ? F10 C40 F12 105.7(15) . . ? F10 C40 F11 104.0(14) . . ? F12 C40 F11 104.7(15) . . ? F10 C40 C37 112.9(16) . . ? F12 C40 C37 119.0(16) . . ? F11 C40 C37 109.3(15) . . ? O5 C41 C54 108.1(10) . 2_665 ? O5 C41 H41A 110.1 . . ? C54 C41 H41A 110.1 2_665 . ? O5 C41 H41B 110.1 . . ? C54 C41 H41B 110.1 2_665 . ? H41A C41 H41B 108.4 . . ? C43 C42 O5 125.9(11) . . ? C43 C42 C47 119.1(12) . . ? O5 C42 C47 114.9(10) . . ? C42 C43 C44 120.6(11) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C45 C44 C43 119.7(12) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? O6 C45 C44 115.6(11) . . ? O6 C45 C46 124.5(11) . . ? C44 C45 C46 119.8(12) . . ? C47 C46 C45 120.5(11) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C42 120.1(11) . . ? C46 C47 H47 119.9 . . ? C42 C47 H47 119.9 . . ? O6 C48 C49 108.2(10) . . ? O6 C48 H48A 110.1 . . ? C49 C48 H48A 110.1 . . ? O6 C48 H48B 110.1 . . ? C49 C48 H48B 110.1 . . ? H48A C48 H48B 108.4 . . ? O7 C49 C48 108.7(9) . . ? O7 C49 H49A 109.9 . . ? C48 C49 H49A 109.9 . . ? O7 C49 H49B 109.9 . . ? C48 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? O7 C50 C51 110.0(9) . . ? O7 C50 H50A 109.7 . . ? C51 C50 H50A 109.7 . . ? O7 C50 H50B 109.7 . . ? C51 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? O8 C51 C50 111.4(10) . . ? O8 C51 H51A 109.3 . . ? C50 C51 H51A 109.3 . . ? O8 C51 H51B 109.3 . . ? C50 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? O8 C52 C53 107.8(10) . . ? O8 C52 H52A 110.1 . . ? C53 C52 H52A 110.1 . . ? O8 C52 H52B 110.1 . . ? C53 C52 H52B 110.1 . . ? H52A C52 H52B 108.5 . . ? O9 C53 C52 110.4(9) . . ? O9 C53 H53A 109.6 . . ? C52 C53 H53A 109.6 . . ? O9 C53 H53B 109.6 . . ? C52 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? O9 C54 C41 110.2(10) . 2_665 ? O9 C54 H54A 109.6 . . ? C41 C54 H54A 109.6 2_665 . ? O9 C54 H54B 109.6 . . ? C41 C54 H54B 109.6 2_665 . ? H54A C54 H54B 108.1 . . ? O10 C55 C68 109.0(11) . 2_766 ? O10 C55 H55A 109.9 . . ? C68 C55 H55A 109.9 2_766 . ? O10 C55 H55B 109.9 . . ? C68 C55 H55B 109.9 2_766 . ? H55A C55 H55B 108.3 . . ? C61 C56 C57 119.0(12) . . ? C61 C56 O10 116.1(11) . . ? C57 C56 O10 124.8(11) . . ? C56 C57 C58 120.2(12) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C59 C58 C57 121.4(12) . . ? C59 C58 H58 119.3 . . ? C57 C58 H58 119.3 . . ? O11 C59 C58 117.6(11) . . ? O11 C59 C60 125.2(11) . . ? C58 C59 C60 117.2(12) . . ? C61 C60 C59 121.0(12) . . ? C61 C60 H60 119.5 . . ? C59 C60 H60 119.5 . . ? C56 C61 C60 121.2(12) . . ? C56 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? O11 C62 C63 109.0(11) . . ? O11 C62 H62A 109.9 . . ? C63 C62 H62A 109.9 . . ? O11 C62 H62B 109.9 . . ? C63 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? O12 C63 C62 110.1(9) . . ? O12 C63 H63A 109.6 . . ? C62 C63 H63A 109.6 . . ? O12 C63 H63B 109.6 . . ? C62 C63 H63B 109.6 . . ? H63A C63 H63B 108.2 . . ? O12 C64 C65 110.6(10) . . ? O12 C64 H64A 109.5 . . ? C65 C64 H64A 109.5 . . ? O12 C64 H64B 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 108.1 . . ? O13 C65 C64 109.5(10) . . ? O13 C65 H65A 109.8 . . ? C64 C65 H65A 109.8 . . ? O13 C65 H65B 109.8 . . ? C64 C65 H65B 109.8 . . ? H65A C65 H65B 108.2 . . ? O13 C66 C67 107.2(10) . . ? O13 C66 H66A 110.3 . . ? C67 C66 H66A 110.3 . . ? O13 C66 H66B 110.3 . . ? C67 C66 H66B 110.3 . . ? H66A C66 H66B 108.5 . . ? O14 C67 C66 110.7(11) . . ? O14 C67 H67A 109.5 . . ? C66 C67 H67A 109.5 . . ? O14 C67 H67B 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 108.1 . . ? O14 C68 C55 111.1(12) . 2_766 ? O14 C68 H68A 109.4 . . ? C55 C68 H68A 109.4 2_766 . ? O14 C68 H68B 109.4 . . ? C55 C68 H68B 109.4 2_766 . ? H68A C68 H68B 108.0 . . ? C74 C69 C70 119.4(13) . . ? C74 C69 C75 123.5(13) . . ? C70 C69 C75 117.1(13) . . ? C71 C70 C69 119.9(13) . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C70 C71 C72 121.8(14) . . ? C70 C71 H71 119.1 . . ? C72 C71 H71 119.1 . . ? C73 C72 C71 116.3(14) . . ? C73 C72 H72 121.9 . . ? C71 C72 H72 121.9 . . ? C72 C73 C74 122.2(14) . . ? C72 C73 H73 118.9 . . ? C74 C73 H73 118.9 . . ? C69 C74 C73 120.4(14) . . ? C69 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C69 C75 H75A 109.5 . . ? C69 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C69 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C81 C76 C77 118.8(15) . . ? C81 C76 C82 121.1(14) . . ? C77 C76 C82 120.1(14) . . ? C78 C77 C76 116.7(14) . . ? C78 C77 H77 121.6 . . ? C76 C77 H77 121.6 . . ? C77 C78 C79 124.5(15) . . ? C77 C78 H78 117.8 . . ? C79 C78 H78 117.8 . . ? C80 C79 C78 117.8(15) . . ? C80 C79 H79 121.1 . . ? C78 C79 H79 121.1 . . ? C79 C80 C81 120.5(15) . . ? C79 C80 H80 119.7 . . ? C81 C80 H80 119.7 . . ? C76 C81 C80 121.6(14) . . ? C76 C81 H81 119.2 . . ? C80 C81 H81 119.2 . . ? C76 C82 H82A 109.5 . . ? C76 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C76 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84A C83A C88A 120.0 . . ? C84A C83A C89A 121.8(14) . . ? C88A C83A C89A 118.1(14) . . ? C85A C84A C83A 120.0 . . ? C85A C84A H84A 120.0 . . ? C83A C84A H84A 120.0 . . ? C84A C85A C86A 120.0 . . ? C84A C85A H85A 120.0 . . ? C86A C85A H85A 120.0 . . ? C85A C86A C87A 120.0 . . ? C85A C86A H86A 120.0 . . ? C87A C86A H86A 120.0 . . ? C88A C87A C86A 120.0 . . ? C88A C87A H87A 120.0 . . ? C86A C87A H87A 120.0 . . ? C87A C88A C83A 120.0 . . ? C87A C88A H88A 120.0 . . ? C83A C88A H88A 120.0 . . ? C83A C89A H89A 109.5 . . ? C83A C89A H89B 109.5 . . ? H89A C89A H89B 109.5 . . ? C83A C89A H89C 109.5 . . ? H89A C89A H89C 109.5 . . ? H89B C89A H89C 109.5 . . ? C84B C83B C88B 120.0 . . ? C84B C83B C89B 115(3) . . ? C88B C83B C89B 125(3) . . ? C85B C84B C83B 120.0 . . ? C85B C84B H84B 120.0 . . ? C83B C84B H84B 120.0 . . ? C86B C85B C84B 120.0 . . ? C86B C85B H85B 120.0 . . ? C84B C85B H85B 120.0 . . ? C85B C86B C87B 120.0 . . ? C85B C86B H86B 120.0 . . ? C87B C86B H86B 120.0 . . ? C88B C87B C86B 120.0 . . ? C88B C87B H87B 120.0 . . ? C86B C87B H87B 120.0 . . ? C87B C88B C83B 120.0 . . ? C87B C88B H88B 120.0 . . ? C83B C88B H88B 120.0 . . ? C83B C89B H89D 109.5 . . ? C83B C89B H89E 109.5 . . ? H89D C89B H89E 109.5 . . ? C83B C89B H89F 109.5 . . ? H89D C89B H89F 109.5 . . ? H89E C89B H89F 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 C1 O1 B1 O2 -4.2(12) . . . . ? C1 O1 B1 N1 -120.4(10) . . . . ? C1 O1 B1 C13 119.0(10) . . . . ? C6 O2 B1 O1 4.0(12) . . . . ? C6 O2 B1 N1 122.6(9) . . . . ? C6 O2 B1 C13 -119.5(11) . . . . ? C7 N1 B1 O1 135.8(11) . . . . ? C11 N1 B1 O1 -41.4(14) . . . . ? C7 N1 B1 O2 17.9(15) . . . . ? C11 N1 B1 O2 -159.3(9) . . . . ? C7 N1 B1 C13 -101.8(12) . . . . ? C11 N1 B1 C13 81.0(12) . . . . ? C26 O4 B2 O3 10.1(15) . . . . ? C26 O4 B2 C33 -120.8(14) . . . . ? C26 O4 B2 N2 121.5(13) . . . . ? C21 O3 B2 O4 -9.7(14) . . . . ? C21 O3 B2 C33 121.0(14) . . . . ? C21 O3 B2 N2 -127.1(11) . . . . ? C27 N2 B2 O4 41.1(18) . . . . ? C31 N2 B2 O4 -137.8(13) . . . . ? C27 N2 B2 O3 153.6(12) . . . . ? C31 N2 B2 O3 -25.3(17) . . . . ? C27 N2 B2 C33 -84.6(15) . . . . ? C31 N2 B2 C33 96.5(15) . . . . ? B1 O1 C1 C2 -174.4(13) . . . . ? B1 O1 C1 C6 2.7(12) . . . . ? O1 C1 C2 C3 176.7(11) . . . . ? C6 C1 C2 C3 -0.1(18) . . . . ? C1 C2 C3 C4 -0.2(18) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 C6 -0.1(19) . . . . ? B1 O2 C6 C5 174.3(12) . . . . ? B1 O2 C6 C1 -2.3(12) . . . . ? C4 C5 C6 O2 -176.6(12) . . . . ? C4 C5 C6 C1 -0.1(17) . . . . ? C2 C1 C6 O2 177.2(10) . . . . ? O1 C1 C6 O2 -0.2(13) . . . . ? C2 C1 C6 C5 0.2(18) . . . . ? O1 C1 C6 C5 -177.1(10) . . . . ? C11 N1 C7 C8 0.4(18) . . . . ? B1 N1 C7 C8 -176.9(11) . . . . ? N1 C7 C8 C9 2.4(18) . . . . ? C7 C8 C9 C10 -3.5(17) . . . . ? C7 C8 C9 C12 176.3(10) . . . . ? C8 C9 C10 C11 2.1(17) . . . . ? C12 C9 C10 C11 -177.7(10) . . . . ? C7 N1 C11 C10 -1.9(16) . . . . ? B1 N1 C11 C10 175.4(10) . . . . ? C9 C10 C11 N1 0.6(17) . . . . ? C10 C9 C12 C12 -1(2) . . . 2_665 ? C8 C9 C12 C12 178.9(13) . . . 2_665 ? O1 B1 C13 C18 1.0(16) . . . . ? O2 B1 C13 C18 122.9(12) . . . . ? N1 B1 C13 C18 -120.5(12) . . . . ? O1 B1 C13 C14 -168.8(10) . . . . ? O2 B1 C13 C14 -46.8(15) . . . . ? N1 B1 C13 C14 69.8(13) . . . . ? C18 C13 C14 C15 1.6(16) . . . . ? B1 C13 C14 C15 172.1(11) . . . . ? C13 C14 C15 C16 -2.9(18) . . . . ? C13 C14 C15 C19 179.7(11) . . . . ? C14 C15 C16 C17 2.9(19) . . . . ? C19 C15 C16 C17 -179.6(12) . . . . ? C15 C16 C17 C18 -1.7(18) . . . . ? C15 C16 C17 C20 -179.8(11) . . . . ? C14 C13 C18 C17 -0.5(17) . . . . ? B1 C13 C18 C17 -170.8(11) . . . . ? C16 C17 C18 C13 0.6(19) . . . . ? C20 C17 C18 C13 178.6(11) . . . . ? C14 C15 C19 F1 61.8(17) . . . . ? C16 C15 C19 F1 -115.7(14) . . . . ? C14 C15 C19 F3 -173.0(12) . . . . ? C16 C15 C19 F3 9.5(18) . . . . ? C14 C15 C19 F2 -55.5(16) . . . . ? C16 C15 C19 F2 127.0(13) . . . . ? C18 C17 C20 F6B -20(2) . . . . ? C16 C17 C20 F6B 158.0(17) . . . . ? C18 C17 C20 F4A 174.1(17) . . . . ? C16 C17 C20 F4A -8(2) . . . . ? C18 C17 C20 F5B 108.4(15) . . . . ? C16 C17 C20 F5B -73.7(16) . . . . ? C18 C17 C20 F4B -144.5(14) . . . . ? C16 C17 C20 F4B 33.4(17) . . . . ? C18 C17 C20 F5A 39.1(18) . . . . ? C16 C17 C20 F5A -143.0(13) . . . . ? C18 C17 C20 F6A -63.5(16) . . . . ? C16 C17 C20 F6A 114.4(14) . . . . ? B2 O3 C21 C26 6.1(17) . . . . ? B2 O3 C21 C22 -170.4(13) . . . . ? C26 C21 C22 C23 3(2) . . . . ? O3 C21 C22 C23 179.4(13) . . . . ? C21 C22 C23 C24 -7(2) . . . . ? C22 C23 C24 C25 4(2) . . . . ? C23 C24 C25 C26 2(2) . . . . ? O3 C21 C26 C25 -173.0(13) . . . . ? C22 C21 C26 C25 4(3) . . . . ? O3 C21 C26 O4 0(2) . . . . ? C22 C21 C26 O4 176.7(12) . . . . ? C24 C25 C26 C21 -6(2) . . . . ? C24 C25 C26 O4 -178.4(14) . . . . ? B2 O4 C26 C21 -7.0(17) . . . . ? B2 O4 C26 C25 166.3(15) . . . . ? C31 N2 C27 C28 0(2) . . . . ? B2 N2 C27 C28 -178.8(12) . . . . ? N2 C27 C28 C29 3(2) . . . . ? C27 C28 C29 C30 -3.9(18) . . . . ? C27 C28 C29 C32 177.0(11) . . . . ? C28 C29 C30 C31 1.2(18) . . . . ? C32 C29 C30 C31 -179.6(11) . . . . ? C27 N2 C31 C30 -3(2) . . . . ? B2 N2 C31 C30 176.0(12) . . . . ? C29 C30 C31 N2 2(2) . . . . ? C28 C29 C32 C32 -5(2) . . . 2_766 ? C30 C29 C32 C32 176.2(14) . . . 2_766 ? O4 B2 C33 C38 -3(2) . . . . ? O3 B2 C33 C38 -127.8(17) . . . . ? N2 B2 C33 C38 119.9(15) . . . . ? O4 B2 C33 C34 154.7(13) . . . . ? O3 B2 C33 C34 30(2) . . . . ? N2 B2 C33 C34 -82.6(16) . . . . ? C38 C33 C34 C35 -9(3) . . . . ? B2 C33 C34 C35 -167.1(16) . . . . ? C33 C34 C35 C36 1(3) . . . . ? C33 C34 C35 C39 180.0(16) . . . . ? C34 C35 C36 C37 9(3) . . . . ? C39 C35 C36 C37 -170.2(16) . . . . ? C35 C36 C37 C38 -10(3) . . . . ? C35 C36 C37 C40 174.1(16) . . . . ? C34 C33 C38 C37 8(3) . . . . ? B2 C33 C38 C37 167.3(15) . . . . ? C36 C37 C38 C33 1(3) . . . . ? C40 C37 C38 C33 177.3(17) . . . . ? C34 C35 C39 F9 -101(2) . . . . ? C36 C35 C39 F9 79(2) . . . . ? C34 C35 C39 F8 135.9(18) . . . . ? C36 C35 C39 F8 -45(2) . . . . ? C34 C35 C39 F7 21(2) . . . . ? C36 C35 C39 F7 -160.0(15) . . . . ? C36 C37 C40 F10 58(2) . . . . ? C38 C37 C40 F10 -118.4(19) . . . . ? C36 C37 C40 F12 -177.8(17) . . . . ? C38 C37 C40 F12 6(3) . . . . ? C36 C37 C40 F11 -58(2) . . . . ? C38 C37 C40 F11 126.4(17) . . . . ? C42 O5 C41 C54 178.4(9) . . . 2_665 ? C41 O5 C42 C43 2.6(16) . . . . ? C41 O5 C42 C47 -175.8(10) . . . . ? O5 C42 C43 C44 -178.4(10) . . . . ? C47 C42 C43 C44 -0.1(17) . . . . ? C42 C43 C44 C45 0.8(16) . . . . ? C48 O6 C45 C44 -177.5(10) . . . . ? C48 O6 C45 C46 -0.2(16) . . . . ? C43 C44 C45 O6 177.7(9) . . . . ? C43 C44 C45 C46 0.3(17) . . . . ? O6 C45 C46 C47 -179.3(10) . . . . ? C44 C45 C46 C47 -2.1(17) . . . . ? C45 C46 C47 C42 2.8(17) . . . . ? C43 C42 C47 C46 -1.7(17) . . . . ? O5 C42 C47 C46 176.8(10) . . . . ? C45 O6 C48 C49 179.3(9) . . . . ? C50 O7 C49 C48 178.3(9) . . . . ? O6 C48 C49 O7 64.0(12) . . . . ? C49 O7 C50 C51 176.7(9) . . . . ? C52 O8 C51 C50 172.7(9) . . . . ? O7 C50 C51 O8 60.7(12) . . . . ? C51 O8 C52 C53 178.8(9) . . . . ? C54 O9 C53 C52 -172.4(10) . . . . ? O8 C52 C53 O9 -69.6(12) . . . . ? C53 O9 C54 C41 -160.6(9) . . . 2_665 ? C56 O10 C55 C68 -178.6(10) . . . 2_766 ? C55 O10 C56 C61 171.7(10) . . . . ? C55 O10 C56 C57 -3.5(17) . . . . ? C61 C56 C57 C58 2.5(18) . . . . ? O10 C56 C57 C58 177.5(10) . . . . ? C56 C57 C58 C59 -1.1(17) . . . . ? C62 O11 C59 C58 179.4(10) . . . . ? C62 O11 C59 C60 0.5(16) . . . . ? C57 C58 C59 O11 -178.7(10) . . . . ? C57 C58 C59 C60 0.3(17) . . . . ? O11 C59 C60 C61 177.9(10) . . . . ? C58 C59 C60 C61 -1.1(17) . . . . ? C57 C56 C61 C60 -3.3(18) . . . . ? O10 C56 C61 C60 -178.7(10) . . . . ? C59 C60 C61 C56 2.6(18) . . . . ? C59 O11 C62 C63 -179.9(9) . . . . ? C64 O12 C63 C62 -163.4(10) . . . . ? O11 C62 C63 O12 -64.1(13) . . . . ? C63 O12 C64 C65 -173.3(10) . . . . ? C66 O13 C65 C64 -179.8(10) . . . . ? O12 C64 C65 O13 -66.7(12) . . . . ? C65 O13 C66 C67 172.6(10) . . . . ? C68 O14 C67 C66 176.7(11) . . . . ? O13 C66 C67 O14 66.4(13) . . . . ? C67 O14 C68 C55 167.4(11) . . . 2_766 ? C74 C69 C70 C71 -2.7(19) . . . . ? C75 C69 C70 C71 -179.8(11) . . . . ? C69 C70 C71 C72 3.3(19) . . . . ? C70 C71 C72 C73 -2.7(19) . . . . ? C71 C72 C73 C74 2(2) . . . . ? C70 C69 C74 C73 2(2) . . . . ? C75 C69 C74 C73 178.5(12) . . . . ? C72 C73 C74 C69 -1(2) . . . . ? C81 C76 C77 C78 2(2) . . . . ? C82 C76 C77 C78 -179.3(13) . . . . ? C76 C77 C78 C79 -2(2) . . . . ? C77 C78 C79 C80 2(2) . . . . ? C78 C79 C80 C81 -3(2) . . . . ? C77 C76 C81 C80 -3(2) . . . . ? C82 C76 C81 C80 178.5(13) . . . . ? C79 C80 C81 C76 3(2) . . . . ? C88A C83A C84A C85A 0.0 . . . . ? C89A C83A C84A C85A -177.4(17) . . . . ? C83A C84A C85A C86A 0.0 . . . . ? C84A C85A C86A C87A 0.0 . . . . ? C85A C86A C87A C88A 0.0 . . . . ? C86A C87A C88A C83A 0.0 . . . . ? C84A C83A C88A C87A 0.0 . . . . ? C89A C83A C88A C87A 177.5(17) . . . . ? C88B C83B C84B C85B 0.0 . . . . ? C89B C83B C84B C85B 179(4) . . . . ? C83B C84B C85B C86B 0.0 . . . . ? C84B C85B C86B C87B 0.0 . . . . ? C85B C86B C87B C88B 0.0 . . . . ? C86B C87B C88B C83B 0.0 . . . . ? C84B C83B C88B C87B 0.0 . . . . ? C89B C83B C88B C87B -179(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.933 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.111 #===END data_compund_3 _database_code_depnum_ccdc_archive 'CCDC 683421' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H40 O10, C38 H22 B2 F12 N2 O4, C7 H8' _chemical_formula_sum 'C73 H70 B2 F12 N2 O14' _chemical_formula_weight 1448.93 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0418(4) _cell_length_b 22.0219(6) _cell_length_c 22.2997(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.386(3) _cell_angle_gamma 90.00 _cell_volume 6852.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 15807 _cell_measurement_theta_min 2.5999 _cell_measurement_theta_max 27.4555 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_T_min 0.88194 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 8.2812 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45866 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.03 _reflns_number_total 12085 _reflns_number_gt 7319 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _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^)+(0.0662P)^2^+17.8066P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12085 _refine_ls_number_parameters 947 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1260 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2075 _refine_ls_wR_factor_gt 0.1601 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.007 _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 0.2323(3) 0.1309(2) 0.0577(2) 0.143(2) Uani 1 1 d . . . F2 F 0.0902(3) 0.15643(15) 0.06295(15) 0.0867(11) Uani 1 1 d . . . F3 F 0.1204(3) 0.09536(16) -0.00224(13) 0.0942(13) Uani 1 1 d . . . F4 F 0.1018(2) -0.11849(13) 0.03892(12) 0.0646(8) Uani 1 1 d . . . F5 F 0.0422(3) -0.13999(16) 0.11935(18) 0.1092(16) Uani 1 1 d . . . F6 F 0.1917(3) -0.14250(14) 0.11778(16) 0.0904(12) Uani 1 1 d . . . F7 F -0.7354(2) 0.30791(16) 0.42194(15) 0.0736(9) Uani 1 1 d . . . F8 F -0.6593(3) 0.22732(14) 0.40978(16) 0.0826(11) Uani 1 1 d . . . F9 F -0.6385(2) 0.27541(16) 0.49352(13) 0.0762(10) Uani 1 1 d . . . F10 F -0.3029(2) 0.41440(18) 0.48330(15) 0.0876(11) Uani 1 1 d . . . F11 F -0.4276(2) 0.45017(15) 0.51664(12) 0.0696(9) Uani 1 1 d . . . F12 F -0.3740(3) 0.48934(15) 0.43958(14) 0.0794(10) Uani 1 1 d . . . O1 O 0.10198(18) -0.01580(12) 0.30540(12) 0.0327(6) Uani 1 1 d . . . O2 O 0.20255(18) 0.06952(12) 0.30165(12) 0.0325(6) Uani 1 1 d . . . O3 O -0.42242(18) 0.38951(12) 0.23147(11) 0.0316(6) Uani 1 1 d . . . O4 O -0.53377(18) 0.30911(12) 0.22032(11) 0.0317(6) Uani 1 1 d . . . N1 N 0.0273(2) 0.08471(14) 0.27569(14) 0.0288(7) Uani 1 1 d . . . N2 N -0.3643(2) 0.28586(14) 0.26197(13) 0.0284(7) Uani 1 1 d . . . B1 B 0.1178(3) 0.0390(2) 0.2704(2) 0.0298(10) Uani 1 1 d . . . B2 B -0.4543(3) 0.3350(2) 0.2607(2) 0.0315(10) Uani 1 1 d . . . C1 C 0.1596(3) -0.00924(17) 0.35857(17) 0.0284(8) Uani 1 1 d . . . C2 C 0.1626(3) -0.04513(18) 0.40881(18) 0.0332(9) Uani 1 1 d . . . H2 H 0.1216 -0.0793 0.4100 0.040 Uiso 1 1 calc R . . C3 C 0.2277(3) -0.0297(2) 0.45806(19) 0.0395(10) Uani 1 1 d . . . H3 H 0.2321 -0.0542 0.4933 0.047 Uiso 1 1 calc R . . C4 C 0.2860(3) 0.0206(2) 0.45648(19) 0.0418(11) Uani 1 1 d . . . H4 H 0.3299 0.0301 0.4907 0.050 Uiso 1 1 calc R . . C5 C 0.2818(3) 0.05778(19) 0.40548(18) 0.0351(9) Uani 1 1 d . . . H5 H 0.3207 0.0930 0.4046 0.042 Uiso 1 1 calc R . . C6 C 0.2188(3) 0.04128(17) 0.35668(17) 0.0298(9) Uani 1 1 d . . . C7 C 0.1235(3) 0.02573(18) 0.20037(18) 0.0313(9) Uani 1 1 d . . . C8 C 0.1336(3) 0.07142(19) 0.15823(18) 0.0338(9) Uani 1 1 d . . . H8 H 0.1379 0.1125 0.1714 0.041 Uiso 1 1 calc R . . C9 C 0.1374(3) 0.05861(19) 0.09764(18) 0.0359(10) Uani 1 1 d . . . C10 C 0.1311(3) -0.0005(2) 0.0772(2) 0.0407(10) Uani 1 1 d . . . H10 H 0.1340 -0.0095 0.0357 0.049 Uiso 1 1 calc R . . C11 C 0.1205(3) -0.04639(19) 0.11811(19) 0.0379(10) Uani 1 1 d . . . C12 C 0.1170(3) -0.03348(19) 0.17870(19) 0.0364(10) Uani 1 1 d . . . H12 H 0.1099 -0.0659 0.2060 0.044 Uiso 1 1 calc R . . C13 C 0.1478(4) 0.1094(2) 0.0545(2) 0.0492(12) Uani 1 1 d . . . C14 C 0.1120(4) -0.1110(2) 0.0979(2) 0.0504(12) Uani 1 1 d . . . C15 C 0.0405(3) 0.14445(18) 0.28453(19) 0.0375(10) Uani 1 1 d . . . H15 H 0.1039 0.1598 0.2917 0.045 Uiso 1 1 calc R . . C16 C -0.0353(3) 0.18399(19) 0.2835(2) 0.0384(10) Uani 1 1 d . . . H16 H -0.0237 0.2261 0.2900 0.046 Uiso 1 1 calc R . . C17 C -0.1289(3) 0.16278(17) 0.27299(16) 0.0283(8) Uani 1 1 d . . . C18 C -0.1411(3) 0.10053(18) 0.26600(17) 0.0321(9) Uani 1 1 d . . . H18 H -0.2038 0.0837 0.2603 0.039 Uiso 1 1 calc R . . C19 C -0.0626(3) 0.06326(18) 0.26739(17) 0.0319(9) Uani 1 1 d . . . H19 H -0.0723 0.0208 0.2623 0.038 Uiso 1 1 calc R . . C20 C -0.2112(3) 0.20533(17) 0.26846(16) 0.0273(8) Uani 1 1 d . . . C21 C -0.1991(3) 0.26688(18) 0.25906(19) 0.0349(9) Uani 1 1 d . . . H21 H -0.1370 0.2823 0.2547 0.042 Uiso 1 1 calc R . . C22 C -0.2756(3) 0.30593(19) 0.25594(18) 0.0347(9) Uani 1 1 d . . . H22 H -0.2657 0.3480 0.2494 0.042 Uiso 1 1 calc R . . C23 C -0.3786(3) 0.22671(18) 0.27016(17) 0.0317(9) Uani 1 1 d . . . H23 H -0.4416 0.2126 0.2740 0.038 Uiso 1 1 calc R . . C24 C -0.3044(3) 0.18547(19) 0.27319(17) 0.0331(9) Uani 1 1 d . . . H24 H -0.3168 0.1435 0.2785 0.040 Uiso 1 1 calc R . . C25 C -0.4628(3) 0.38513(17) 0.17306(17) 0.0294(9) Uani 1 1 d . . . C26 C -0.4432(3) 0.41987(19) 0.12468(19) 0.0373(10) Uani 1 1 d . . . H26 H -0.3958 0.4508 0.1290 0.045 Uiso 1 1 calc R . . C27 C -0.4956(3) 0.4081(2) 0.0690(2) 0.0438(11) Uani 1 1 d . . . H27 H -0.4842 0.4317 0.0349 0.053 Uiso 1 1 calc R . . C28 C -0.5639(3) 0.3626(2) 0.06268(19) 0.0439(11) Uani 1 1 d . . . H28 H -0.5988 0.3556 0.0243 0.053 Uiso 1 1 calc R . . C29 C -0.5824(3) 0.32666(19) 0.11203(18) 0.0376(10) Uani 1 1 d . . . H29 H -0.6292 0.2953 0.1079 0.045 Uiso 1 1 calc R . . C30 C -0.5299(3) 0.33868(17) 0.16665(17) 0.0301(9) Uani 1 1 d . . . C31 C -0.4787(3) 0.34410(17) 0.32868(17) 0.0294(9) Uani 1 1 d . . . C32 C -0.5505(3) 0.31095(18) 0.35183(18) 0.0342(9) Uani 1 1 d . . . H32 H -0.5863 0.2824 0.3266 0.041 Uiso 1 1 calc R . . C33 C -0.5712(3) 0.31851(19) 0.41101(18) 0.0345(9) Uani 1 1 d . . . C34 C -0.5210(3) 0.36035(19) 0.44805(18) 0.0361(10) Uani 1 1 d . . . H34 H -0.5356 0.3662 0.4882 0.043 Uiso 1 1 calc R . . C35 C -0.4489(3) 0.39389(19) 0.42604(18) 0.0358(9) Uani 1 1 d . . . C36 C -0.4276(3) 0.38542(18) 0.36702(18) 0.0330(9) Uani 1 1 d . . . H36 H -0.3773 0.4082 0.3527 0.040 Uiso 1 1 calc R . . C37 C -0.6498(3) 0.2823(2) 0.4339(2) 0.0462(11) Uani 1 1 d . . . C38 C -0.3890(4) 0.4368(2) 0.4660(2) 0.0491(12) Uani 1 1 d . . . O5 O -0.37644(19) 0.16019(12) 0.12390(13) 0.0365(7) Uani 1 1 d . . . O6 O -0.5233(2) 0.12349(14) 0.19934(15) 0.0487(8) Uani 1 1 d . . . O7 O -0.4648(4) 0.08722(19) 0.31331(17) 0.0875(14) Uani 1 1 d . . . O8 O -0.3964(2) 0.17998(15) 0.39778(14) 0.0522(8) Uani 1 1 d . . . O9 O -0.2000(2) 0.17041(13) 0.44324(15) 0.0501(8) Uani 1 1 d . . . O10 O -0.1258(2) 0.06772(13) 0.42080(15) 0.0466(8) Uani 1 1 d . . . O11 O -0.2077(2) -0.01921(16) 0.33287(17) 0.0609(9) Uani 1 1 d . . . O12 O -0.2752(4) -0.0400(3) 0.2009(3) 0.118(2) Uani 1 1 d . . . O13A O -0.1974(5) 0.0039(3) 0.0753(2) 0.034(2) Uani 0.515(12) 1 d P A 1 O13B O -0.1611(6) -0.0055(4) 0.1443(3) 0.057(3) Uani 0.485(12) 1 d P A 2 O14 O -0.2055(2) 0.11929(13) 0.12283(14) 0.0420(7) Uani 1 1 d . A . C39 C -0.3087(3) 0.20293(18) 0.11586(17) 0.0308(9) Uani 1 1 d . . . C40 C -0.2148(3) 0.18052(18) 0.11546(17) 0.0326(9) Uani 1 1 d . . . C41 C -0.1409(3) 0.2204(2) 0.10902(19) 0.0395(10) Uani 1 1 d . . . H41 H -0.0772 0.2056 0.1095 0.047 Uiso 1 1 calc R . . C42 C -0.1594(3) 0.2817(2) 0.1018(2) 0.0493(12) Uani 1 1 d . . . H42 H -0.1083 0.3090 0.0973 0.059 Uiso 1 1 calc R . . C43 C -0.2516(3) 0.3036(2) 0.1012(2) 0.0461(11) Uani 1 1 d . . . H43 H -0.2639 0.3458 0.0960 0.055 Uiso 1 1 calc R . . C44 C -0.3261(3) 0.26398(18) 0.10829(18) 0.0349(9) Uani 1 1 d . . . H44 H -0.3895 0.2791 0.1079 0.042 Uiso 1 1 calc R . . C45 C -0.4734(3) 0.18046(19) 0.11954(19) 0.0361(9) Uani 1 1 d . . . H45A H -0.4947 0.1942 0.0779 0.043 Uiso 1 1 calc R . . H45B H -0.4796 0.2148 0.1475 0.043 Uiso 1 1 calc R . . C46 C -0.5326(3) 0.1280(2) 0.1359(2) 0.0481(12) Uani 1 1 d . . . H46A H -0.6005 0.1343 0.1202 0.058 Uiso 1 1 calc R . . H46B H -0.5100 0.0901 0.1182 0.058 Uiso 1 1 calc R . . C47 C -0.5570(4) 0.0697(2) 0.2223(3) 0.0681(16) Uani 1 1 d . . . H47A H -0.5182 0.0352 0.2099 0.082 Uiso 1 1 calc R . . H47B H -0.6242 0.0630 0.2048 0.082 Uiso 1 1 calc R . . C48 C -0.5527(5) 0.0709(3) 0.2861(3) 0.087(2) Uani 1 1 d . . . H48A H -0.6011 0.0999 0.2979 0.104 Uiso 1 1 calc R . . H48B H -0.5691 0.0301 0.3006 0.104 Uiso 1 1 calc R . . C49 C -0.4612(6) 0.0846(4) 0.3764(3) 0.107(3) Uani 1 1 d . . . H49A H -0.5241 0.0979 0.3877 0.128 Uiso 1 1 calc R . . H49B H -0.4526 0.0416 0.3888 0.128 Uiso 1 1 calc R . . C50 C -0.3923(6) 0.1177(3) 0.4086(3) 0.103(3) Uani 1 1 d . . . H50A H -0.3290 0.1026 0.3997 0.124 Uiso 1 1 calc R . . H50B H -0.3968 0.1108 0.4521 0.124 Uiso 1 1 calc R . . C51 C -0.3517(4) 0.2164(2) 0.4449(2) 0.0541(13) Uani 1 1 d . . . H51A H -0.3588 0.1964 0.4839 0.065 Uiso 1 1 calc R . . H51B H -0.3854 0.2559 0.4446 0.065 Uiso 1 1 calc R . . C52 C -0.2473(4) 0.2278(2) 0.4409(2) 0.0494(12) Uani 1 1 d . . . H52A H -0.2386 0.2489 0.4027 0.059 Uiso 1 1 calc R . . H52B H -0.2203 0.2537 0.4750 0.059 Uiso 1 1 calc R . . C53 C -0.1020(3) 0.1704(2) 0.4457(2) 0.0437(11) Uani 1 1 d . . . C54 C -0.0439(4) 0.2203(2) 0.4576(2) 0.0549(13) Uani 1 1 d . . . H54 H -0.0714 0.2590 0.4633 0.066 Uiso 1 1 calc R . . C55 C 0.0551(4) 0.2140(3) 0.4612(3) 0.0690(16) Uani 1 1 d . . . H55 H 0.0951 0.2486 0.4689 0.083 Uiso 1 1 calc R . . C56 C 0.0955(4) 0.1581(2) 0.4537(3) 0.0627(15) Uani 1 1 d . . . H56 H 0.1633 0.1538 0.4572 0.075 Uiso 1 1 calc R . . C57 C 0.0372(3) 0.1079(2) 0.4411(2) 0.0462(11) Uani 1 1 d . . . H57 H 0.0653 0.0693 0.4359 0.055 Uiso 1 1 calc R . . C58 C -0.0609(3) 0.11335(19) 0.43603(19) 0.0406(10) Uani 1 1 d . . . C59 C -0.0888(3) 0.00819(18) 0.4136(2) 0.0443(11) Uani 1 1 d . . . H59A H -0.0554 -0.0065 0.4523 0.053 Uiso 1 1 calc R . . H59B H -0.0426 0.0085 0.3831 0.053 Uiso 1 1 calc R . . C60 C -0.1718(4) -0.0322(2) 0.3934(2) 0.0567(14) Uani 1 1 d . . . H60A H -0.1512 -0.0752 0.3968 0.068 Uiso 1 1 calc R . . H60B H -0.2231 -0.0261 0.4199 0.068 Uiso 1 1 calc R . . C61 C -0.2913(4) -0.0541(3) 0.3079(4) 0.100(3) Uani 1 1 d . . . H61A H -0.3437 -0.0504 0.3339 0.119 Uiso 1 1 calc R . . H61B H -0.2747 -0.0976 0.3044 0.119 Uiso 1 1 calc R . . C62 C -0.3227(5) -0.0253(5) 0.2424(3) 0.133(4) Uani 1 1 d . . . H62A H -0.3904 -0.0365 0.2302 0.159 Uiso 1 1 calc R . . H62B H -0.3203 0.0195 0.2464 0.159 Uiso 1 1 calc R . . C63 C -0.3137(6) -0.0233(4) 0.1438(3) 0.099(2) Uani 1 1 d . A . H63A H -0.3228 0.0213 0.1424 0.119 Uiso 1 1 calc R . . H63B H -0.3773 -0.0426 0.1346 0.119 Uiso 1 1 calc R . . C64 C -0.2541(6) -0.0405(4) 0.0997(6) 0.152(5) Uani 1 1 d . . . H64A H -0.2105 -0.0727 0.1175 0.182 Uiso 1 1 calc R A 1 H64B H -0.2954 -0.0592 0.0658 0.182 Uiso 1 1 calc R A 1 C65A C -0.1294(11) 0.0253(7) 0.1222(6) 0.032(3) Uani 0.515(12) 1 d P A 1 H65A H -0.0677 0.0038 0.1214 0.038 Uiso 0.515(12) 1 calc PR A 1 H65B H -0.1527 0.0182 0.1619 0.038 Uiso 0.515(12) 1 calc PR A 1 C65B C -0.1307(16) 0.0264(10) 0.0956(7) 0.049(5) Uani 0.485(12) 1 d P A 2 H65C H -0.1792 0.0226 0.0601 0.059 Uiso 0.485(12) 1 calc PR A 2 H65D H -0.0698 0.0089 0.0850 0.059 Uiso 0.485(12) 1 calc PR A 2 C66 C -0.1162(3) 0.09285(19) 0.1121(2) 0.0385(10) Uani 1 1 d . . . H66A H -0.0633 0.1092 0.1405 0.046 Uiso 1 1 calc R A 1 H66B H -0.1022 0.1009 0.0703 0.046 Uiso 1 1 calc R A 1 C67 C 0.1989(4) 0.2592(3) 0.2213(4) 0.0776(19) Uani 1 1 d . . . C68 C 0.1691(4) 0.2884(3) 0.2696(3) 0.0718(16) Uani 1 1 d . . . H68 H 0.1952 0.2784 0.3095 0.086 Uiso 1 1 calc R . . C69 C 0.0946(6) 0.3363(4) 0.2585(5) 0.112(3) Uani 1 1 d . . . H69 H 0.0739 0.3588 0.2910 0.135 Uiso 1 1 calc R . . C70 C 0.0569(5) 0.3470(4) 0.2009(6) 0.107(3) Uani 1 1 d . . . H70 H 0.0083 0.3767 0.1919 0.128 Uiso 1 1 calc R . . C71 C 0.0920(7) 0.3128(5) 0.1545(5) 0.109(3) Uani 1 1 d . . . H71 H 0.0650 0.3204 0.1143 0.131 Uiso 1 1 calc R . . C72 C 0.1575(6) 0.2725(4) 0.1629(4) 0.098(3) Uani 1 1 d . . . H72 H 0.1781 0.2516 0.1293 0.118 Uiso 1 1 calc R . . C73 C 0.2726(5) 0.2141(3) 0.2272(5) 0.127(4) Uani 1 1 d . . . H73A H 0.3352 0.2339 0.2349 0.190 Uiso 1 1 calc R . . H73B H 0.2699 0.1904 0.1899 0.190 Uiso 1 1 calc R . . H73C H 0.2630 0.1870 0.2609 0.190 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 0.064(2) 0.179(5) 0.179(4) 0.129(4) -0.024(3) -0.051(3) F2 0.133(3) 0.058(2) 0.075(2) 0.0238(17) 0.042(2) 0.022(2) F3 0.171(4) 0.072(2) 0.0404(18) 0.0055(16) 0.014(2) -0.013(2) F4 0.098(2) 0.0511(17) 0.0421(16) -0.0123(13) -0.0019(15) 0.0004(16) F5 0.166(4) 0.064(2) 0.113(3) -0.044(2) 0.082(3) -0.057(2) F6 0.128(3) 0.0514(19) 0.083(2) -0.0134(17) -0.028(2) 0.040(2) F7 0.0418(17) 0.094(2) 0.087(2) 0.0241(19) 0.0167(16) -0.0023(16) F8 0.106(3) 0.056(2) 0.096(2) -0.0144(18) 0.054(2) -0.0281(18) F9 0.078(2) 0.108(3) 0.0439(17) 0.0216(17) 0.0091(15) -0.0252(19) F10 0.059(2) 0.118(3) 0.079(2) -0.043(2) -0.0226(17) 0.005(2) F11 0.085(2) 0.082(2) 0.0452(16) -0.0271(15) 0.0199(15) -0.0157(17) F12 0.117(3) 0.068(2) 0.0529(18) -0.0127(16) 0.0077(18) -0.040(2) O1 0.0316(15) 0.0314(15) 0.0340(15) 0.0019(12) -0.0013(12) -0.0010(12) O2 0.0300(15) 0.0317(15) 0.0354(15) 0.0041(12) 0.0021(12) 0.0015(12) O3 0.0304(14) 0.0327(15) 0.0315(15) -0.0037(12) 0.0020(12) 0.0010(12) O4 0.0296(14) 0.0358(15) 0.0292(14) -0.0007(12) 0.0012(11) 0.0013(12) N1 0.0293(18) 0.0303(18) 0.0272(17) 0.0025(14) 0.0046(14) 0.0009(14) N2 0.0257(17) 0.0340(19) 0.0255(16) -0.0032(14) 0.0016(13) -0.0008(14) B1 0.029(2) 0.025(2) 0.035(2) 0.0011(19) 0.0018(19) -0.0001(18) B2 0.026(2) 0.034(3) 0.034(2) -0.002(2) 0.0013(19) -0.0006(19) C1 0.030(2) 0.026(2) 0.029(2) -0.0015(16) 0.0051(17) 0.0082(16) C2 0.035(2) 0.026(2) 0.039(2) 0.0011(17) 0.0067(19) 0.0072(17) C3 0.047(3) 0.042(3) 0.031(2) 0.0039(19) 0.008(2) 0.014(2) C4 0.041(3) 0.053(3) 0.030(2) -0.007(2) 0.0012(19) 0.007(2) C5 0.031(2) 0.037(2) 0.038(2) -0.0073(18) 0.0019(18) 0.0018(18) C6 0.027(2) 0.030(2) 0.033(2) -0.0016(17) 0.0077(17) 0.0072(17) C7 0.0213(19) 0.037(2) 0.035(2) -0.0012(18) 0.0029(16) 0.0062(17) C8 0.032(2) 0.035(2) 0.035(2) -0.0013(18) 0.0042(18) 0.0014(18) C9 0.034(2) 0.039(2) 0.036(2) 0.0033(18) 0.0080(18) 0.0022(18) C10 0.040(2) 0.046(3) 0.036(2) -0.004(2) 0.0045(19) 0.007(2) C11 0.035(2) 0.036(2) 0.042(2) -0.0021(19) 0.0040(19) 0.0088(19) C12 0.034(2) 0.036(2) 0.039(2) 0.0034(19) 0.0033(18) 0.0058(18) C13 0.062(3) 0.046(3) 0.042(3) -0.003(2) 0.015(2) -0.009(2) C14 0.066(3) 0.045(3) 0.040(3) -0.002(2) 0.002(2) 0.009(3) C15 0.027(2) 0.034(2) 0.051(3) -0.004(2) -0.0005(19) -0.0026(18) C16 0.032(2) 0.031(2) 0.052(3) -0.0059(19) 0.0015(19) 0.0002(18) C17 0.031(2) 0.033(2) 0.0218(18) -0.0008(16) 0.0049(16) 0.0021(17) C18 0.025(2) 0.036(2) 0.035(2) 0.0037(17) 0.0026(17) -0.0026(17) C19 0.033(2) 0.029(2) 0.034(2) 0.0024(17) 0.0037(17) -0.0023(17) C20 0.028(2) 0.033(2) 0.0205(18) -0.0030(16) 0.0027(15) 0.0004(17) C21 0.025(2) 0.034(2) 0.046(2) -0.0097(19) 0.0027(18) -0.0036(17) C22 0.031(2) 0.031(2) 0.042(2) -0.0063(18) 0.0044(18) -0.0029(18) C23 0.027(2) 0.038(2) 0.032(2) 0.0014(17) 0.0070(17) -0.0012(17) C24 0.034(2) 0.034(2) 0.031(2) 0.0013(17) 0.0059(17) -0.0002(18) C25 0.030(2) 0.026(2) 0.032(2) -0.0043(16) 0.0039(17) 0.0066(17) C26 0.040(2) 0.030(2) 0.043(2) -0.0006(19) 0.008(2) 0.0075(18) C27 0.056(3) 0.040(3) 0.036(2) 0.005(2) 0.005(2) 0.012(2) C28 0.057(3) 0.042(3) 0.031(2) 0.0000(19) -0.003(2) 0.017(2) C29 0.034(2) 0.038(2) 0.040(2) -0.0073(19) -0.0020(19) 0.0071(19) C30 0.029(2) 0.030(2) 0.032(2) -0.0021(17) 0.0056(17) 0.0087(17) C31 0.026(2) 0.031(2) 0.031(2) -0.0016(17) 0.0026(16) 0.0088(17) C32 0.033(2) 0.034(2) 0.035(2) -0.0011(18) 0.0005(18) 0.0039(18) C33 0.033(2) 0.037(2) 0.034(2) 0.0038(18) 0.0051(18) 0.0062(18) C34 0.043(2) 0.039(2) 0.026(2) -0.0005(18) 0.0030(18) 0.010(2) C35 0.034(2) 0.041(2) 0.032(2) -0.0047(18) 0.0016(18) 0.0060(19) C36 0.030(2) 0.034(2) 0.035(2) -0.0019(18) 0.0061(17) 0.0045(17) C37 0.047(3) 0.054(3) 0.039(3) 0.005(2) 0.011(2) 0.001(2) C38 0.050(3) 0.060(3) 0.039(3) -0.012(2) 0.007(2) -0.001(2) O5 0.0301(15) 0.0312(15) 0.0480(17) -0.0003(13) 0.0035(13) 0.0004(12) O6 0.0477(19) 0.0418(18) 0.059(2) 0.0048(15) 0.0159(16) -0.0101(15) O7 0.132(4) 0.076(3) 0.052(2) 0.017(2) 0.001(2) -0.048(3) O8 0.057(2) 0.059(2) 0.0410(18) 0.0071(16) 0.0057(15) 0.0121(17) O9 0.051(2) 0.0296(16) 0.073(2) 0.0011(15) 0.0224(17) 0.0098(14) O10 0.0533(19) 0.0279(16) 0.063(2) 0.0013(14) 0.0263(16) 0.0036(14) O11 0.053(2) 0.061(2) 0.070(2) 0.0018(18) 0.0137(18) -0.0226(17) O12 0.079(3) 0.125(5) 0.151(5) 0.060(4) 0.017(4) -0.012(3) O13A 0.040(4) 0.033(3) 0.028(3) -0.001(2) -0.003(3) -0.005(3) O13B 0.071(6) 0.052(5) 0.045(5) 0.003(4) -0.006(4) 0.004(4) O14 0.0327(16) 0.0323(16) 0.061(2) 0.0045(14) 0.0068(14) 0.0043(13) C39 0.034(2) 0.033(2) 0.026(2) -0.0019(16) 0.0070(17) -0.0041(18) C40 0.038(2) 0.029(2) 0.031(2) 0.0032(17) 0.0062(18) -0.0002(18) C41 0.034(2) 0.042(3) 0.043(2) 0.000(2) 0.008(2) -0.003(2) C42 0.049(3) 0.036(3) 0.066(3) 0.000(2) 0.018(2) -0.011(2) C43 0.057(3) 0.032(2) 0.052(3) 0.001(2) 0.016(2) 0.000(2) C44 0.043(2) 0.029(2) 0.033(2) -0.0028(17) 0.0058(19) 0.0039(18) C45 0.031(2) 0.039(2) 0.036(2) -0.0031(18) -0.0025(18) 0.0041(18) C46 0.038(3) 0.055(3) 0.051(3) -0.007(2) 0.001(2) -0.008(2) C47 0.064(4) 0.049(3) 0.090(4) 0.015(3) 0.003(3) -0.016(3) C48 0.064(4) 0.082(5) 0.115(6) 0.047(4) 0.021(4) -0.016(3) C49 0.130(7) 0.113(6) 0.075(5) 0.040(4) -0.002(4) -0.043(5) C50 0.156(7) 0.071(4) 0.070(4) 0.030(3) -0.045(5) -0.023(5) C51 0.057(3) 0.059(3) 0.048(3) -0.007(2) 0.010(2) 0.021(3) C52 0.066(3) 0.034(3) 0.049(3) 0.000(2) 0.012(2) 0.014(2) C53 0.048(3) 0.035(2) 0.052(3) 0.008(2) 0.022(2) 0.007(2) C54 0.063(3) 0.034(3) 0.071(3) -0.008(2) 0.023(3) 0.001(2) C55 0.061(4) 0.056(3) 0.094(4) -0.020(3) 0.024(3) -0.011(3) C56 0.049(3) 0.059(3) 0.082(4) -0.022(3) 0.016(3) 0.003(3) C57 0.050(3) 0.041(3) 0.050(3) -0.005(2) 0.015(2) 0.007(2) C58 0.051(3) 0.033(2) 0.041(2) 0.0021(19) 0.018(2) 0.001(2) C59 0.064(3) 0.030(2) 0.041(2) 0.0040(19) 0.014(2) 0.014(2) C60 0.075(4) 0.036(3) 0.064(3) 0.007(2) 0.031(3) -0.002(2) C61 0.049(3) 0.064(4) 0.190(8) 0.027(5) 0.032(4) -0.033(3) C62 0.053(4) 0.252(11) 0.084(5) -0.125(6) -0.026(4) 0.047(5) C63 0.105(6) 0.107(6) 0.078(5) 0.012(4) -0.031(4) -0.004(5) C64 0.072(5) 0.116(7) 0.275(14) 0.063(8) 0.052(7) -0.013(5) C65A 0.028(6) 0.032(6) 0.035(8) 0.006(8) 0.001(7) 0.006(4) C65B 0.055(10) 0.053(9) 0.039(9) 0.009(10) 0.007(10) 0.020(7) C66 0.033(2) 0.040(2) 0.042(2) 0.0010(19) 0.0047(19) 0.0060(19) C67 0.054(4) 0.056(4) 0.125(6) -0.009(4) 0.019(4) -0.027(3) C68 0.061(4) 0.078(4) 0.074(4) -0.002(3) 0.001(3) -0.020(3) C69 0.084(6) 0.106(7) 0.150(8) -0.029(6) 0.026(6) -0.053(5) C70 0.059(4) 0.078(5) 0.177(9) 0.039(6) -0.017(6) -0.016(4) C71 0.097(7) 0.104(7) 0.125(7) 0.010(6) 0.010(6) -0.022(5) C72 0.089(5) 0.119(7) 0.082(5) 0.013(5) -0.006(4) -0.057(5) C73 0.065(4) 0.067(5) 0.253(11) -0.017(6) 0.041(6) -0.023(4) _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 C13 1.272(6) . ? F2 C13 1.341(6) . ? F3 C13 1.317(5) . ? F4 C14 1.318(5) . ? F5 C14 1.305(6) . ? F6 C14 1.349(6) . ? F7 C37 1.327(5) . ? F8 C37 1.326(5) . ? F9 C37 1.331(5) . ? F10 C38 1.323(6) . ? F11 C38 1.338(5) . ? F12 C38 1.327(6) . ? O1 C1 1.367(5) . ? O1 B1 1.467(5) . ? O2 C6 1.372(5) . ? O2 B1 1.473(5) . ? O3 C25 1.365(4) . ? O3 B2 1.459(5) . ? O4 C30 1.369(5) . ? O4 B2 1.469(5) . ? N1 C15 1.340(5) . ? N1 C19 1.341(5) . ? N1 B1 1.636(5) . ? N2 C23 1.334(5) . ? N2 C22 1.342(5) . ? N2 B2 1.662(5) . ? B1 C7 1.600(6) . ? B2 C31 1.603(6) . ? C1 C2 1.368(5) . ? C1 C6 1.392(5) . ? C2 C3 1.390(6) . ? C2 H2 0.9500 . ? C3 C4 1.380(6) . ? C3 H3 0.9500 . ? C4 C5 1.398(6) . ? C4 H4 0.9500 . ? C5 C6 1.373(5) . ? C5 H5 0.9500 . ? C7 C12 1.390(6) . ? C7 C8 1.395(6) . ? C8 C9 1.387(6) . ? C8 H8 0.9500 . ? C9 C10 1.380(6) . ? C9 C13 1.493(6) . ? C10 C11 1.381(6) . ? C10 H10 0.9500 . ? C11 C12 1.387(6) . ? C11 C14 1.493(6) . ? C12 H12 0.9500 . ? C15 C16 1.373(6) . ? C15 H15 0.9500 . ? C16 C17 1.391(5) . ? C16 H16 0.9500 . ? C17 C18 1.388(5) . ? C17 C20 1.482(5) . ? C18 C19 1.372(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.385(5) . ? C20 C24 1.396(5) . ? C21 C22 1.372(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.378(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.375(6) . ? C25 C30 1.388(5) . ? C26 C27 1.394(6) . ? C26 H26 0.9500 . ? C27 C28 1.382(6) . ? C27 H27 0.9500 . ? C28 C29 1.403(6) . ? C28 H28 0.9500 . ? C29 C30 1.377(5) . ? C29 H29 0.9500 . ? C31 C32 1.389(6) . ? C31 C36 1.392(5) . ? C32 C33 1.393(5) . ? C32 H32 0.9500 . ? C33 C34 1.378(6) . ? C33 C37 1.496(6) . ? C34 C35 1.386(6) . ? C34 H34 0.9500 . ? C35 C36 1.394(5) . ? C35 C38 1.492(6) . ? C36 H36 0.9500 . ? O5 C39 1.364(5) . ? O5 C45 1.425(5) . ? O6 C47 1.395(6) . ? O6 C46 1.409(5) . ? O7 C48 1.362(7) . ? O7 C49 1.403(7) . ? O8 C50 1.392(7) . ? O8 C51 1.413(6) . ? O9 C53 1.371(5) . ? O9 C52 1.427(5) . ? O10 C58 1.373(5) . ? O10 C59 1.426(5) . ? O11 C60 1.417(6) . ? O11 C61 1.460(7) . ? O12 C62 1.242(7) . ? O12 C63 1.378(8) . ? O13A C64 1.408(10) . ? O13A C65A 1.417(16) . ? O13B C65B 1.399(18) . ? O13B C64 1.732(13) . ? O14 C40 1.363(5) . ? O14 C66 1.426(5) . ? C39 C44 1.373(5) . ? C39 C40 1.409(5) . ? C40 C41 1.379(6) . ? C41 C42 1.381(6) . ? C41 H41 0.9500 . ? C42 C43 1.381(6) . ? C42 H42 0.9500 . ? C43 C44 1.385(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.493(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.418(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.354(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.500(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.377(7) . ? C53 C58 1.409(6) . ? C54 C55 1.390(7) . ? C54 H54 0.9500 . ? C55 C56 1.375(7) . ? C55 H55 0.9500 . ? C56 C57 1.386(7) . ? C56 H56 0.9500 . ? C57 C58 1.374(6) . ? C57 H57 0.9500 . ? C59 C60 1.495(7) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.608(11) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.412(12) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65A C66 1.518(17) . ? C65A H65A 0.9900 . ? C65A H65B 0.9900 . ? C65B C66 1.52(2) . ? C65B H65C 0.9900 . ? C65B H65D 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.359(9) . ? C67 C72 1.398(10) . ? C67 C73 1.431(9) . ? C68 C69 1.486(11) . ? C68 H68 0.9500 . ? C69 C70 1.356(11) . ? C69 H69 0.9500 . ? C70 C71 1.410(12) . ? C70 H70 0.9500 . ? C71 C72 1.277(11) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 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 105.3(3) . . ? C6 O2 B1 105.1(3) . . ? C25 O3 B2 104.6(3) . . ? C30 O4 B2 104.5(3) . . ? C15 N1 C19 118.6(3) . . ? C15 N1 B1 121.2(3) . . ? C19 N1 B1 120.0(3) . . ? C23 N2 C22 119.4(3) . . ? C23 N2 B2 120.9(3) . . ? C22 N2 B2 119.7(3) . . ? O1 B1 O2 106.6(3) . . ? O1 B1 C7 113.3(3) . . ? O2 B1 C7 114.8(3) . . ? O1 B1 N1 107.7(3) . . ? O2 B1 N1 106.2(3) . . ? C7 B1 N1 107.8(3) . . ? O3 B2 O4 107.2(3) . . ? O3 B2 C31 115.4(3) . . ? O4 B2 C31 113.6(3) . . ? O3 B2 N2 105.8(3) . . ? O4 B2 N2 106.3(3) . . ? C31 B2 N2 107.9(3) . . ? O1 C1 C2 127.6(4) . . ? O1 C1 C6 110.9(3) . . ? C2 C1 C6 121.5(4) . . ? C1 C2 C3 117.6(4) . . ? C1 C2 H2 121.2 . . ? C3 C2 H2 121.2 . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 121.3(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 117.1(4) . . ? C6 C5 H5 121.5 . . ? C4 C5 H5 121.5 . . ? O2 C6 C5 128.1(4) . . ? O2 C6 C1 110.4(3) . . ? C5 C6 C1 121.4(4) . . ? C12 C7 C8 116.8(4) . . ? C12 C7 B1 120.1(4) . . ? C8 C7 B1 123.1(4) . . ? C9 C8 C7 121.8(4) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C8 120.4(4) . . ? C10 C9 C13 120.0(4) . . ? C8 C9 C13 119.6(4) . . ? C9 C10 C11 118.6(4) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C10 C11 C12 120.8(4) . . ? C10 C11 C14 120.6(4) . . ? C12 C11 C14 118.6(4) . . ? C11 C12 C7 121.5(4) . . ? C11 C12 H12 119.2 . . ? C7 C12 H12 119.2 . . ? F1 C13 F3 108.2(5) . . ? F1 C13 F2 106.1(5) . . ? F3 C13 F2 101.6(4) . . ? F1 C13 C9 113.5(4) . . ? F3 C13 C9 113.9(4) . . ? F2 C13 C9 112.6(4) . . ? F5 C14 F4 107.6(4) . . ? F5 C14 F6 104.9(4) . . ? F4 C14 F6 104.9(4) . . ? F5 C14 C11 113.2(4) . . ? F4 C14 C11 114.6(4) . . ? F6 C14 C11 110.8(4) . . ? N1 C15 C16 121.7(4) . . ? N1 C15 H15 119.1 . . ? C16 C15 H15 119.1 . . ? C15 C16 C17 120.4(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 116.9(4) . . ? C18 C17 C20 122.1(3) . . ? C16 C17 C20 120.9(4) . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? N1 C19 C18 122.3(4) . . ? N1 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C21 C20 C24 116.7(4) . . ? C21 C20 C17 121.4(3) . . ? C24 C20 C17 121.8(4) . . ? C22 C21 C20 120.8(4) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? N2 C22 C21 121.3(4) . . ? N2 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? N2 C23 C24 121.7(4) . . ? N2 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C20 120.0(4) . . ? C23 C24 H24 120.0 . . ? C20 C24 H24 120.0 . . ? O3 C25 C26 127.7(4) . . ? O3 C25 C30 110.8(3) . . ? C26 C25 C30 121.5(4) . . ? C25 C26 C27 117.6(4) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? C28 C27 C26 121.2(4) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 121.0(4) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C28 117.2(4) . . ? C30 C29 H29 121.4 . . ? C28 C29 H29 121.4 . . ? O4 C30 C29 127.8(4) . . ? O4 C30 C25 110.7(3) . . ? C29 C30 C25 121.6(4) . . ? C32 C31 C36 117.4(4) . . ? C32 C31 B2 121.7(4) . . ? C36 C31 B2 120.8(4) . . ? C31 C32 C33 121.7(4) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C34 C33 C32 120.1(4) . . ? C34 C33 C37 120.0(4) . . ? C32 C33 C37 119.9(4) . . ? C33 C34 C35 119.3(4) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 120.3(4) . . ? C34 C35 C38 120.7(4) . . ? C36 C35 C38 118.9(4) . . ? C31 C36 C35 121.1(4) . . ? C31 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? F8 C37 F7 105.0(4) . . ? F8 C37 F9 107.2(4) . . ? F7 C37 F9 104.7(4) . . ? F8 C37 C33 113.2(4) . . ? F7 C37 C33 113.1(4) . . ? F9 C37 C33 113.1(4) . . ? F10 C38 F12 105.6(4) . . ? F10 C38 F11 106.2(4) . . ? F12 C38 F11 106.3(4) . . ? F10 C38 C35 112.0(4) . . ? F12 C38 C35 113.2(4) . . ? F11 C38 C35 112.9(4) . . ? C39 O5 C45 116.7(3) . . ? C47 O6 C46 115.5(4) . . ? C48 O7 C49 111.5(5) . . ? C50 O8 C51 115.0(4) . . ? C53 O9 C52 117.6(3) . . ? C58 O10 C59 117.5(3) . . ? C60 O11 C61 116.2(4) . . ? C62 O12 C63 115.6(7) . . ? C64 O13A C65A 108.0(9) . . ? C65B O13B C64 93.1(10) . . ? C40 O14 C66 117.3(3) . . ? O5 C39 C44 125.1(4) . . ? O5 C39 C40 115.2(3) . . ? C44 C39 C40 119.7(4) . . ? O14 C40 C41 125.4(4) . . ? O14 C40 C39 115.0(3) . . ? C41 C40 C39 119.6(4) . . ? C40 C41 C42 120.0(4) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 120.5(4) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 119.9(4) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C39 C44 C43 120.3(4) . . ? C39 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? O5 C45 C46 107.1(3) . . ? O5 C45 H45A 110.3 . . ? C46 C45 H45A 110.3 . . ? O5 C45 H45B 110.3 . . ? C46 C45 H45B 110.3 . . ? H45A C45 H45B 108.6 . . ? O6 C46 C45 108.0(4) . . ? O6 C46 H46A 110.1 . . ? C45 C46 H46A 110.1 . . ? O6 C46 H46B 110.1 . . ? C45 C46 H46B 110.1 . . ? H46A C46 H46B 108.4 . . ? O6 C47 C48 111.9(5) . . ? O6 C47 H47A 109.2 . . ? C48 C47 H47A 109.2 . . ? O6 C47 H47B 109.2 . . ? C48 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? O7 C48 C47 112.8(5) . . ? O7 C48 H48A 109.0 . . ? C47 C48 H48A 109.0 . . ? O7 C48 H48B 109.0 . . ? C47 C48 H48B 109.0 . . ? H48A C48 H48B 107.8 . . ? C50 C49 O7 117.0(6) . . ? C50 C49 H49A 108.0 . . ? O7 C49 H49A 108.0 . . ? C50 C49 H49B 108.0 . . ? O7 C49 H49B 108.0 . . ? H49A C49 H49B 107.3 . . ? C49 C50 O8 115.2(6) . . ? C49 C50 H50A 108.5 . . ? O8 C50 H50A 108.5 . . ? C49 C50 H50B 108.5 . . ? O8 C50 H50B 108.5 . . ? H50A C50 H50B 107.5 . . ? O8 C51 C52 114.0(4) . . ? O8 C51 H51A 108.7 . . ? C52 C51 H51A 108.7 . . ? O8 C51 H51B 108.7 . . ? C52 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? O9 C52 C51 107.7(4) . . ? O9 C52 H52A 110.2 . . ? C51 C52 H52A 110.2 . . ? O9 C52 H52B 110.2 . . ? C51 C52 H52B 110.2 . . ? H52A C52 H52B 108.5 . . ? O9 C53 C54 125.4(4) . . ? O9 C53 C58 114.9(4) . . ? C54 C53 C58 119.8(4) . . ? C53 C54 C55 120.0(5) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 120.3(5) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C55 C56 C57 119.8(5) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C58 C57 C56 120.8(4) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? O10 C58 C57 126.0(4) . . ? O10 C58 C53 114.7(4) . . ? C57 C58 C53 119.3(4) . . ? O10 C59 C60 107.5(4) . . ? O10 C59 H59A 110.2 . . ? C60 C59 H59A 110.2 . . ? O10 C59 H59B 110.2 . . ? C60 C59 H59B 110.2 . . ? H59A C59 H59B 108.5 . . ? O11 C60 C59 110.4(4) . . ? O11 C60 H60A 109.6 . . ? C59 C60 H60A 109.6 . . ? O11 C60 H60B 109.6 . . ? C59 C60 H60B 109.6 . . ? H60A C60 H60B 108.1 . . ? O11 C61 C62 105.4(5) . . ? O11 C61 H61A 110.7 . . ? C62 C61 H61A 110.7 . . ? O11 C61 H61B 110.7 . . ? C62 C61 H61B 110.7 . . ? H61A C61 H61B 108.8 . . ? O12 C62 C61 117.2(7) . . ? O12 C62 H62A 108.0 . . ? C61 C62 H62A 108.0 . . ? O12 C62 H62B 108.0 . . ? C61 C62 H62B 108.0 . . ? H62A C62 H62B 107.2 . . ? O12 C63 C64 111.8(8) . . ? O12 C63 H63A 109.3 . . ? C64 C63 H63A 109.3 . . ? O12 C63 H63B 109.3 . . ? C64 C63 H63B 109.3 . . ? H63A C63 H63B 107.9 . . ? O13A C64 C63 119.1(9) . . ? O13A C64 O13B 59.4(5) . . ? C63 C64 O13B 87.0(8) . . ? O13A C64 H64A 107.5 . . ? C63 C64 H64A 107.5 . . ? O13B C64 H64A 72.3 . . ? O13A C64 H64B 107.5 . . ? C63 C64 H64B 107.5 . . ? O13B C64 H64B 164.6 . . ? H64A C64 H64B 107.0 . . ? O13A C65A C66 107.5(10) . . ? O13A C65A H65A 110.2 . . ? C66 C65A H65A 110.2 . . ? O13A C65A H65B 110.2 . . ? C66 C65A H65B 110.2 . . ? H65A C65A H65B 108.5 . . ? O13B C65B C66 109.9(12) . . ? O13B C65B H65C 109.7 . . ? C66 C65B H65C 109.7 . . ? O13B C65B H65D 109.7 . . ? C66 C65B H65D 109.7 . . ? H65C C65B H65D 108.2 . . ? O14 C66 C65B 109.8(9) . . ? O14 C66 C65A 104.5(6) . . ? C65B C66 C65A 22.5(5) . . ? O14 C66 H66A 110.8 . . ? C65B C66 H66A 125.2 . . ? C65A C66 H66A 110.8 . . ? O14 C66 H66B 110.8 . . ? C65B C66 H66B 88.9 . . ? C65A C66 H66B 110.8 . . ? H66A C66 H66B 108.9 . . ? C68 C67 C72 120.5(7) . . ? C68 C67 C73 122.6(8) . . ? C72 C67 C73 116.9(8) . . ? C67 C68 C69 118.4(7) . . ? C67 C68 H68 120.8 . . ? C69 C68 H68 120.8 . . ? C70 C69 C68 118.3(8) . . ? C70 C69 H69 120.8 . . ? C68 C69 H69 120.8 . . ? C69 C70 C71 118.1(8) . . ? C69 C70 H70 121.0 . . ? C71 C70 H70 121.0 . . ? C72 C71 C70 124.7(10) . . ? C72 C71 H71 117.7 . . ? C70 C71 H71 117.7 . . ? C71 C72 C67 119.9(9) . . ? C71 C72 H72 120.0 . . ? C67 C72 H72 120.0 . . ? C67 C73 H73A 109.5 . . ? C67 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C67 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 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 C1 O1 B1 O2 12.1(4) . . . . ? C1 O1 B1 C7 139.4(3) . . . . ? C1 O1 B1 N1 -101.5(3) . . . . ? C6 O2 B1 O1 -12.4(4) . . . . ? C6 O2 B1 C7 -138.8(3) . . . . ? C6 O2 B1 N1 102.2(3) . . . . ? C15 N1 B1 O1 137.3(4) . . . . ? C19 N1 B1 O1 -46.9(4) . . . . ? C15 N1 B1 O2 23.4(5) . . . . ? C19 N1 B1 O2 -160.8(3) . . . . ? C15 N1 B1 C7 -100.1(4) . . . . ? C19 N1 B1 C7 75.7(4) . . . . ? C25 O3 B2 O4 -14.8(4) . . . . ? C25 O3 B2 C31 -142.5(3) . . . . ? C25 O3 B2 N2 98.4(3) . . . . ? C30 O4 B2 O3 13.5(4) . . . . ? C30 O4 B2 C31 142.2(3) . . . . ? C30 O4 B2 N2 -99.3(3) . . . . ? C23 N2 B2 O3 -161.4(3) . . . . ? C22 N2 B2 O3 20.0(4) . . . . ? C23 N2 B2 O4 -47.6(4) . . . . ? C22 N2 B2 O4 133.8(3) . . . . ? C23 N2 B2 C31 74.6(4) . . . . ? C22 N2 B2 C31 -104.0(4) . . . . ? B1 O1 C1 C2 172.2(4) . . . . ? B1 O1 C1 C6 -7.4(4) . . . . ? O1 C1 C2 C3 179.9(4) . . . . ? C6 C1 C2 C3 -0.6(5) . . . . ? C1 C2 C3 C4 1.0(6) . . . . ? C2 C3 C4 C5 0.0(6) . . . . ? C3 C4 C5 C6 -1.5(6) . . . . ? B1 O2 C6 C5 -171.0(4) . . . . ? B1 O2 C6 C1 8.2(4) . . . . ? C4 C5 C6 O2 -179.0(4) . . . . ? C4 C5 C6 C1 1.9(6) . . . . ? O1 C1 C6 O2 -0.5(4) . . . . ? C2 C1 C6 O2 179.8(3) . . . . ? O1 C1 C6 C5 178.7(3) . . . . ? C2 C1 C6 C5 -0.9(6) . . . . ? O1 B1 C7 C12 -2.2(5) . . . . ? O2 B1 C7 C12 120.7(4) . . . . ? N1 B1 C7 C12 -121.2(4) . . . . ? O1 B1 C7 C8 176.9(3) . . . . ? O2 B1 C7 C8 -60.3(5) . . . . ? N1 B1 C7 C8 57.8(5) . . . . ? C12 C7 C8 C9 -0.3(6) . . . . ? B1 C7 C8 C9 -179.4(4) . . . . ? C7 C8 C9 C10 0.2(6) . . . . ? C7 C8 C9 C13 179.7(4) . . . . ? C8 C9 C10 C11 0.2(6) . . . . ? C13 C9 C10 C11 -179.3(4) . . . . ? C9 C10 C11 C12 -0.4(6) . . . . ? C9 C10 C11 C14 179.1(4) . . . . ? C10 C11 C12 C7 0.3(6) . . . . ? C14 C11 C12 C7 -179.3(4) . . . . ? C8 C7 C12 C11 0.1(6) . . . . ? B1 C7 C12 C11 179.3(4) . . . . ? C10 C9 C13 F1 -104.3(6) . . . . ? C8 C9 C13 F1 76.1(6) . . . . ? C10 C9 C13 F3 20.2(6) . . . . ? C8 C9 C13 F3 -159.3(4) . . . . ? C10 C9 C13 F2 135.1(4) . . . . ? C8 C9 C13 F2 -44.4(6) . . . . ? C10 C11 C14 F5 -133.1(5) . . . . ? C12 C11 C14 F5 46.5(6) . . . . ? C10 C11 C14 F4 -9.2(7) . . . . ? C12 C11 C14 F4 170.4(4) . . . . ? C10 C11 C14 F6 109.3(5) . . . . ? C12 C11 C14 F6 -71.1(5) . . . . ? C19 N1 C15 C16 -1.9(6) . . . . ? B1 N1 C15 C16 173.9(4) . . . . ? N1 C15 C16 C17 -0.1(7) . . . . ? C15 C16 C17 C18 2.3(6) . . . . ? C15 C16 C17 C20 -176.6(4) . . . . ? C16 C17 C18 C19 -2.4(6) . . . . ? C20 C17 C18 C19 176.5(3) . . . . ? C15 N1 C19 C18 1.8(6) . . . . ? B1 N1 C19 C18 -174.1(3) . . . . ? C17 C18 C19 N1 0.4(6) . . . . ? C18 C17 C20 C21 -162.2(4) . . . . ? C16 C17 C20 C21 16.7(6) . . . . ? C18 C17 C20 C24 17.6(5) . . . . ? C16 C17 C20 C24 -163.6(4) . . . . ? C24 C20 C21 C22 1.3(6) . . . . ? C17 C20 C21 C22 -178.9(4) . . . . ? C23 N2 C22 C21 -1.1(6) . . . . ? B2 N2 C22 C21 177.5(4) . . . . ? C20 C21 C22 N2 0.1(6) . . . . ? C22 N2 C23 C24 0.6(6) . . . . ? B2 N2 C23 C24 -178.0(3) . . . . ? N2 C23 C24 C20 0.9(6) . . . . ? C21 C20 C24 C23 -1.8(5) . . . . ? C17 C20 C24 C23 178.5(3) . . . . ? B2 O3 C25 C26 -169.0(4) . . . . ? B2 O3 C25 C30 10.7(4) . . . . ? O3 C25 C26 C27 -178.4(4) . . . . ? C30 C25 C26 C27 2.0(6) . . . . ? C25 C26 C27 C28 -0.7(6) . . . . ? C26 C27 C28 C29 -0.3(7) . . . . ? C27 C28 C29 C30 0.1(6) . . . . ? B2 O4 C30 C29 172.5(4) . . . . ? B2 O4 C30 C25 -7.2(4) . . . . ? C28 C29 C30 O4 -178.5(4) . . . . ? C28 C29 C30 C25 1.2(6) . . . . ? O3 C25 C30 O4 -2.3(4) . . . . ? C26 C25 C30 O4 177.4(3) . . . . ? O3 C25 C30 C29 178.0(3) . . . . ? C26 C25 C30 C29 -2.3(6) . . . . ? O3 B2 C31 C32 146.9(4) . . . . ? O4 B2 C31 C32 22.5(5) . . . . ? N2 B2 C31 C32 -95.1(4) . . . . ? O3 B2 C31 C36 -33.7(5) . . . . ? O4 B2 C31 C36 -158.1(3) . . . . ? N2 B2 C31 C36 84.3(4) . . . . ? C36 C31 C32 C33 0.1(6) . . . . ? B2 C31 C32 C33 179.6(4) . . . . ? C31 C32 C33 C34 1.0(6) . . . . ? C31 C32 C33 C37 179.3(4) . . . . ? C32 C33 C34 C35 -1.1(6) . . . . ? C37 C33 C34 C35 -179.5(4) . . . . ? C33 C34 C35 C36 0.1(6) . . . . ? C33 C34 C35 C38 -176.1(4) . . . . ? C32 C31 C36 C35 -1.1(6) . . . . ? B2 C31 C36 C35 179.5(4) . . . . ? C34 C35 C36 C31 1.0(6) . . . . ? C38 C35 C36 C31 177.3(4) . . . . ? C34 C33 C37 F8 -148.5(4) . . . . ? C32 C33 C37 F8 33.1(6) . . . . ? C34 C33 C37 F7 92.3(5) . . . . ? C32 C33 C37 F7 -86.1(5) . . . . ? C34 C33 C37 F9 -26.4(6) . . . . ? C32 C33 C37 F9 155.2(4) . . . . ? C34 C35 C38 F10 103.6(5) . . . . ? C36 C35 C38 F10 -72.7(5) . . . . ? C34 C35 C38 F12 -137.1(4) . . . . ? C36 C35 C38 F12 46.5(6) . . . . ? C34 C35 C38 F11 -16.3(6) . . . . ? C36 C35 C38 F11 167.4(4) . . . . ? C45 O5 C39 C44 4.9(5) . . . . ? C45 O5 C39 C40 -174.9(3) . . . . ? C66 O14 C40 C41 -12.1(6) . . . . ? C66 O14 C40 C39 169.1(3) . . . . ? O5 C39 C40 O14 0.4(5) . . . . ? C44 C39 C40 O14 -179.5(3) . . . . ? O5 C39 C40 C41 -178.5(4) . . . . ? C44 C39 C40 C41 1.7(6) . . . . ? O14 C40 C41 C42 -180.0(4) . . . . ? C39 C40 C41 C42 -1.2(6) . . . . ? C40 C41 C42 C43 0.2(7) . . . . ? C41 C42 C43 C44 0.5(7) . . . . ? O5 C39 C44 C43 179.2(4) . . . . ? C40 C39 C44 C43 -1.0(6) . . . . ? C42 C43 C44 C39 0.0(7) . . . . ? C39 O5 C45 C46 -174.4(3) . . . . ? C47 O6 C46 C45 -166.9(4) . . . . ? O5 C45 C46 O6 79.8(4) . . . . ? C46 O6 C47 C48 -175.0(5) . . . . ? C49 O7 C48 C47 -176.6(6) . . . . ? O6 C47 C48 O7 -51.4(8) . . . . ? C48 O7 C49 C50 -158.6(8) . . . . ? O7 C49 C50 O8 59.9(11) . . . . ? C51 O8 C50 C49 156.9(6) . . . . ? C50 O8 C51 C52 88.7(6) . . . . ? C53 O9 C52 C51 -174.3(4) . . . . ? O8 C51 C52 O9 -60.1(5) . . . . ? C52 O9 C53 C54 13.0(7) . . . . ? C52 O9 C53 C58 -168.1(4) . . . . ? O9 C53 C54 C55 177.5(5) . . . . ? C58 C53 C54 C55 -1.3(8) . . . . ? C53 C54 C55 C56 -0.8(9) . . . . ? C54 C55 C56 C57 1.5(9) . . . . ? C55 C56 C57 C58 0.0(8) . . . . ? C59 O10 C58 C57 4.6(6) . . . . ? C59 O10 C58 C53 -176.7(4) . . . . ? C56 C57 C58 O10 176.6(4) . . . . ? C56 C57 C58 C53 -2.0(7) . . . . ? O9 C53 C58 O10 5.0(6) . . . . ? C54 C53 C58 O10 -176.1(4) . . . . ? O9 C53 C58 C57 -176.2(4) . . . . ? C54 C53 C58 C57 2.7(7) . . . . ? C58 O10 C59 C60 -176.5(4) . . . . ? C61 O11 C60 C59 -178.0(4) . . . . ? O10 C59 C60 O11 71.9(5) . . . . ? C60 O11 C61 C62 174.1(5) . . . . ? C63 O12 C62 C61 169.1(6) . . . . ? O11 C61 C62 O12 78.1(9) . . . . ? C62 O12 C63 C64 178.7(8) . . . . ? C65A O13A C64 C63 65.0(11) . . . . ? C65A O13A C64 O13B -1.5(8) . . . . ? O12 C63 C64 O13A -103.0(10) . . . . ? O12 C63 C64 O13B -50.8(8) . . . . ? C65B O13B C64 O13A -5.0(9) . . . . ? C65B O13B C64 C63 -131.7(10) . . . . ? C64 O13A C65A C66 -143.4(8) . . . . ? C64 O13B C65B C66 131.5(12) . . . . ? C40 O14 C66 C65B -155.6(7) . . . . ? C40 O14 C66 C65A -178.5(6) . . . . ? O13B C65B C66 O14 -63.8(14) . . . . ? O13B C65B C66 C65A 16(2) . . . . ? O13A C65A C66 O14 67.9(10) . . . . ? O13A C65A C66 C65B -39(3) . . . . ? C72 C67 C68 C69 -2.4(8) . . . . ? C73 C67 C68 C69 177.7(5) . . . . ? C67 C68 C69 C70 2.6(9) . . . . ? C68 C69 C70 C71 -1.2(10) . . . . ? C69 C70 C71 C72 -0.5(12) . . . . ? C70 C71 C72 C67 0.8(12) . . . . ? C68 C67 C72 C71 0.8(10) . . . . ? C73 C67 C72 C71 -179.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.074 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.067 #===END