# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chuan-Feng Chen' _publ_contact_author_email CCHEN@ICCAS.AC.CN _publ_section_title ; Complexation between pentiptycene-based mono(crown ether)s and tetracationic cyclobis(paraquat-p-phenylene): who is the host or the guest? ; loop_ _publ_author_name 'Chuan-Feng Chen.' 'Jing Cao.' 'Hai-Yan Lu.' 'Jun-Feng Xiang.' # Attachment 'complex_1-3.cif' data_r90718e _database_code_depnum_ccdc_archive 'CCDC 755777' #TrackingRef 'complex_1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C102 H104 F24 N8 O12 P4' _chemical_formula_weight 2213.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.719(3) _cell_length_b 26.481(5) _cell_length_c 27.621(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.51(3) _cell_angle_gamma 90.00 _cell_volume 9988(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 20279 _cell_measurement_theta_min 1.669 _cell_measurement_theta_max 27.091 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4576 _exptl_absorpt_coefficient_mu 0.187 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9743 _exptl_absorpt_correction_T_max 0.9889 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 67812 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.02 _reflns_number_total 17609 _reflns_number_gt 13327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _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^)+(0.0839P)^2^+8.0852P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17609 _refine_ls_number_parameters 1394 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1569 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.04119(6) 0.39020(3) 0.51889(3) 0.03116(19) Uani 1 1 d . . . P2 P 0.10294(6) 0.33952(3) 0.85155(3) 0.0350(2) Uani 1 1 d . . . P3 P 0.14579(6) 0.10939(3) 0.55345(3) 0.0336(2) Uani 1 1 d . . . P4 P 0.14095(6) 0.05960(3) 0.76571(3) 0.0336(2) Uani 1 1 d D . . F1 F -0.01723(14) 0.39620(8) 0.56625(7) 0.0488(5) Uani 1 1 d . . . F2 F 0.14068(14) 0.38469(10) 0.55308(7) 0.0600(6) Uani 1 1 d . . . F3 F 0.02413(15) 0.33067(7) 0.52079(8) 0.0535(5) Uani 1 1 d . . . F4 F 0.09800(13) 0.38264(8) 0.47182(6) 0.0495(5) Uani 1 1 d . . . F5 F -0.05991(13) 0.39571(8) 0.48524(7) 0.0509(5) Uani 1 1 d . . . F6 F 0.05487(18) 0.44927(8) 0.51725(8) 0.0623(6) Uani 1 1 d . . . F7 F -0.01315(14) 0.33862(13) 0.83919(10) 0.0959(11) Uani 1 1 d . . . F8 F 0.0988(2) 0.38702(8) 0.88541(10) 0.0933(10) Uani 1 1 d . . . F9 F 0.08992(12) 0.30304(7) 0.89640(6) 0.0340(4) Uani 1 1 d . . . F10 F 0.21817(13) 0.33734(8) 0.86207(7) 0.0468(5) Uani 1 1 d . . . F11 F 0.10948(16) 0.29042(9) 0.81761(7) 0.0607(6) Uani 1 1 d . . . F12 F 0.11319(15) 0.37460(10) 0.80522(8) 0.0652(7) Uani 1 1 d . . . F13 F 0.1126(2) 0.16468(9) 0.56656(10) 0.0799(8) Uani 1 1 d . . . F14 F 0.05153(17) 0.08619(11) 0.57189(10) 0.0813(8) Uani 1 1 d . . . F15 F 0.2011(2) 0.10507(9) 0.60663(9) 0.0793(8) Uani 1 1 d . . . F16 F 0.18481(18) 0.05463(8) 0.54257(9) 0.0665(6) Uani 1 1 d . . . F17 F 0.24205(15) 0.13394(9) 0.53533(9) 0.0699(7) Uani 1 1 d . . . F18 F 0.09550(18) 0.11341(12) 0.50041(8) 0.0806(8) Uani 1 1 d . . . F19 F 0.09178(17) 0.01066(8) 0.74029(8) 0.0604(6) Uani 1 1 d D A . F20 F 0.19017(19) 0.10822(10) 0.79054(10) 0.0859(9) Uani 1 1 d D A . F21 F 0.0383(4) 0.0818(3) 0.7709(4) 0.093(4) Uani 0.61(2) 1 d PD A 1 F22 F 0.1494(11) 0.0331(4) 0.8160(2) 0.093(3) Uani 0.61(2) 1 d PD A 1 F23 F 0.2460(4) 0.0397(4) 0.7569(4) 0.084(3) Uani 0.61(2) 1 d PD A 1 F24 F 0.1386(7) 0.0838(4) 0.7135(2) 0.070(3) Uani 0.61(2) 1 d PD A 1 F21' F 0.0483(11) 0.0909(6) 0.7535(10) 0.142(8) Uani 0.39(2) 1 d P A 2 F22' F 0.085(2) 0.0427(6) 0.8130(6) 0.116(7) Uani 0.39(2) 1 d P A 2 F23' F 0.2264(16) 0.0238(7) 0.7811(11) 0.147(9) Uani 0.39(2) 1 d P A 2 F24' F 0.183(2) 0.0768(7) 0.7206(7) 0.129(8) Uani 0.39(2) 1 d P A 2 O1 O 0.79404(14) 0.21113(8) 0.52191(7) 0.0309(5) Uani 1 1 d . . . O2 O 0.80364(15) 0.10761(8) 0.50821(7) 0.0337(5) Uani 1 1 d . . . O3 O 0.81997(14) 0.03286(8) 0.58827(7) 0.0314(5) Uani 1 1 d . . . O4 O 0.81522(12) -0.02520(7) 0.67363(6) 0.0235(4) Uani 1 1 d . . . O5 O 0.62165(13) -0.04250(7) 0.67590(6) 0.0263(4) Uani 1 1 d . . . O6 O 0.51919(13) 0.02921(8) 0.57212(7) 0.0287(4) Uani 1 1 d . . . O7 O 0.46592(13) 0.12152(7) 0.52033(6) 0.0254(4) Uani 1 1 d . . . O8 O 0.59389(14) 0.20603(7) 0.51671(8) 0.0326(5) Uani 1 1 d . . . O9 O 0.88869(12) 0.17071(7) 0.81881(6) 0.0218(4) Uani 1 1 d . . . O10 O 1.00257(15) 0.12908(9) 0.90476(8) 0.0399(5) Uani 1 1 d . . . O11 O 0.48719(12) 0.13826(7) 0.81946(6) 0.0197(4) Uani 1 1 d . . . O12 O 0.37449(14) 0.21747(8) 0.86681(8) 0.0328(5) Uani 1 1 d . . . N1 N 0.08395(15) 0.62321(8) 0.30643(8) 0.0236(5) Uani 1 1 d . . . N2 N 0.58157(15) 0.59306(9) 0.28088(8) 0.0247(5) Uani 1 1 d . . . N3 N 0.67616(15) 0.83365(9) 0.32389(9) 0.0270(5) Uani 1 1 d . . . N4 N 0.18080(15) 0.86437(8) 0.34703(8) 0.0226(5) Uani 1 1 d . . . C1 C 0.7386(2) 0.25450(11) 0.52472(10) 0.0270(6) Uani 1 1 d . . . C2 C 0.7868(2) 0.30023(12) 0.53088(10) 0.0322(7) Uani 1 1 d . . . H2 H 0.8546 0.3014 0.5310 0.039 Uiso 1 1 calc R . . C3 C 0.7344(2) 0.34447(12) 0.53685(11) 0.0368(7) Uani 1 1 d . . . H3 H 0.7670 0.3752 0.5409 0.044 Uiso 1 1 calc R . . C4 C 0.6342(2) 0.34245(11) 0.53673(11) 0.0350(7) Uani 1 1 d . . . H4 H 0.5992 0.3718 0.5415 0.042 Uiso 1 1 calc R . . C5 C 0.5848(2) 0.29685(11) 0.52948(11) 0.0319(7) Uani 1 1 d . . . H5 H 0.5169 0.2959 0.5287 0.038 Uiso 1 1 calc R . . C6 C 0.6365(2) 0.25286(11) 0.52336(10) 0.0277(6) Uani 1 1 d . . . C7 C 0.4946(2) 0.20553(11) 0.49498(11) 0.0307(7) Uani 1 1 d . . . H7A H 0.4876 0.2282 0.4673 0.037 Uiso 1 1 calc R . . H7B H 0.4509 0.2168 0.5184 0.037 Uiso 1 1 calc R . . C8 C 0.4691(2) 0.15307(12) 0.47898(10) 0.0338(7) Uani 1 1 d . . . H8A H 0.4058 0.1529 0.4600 0.041 Uiso 1 1 calc R . . H8B H 0.5176 0.1405 0.4587 0.041 Uiso 1 1 calc R . . C9 C 0.43086(19) 0.07283(11) 0.50674(10) 0.0276(6) Uani 1 1 d . . . H9A H 0.4753 0.0567 0.4862 0.033 Uiso 1 1 calc R . . H9B H 0.3671 0.0755 0.4884 0.033 Uiso 1 1 calc R . . C10 C 0.42330(19) 0.04194(11) 0.55142(10) 0.0270(6) Uani 1 1 d . . . H10A H 0.3894 0.0610 0.5747 0.032 Uiso 1 1 calc R . . H10B H 0.3863 0.0114 0.5432 0.032 Uiso 1 1 calc R . . C11 C 0.51732(19) 0.00192(11) 0.61606(10) 0.0275(6) Uani 1 1 d . . . H11A H 0.4671 -0.0240 0.6125 0.033 Uiso 1 1 calc R . . H11B H 0.5029 0.0244 0.6421 0.033 Uiso 1 1 calc R . . C12 C 0.6158(2) -0.02173(12) 0.62753(10) 0.0294(6) Uani 1 1 d . . . H12A H 0.6254 -0.0482 0.6042 0.035 Uiso 1 1 calc R . . H12B H 0.6666 0.0034 0.6255 0.035 Uiso 1 1 calc R . . C13 C 0.67052(18) -0.01270(10) 0.71151(9) 0.0203(5) Uani 1 1 d . . . C14 C 0.77161(18) -0.00456(10) 0.71148(9) 0.0200(5) Uani 1 1 d . . . C15 C 0.90334(19) -0.00195(11) 0.65947(10) 0.0254(6) Uani 1 1 d . . . H15A H 0.9603 -0.0212 0.6723 0.030 Uiso 1 1 calc R . . H15B H 0.9095 0.0321 0.6723 0.030 Uiso 1 1 calc R . . C16 C 0.8969(2) -0.00091(11) 0.60488(10) 0.0305(7) Uani 1 1 d . . . H16A H 0.9584 0.0105 0.5941 0.037 Uiso 1 1 calc R . . H16B H 0.8832 -0.0345 0.5919 0.037 Uiso 1 1 calc R . . C17 C 0.7816(2) 0.02581(13) 0.53885(11) 0.0375(7) Uani 1 1 d . . . H17A H 0.7126 0.0347 0.5356 0.045 Uiso 1 1 calc R . . H17B H 0.7867 -0.0096 0.5306 0.045 Uiso 1 1 calc R . . C18 C 0.8329(2) 0.05661(11) 0.50341(11) 0.0342(7) Uani 1 1 d . . . H18A H 0.9033 0.0536 0.5104 0.041 Uiso 1 1 calc R . . H18B H 0.8151 0.0448 0.4705 0.041 Uiso 1 1 calc R . . C19 C 0.8478(2) 0.14134(11) 0.47708(10) 0.0313(7) Uani 1 1 d . . . H19A H 0.8481 0.1266 0.4449 0.038 Uiso 1 1 calc R . . H19B H 0.9150 0.1479 0.4897 0.038 Uiso 1 1 calc R . . C20 C 0.7907(2) 0.18935(12) 0.47418(10) 0.0332(7) Uani 1 1 d . . . H20A H 0.8184 0.2127 0.4521 0.040 Uiso 1 1 calc R . . H20B H 0.7233 0.1826 0.4619 0.040 Uiso 1 1 calc R . . C21 C 0.62039(18) 0.00373(9) 0.74993(9) 0.0198(5) Uani 1 1 d . . . H21 H 0.5535 -0.0021 0.7497 0.024 Uiso 1 1 calc R . . C22 C 0.67085(18) 0.02882(9) 0.78844(9) 0.0193(5) Uani 1 1 d . . . C23 C 0.62774(18) 0.05151(10) 0.83285(9) 0.0199(5) Uani 1 1 d . . . H23 H 0.5573 0.0455 0.8329 0.024 Uiso 1 1 calc R . . C24 C 0.68771(19) 0.02956(10) 0.87740(9) 0.0219(6) Uani 1 1 d . . . C25 C 0.6511(2) 0.00354(10) 0.91522(10) 0.0255(6) Uani 1 1 d . . . H25 H 0.5839 -0.0004 0.9161 0.031 Uiso 1 1 calc R . . C26 C 0.7167(2) -0.01658(11) 0.95186(10) 0.0298(6) Uani 1 1 d . . . H26 H 0.6931 -0.0338 0.9776 0.036 Uiso 1 1 calc R . . C27 C 0.8169(2) -0.01109(11) 0.95018(10) 0.0314(7) Uani 1 1 d . . . H27 H 0.8601 -0.0257 0.9742 0.038 Uiso 1 1 calc R . . C28 C 0.8531(2) 0.01627(10) 0.91260(10) 0.0265(6) Uani 1 1 d . . . H28 H 0.9202 0.0205 0.9117 0.032 Uiso 1 1 calc R . . C29 C 0.78816(19) 0.03709(10) 0.87674(9) 0.0221(6) Uani 1 1 d . . . C30 C 0.81463(18) 0.06714(10) 0.83281(9) 0.0198(5) Uani 1 1 d . . . H30 H 0.8851 0.0732 0.8330 0.024 Uiso 1 1 calc R . . C31 C 0.77161(17) 0.03742(9) 0.78840(9) 0.0187(5) Uani 1 1 d . . . C32 C 0.82228(18) 0.02074(10) 0.75057(9) 0.0200(5) Uani 1 1 d . . . H32 H 0.8893 0.0263 0.7511 0.024 Uiso 1 1 calc R . . C33 C 0.65351(17) 0.10735(10) 0.83022(9) 0.0184(5) Uani 1 1 d . . . C34 C 0.58726(17) 0.14718(10) 0.82228(9) 0.0175(5) Uani 1 1 d . . . C35 C 0.62215(17) 0.19479(10) 0.81227(9) 0.0191(5) Uani 1 1 d . . . C36 C 0.56089(17) 0.24159(9) 0.79768(9) 0.0185(5) Uani 1 1 d . . . H36 H 0.4904 0.2360 0.7984 0.022 Uiso 1 1 calc R . . C37 C 0.60032(17) 0.28393(10) 0.83121(9) 0.0189(5) Uani 1 1 d . . . C38 C 0.54634(19) 0.31368(10) 0.86009(9) 0.0236(6) Uani 1 1 d . . . H38 H 0.4795 0.3083 0.8608 0.028 Uiso 1 1 calc R . . C39 C 0.5936(2) 0.35181(11) 0.88815(10) 0.0271(6) Uani 1 1 d . . . H39 H 0.5579 0.3725 0.9071 0.032 Uiso 1 1 calc R . . C40 C 0.6938(2) 0.35894(11) 0.88792(10) 0.0275(6) Uani 1 1 d . . . H40 H 0.7248 0.3840 0.9074 0.033 Uiso 1 1 calc R . . C41 C 0.74846(19) 0.32916(10) 0.85902(9) 0.0226(6) Uani 1 1 d . . . H41 H 0.8156 0.3341 0.8590 0.027 Uiso 1 1 calc R . . C42 C 0.70111(18) 0.29192(10) 0.83022(9) 0.0196(5) Uani 1 1 d . . . C43 C 0.74761(18) 0.25607(10) 0.79554(9) 0.0200(5) Uani 1 1 d . . . H43 H 0.8181 0.2616 0.7948 0.024 Uiso 1 1 calc R . . C44 C 0.72311(17) 0.20305(10) 0.81183(9) 0.0184(5) Uani 1 1 d . . . C45 C 0.78929(17) 0.16370(10) 0.82178(9) 0.0185(5) Uani 1 1 d . . . C46 C 0.75456(17) 0.11563(10) 0.83027(9) 0.0189(5) Uani 1 1 d . . . C47 C 0.58895(18) 0.25598(9) 0.74723(9) 0.0201(5) Uani 1 1 d . . . C48 C 0.52564(19) 0.26231(10) 0.70533(10) 0.0235(6) Uani 1 1 d . . . H48 H 0.4584 0.2591 0.7065 0.028 Uiso 1 1 calc R . . C49 C 0.5635(2) 0.27355(11) 0.66140(10) 0.0263(6) Uani 1 1 d . . . H49 H 0.5214 0.2784 0.6333 0.032 Uiso 1 1 calc R . . C50 C 0.66421(19) 0.27755(10) 0.65963(10) 0.0254(6) Uani 1 1 d . . . H50 H 0.6893 0.2840 0.6301 0.030 Uiso 1 1 calc R . . C51 C 0.72811(19) 0.27197(10) 0.70212(10) 0.0224(6) Uani 1 1 d . . . H51 H 0.7954 0.2747 0.7010 0.027 Uiso 1 1 calc R . . C52 C 0.68970(18) 0.26232(10) 0.74573(9) 0.0199(5) Uani 1 1 d . . . C53 C 0.9390(2) 0.19913(12) 0.85870(12) 0.0342(7) Uani 1 1 d . . . H53A H 0.8960 0.2036 0.8843 0.041 Uiso 1 1 calc R . . H53B H 0.9564 0.2323 0.8473 0.041 Uiso 1 1 calc R . . C54 C 1.02903(19) 0.17179(11) 0.87820(11) 0.0308(7) Uani 1 1 d . . . H54A H 1.0656 0.1612 0.8516 0.037 Uiso 1 1 calc R . . H54B H 1.0703 0.1940 0.8992 0.037 Uiso 1 1 calc R . . C55 C 1.0861(3) 0.09882(14) 0.91952(13) 0.0508(9) Uani 1 1 d . . . H55A H 1.1112 0.0844 0.8914 0.076 Uiso 1 1 calc R . . H55B H 1.0677 0.0723 0.9405 0.076 Uiso 1 1 calc R . . H55C H 1.1357 0.1194 0.9366 0.076 Uiso 1 1 calc R . . C56 C 0.44947(19) 0.13343(11) 0.86665(10) 0.0243(6) Uani 1 1 d . . . H56A H 0.4922 0.1114 0.8871 0.029 Uiso 1 1 calc R . . H56B H 0.3852 0.1179 0.8625 0.029 Uiso 1 1 calc R . . C57 C 0.4421(2) 0.18376(11) 0.89158(10) 0.0293(6) Uani 1 1 d . . . H57A H 0.4230 0.1781 0.9241 0.035 Uiso 1 1 calc R . . H57B H 0.5063 0.1995 0.8949 0.035 Uiso 1 1 calc R . . C58 C 0.2758(2) 0.20508(13) 0.87395(12) 0.0356(7) Uani 1 1 d . . . H58A H 0.2572 0.1747 0.8565 0.053 Uiso 1 1 calc R . . H58B H 0.2334 0.2321 0.8622 0.053 Uiso 1 1 calc R . . H58C H 0.2702 0.2001 0.9080 0.053 Uiso 1 1 calc R . . C59 C 0.11534(19) 0.62449(10) 0.26169(10) 0.0241(6) Uani 1 1 d . . . H59 H 0.0721 0.6330 0.2350 0.029 Uiso 1 1 calc R . . C60 C 0.21071(18) 0.61326(10) 0.25548(10) 0.0221(6) Uani 1 1 d . . . H60 H 0.2319 0.6145 0.2245 0.027 Uiso 1 1 calc R . . C61 C 0.27665(18) 0.59993(10) 0.29519(10) 0.0208(5) Uani 1 1 d . . . C62 C 0.23891(19) 0.59472(11) 0.33995(10) 0.0259(6) Uani 1 1 d . . . H62 H 0.2788 0.5830 0.3667 0.031 Uiso 1 1 calc R . . C63 C 0.1428(2) 0.60688(11) 0.34467(10) 0.0279(6) Uani 1 1 d . . . H63 H 0.1184 0.6037 0.3748 0.033 Uiso 1 1 calc R . . C64 C 0.38258(19) 0.59470(10) 0.28964(10) 0.0216(6) Uani 1 1 d . . . C65 C 0.42009(19) 0.60785(10) 0.24623(10) 0.0244(6) Uani 1 1 d . . . H65 H 0.3777 0.6174 0.2195 0.029 Uiso 1 1 calc R . . C66 C 0.51913(19) 0.60676(11) 0.24271(10) 0.0260(6) Uani 1 1 d . . . H66 H 0.5433 0.6156 0.2136 0.031 Uiso 1 1 calc R . . C67 C 0.5479(2) 0.57854(11) 0.32255(11) 0.0308(7) Uani 1 1 d . . . H67 H 0.5918 0.5679 0.3483 0.037 Uiso 1 1 calc R . . C68 C 0.44960(19) 0.57900(11) 0.32801(10) 0.0286(6) Uani 1 1 d . . . H68 H 0.4275 0.5689 0.3573 0.034 Uiso 1 1 calc R . . C69 C 0.68957(19) 0.59830(11) 0.27730(11) 0.0301(7) Uani 1 1 d . . . H69A H 0.7052 0.5884 0.2451 0.036 Uiso 1 1 calc R . . H69B H 0.7255 0.5765 0.3010 0.036 Uiso 1 1 calc R . . C70 C 0.71830(17) 0.65272(11) 0.28690(10) 0.0251(6) Uani 1 1 d . . . C71 C 0.74486(18) 0.66954(11) 0.33385(10) 0.0281(6) Uani 1 1 d . . . H71 H 0.7492 0.6467 0.3595 0.034 Uiso 1 1 calc R . . C72 C 0.76505(19) 0.72015(12) 0.34288(11) 0.0287(6) Uani 1 1 d . . . H72 H 0.7837 0.7309 0.3745 0.034 Uiso 1 1 calc R . . C73 C 0.75759(17) 0.75496(11) 0.30499(10) 0.0257(6) Uani 1 1 d . . . C74 C 0.73301(18) 0.73791(11) 0.25782(10) 0.0273(6) Uani 1 1 d . . . H74 H 0.7297 0.7607 0.2321 0.033 Uiso 1 1 calc R . . C75 C 0.71355(18) 0.68753(11) 0.24879(10) 0.0275(6) Uani 1 1 d . . . H75 H 0.6971 0.6766 0.2170 0.033 Uiso 1 1 calc R . . C76 C 0.77295(19) 0.81039(11) 0.31495(12) 0.0315(7) Uani 1 1 d . . . H76A H 0.7987 0.8265 0.2873 0.038 Uiso 1 1 calc R . . H76B H 0.8197 0.8150 0.3432 0.038 Uiso 1 1 calc R . . C77 C 0.6400(2) 0.82471(11) 0.36666(10) 0.0289(6) Uani 1 1 d . . . H77 H 0.6794 0.8095 0.3918 0.035 Uiso 1 1 calc R . . C78 C 0.54572(19) 0.83778(11) 0.37370(10) 0.0256(6) Uani 1 1 d . . . H78 H 0.5215 0.8314 0.4034 0.031 Uiso 1 1 calc R . . C79 C 0.48634(19) 0.86067(10) 0.33635(10) 0.0221(6) Uani 1 1 d . . . C80 C 0.52858(19) 0.87326(11) 0.29399(10) 0.0255(6) Uani 1 1 d . . . H80 H 0.4927 0.8914 0.2696 0.031 Uiso 1 1 calc R . . C81 C 0.62307(19) 0.85894(11) 0.28828(10) 0.0279(6) Uani 1 1 d . . . H81 H 0.6504 0.8668 0.2597 0.034 Uiso 1 1 calc R . . C82 C 0.37984(19) 0.86660(10) 0.34055(9) 0.0211(6) Uani 1 1 d . . . C83 C 0.3424(2) 0.86761(10) 0.38546(10) 0.0248(6) Uani 1 1 d . . . H83 H 0.3846 0.8694 0.4138 0.030 Uiso 1 1 calc R . . C84 C 0.2425(2) 0.86604(10) 0.38796(10) 0.0258(6) Uani 1 1 d . . . H84 H 0.2176 0.8661 0.4181 0.031 Uiso 1 1 calc R . . C85 C 0.21485(19) 0.86542(10) 0.30286(10) 0.0229(6) Uani 1 1 d . . . H85 H 0.1710 0.8652 0.2750 0.027 Uiso 1 1 calc R . . C86 C 0.31360(18) 0.86674(10) 0.29868(10) 0.0224(6) Uani 1 1 d . . . H86 H 0.3366 0.8677 0.2681 0.027 Uiso 1 1 calc R . . C87 C 0.07290(19) 0.85825(11) 0.35005(11) 0.0275(6) Uani 1 1 d . . . H87A H 0.0371 0.8797 0.3261 0.033 Uiso 1 1 calc R . . H87B H 0.0565 0.8684 0.3820 0.033 Uiso 1 1 calc R . . C88 C 0.04406(17) 0.80389(10) 0.34087(10) 0.0233(6) Uani 1 1 d . . . C89 C 0.01603(18) 0.78709(11) 0.29393(10) 0.0250(6) Uani 1 1 d . . . H89 H 0.0109 0.8099 0.2682 0.030 Uiso 1 1 calc R . . C90 C -0.00438(18) 0.73628(11) 0.28525(10) 0.0253(6) Uani 1 1 d . . . H90 H -0.0223 0.7252 0.2537 0.030 Uiso 1 1 calc R . . C91 C 0.00184(17) 0.70201(10) 0.32346(10) 0.0225(6) Uani 1 1 d . . . C92 C 0.02699(19) 0.71926(11) 0.37041(10) 0.0256(6) Uani 1 1 d . . . H92 H 0.0298 0.6966 0.3963 0.031 Uiso 1 1 calc R . . C93 C 0.04795(18) 0.76986(11) 0.37928(10) 0.0257(6) Uani 1 1 d . . . H93 H 0.0646 0.7810 0.4109 0.031 Uiso 1 1 calc R . . C94 C -0.01372(18) 0.64604(11) 0.31400(11) 0.0269(6) Uani 1 1 d . . . H94A H -0.0405 0.6302 0.3415 0.032 Uiso 1 1 calc R . . H94B H -0.0593 0.6410 0.2853 0.032 Uiso 1 1 calc R . . N5 N 0.0834(2) 0.46779(13) 0.66393(13) 0.0590(9) Uani 1 1 d . . . N6 N 0.2006(2) 0.76251(12) -0.04188(11) 0.0482(7) Uani 1 1 d . . . N7 N 0.0785(3) 0.93949(16) 0.93797(13) 0.0707(10) Uani 1 1 d . . . N8 N 0.1130(2) 0.92304(12) 0.64525(11) 0.0502(8) Uani 1 1 d . . . C95 C 0.1253(2) 0.48627(14) 0.63486(15) 0.0447(9) Uani 1 1 d . . . C96 C 0.1776(3) 0.51010(15) 0.59766(15) 0.0561(10) Uani 1 1 d . . . H96A H 0.1321 0.5280 0.5753 0.084 Uiso 1 1 calc R . . H96B H 0.2103 0.4847 0.5804 0.084 Uiso 1 1 calc R . . H96C H 0.2251 0.5333 0.6127 0.084 Uiso 1 1 calc R . . C97 C 0.2636(3) 0.75492(13) -0.01295(13) 0.0423(8) Uani 1 1 d . . . C98 C 0.3437(3) 0.74558(15) 0.02414(15) 0.0613(11) Uani 1 1 d . . . H98A H 0.3942 0.7703 0.0215 0.092 Uiso 1 1 d R . . H98B H 0.3698 0.7124 0.0197 0.092 Uiso 1 1 d R . . H98C H 0.3202 0.7478 0.0557 0.092 Uiso 1 1 d R . . C99 C 0.1154(2) 0.91564(15) 0.96875(13) 0.0447(8) Uani 1 1 d . . . C100 C 0.1615(2) 0.88465(13) 1.00796(13) 0.0453(8) Uani 1 1 d . . . H10C H 0.1174 0.8806 1.0327 0.068 Uiso 1 1 calc R . . H10D H 0.2205 0.9007 1.0217 0.068 Uiso 1 1 calc R . . H10E H 0.1770 0.8521 0.9954 0.068 Uiso 1 1 calc R . . C101 C 0.1748(2) 0.95133(13) 0.64572(11) 0.0359(7) Uani 1 1 d . . . C102 C 0.2552(3) 0.98684(15) 0.64655(15) 0.0537(10) Uani 1 1 d . . . H10F H 0.3108 0.9735 0.6662 0.080 Uiso 1 1 calc R . . H10G H 0.2360 1.0183 0.6600 0.080 Uiso 1 1 calc R . . H10H H 0.2722 0.9922 0.6140 0.080 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 P1 0.0359(4) 0.0331(5) 0.0258(4) -0.0001(3) 0.0095(3) -0.0032(3) P2 0.0332(4) 0.0454(5) 0.0268(4) 0.0075(4) 0.0059(3) 0.0083(4) P3 0.0308(4) 0.0349(5) 0.0357(4) -0.0053(4) 0.0057(3) 0.0027(3) P4 0.0354(4) 0.0329(5) 0.0320(4) -0.0029(3) 0.0003(3) -0.0042(3) F1 0.0622(12) 0.0502(12) 0.0377(11) -0.0007(9) 0.0245(9) 0.0094(10) F2 0.0455(11) 0.0943(18) 0.0388(11) -0.0071(11) -0.0036(9) 0.0080(11) F3 0.0699(13) 0.0330(11) 0.0615(13) 0.0002(10) 0.0270(11) 0.0003(10) F4 0.0438(10) 0.0757(15) 0.0313(10) -0.0027(10) 0.0157(8) -0.0076(10) F5 0.0435(10) 0.0633(14) 0.0454(12) -0.0095(10) 0.0012(9) 0.0092(10) F6 0.0939(17) 0.0371(12) 0.0565(14) 0.0000(10) 0.0096(12) -0.0181(11) F7 0.0307(11) 0.169(3) 0.0897(18) 0.083(2) 0.0171(11) 0.0267(14) F8 0.182(3) 0.0304(12) 0.0811(18) 0.0050(12) 0.0820(19) 0.0165(15) F9 0.0412(9) 0.0342(10) 0.0267(9) 0.0020(8) 0.0040(7) 0.0021(8) F10 0.0349(9) 0.0641(14) 0.0404(11) 0.0052(10) -0.0016(8) -0.0097(9) F11 0.0683(13) 0.0810(17) 0.0337(11) -0.0217(11) 0.0097(9) -0.0229(12) F12 0.0589(13) 0.0913(18) 0.0480(13) 0.0399(12) 0.0180(10) 0.0193(12) F13 0.109(2) 0.0461(14) 0.0907(19) 0.0016(13) 0.0394(15) 0.0321(14) F14 0.0636(14) 0.100(2) 0.0875(18) -0.0169(16) 0.0425(13) -0.0290(14) F15 0.125(2) 0.0524(15) 0.0540(14) -0.0070(12) -0.0276(14) -0.0138(14) F16 0.0875(16) 0.0407(13) 0.0712(16) -0.0173(11) 0.0077(12) 0.0092(12) F17 0.0481(12) 0.0702(17) 0.0954(19) -0.0035(14) 0.0272(12) -0.0080(11) F18 0.0746(16) 0.121(2) 0.0433(13) 0.0133(14) -0.0116(11) 0.0018(15) F19 0.0841(15) 0.0376(12) 0.0582(14) -0.0077(10) 0.0000(11) -0.0179(11) F20 0.0822(17) 0.0828(19) 0.094(2) -0.0530(16) 0.0155(14) -0.0396(15) F21 0.037(3) 0.077(5) 0.173(8) -0.069(6) 0.050(4) -0.020(3) F22 0.158(8) 0.095(5) 0.025(3) 0.013(3) -0.007(4) -0.028(6) F23 0.046(3) 0.093(6) 0.113(6) -0.021(4) 0.001(3) 0.023(3) F24 0.118(6) 0.047(3) 0.042(3) 0.018(3) -0.005(4) -0.017(4) F21' 0.090(10) 0.094(8) 0.232(18) 0.032(10) -0.032(10) 0.062(8) F22' 0.203(18) 0.094(9) 0.061(7) -0.008(6) 0.071(9) -0.039(11) F23' 0.118(13) 0.105(10) 0.20(2) 0.007(12) -0.090(12) 0.052(10) F24' 0.203(19) 0.087(12) 0.120(13) -0.050(9) 0.134(12) -0.086(12) O1 0.0372(11) 0.0295(11) 0.0248(11) -0.0012(9) -0.0035(8) 0.0057(9) O2 0.0507(12) 0.0261(11) 0.0259(11) 0.0003(9) 0.0122(9) 0.0024(10) O3 0.0450(12) 0.0256(11) 0.0236(10) 0.0003(8) 0.0035(9) 0.0028(9) O4 0.0262(9) 0.0208(10) 0.0245(10) -0.0029(8) 0.0072(7) 0.0004(8) O5 0.0331(10) 0.0254(11) 0.0197(10) -0.0029(8) -0.0009(8) -0.0050(8) O6 0.0233(9) 0.0321(11) 0.0300(11) 0.0057(9) -0.0008(8) 0.0005(8) O7 0.0300(10) 0.0249(10) 0.0214(10) -0.0017(8) 0.0026(8) -0.0051(8) O8 0.0314(10) 0.0229(11) 0.0419(12) 0.0007(9) -0.0043(9) 0.0001(9) O9 0.0160(8) 0.0216(10) 0.0279(10) -0.0019(8) 0.0032(7) -0.0021(7) O10 0.0356(11) 0.0444(14) 0.0384(13) 0.0098(10) -0.0040(9) -0.0056(10) O11 0.0179(8) 0.0219(10) 0.0199(9) 0.0004(8) 0.0051(7) -0.0016(7) O12 0.0292(10) 0.0298(11) 0.0410(12) 0.0035(9) 0.0118(9) 0.0025(9) N1 0.0237(11) 0.0185(12) 0.0292(13) -0.0036(10) 0.0058(9) -0.0027(9) N2 0.0233(11) 0.0194(12) 0.0312(13) -0.0018(10) 0.0024(9) 0.0010(9) N3 0.0214(11) 0.0274(13) 0.0319(13) -0.0067(11) 0.0016(10) -0.0042(10) N4 0.0252(11) 0.0168(11) 0.0267(12) -0.0018(9) 0.0066(9) 0.0016(9) C1 0.0330(14) 0.0269(15) 0.0209(14) 0.0018(12) 0.0006(11) 0.0053(12) C2 0.0344(15) 0.0329(17) 0.0283(16) 0.0033(13) -0.0021(12) -0.0028(13) C3 0.0507(19) 0.0246(16) 0.0341(17) 0.0023(13) -0.0014(14) -0.0045(14) C4 0.0484(18) 0.0209(15) 0.0355(17) 0.0031(13) 0.0030(14) 0.0065(14) C5 0.0337(15) 0.0303(17) 0.0310(16) 0.0036(13) -0.0006(12) 0.0041(13) C6 0.0366(15) 0.0224(15) 0.0236(15) 0.0003(12) 0.0007(12) -0.0005(12) C7 0.0311(14) 0.0306(17) 0.0294(16) 0.0064(13) -0.0026(12) -0.0013(13) C8 0.0422(17) 0.0377(18) 0.0208(15) 0.0061(13) -0.0008(12) -0.0076(14) C9 0.0258(13) 0.0269(15) 0.0291(15) -0.0054(12) -0.0020(11) -0.0010(12) C10 0.0226(13) 0.0230(15) 0.0343(16) -0.0012(12) -0.0022(11) -0.0020(11) C11 0.0281(14) 0.0237(15) 0.0308(15) 0.0031(12) 0.0044(12) 0.0006(12) C12 0.0301(14) 0.0373(17) 0.0204(14) -0.0006(13) 0.0003(11) 0.0018(13) C13 0.0260(13) 0.0161(13) 0.0181(13) 0.0007(10) -0.0012(10) -0.0016(11) C14 0.0248(13) 0.0153(13) 0.0205(13) 0.0023(10) 0.0055(10) 0.0030(11) C15 0.0242(13) 0.0239(15) 0.0293(15) 0.0028(12) 0.0085(11) 0.0014(11) C16 0.0387(15) 0.0229(15) 0.0322(16) 0.0016(13) 0.0149(13) 0.0016(13) C17 0.0509(18) 0.0334(18) 0.0273(16) -0.0028(14) -0.0011(13) -0.0070(15) C18 0.0561(19) 0.0232(16) 0.0237(15) -0.0034(12) 0.0055(13) 0.0027(14) C19 0.0370(15) 0.0319(17) 0.0257(15) 0.0008(13) 0.0068(12) 0.0022(13) C20 0.0424(16) 0.0317(17) 0.0254(15) 0.0025(13) 0.0028(12) 0.0030(14) C21 0.0204(12) 0.0143(13) 0.0249(14) 0.0018(11) 0.0024(10) -0.0004(10) C22 0.0231(12) 0.0139(13) 0.0212(13) 0.0041(10) 0.0035(10) 0.0028(10) C23 0.0185(12) 0.0161(13) 0.0256(14) 0.0004(11) 0.0048(10) -0.0004(10) C24 0.0294(13) 0.0150(13) 0.0217(14) -0.0028(11) 0.0037(11) 0.0025(11) C25 0.0363(15) 0.0182(14) 0.0230(14) -0.0004(11) 0.0088(11) -0.0004(12) C26 0.0501(17) 0.0191(14) 0.0207(14) 0.0006(12) 0.0069(12) 0.0027(13) C27 0.0462(17) 0.0227(15) 0.0237(15) 0.0013(12) -0.0044(12) 0.0055(13) C28 0.0331(14) 0.0213(14) 0.0243(14) -0.0015(12) -0.0018(11) 0.0012(12) C29 0.0288(13) 0.0165(13) 0.0209(14) -0.0014(11) 0.0014(11) 0.0012(11) C30 0.0195(12) 0.0194(14) 0.0203(13) 0.0002(11) 0.0003(10) 0.0018(11) C31 0.0205(12) 0.0129(12) 0.0224(13) 0.0016(10) 0.0004(10) 0.0014(10) C32 0.0181(12) 0.0174(13) 0.0243(14) 0.0032(11) 0.0012(10) 0.0014(10) C33 0.0218(12) 0.0158(13) 0.0181(13) -0.0004(10) 0.0041(10) -0.0020(10) C34 0.0175(11) 0.0199(13) 0.0154(12) -0.0001(10) 0.0033(9) -0.0005(10) C35 0.0193(12) 0.0209(14) 0.0174(13) -0.0011(11) 0.0026(10) 0.0023(11) C36 0.0186(12) 0.0136(13) 0.0236(14) 0.0009(10) 0.0028(10) 0.0007(10) C37 0.0219(12) 0.0169(13) 0.0179(13) 0.0038(10) 0.0010(10) 0.0005(10) C38 0.0255(13) 0.0236(15) 0.0222(14) 0.0017(11) 0.0057(11) 0.0038(11) C39 0.0323(14) 0.0243(15) 0.0248(15) -0.0022(12) 0.0042(11) 0.0040(12) C40 0.0373(15) 0.0211(14) 0.0235(14) -0.0015(12) -0.0010(12) -0.0013(12) C41 0.0255(13) 0.0200(14) 0.0221(14) 0.0009(11) 0.0006(10) -0.0009(11) C42 0.0235(12) 0.0172(13) 0.0180(13) 0.0033(10) 0.0018(10) 0.0023(11) C43 0.0190(12) 0.0179(14) 0.0235(14) 0.0002(11) 0.0035(10) -0.0019(10) C44 0.0206(12) 0.0174(13) 0.0171(13) -0.0004(10) 0.0012(10) 0.0002(10) C45 0.0171(11) 0.0200(13) 0.0186(13) -0.0021(11) 0.0026(9) -0.0014(10) C46 0.0197(12) 0.0187(13) 0.0181(13) 0.0005(10) 0.0002(10) 0.0002(10) C47 0.0241(13) 0.0127(12) 0.0240(14) 0.0008(11) 0.0055(10) -0.0003(10) C48 0.0233(13) 0.0207(14) 0.0261(14) -0.0025(11) 0.0001(11) -0.0010(11) C49 0.0324(14) 0.0259(15) 0.0196(14) 0.0000(12) -0.0024(11) -0.0033(12) C50 0.0336(14) 0.0211(14) 0.0223(14) -0.0003(11) 0.0070(11) -0.0044(12) C51 0.0241(12) 0.0177(14) 0.0259(14) -0.0007(11) 0.0056(11) -0.0028(11) C52 0.0221(12) 0.0138(13) 0.0235(14) -0.0015(11) 0.0015(10) 0.0002(10) C53 0.0268(14) 0.0259(16) 0.0478(19) -0.0094(14) -0.0066(13) -0.0025(13) C54 0.0240(13) 0.0328(17) 0.0347(16) -0.0010(13) -0.0020(12) -0.0017(12) C55 0.055(2) 0.050(2) 0.043(2) 0.0074(17) -0.0190(16) 0.0062(18) C56 0.0226(13) 0.0261(15) 0.0256(14) 0.0055(12) 0.0100(11) 0.0016(11) C57 0.0263(14) 0.0334(17) 0.0288(15) -0.0014(13) 0.0058(11) 0.0012(13) C58 0.0281(14) 0.0385(18) 0.0409(18) -0.0043(15) 0.0068(13) 0.0038(13) C59 0.0269(13) 0.0199(14) 0.0252(14) -0.0021(11) 0.0009(11) -0.0029(11) C60 0.0253(13) 0.0184(13) 0.0232(14) -0.0021(11) 0.0053(11) -0.0029(11) C61 0.0247(13) 0.0133(13) 0.0245(14) -0.0025(11) 0.0029(10) -0.0011(11) C62 0.0300(14) 0.0240(15) 0.0240(14) 0.0041(12) 0.0050(11) 0.0026(12) C63 0.0302(14) 0.0274(16) 0.0273(15) 0.0029(12) 0.0101(12) -0.0007(12) C64 0.0268(13) 0.0148(13) 0.0232(14) -0.0022(11) 0.0024(11) -0.0007(11) C65 0.0241(13) 0.0229(14) 0.0258(14) 0.0012(12) 0.0012(11) 0.0018(11) C66 0.0262(13) 0.0239(15) 0.0282(15) -0.0003(12) 0.0045(11) 0.0006(12) C67 0.0282(14) 0.0311(17) 0.0324(16) 0.0052(13) -0.0006(12) 0.0016(13) C68 0.0284(14) 0.0312(16) 0.0263(15) 0.0068(13) 0.0034(11) -0.0006(12) C69 0.0194(13) 0.0317(17) 0.0394(17) -0.0036(13) 0.0035(12) 0.0036(12) C70 0.0149(12) 0.0305(16) 0.0305(15) -0.0020(12) 0.0054(10) 0.0032(11) C71 0.0207(13) 0.0344(17) 0.0293(15) 0.0009(13) 0.0035(11) 0.0037(12) C72 0.0216(13) 0.0367(17) 0.0277(15) -0.0057(13) 0.0023(11) 0.0041(12) C73 0.0141(12) 0.0303(16) 0.0332(16) -0.0064(13) 0.0042(11) 0.0014(11) C74 0.0218(13) 0.0332(16) 0.0280(15) 0.0026(13) 0.0078(11) -0.0006(12) C75 0.0214(13) 0.0352(17) 0.0267(15) -0.0044(13) 0.0059(11) 0.0001(12) C76 0.0184(13) 0.0305(17) 0.0458(18) -0.0089(14) 0.0043(12) -0.0015(12) C77 0.0288(14) 0.0294(16) 0.0276(15) -0.0057(13) -0.0025(12) 0.0000(12) C78 0.0290(14) 0.0269(15) 0.0206(14) -0.0039(12) 0.0003(11) 0.0015(12) C79 0.0269(13) 0.0163(13) 0.0233(14) -0.0064(11) 0.0034(11) -0.0054(11) C80 0.0265(13) 0.0252(15) 0.0246(14) -0.0015(12) 0.0010(11) -0.0025(12) C81 0.0270(14) 0.0275(16) 0.0296(15) -0.0031(13) 0.0044(12) -0.0073(12) C82 0.0271(13) 0.0128(13) 0.0237(14) 0.0001(11) 0.0036(11) 0.0004(11) C83 0.0317(14) 0.0225(14) 0.0201(14) -0.0021(11) 0.0021(11) 0.0000(12) C84 0.0323(14) 0.0217(14) 0.0243(15) -0.0029(12) 0.0084(11) 0.0008(12) C85 0.0253(13) 0.0203(14) 0.0229(14) -0.0008(11) 0.0022(11) 0.0005(11) C86 0.0258(13) 0.0217(14) 0.0203(13) 0.0010(11) 0.0047(10) 0.0002(11) C87 0.0228(13) 0.0233(15) 0.0377(17) -0.0012(13) 0.0105(12) 0.0043(11) C88 0.0154(11) 0.0250(15) 0.0303(15) -0.0020(12) 0.0066(10) 0.0028(11) C89 0.0232(13) 0.0241(15) 0.0285(15) 0.0046(12) 0.0060(11) 0.0036(11) C90 0.0213(12) 0.0327(16) 0.0218(14) -0.0027(12) 0.0014(10) 0.0021(12) C91 0.0145(11) 0.0225(14) 0.0312(15) -0.0017(12) 0.0051(10) -0.0011(10) C92 0.0267(13) 0.0261(15) 0.0245(15) 0.0032(12) 0.0044(11) 0.0004(12) C93 0.0250(13) 0.0292(16) 0.0230(14) -0.0025(12) 0.0028(11) -0.0011(12) C94 0.0186(12) 0.0279(16) 0.0350(16) -0.0057(13) 0.0066(11) -0.0030(11) N5 0.062(2) 0.0434(19) 0.070(2) 0.0006(17) -0.0046(18) -0.0097(16) N6 0.0554(18) 0.0434(18) 0.0476(18) -0.0038(15) 0.0145(15) -0.0047(15) N7 0.073(2) 0.091(3) 0.045(2) -0.008(2) -0.0089(17) -0.001(2) N8 0.0476(17) 0.056(2) 0.0499(18) -0.0086(15) 0.0199(14) -0.0073(16) C95 0.0391(18) 0.0341(19) 0.058(2) -0.0087(18) -0.0111(17) 0.0027(16) C96 0.052(2) 0.053(2) 0.063(3) -0.014(2) 0.0054(18) -0.0062(19) C97 0.055(2) 0.0342(19) 0.039(2) 0.0005(15) 0.0131(17) -0.0092(16) C98 0.077(3) 0.048(2) 0.056(2) 0.0117(19) -0.010(2) -0.016(2) C99 0.0415(18) 0.054(2) 0.038(2) -0.0150(18) 0.0041(15) -0.0093(17) C100 0.0488(19) 0.038(2) 0.052(2) -0.0104(17) 0.0155(16) 0.0045(16) C101 0.0367(17) 0.0410(19) 0.0317(17) 0.0017(14) 0.0118(13) 0.0060(15) C102 0.054(2) 0.049(2) 0.061(2) 0.0054(19) 0.0180(18) -0.0088(18) _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 P1 F6 1.577(2) . ? P1 F2 1.590(2) . ? P1 F4 1.5911(19) . ? P1 F3 1.595(2) . ? P1 F5 1.601(2) . ? P1 F1 1.6063(19) . ? P2 F8 1.572(2) . ? P2 F10 1.5808(19) . ? P2 F9 1.5944(18) . ? P2 F7 1.597(2) . ? P2 F12 1.598(2) . ? P2 F11 1.610(2) . ? P3 F14 1.561(2) . ? P3 F18 1.562(2) . ? P3 F16 1.584(2) . ? P3 F13 1.586(2) . ? P3 F15 1.592(2) . ? P3 F17 1.595(2) . ? P4 F24' 1.496(12) . ? P4 F21' 1.528(10) . ? P4 F23' 1.536(11) . ? P4 F21 1.546(5) . ? P4 F22 1.550(5) . ? P4 F23 1.574(5) . ? P4 F24 1.576(5) . ? P4 F20 1.580(2) . ? P4 F19 1.593(2) . ? P4 F22' 1.636(11) . ? O1 C1 1.384(3) . ? O1 C20 1.436(3) . ? O2 C19 1.416(3) . ? O2 C18 1.419(3) . ? O3 C16 1.425(3) . ? O3 C17 1.427(3) . ? O4 C14 1.367(3) . ? O4 C15 1.444(3) . ? O5 C13 1.383(3) . ? O5 C12 1.440(3) . ? O6 C11 1.415(3) . ? O6 C10 1.424(3) . ? O7 C9 1.414(3) . ? O7 C8 1.419(3) . ? O8 C6 1.375(3) . ? O8 C7 1.435(3) . ? O9 C45 1.386(3) . ? O9 C53 1.453(3) . ? O10 C54 1.414(4) . ? O10 C55 1.426(4) . ? O11 C34 1.388(3) . ? O11 C56 1.453(3) . ? O12 C57 1.416(3) . ? O12 C58 1.425(3) . ? N1 C63 1.338(4) . ? N1 C59 1.347(3) . ? N1 C94 1.503(3) . ? N2 C67 1.337(4) . ? N2 C66 1.343(4) . ? N2 C69 1.501(3) . ? N3 C81 1.345(4) . ? N3 C77 1.346(4) . ? N3 C76 1.506(3) . ? N4 C84 1.346(4) . ? N4 C85 1.348(3) . ? N4 C87 1.499(3) . ? C1 C2 1.382(4) . ? C1 C6 1.399(4) . ? C2 C3 1.393(4) . ? C2 H2 0.9300 . ? C3 C4 1.376(4) . ? C3 H3 0.9300 . ? C4 C5 1.390(4) . ? C4 H4 0.9300 . ? C5 C6 1.383(4) . ? C5 H5 0.9300 . ? C7 C8 1.489(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.493(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.495(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C21 1.389(4) . ? C13 C14 1.404(3) . ? C14 C32 1.398(4) . ? C15 C16 1.502(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.501(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.492(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.382(4) . ? C21 H21 0.9300 . ? C22 C31 1.401(3) . ? C22 C23 1.535(3) . ? C23 C33 1.524(3) . ? C23 C24 1.528(4) . ? C23 H23 0.9800 . ? C24 C25 1.385(4) . ? C24 C29 1.394(4) . ? C25 C26 1.394(4) . ? C25 H25 0.9300 . ? C26 C27 1.388(4) . ? C26 H26 0.9300 . ? C27 C28 1.395(4) . ? C27 H27 0.9300 . ? C28 C29 1.382(4) . ? C28 H28 0.9300 . ? C29 C30 1.524(4) . ? C30 C46 1.524(4) . ? C30 C31 1.527(4) . ? C30 H30 0.9800 . ? C31 C32 1.382(4) . ? C32 H32 0.9300 . ? C33 C34 1.396(4) . ? C33 C46 1.403(3) . ? C34 C35 1.386(4) . ? C35 C44 1.403(3) . ? C35 C36 1.529(3) . ? C36 C37 1.520(4) . ? C36 C47 1.529(3) . ? C36 H36 0.9800 . ? C37 C38 1.385(4) . ? C37 C42 1.402(3) . ? C38 C39 1.395(4) . ? C38 H38 0.9300 . ? C39 C40 1.387(4) . ? C39 H39 0.9300 . ? C40 C41 1.392(4) . ? C40 H40 0.9300 . ? C41 C42 1.389(4) . ? C41 H41 0.9300 . ? C42 C43 1.531(4) . ? C43 C44 1.522(3) . ? C43 C52 1.530(4) . ? C43 H43 0.9800 . ? C44 C45 1.392(4) . ? C45 C46 1.387(4) . ? C47 C48 1.389(4) . ? C47 C52 1.397(3) . ? C48 C49 1.397(4) . ? C48 H48 0.9300 . ? C49 C50 1.391(4) . ? C49 H49 0.9300 . ? C50 C51 1.404(4) . ? C50 H50 0.9300 . ? C51 C52 1.384(4) . ? C51 H51 0.9300 . ? C53 C54 1.487(4) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C57 1.508(4) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.368(4) . ? C59 H59 0.9300 . ? C60 C61 1.398(4) . ? C60 H60 0.9300 . ? C61 C62 1.392(4) . ? C61 C64 1.482(3) . ? C62 C63 1.376(4) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 C65 1.394(4) . ? C64 C68 1.398(4) . ? C65 C66 1.372(4) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C68 1.371(4) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C70 1.511(4) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 C71 1.387(4) . ? C70 C75 1.396(4) . ? C71 C72 1.386(4) . ? C71 H71 0.9300 . ? C72 C73 1.391(4) . ? C72 H72 0.9300 . ? C73 C74 1.389(4) . ? C73 C76 1.504(4) . ? C74 C75 1.378(4) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C77 C78 1.370(4) . ? C77 H77 0.9300 . ? C78 C79 1.391(4) . ? C78 H78 0.9300 . ? C79 C80 1.395(4) . ? C79 C82 1.485(4) . ? C80 C81 1.374(4) . ? C80 H80 0.9300 . ? C81 H81 0.9300 . ? C82 C83 1.388(4) . ? C82 C86 1.401(4) . ? C83 C84 1.380(4) . ? C83 H83 0.9300 . ? C84 H84 0.9300 . ? C85 C86 1.371(4) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C87 C88 1.508(4) . ? C87 H87A 0.9700 . ? C87 H87B 0.9700 . ? C88 C93 1.389(4) . ? C88 C89 1.390(4) . ? C89 C90 1.391(4) . ? C89 H89 0.9300 . ? C90 C91 1.388(4) . ? C90 H90 0.9300 . ? C91 C92 1.387(4) . ? C91 C94 1.516(4) . ? C92 C93 1.387(4) . ? C92 H92 0.9300 . ? C93 H93 0.9300 . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? N5 C95 1.142(5) . ? N6 C97 1.137(4) . ? N7 C99 1.138(5) . ? N8 C101 1.130(4) . ? C95 C96 1.453(6) . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? C97 C98 1.450(5) . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C99 C100 1.454(5) . ? C100 H10C 0.9600 . ? C100 H10D 0.9600 . ? C100 H10E 0.9600 . ? C101 C102 1.448(5) . ? C102 H10F 0.9600 . ? C102 H10G 0.9600 . ? C102 H10H 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F6 P1 F2 90.58(13) . . ? F6 P1 F4 91.85(12) . . ? F2 P1 F4 90.80(11) . . ? F6 P1 F3 178.36(13) . . ? F2 P1 F3 90.59(13) . . ? F4 P1 F3 89.29(11) . . ? F6 P1 F5 89.52(12) . . ? F2 P1 F5 179.07(12) . . ? F4 P1 F5 90.12(11) . . ? F3 P1 F5 89.29(12) . . ? F6 P1 F1 89.73(12) . . ? F2 P1 F1 89.56(11) . . ? F4 P1 F1 178.38(12) . . ? F3 P1 F1 89.13(11) . . ? F5 P1 F1 89.52(11) . . ? F8 P2 F10 90.73(15) . . ? F8 P2 F9 90.53(11) . . ? F10 P2 F9 91.12(10) . . ? F8 P2 F7 92.68(18) . . ? F10 P2 F7 176.57(17) . . ? F9 P2 F7 88.46(11) . . ? F8 P2 F12 91.28(14) . . ? F10 P2 F12 90.30(11) . . ? F9 P2 F12 177.68(13) . . ? F7 P2 F12 90.01(12) . . ? F8 P2 F11 178.67(16) . . ? F10 P2 F11 88.10(11) . . ? F9 P2 F11 88.84(11) . . ? F7 P2 F11 88.49(16) . . ? F12 P2 F11 89.37(13) . . ? F14 P3 F18 91.58(15) . . ? F14 P3 F16 90.41(15) . . ? F18 P3 F16 90.65(15) . . ? F14 P3 F13 91.34(15) . . ? F18 P3 F13 92.32(16) . . ? F16 P3 F13 176.50(15) . . ? F14 P3 F15 90.41(16) . . ? F18 P3 F15 177.73(16) . . ? F16 P3 F15 88.24(13) . . ? F13 P3 F15 88.72(15) . . ? F14 P3 F17 178.92(15) . . ? F18 P3 F17 89.00(15) . . ? F16 P3 F17 90.50(13) . . ? F13 P3 F17 87.72(14) . . ? F15 P3 F17 89.02(15) . . ? F24' P4 F21' 91.9(10) . . ? F24' P4 F23' 94.0(10) . . ? F21' P4 F23' 173.2(10) . . ? F24' P4 F21 113.1(11) . . ? F21' P4 F21 21.2(10) . . ? F23' P4 F21 152.6(12) . . ? F24' P4 F22 151.9(10) . . ? F21' P4 F22 115.6(9) . . ? F23' P4 F22 58.9(10) . . ? F21 P4 F22 94.6(5) . . ? F24' P4 F23 62.4(10) . . ? F21' P4 F23 154.3(9) . . ? F23' P4 F23 31.9(10) . . ? F21 P4 F23 175.5(5) . . ? F22 P4 F23 89.8(4) . . ? F24' P4 F24 24.5(12) . . ? F21' P4 F24 68.5(10) . . ? F23' P4 F24 116.9(12) . . ? F21 P4 F24 89.4(5) . . ? F22 P4 F24 175.8(6) . . ? F23 P4 F24 86.2(4) . . ? F24' P4 F20 85.9(7) . . ? F21' P4 F20 88.0(7) . . ? F23' P4 F20 95.7(7) . . ? F21 P4 F20 90.3(3) . . ? F22 P4 F20 89.3(3) . . ? F23 P4 F20 88.8(4) . . ? F24 P4 F20 92.0(4) . . ? F24' P4 F19 93.6(7) . . ? F21' P4 F19 92.1(7) . . ? F23' P4 F19 84.2(7) . . ? F21 P4 F19 90.0(3) . . ? F22 P4 F19 91.1(3) . . ? F23 P4 F19 90.9(4) . . ? F24 P4 F19 87.6(4) . . ? F20 P4 F19 179.54(15) . . ? F24' P4 F22' 175.1(9) . . ? F21' P4 F22' 83.3(8) . . ? F23' P4 F22' 90.7(9) . . ? F21 P4 F22' 62.1(9) . . ? F22 P4 F22' 33.0(7) . . ? F23 P4 F22' 122.3(8) . . ? F24 P4 F22' 150.6(10) . . ? F20 P4 F22' 95.1(6) . . ? F19 P4 F22' 85.4(6) . . ? C1 O1 C20 114.6(2) . . ? C19 O2 C18 113.7(2) . . ? C16 O3 C17 114.8(2) . . ? C14 O4 C15 118.4(2) . . ? C13 O5 C12 115.0(2) . . ? C11 O6 C10 111.9(2) . . ? C9 O7 C8 111.0(2) . . ? C6 O8 C7 116.0(2) . . ? C45 O9 C53 115.0(2) . . ? C54 O10 C55 111.0(2) . . ? C34 O11 C56 113.58(19) . . ? C57 O12 C58 112.0(2) . . ? C63 N1 C59 120.7(2) . . ? C63 N1 C94 119.9(2) . . ? C59 N1 C94 119.0(2) . . ? C67 N2 C66 120.4(2) . . ? C67 N2 C69 120.5(2) . . ? C66 N2 C69 118.9(2) . . ? C81 N3 C77 120.7(2) . . ? C81 N3 C76 120.5(2) . . ? C77 N3 C76 118.5(2) . . ? C84 N4 C85 121.0(2) . . ? C84 N4 C87 120.1(2) . . ? C85 N4 C87 118.8(2) . . ? C2 C1 O1 118.3(2) . . ? C2 C1 C6 119.8(3) . . ? O1 C1 C6 121.8(3) . . ? C1 C2 C3 120.3(3) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 119.6(3) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? O8 C6 C5 124.0(3) . . ? O8 C6 C1 116.3(2) . . ? C5 C6 C1 119.6(3) . . ? O8 C7 C8 108.6(2) . . ? O8 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? O8 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.3 . . ? O7 C8 C7 109.6(2) . . ? O7 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? O7 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? O7 C9 C10 109.2(2) . . ? O7 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? O7 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.3 . . ? O6 C10 C9 109.1(2) . . ? O6 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? O6 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O6 C11 C12 107.8(2) . . ? O6 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O6 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? O5 C12 C11 109.0(2) . . ? O5 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? O5 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? O5 C13 C21 118.7(2) . . ? O5 C13 C14 119.9(2) . . ? C21 C13 C14 120.9(2) . . ? O4 C14 C32 124.1(2) . . ? O4 C14 C13 116.4(2) . . ? C32 C14 C13 119.4(2) . . ? O4 C15 C16 108.0(2) . . ? O4 C15 H15A 110.1 . . ? C16 C15 H15A 110.1 . . ? O4 C15 H15B 110.1 . . ? C16 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? O3 C16 C15 107.8(2) . . ? O3 C16 H16A 110.2 . . ? C15 C16 H16A 110.2 . . ? O3 C16 H16B 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? O3 C17 C18 113.5(3) . . ? O3 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? O3 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? O2 C18 C17 107.6(2) . . ? O2 C18 H18A 110.2 . . ? C17 C18 H18A 110.2 . . ? O2 C18 H18B 110.2 . . ? C17 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? O2 C19 C20 108.5(2) . . ? O2 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? O2 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? O1 C20 C19 108.8(2) . . ? O1 C20 H20A 109.9 . . ? C19 C20 H20A 109.9 . . ? O1 C20 H20B 109.9 . . ? C19 C20 H20B 109.9 . . ? H20A C20 H20B 108.3 . . ? C22 C21 C13 119.4(2) . . ? C22 C21 H21 120.3 . . ? C13 C21 H21 120.3 . . ? C21 C22 C31 119.9(2) . . ? C21 C22 C23 126.9(2) . . ? C31 C22 C23 113.1(2) . . ? C33 C23 C24 107.4(2) . . ? C33 C23 C22 103.5(2) . . ? C24 C23 C22 106.0(2) . . ? C33 C23 H23 113.1 . . ? C24 C23 H23 113.1 . . ? C22 C23 H23 113.1 . . ? C25 C24 C29 120.8(2) . . ? C25 C24 C23 126.2(2) . . ? C29 C24 C23 113.0(2) . . ? C24 C25 C26 118.8(3) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C27 C26 C25 120.5(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 120.2(3) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 119.3(3) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C24 120.2(3) . . ? C28 C29 C30 126.4(2) . . ? C24 C29 C30 113.4(2) . . ? C46 C30 C29 107.9(2) . . ? C46 C30 C31 103.39(19) . . ? C29 C30 C31 105.5(2) . . ? C46 C30 H30 113.1 . . ? C29 C30 H30 113.1 . . ? C31 C30 H30 113.1 . . ? C32 C31 C22 121.1(2) . . ? C32 C31 C30 126.0(2) . . ? C22 C31 C30 112.8(2) . . ? C31 C32 C14 119.2(2) . . ? C31 C32 H32 120.4 . . ? C14 C32 H32 120.4 . . ? C34 C33 C46 120.7(2) . . ? C34 C33 C23 126.2(2) . . ? C46 C33 C23 112.7(2) . . ? C35 C34 O11 120.2(2) . . ? C35 C34 C33 119.1(2) . . ? O11 C34 C33 120.4(2) . . ? C34 C35 C44 120.2(2) . . ? C34 C35 C36 126.7(2) . . ? C44 C35 C36 112.9(2) . . ? C37 C36 C35 106.4(2) . . ? C37 C36 C47 105.4(2) . . ? C35 C36 C47 105.20(19) . . ? C37 C36 H36 113.1 . . ? C35 C36 H36 113.1 . . ? C47 C36 H36 113.1 . . ? C38 C37 C42 120.5(2) . . ? C38 C37 C36 126.3(2) . . ? C42 C37 C36 113.2(2) . . ? C37 C38 C39 119.1(2) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C40 C39 C38 120.3(3) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 120.9(3) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C42 C41 C40 118.8(2) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C41 C42 C37 120.3(2) . . ? C41 C42 C43 126.8(2) . . ? C37 C42 C43 112.9(2) . . ? C44 C43 C52 104.8(2) . . ? C44 C43 C42 105.7(2) . . ? C52 C43 C42 106.5(2) . . ? C44 C43 H43 113.1 . . ? C52 C43 H43 113.1 . . ? C42 C43 H43 113.1 . . ? C45 C44 C35 120.5(2) . . ? C45 C44 C43 126.2(2) . . ? C35 C44 C43 113.1(2) . . ? O9 C45 C46 119.3(2) . . ? O9 C45 C44 121.0(2) . . ? C46 C45 C44 119.5(2) . . ? C45 C46 C33 119.9(2) . . ? C45 C46 C30 126.0(2) . . ? C33 C46 C30 113.5(2) . . ? C48 C47 C52 120.2(2) . . ? C48 C47 C36 126.7(2) . . ? C52 C47 C36 113.2(2) . . ? C47 C48 C49 119.6(2) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C50 C49 C48 120.0(2) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.3(2) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C52 C51 C50 119.2(2) . . ? C52 C51 H51 120.4 . . ? C50 C51 H51 120.4 . . ? C51 C52 C47 120.6(2) . . ? C51 C52 C43 126.5(2) . . ? C47 C52 C43 113.0(2) . . ? O9 C53 C54 109.9(2) . . ? O9 C53 H53A 109.7 . . ? C54 C53 H53A 109.7 . . ? O9 C53 H53B 109.7 . . ? C54 C53 H53B 109.7 . . ? H53A C53 H53B 108.2 . . ? O10 C54 C53 109.4(2) . . ? O10 C54 H54A 109.8 . . ? C53 C54 H54A 109.8 . . ? O10 C54 H54B 109.8 . . ? C53 C54 H54B 109.8 . . ? H54A C54 H54B 108.2 . . ? O10 C55 H55A 109.5 . . ? O10 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O10 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O11 C56 C57 112.1(2) . . ? O11 C56 H56A 109.2 . . ? C57 C56 H56A 109.2 . . ? O11 C56 H56B 109.2 . . ? C57 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? O12 C57 C56 114.0(2) . . ? O12 C57 H57A 108.8 . . ? C56 C57 H57A 108.8 . . ? O12 C57 H57B 108.8 . . ? C56 C57 H57B 108.8 . . ? H57A C57 H57B 107.7 . . ? O12 C58 H58A 109.5 . . ? O12 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O12 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N1 C59 C60 120.2(3) . . ? N1 C59 H59 119.9 . . ? C60 C59 H59 119.9 . . ? C59 C60 C61 120.7(2) . . ? C59 C60 H60 119.6 . . ? C61 C60 H60 119.6 . . ? C62 C61 C60 117.0(2) . . ? C62 C61 C64 122.3(2) . . ? C60 C61 C64 120.6(2) . . ? C63 C62 C61 120.2(3) . . ? C63 C62 H62 119.9 . . ? C61 C62 H62 119.9 . . ? N1 C63 C62 120.8(3) . . ? N1 C63 H63 119.6 . . ? C62 C63 H63 119.6 . . ? C65 C64 C68 117.1(2) . . ? C65 C64 C61 120.8(2) . . ? C68 C64 C61 122.0(2) . . ? C66 C65 C64 120.4(3) . . ? C66 C65 H65 119.8 . . ? C64 C65 H65 119.8 . . ? N2 C66 C65 120.8(3) . . ? N2 C66 H66 119.6 . . ? C65 C66 H66 119.6 . . ? N2 C67 C68 121.1(3) . . ? N2 C67 H67 119.4 . . ? C68 C67 H67 119.4 . . ? C67 C68 C64 120.1(3) . . ? C67 C68 H68 120.0 . . ? C64 C68 H68 120.0 . . ? N2 C69 C70 108.6(2) . . ? N2 C69 H69A 110.0 . . ? C70 C69 H69A 110.0 . . ? N2 C69 H69B 110.0 . . ? C70 C69 H69B 110.0 . . ? H69A C69 H69B 108.3 . . ? C71 C70 C75 118.8(3) . . ? C71 C70 C69 120.8(3) . . ? C75 C70 C69 120.3(3) . . ? C72 C71 C70 120.6(3) . . ? C72 C71 H71 119.7 . . ? C70 C71 H71 119.7 . . ? C71 C72 C73 120.4(3) . . ? C71 C72 H72 119.8 . . ? C73 C72 H72 119.8 . . ? C74 C73 C72 118.9(3) . . ? C74 C73 C76 120.4(3) . . ? C72 C73 C76 120.7(3) . . ? C75 C74 C73 120.6(3) . . ? C75 C74 H74 119.7 . . ? C73 C74 H74 119.7 . . ? C74 C75 C70 120.6(3) . . ? C74 C75 H75 119.7 . . ? C70 C75 H75 119.7 . . ? C73 C76 N3 108.6(2) . . ? C73 C76 H76A 110.0 . . ? N3 C76 H76A 110.0 . . ? C73 C76 H76B 110.0 . . ? N3 C76 H76B 110.0 . . ? H76A C76 H76B 108.4 . . ? N3 C77 C78 120.9(3) . . ? N3 C77 H77 119.6 . . ? C78 C77 H77 119.6 . . ? C77 C78 C79 119.9(3) . . ? C77 C78 H78 120.1 . . ? C79 C78 H78 120.1 . . ? C78 C79 C80 117.7(2) . . ? C78 C79 C82 119.9(2) . . ? C80 C79 C82 122.1(2) . . ? C81 C80 C79 120.2(3) . . ? C81 C80 H80 119.9 . . ? C79 C80 H80 119.9 . . ? N3 C81 C80 120.3(3) . . ? N3 C81 H81 119.9 . . ? C80 C81 H81 119.9 . . ? C83 C82 C86 118.1(2) . . ? C83 C82 C79 121.6(2) . . ? C86 C82 C79 120.1(2) . . ? C84 C83 C82 119.9(3) . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? N4 C84 C83 120.4(2) . . ? N4 C84 H84 119.8 . . ? C83 C84 H84 119.8 . . ? N4 C85 C86 120.5(2) . . ? N4 C85 H85 119.7 . . ? C86 C85 H85 119.7 . . ? C85 C86 C82 119.9(2) . . ? C85 C86 H86 120.0 . . ? C82 C86 H86 120.0 . . ? N4 C87 C88 109.8(2) . . ? N4 C87 H87A 109.7 . . ? C88 C87 H87A 109.7 . . ? N4 C87 H87B 109.7 . . ? C88 C87 H87B 109.7 . . ? H87A C87 H87B 108.2 . . ? C93 C88 C89 119.5(3) . . ? C93 C88 C87 120.0(3) . . ? C89 C88 C87 120.5(3) . . ? C88 C89 C90 120.2(3) . . ? C88 C89 H89 119.9 . . ? C90 C89 H89 119.9 . . ? C91 C90 C89 120.3(3) . . ? C91 C90 H90 119.8 . . ? C89 C90 H90 119.8 . . ? C92 C91 C90 119.1(3) . . ? C92 C91 C94 120.1(2) . . ? C90 C91 C94 120.7(3) . . ? C93 C92 C91 120.8(3) . . ? C93 C92 H92 119.6 . . ? C91 C92 H92 119.6 . . ? C92 C93 C88 120.0(3) . . ? C92 C93 H93 120.0 . . ? C88 C93 H93 120.0 . . ? N1 C94 C91 107.7(2) . . ? N1 C94 H94A 110.2 . . ? C91 C94 H94A 110.2 . . ? N1 C94 H94B 110.2 . . ? C91 C94 H94B 110.2 . . ? H94A C94 H94B 108.5 . . ? N5 C95 C96 179.3(4) . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? N6 C97 C98 179.6(5) . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.4 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N7 C99 C100 179.2(4) . . ? C99 C100 H10C 109.5 . . ? C99 C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? C99 C100 H10E 109.5 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? N8 C101 C102 178.9(4) . . ? C101 C102 H10F 109.5 . . ? C101 C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? C101 C102 H10H 109.5 . . ? H10F C102 H10H 109.5 . . ? H10G C102 H10H 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 C20 O1 C1 C2 -107.5(3) . . . . ? C20 O1 C1 C6 75.0(3) . . . . ? O1 C1 C2 C3 -176.1(3) . . . . ? C6 C1 C2 C3 1.5(4) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C2 C3 C4 C5 -1.6(5) . . . . ? C3 C4 C5 C6 1.4(5) . . . . ? C7 O8 C6 C5 27.0(4) . . . . ? C7 O8 C6 C1 -154.2(2) . . . . ? C4 C5 C6 O8 179.0(3) . . . . ? C4 C5 C6 C1 0.3(4) . . . . ? C2 C1 C6 O8 179.5(2) . . . . ? O1 C1 C6 O8 -3.0(4) . . . . ? C2 C1 C6 C5 -1.7(4) . . . . ? O1 C1 C6 C5 175.8(2) . . . . ? C6 O8 C7 C8 165.7(2) . . . . ? C9 O7 C8 C7 173.2(2) . . . . ? O8 C7 C8 O7 67.8(3) . . . . ? C8 O7 C9 C10 -176.7(2) . . . . ? C11 O6 C10 C9 177.1(2) . . . . ? O7 C9 C10 O6 -72.0(3) . . . . ? C10 O6 C11 C12 164.6(2) . . . . ? C13 O5 C12 C11 -99.5(3) . . . . ? O6 C11 C12 O5 170.3(2) . . . . ? C12 O5 C13 C21 120.1(3) . . . . ? C12 O5 C13 C14 -67.3(3) . . . . ? C15 O4 C14 C32 -30.3(4) . . . . ? C15 O4 C14 C13 153.9(2) . . . . ? O5 C13 C14 O4 3.3(4) . . . . ? C21 C13 C14 O4 175.7(2) . . . . ? O5 C13 C14 C32 -172.8(2) . . . . ? C21 C13 C14 C32 -0.4(4) . . . . ? C14 O4 C15 C16 -138.3(2) . . . . ? C17 O3 C16 C15 -159.6(2) . . . . ? O4 C15 C16 O3 67.0(3) . . . . ? C16 O3 C17 C18 -90.3(3) . . . . ? C19 O2 C18 C17 179.2(2) . . . . ? O3 C17 C18 O2 -73.2(3) . . . . ? C18 O2 C19 C20 163.1(2) . . . . ? C1 O1 C20 C19 -176.3(2) . . . . ? O2 C19 C20 O1 61.5(3) . . . . ? O5 C13 C21 C22 173.0(2) . . . . ? C14 C13 C21 C22 0.5(4) . . . . ? C13 C21 C22 C31 0.0(4) . . . . ? C13 C21 C22 C23 177.4(2) . . . . ? C21 C22 C23 C33 -120.2(3) . . . . ? C31 C22 C23 C33 57.3(3) . . . . ? C21 C22 C23 C24 127.0(3) . . . . ? C31 C22 C23 C24 -55.5(3) . . . . ? C33 C23 C24 C25 125.3(3) . . . . ? C22 C23 C24 C25 -124.6(3) . . . . ? C33 C23 C24 C29 -56.1(3) . . . . ? C22 C23 C24 C29 54.0(3) . . . . ? C29 C24 C25 C26 -2.2(4) . . . . ? C23 C24 C25 C26 176.3(2) . . . . ? C24 C25 C26 C27 -0.7(4) . . . . ? C25 C26 C27 C28 2.3(4) . . . . ? C26 C27 C28 C29 -1.0(4) . . . . ? C27 C28 C29 C24 -1.8(4) . . . . ? C27 C28 C29 C30 -178.9(3) . . . . ? C25 C24 C29 C28 3.5(4) . . . . ? C23 C24 C29 C28 -175.2(2) . . . . ? C25 C24 C29 C30 -179.1(2) . . . . ? C23 C24 C29 C30 2.2(3) . . . . ? C28 C29 C30 C46 -130.3(3) . . . . ? C24 C29 C30 C46 52.5(3) . . . . ? C28 C29 C30 C31 119.7(3) . . . . ? C24 C29 C30 C31 -57.5(3) . . . . ? C21 C22 C31 C32 -0.7(4) . . . . ? C23 C22 C31 C32 -178.4(2) . . . . ? C21 C22 C31 C30 178.0(2) . . . . ? C23 C22 C31 C30 0.3(3) . . . . ? C46 C30 C31 C32 121.2(3) . . . . ? C29 C30 C31 C32 -125.6(3) . . . . ? C46 C30 C31 C22 -57.5(3) . . . . ? C29 C30 C31 C22 55.7(3) . . . . ? C22 C31 C32 C14 0.8(4) . . . . ? C30 C31 C32 C14 -177.7(2) . . . . ? O4 C14 C32 C31 -176.0(2) . . . . ? C13 C14 C32 C31 -0.3(4) . . . . ? C24 C23 C33 C34 -133.5(3) . . . . ? C22 C23 C33 C34 114.7(3) . . . . ? C24 C23 C33 C46 54.5(3) . . . . ? C22 C23 C33 C46 -57.4(3) . . . . ? C56 O11 C34 C35 -105.9(3) . . . . ? C56 O11 C34 C33 80.7(3) . . . . ? C46 C33 C34 C35 2.8(4) . . . . ? C23 C33 C34 C35 -168.6(2) . . . . ? C46 C33 C34 O11 176.2(2) . . . . ? C23 C33 C34 O11 4.8(4) . . . . ? O11 C34 C35 C44 -175.6(2) . . . . ? C33 C34 C35 C44 -2.2(4) . . . . ? O11 C34 C35 C36 0.0(4) . . . . ? C33 C34 C35 C36 173.5(2) . . . . ? C34 C35 C36 C37 129.6(3) . . . . ? C44 C35 C36 C37 -54.5(3) . . . . ? C34 C35 C36 C47 -118.9(3) . . . . ? C44 C35 C36 C47 57.0(3) . . . . ? C35 C36 C37 C38 -125.8(3) . . . . ? C47 C36 C37 C38 122.8(3) . . . . ? C35 C36 C37 C42 55.3(3) . . . . ? C47 C36 C37 C42 -56.1(3) . . . . ? C42 C37 C38 C39 0.1(4) . . . . ? C36 C37 C38 C39 -178.7(2) . . . . ? C37 C38 C39 C40 -1.5(4) . . . . ? C38 C39 C40 C41 1.5(4) . . . . ? C39 C40 C41 C42 0.0(4) . . . . ? C40 C41 C42 C37 -1.4(4) . . . . ? C40 C41 C42 C43 178.9(2) . . . . ? C38 C37 C42 C41 1.3(4) . . . . ? C36 C37 C42 C41 -179.7(2) . . . . ? C38 C37 C42 C43 -178.9(2) . . . . ? C36 C37 C42 C43 0.0(3) . . . . ? C41 C42 C43 C44 123.8(3) . . . . ? C37 C42 C43 C44 -55.9(3) . . . . ? C41 C42 C43 C52 -125.2(3) . . . . ? C37 C42 C43 C52 55.1(3) . . . . ? C34 C35 C44 C45 -0.5(4) . . . . ? C36 C35 C44 C45 -176.7(2) . . . . ? C34 C35 C44 C43 174.5(2) . . . . ? C36 C35 C44 C43 -1.7(3) . . . . ? C52 C43 C44 C45 119.2(3) . . . . ? C42 C43 C44 C45 -128.6(3) . . . . ? C52 C43 C44 C35 -55.5(3) . . . . ? C42 C43 C44 C35 56.7(3) . . . . ? C53 O9 C45 C46 -111.2(3) . . . . ? C53 O9 C45 C44 74.9(3) . . . . ? C35 C44 C45 O9 176.4(2) . . . . ? C43 C44 C45 O9 2.0(4) . . . . ? C35 C44 C45 C46 2.6(4) . . . . ? C43 C44 C45 C46 -171.8(2) . . . . ? O9 C45 C46 C33 -175.8(2) . . . . ? C44 C45 C46 C33 -1.9(4) . . . . ? O9 C45 C46 C30 -5.4(4) . . . . ? C44 C45 C46 C30 168.6(2) . . . . ? C34 C33 C46 C45 -0.8(4) . . . . ? C23 C33 C46 C45 171.8(2) . . . . ? C34 C33 C46 C30 -172.4(2) . . . . ? C23 C33 C46 C30 0.1(3) . . . . ? C29 C30 C46 C45 135.1(3) . . . . ? C31 C30 C46 C45 -113.5(3) . . . . ? C29 C30 C46 C33 -53.9(3) . . . . ? C31 C30 C46 C33 57.5(3) . . . . ? C37 C36 C47 C48 -122.7(3) . . . . ? C35 C36 C47 C48 125.1(3) . . . . ? C37 C36 C47 C52 58.0(3) . . . . ? C35 C36 C47 C52 -54.3(3) . . . . ? C52 C47 C48 C49 1.9(4) . . . . ? C36 C47 C48 C49 -177.4(2) . . . . ? C47 C48 C49 C50 1.0(4) . . . . ? C48 C49 C50 C51 -2.1(4) . . . . ? C49 C50 C51 C52 0.1(4) . . . . ? C50 C51 C52 C47 2.8(4) . . . . ? C50 C51 C52 C43 -178.9(2) . . . . ? C48 C47 C52 C51 -3.9(4) . . . . ? C36 C47 C52 C51 175.5(2) . . . . ? C48 C47 C52 C43 177.6(2) . . . . ? C36 C47 C52 C43 -3.0(3) . . . . ? C44 C43 C52 C51 -120.0(3) . . . . ? C42 C43 C52 C51 128.3(3) . . . . ? C44 C43 C52 C47 58.4(3) . . . . ? C42 C43 C52 C47 -53.3(3) . . . . ? C45 O9 C53 C54 130.8(2) . . . . ? C55 O10 C54 C53 173.6(3) . . . . ? O9 C53 C54 O10 -72.9(3) . . . . ? C34 O11 C56 C57 75.1(3) . . . . ? C58 O12 C57 C56 77.3(3) . . . . ? O11 C56 C57 O12 64.2(3) . . . . ? C63 N1 C59 C60 -5.7(4) . . . . ? C94 N1 C59 C60 167.1(2) . . . . ? N1 C59 C60 C61 0.5(4) . . . . ? C59 C60 C61 C62 5.1(4) . . . . ? C59 C60 C61 C64 -171.5(2) . . . . ? C60 C61 C62 C63 -5.7(4) . . . . ? C64 C61 C62 C63 170.8(3) . . . . ? C59 N1 C63 C62 5.0(4) . . . . ? C94 N1 C63 C62 -167.7(3) . . . . ? C61 C62 C63 N1 0.9(4) . . . . ? C62 C61 C64 C65 -169.8(3) . . . . ? C60 C61 C64 C65 6.5(4) . . . . ? C62 C61 C64 C68 6.9(4) . . . . ? C60 C61 C64 C68 -176.8(3) . . . . ? C68 C64 C65 C66 -2.1(4) . . . . ? C61 C64 C65 C66 174.7(2) . . . . ? C67 N2 C66 C65 2.3(4) . . . . ? C69 N2 C66 C65 -172.8(3) . . . . ? C64 C65 C66 N2 0.0(4) . . . . ? C66 N2 C67 C68 -2.4(4) . . . . ? C69 N2 C67 C68 172.7(3) . . . . ? N2 C67 C68 C64 0.2(5) . . . . ? C65 C64 C68 C67 2.0(4) . . . . ? C61 C64 C68 C67 -174.8(3) . . . . ? C67 N2 C69 C70 -94.7(3) . . . . ? C66 N2 C69 C70 80.4(3) . . . . ? N2 C69 C70 C71 88.4(3) . . . . ? N2 C69 C70 C75 -88.2(3) . . . . ? C75 C70 C71 C72 0.9(4) . . . . ? C69 C70 C71 C72 -175.8(2) . . . . ? C70 C71 C72 C73 0.9(4) . . . . ? C71 C72 C73 C74 -2.3(4) . . . . ? C71 C72 C73 C76 176.0(2) . . . . ? C72 C73 C74 C75 1.8(4) . . . . ? C76 C73 C74 C75 -176.4(2) . . . . ? C73 C74 C75 C70 -0.1(4) . . . . ? C71 C70 C75 C74 -1.3(4) . . . . ? C69 C70 C75 C74 175.4(2) . . . . ? C74 C73 C76 N3 89.1(3) . . . . ? C72 C73 C76 N3 -89.1(3) . . . . ? C81 N3 C76 C73 -99.4(3) . . . . ? C77 N3 C76 C73 74.6(3) . . . . ? C81 N3 C77 C78 4.9(4) . . . . ? C76 N3 C77 C78 -169.2(3) . . . . ? N3 C77 C78 C79 -0.1(4) . . . . ? C77 C78 C79 C80 -5.2(4) . . . . ? C77 C78 C79 C82 169.2(3) . . . . ? C78 C79 C80 C81 6.0(4) . . . . ? C82 C79 C80 C81 -168.3(2) . . . . ? C77 N3 C81 C80 -4.1(4) . . . . ? C76 N3 C81 C80 169.8(2) . . . . ? C79 C80 C81 N3 -1.4(4) . . . . ? C78 C79 C82 C83 24.0(4) . . . . ? C80 C79 C82 C83 -161.9(3) . . . . ? C78 C79 C82 C86 -150.3(3) . . . . ? C80 C79 C82 C86 23.8(4) . . . . ? C86 C82 C83 C84 3.4(4) . . . . ? C79 C82 C83 C84 -170.9(2) . . . . ? C85 N4 C84 C83 -1.6(4) . . . . ? C87 N4 C84 C83 174.8(2) . . . . ? C82 C83 C84 N4 -1.1(4) . . . . ? C84 N4 C85 C86 1.9(4) . . . . ? C87 N4 C85 C86 -174.6(2) . . . . ? N4 C85 C86 C82 0.5(4) . . . . ? C83 C82 C86 C85 -3.1(4) . . . . ? C79 C82 C86 C85 171.3(2) . . . . ? C84 N4 C87 C88 -99.7(3) . . . . ? C85 N4 C87 C88 76.8(3) . . . . ? N4 C87 C88 C93 88.4(3) . . . . ? N4 C87 C88 C89 -89.8(3) . . . . ? C93 C88 C89 C90 -2.4(4) . . . . ? C87 C88 C89 C90 175.8(2) . . . . ? C88 C89 C90 C91 0.8(4) . . . . ? C89 C90 C91 C92 1.1(4) . . . . ? C89 C90 C91 C94 -175.9(2) . . . . ? C90 C91 C92 C93 -1.5(4) . . . . ? C94 C91 C92 C93 175.6(2) . . . . ? C91 C92 C93 C88 -0.1(4) . . . . ? C89 C88 C93 C92 2.1(4) . . . . ? C87 C88 C93 C92 -176.2(2) . . . . ? C63 N1 C94 C91 87.5(3) . . . . ? C59 N1 C94 C91 -85.4(3) . . . . ? C92 C91 C94 N1 -87.6(3) . . . . ? C90 C91 C94 N1 89.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.779 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.061 # Attachment 'complex_2-3.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 755778' #TrackingRef 'complex_2-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H103 F24 N7 O12 P4' _chemical_formula_weight 2222.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.542(4) _cell_length_b 29.698(6) _cell_length_c 19.395(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.39(3) _cell_angle_gamma 90.00 _cell_volume 10101(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20543 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 26.01 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4592 _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9640 _exptl_absorpt_correction_T_max 0.9764 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; Because of lack of heavy atoms in the complex and the presence of disordered PF6-, the quality of the X-ray diffraction data was not very well. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64094 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.01 _reflns_number_total 19815 _reflns_number_gt 17219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 19815 _refine_ls_number_parameters 1361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.1119 _refine_ls_wR_factor_ref 0.3012 _refine_ls_wR_factor_gt 0.2934 _refine_ls_goodness_of_fit_ref 1.813 _refine_ls_restrained_S_all 1.813 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.003 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 P1 P 0.92026(8) 0.09631(4) 0.15450(7) 0.0546(4) Uani 1 1 d . . . P2 P 0.19516(8) 0.10378(4) 0.38631(7) 0.0511(3) Uani 1 1 d . . . P3 P 0.34443(7) 0.16039(4) 0.71228(6) 0.0473(3) Uani 1 1 d . . . P4 P 0.35892(9) 0.09295(5) -0.00061(8) 0.0622(4) Uani 1 1 d . . . F1 F 0.9869(4) 0.1229(2) 0.1312(4) 0.242(5) Uani 1 1 d . . . F2 F 0.9555(5) 0.0715(2) 0.2128(3) 0.240(5) Uani 1 1 d . . . F3 F 0.8465(4) 0.07033(17) 0.1733(3) 0.173(3) Uani 1 1 d . . . F4 F 0.8683(4) 0.11679(18) 0.0976(3) 0.173(3) Uani 1 1 d . . . F5 F 0.8978(2) 0.13596(12) 0.2042(2) 0.0983(13) Uani 1 1 d . . . F6 F 0.9410(2) 0.05662(11) 0.10303(19) 0.0884(11) Uani 1 1 d . . . F7 F 0.1749(3) 0.05777(10) 0.42320(19) 0.0950(12) Uani 1 1 d . . . F8 F 0.2760(2) 0.10542(12) 0.4223(2) 0.0932(12) Uani 1 1 d . . . F9 F 0.11232(18) 0.10246(12) 0.34880(18) 0.0803(10) Uani 1 1 d . . . F10 F 0.21165(16) 0.15007(9) 0.34896(15) 0.0578(7) Uani 1 1 d . . . F11 F 0.22909(19) 0.07697(10) 0.32194(16) 0.0699(9) Uani 1 1 d . . . F12 F 0.1594(2) 0.13102(10) 0.44893(15) 0.0746(9) Uani 1 1 d . . . F13 F 0.3401(3) 0.16570(13) 0.63384(18) 0.1184(16) Uani 1 1 d . . . F14 F 0.2570(2) 0.15998(12) 0.7172(3) 0.137(2) Uani 1 1 d . . . F15 F 0.3540(4) 0.15470(13) 0.7922(2) 0.146(2) Uani 1 1 d . . . F16 F 0.4334(2) 0.16161(13) 0.7102(3) 0.128(2) Uani 1 1 d . . . F17 F 0.3452(2) 0.10753(10) 0.70169(19) 0.0829(11) Uani 1 1 d . . . F18 F 0.34514(15) 0.21373(9) 0.72316(16) 0.0599(7) Uani 1 1 d . . . F19 F 0.3245(3) 0.14047(12) -0.0167(3) 0.1316(19) Uani 1 1 d . . . F20 F 0.3167(3) 0.09242(14) 0.0708(2) 0.1103(14) Uani 1 1 d . . . F21 F 0.4313(2) 0.11549(13) 0.0364(2) 0.0998(13) Uani 1 1 d . . . F22 F 0.3914(2) 0.04407(12) 0.0189(2) 0.0964(12) Uani 1 1 d . . . F23 F 0.4043(2) 0.09145(15) -0.06988(19) 0.1038(14) Uani 1 1 d . . . F24 F 0.2889(2) 0.06947(12) -0.0371(2) 0.0874(11) Uani 1 1 d . . . O1 O -0.15000(15) 0.31125(9) 0.70670(14) 0.0365(6) Uani 1 1 d . . . O2 O -0.0455(2) 0.39245(12) 0.81204(18) 0.0602(9) Uani 1 1 d . . . O3 O 0.02098(14) 0.15595(9) 0.75588(13) 0.0334(6) Uani 1 1 d . . . O4 O 0.08041(18) 0.07982(11) 0.8270(2) 0.0660(10) Uani 1 1 d . . . O5 O -0.07157(18) 0.14758(10) 0.43068(15) 0.0471(7) Uani 1 1 d . . . O6 O -0.1609(2) 0.06722(16) 0.4074(2) 0.0861(13) Uani 1 1 d . . . O7 O -0.2826(2) 0.00379(14) 0.3740(2) 0.0765(12) Uani 1 1 d . . . O8 O -0.3880(2) 0.02711(11) 0.49064(19) 0.0622(9) Uani 1 1 d . . . O9 O -0.14729(16) 0.22058(10) 0.40930(14) 0.0442(7) Uani 1 1 d . . . O10 O -0.31753(16) 0.23000(11) 0.38197(14) 0.0459(7) Uani 1 1 d . . . O11 O -0.43978(16) 0.17816(10) 0.43319(16) 0.0469(7) Uani 1 1 d . . . O12 O -0.46102(19) 0.09922(10) 0.51533(17) 0.0528(8) Uani 1 1 d . . . N1 N -0.27827(19) 0.22287(12) 0.55852(17) 0.0385(8) Uani 1 1 d . . . N2 N -0.1096(2) 0.03307(12) 0.70483(18) 0.0427(8) Uani 1 1 d . . . N3 N -0.2931(2) 0.08239(12) 0.99192(17) 0.0420(8) Uani 1 1 d . . . N4 N -0.4757(2) 0.26543(12) 0.83939(17) 0.0402(8) Uani 1 1 d . . . C1 C -0.2062(4) 0.0682(3) 0.3468(3) 0.0860(19) Uani 1 1 d . . . H1A H -0.1829 0.0494 0.3108 0.103 Uiso 1 1 calc R . . H1B H -0.2108 0.0994 0.3294 0.103 Uiso 1 1 calc R . . C2 C 0.1228(4) 0.03897(19) 0.8305(5) 0.106(3) Uani 1 1 d . . . H2A H 0.0898 0.0146 0.8460 0.160 Uiso 1 1 calc R . . H2B H 0.1659 0.0425 0.8631 0.160 Uiso 1 1 calc R . . H2C H 0.1419 0.0317 0.7847 0.160 Uiso 1 1 calc R . . C3 C -0.2847(3) 0.0497(2) 0.3642(4) 0.0774(17) Uani 1 1 d . . . H3A H -0.3027 0.0645 0.4066 0.093 Uiso 1 1 calc R . . H3B H -0.3213 0.0569 0.3261 0.093 Uiso 1 1 calc R . . C4 C -0.3515(3) -0.0157(2) 0.3956(3) 0.0714(16) Uani 1 1 d . . . H4A H -0.3540 -0.0472 0.3788 0.086 Uiso 1 1 calc R . . H4B H -0.3947 0.0009 0.3740 0.086 Uiso 1 1 calc R . . C5 C -0.0806(4) 0.0719(2) 0.3945(4) 0.0802(18) Uani 1 1 d . . . H5A H -0.0734 0.0843 0.3477 0.096 Uiso 1 1 calc R . . H5B H -0.0554 0.0421 0.3973 0.096 Uiso 1 1 calc R . . C6 C 0.0277(3) 0.41323(19) 0.8138(3) 0.0696(16) Uani 1 1 d . . . H6A H 0.0361 0.4282 0.8583 0.104 Uiso 1 1 calc R . . H6B H 0.0303 0.4355 0.7766 0.104 Uiso 1 1 calc R . . H6C H 0.0671 0.3903 0.8076 0.104 Uiso 1 1 calc R . . C7 C -0.3607(3) -0.01584(18) 0.4714(3) 0.0659(15) Uani 1 1 d . . . H7A H -0.3973 -0.0395 0.4846 0.079 Uiso 1 1 calc R . . H7B H -0.3111 -0.0221 0.4950 0.079 Uiso 1 1 calc R . . C8 C -0.4461(3) 0.07354(15) 0.5730(2) 0.0467(10) Uani 1 1 d . . . C9 C -0.3884(3) -0.01478(16) 0.7372(3) 0.0573(13) Uani 1 1 d . . . H9A H -0.3570 -0.0403 0.7297 0.069 Uiso 1 1 calc R . . C10 C -0.4594(3) 0.03014(18) 0.8128(3) 0.0586(13) Uani 1 1 d . . . H10A H -0.4786 0.0350 0.8575 0.070 Uiso 1 1 calc R . . C11 C -0.1702(3) 0.26086(17) 1.0118(2) 0.0539(12) Uani 1 1 d . . . H11A H -0.1840 0.2802 1.0485 0.065 Uiso 1 1 calc R . . C12 C -0.3854(3) 0.00451(16) 0.6121(3) 0.0529(12) Uani 1 1 d . . . H12A H -0.3571 -0.0220 0.6030 0.064 Uiso 1 1 calc R . . C13 C -0.4482(2) 0.20744(17) 0.3753(2) 0.0492(11) Uani 1 1 d . . . H13A H -0.4639 0.2377 0.3912 0.059 Uiso 1 1 calc R . . H13B H -0.4887 0.1957 0.3437 0.059 Uiso 1 1 calc R . . C14 C -0.1265(2) 0.04359(16) 0.9344(2) 0.0453(10) Uani 1 1 d . . . H14A H -0.1013 0.0610 0.9691 0.054 Uiso 1 1 calc R . . C15 C -0.1771(3) 0.02868(15) 0.6686(2) 0.0482(11) Uani 1 1 d . . . H15A H -0.2042 0.0010 0.6696 0.058 Uiso 1 1 calc R . . C16 C -0.4692(3) 0.08227(16) 0.6376(2) 0.0486(11) Uani 1 1 d . . . H16A H -0.4976 0.1088 0.6461 0.058 Uiso 1 1 calc R . . C17 C -0.5123(3) 0.16444(16) 0.4591(3) 0.0521(11) Uani 1 1 d . . . H17A H -0.5386 0.1446 0.4251 0.063 Uiso 1 1 calc R . . H17B H -0.5448 0.1913 0.4661 0.063 Uiso 1 1 calc R . . C18 C -0.4137(3) -0.00704(17) 0.8006(3) 0.0594(13) Uani 1 1 d . . . H18A H -0.4004 -0.0270 0.8373 0.071 Uiso 1 1 calc R . . C19 C -0.4517(2) 0.05241(15) 0.6932(2) 0.0433(10) Uani 1 1 d . . . C20 C -0.4419(2) 0.25558(15) 0.6145(2) 0.0447(10) Uani 1 1 d . . . H20A H -0.4614 0.2355 0.5803 0.054 Uiso 1 1 calc R . . C21 C -0.0860(3) -0.00235(15) 0.7558(2) 0.0479(11) Uani 1 1 d . . . H21A H -0.0299 -0.0020 0.7625 0.057 Uiso 1 1 calc R . . H21B H -0.1012 -0.0324 0.7381 0.057 Uiso 1 1 calc R . . C22 C -0.1976(3) -0.00885(15) 0.8335(2) 0.0483(11) Uani 1 1 d . . . H22A H -0.2221 -0.0273 0.7996 0.058 Uiso 1 1 calc R . . C23 C -0.0880(3) 0.03249(15) 0.8736(2) 0.0454(10) Uani 1 1 d . . . H23A H -0.0376 0.0430 0.8670 0.055 Uiso 1 1 calc R . . C24 C -0.4070(3) 0.01374(16) 0.6810(3) 0.0512(11) Uani 1 1 d . . . C25 C -0.2352(3) 0.00301(16) 0.8924(2) 0.0503(11) Uani 1 1 d . . . H25A H -0.2861 -0.0070 0.8981 0.060 Uiso 1 1 calc R . . C26 C -0.4769(3) 0.05999(16) 0.7605(2) 0.0490(11) Uani 1 1 d . . . H26A H -0.5065 0.0860 0.7700 0.059 Uiso 1 1 calc R . . C27 C -0.5010(3) 0.13959(15) 0.5269(3) 0.0530(12) Uani 1 1 d . . . H27A H -0.4719 0.1587 0.5600 0.064 Uiso 1 1 calc R . . H27B H -0.5512 0.1328 0.5468 0.064 Uiso 1 1 calc R . . C28 C -0.3868(3) 0.31564(15) 0.7122(2) 0.0457(10) Uani 1 1 d . . . H28A H -0.3683 0.3368 0.7453 0.055 Uiso 1 1 calc R . . C29 C -0.0604(3) 0.37002(16) 0.7494(2) 0.0541(13) Uani 1 1 d . . . H29A H -0.0214 0.3466 0.7417 0.065 Uiso 1 1 calc R . . H29B H -0.0598 0.3915 0.7104 0.065 Uiso 1 1 calc R . . C30 C -0.2056(3) 0.06389(15) 0.6310(2) 0.0494(11) Uani 1 1 d . . . H30A H -0.2529 0.0607 0.6066 0.059 Uiso 1 1 calc R . . C31 C -0.2956(2) 0.18323(16) 0.5277(2) 0.0452(10) Uani 1 1 d . . . H31A H -0.3340 0.1823 0.4923 0.054 Uiso 1 1 calc R . . C32 C -0.0457(3) 0.10330(15) 0.4478(3) 0.0516(11) Uani 1 1 d . . . H32A H -0.0622 0.0949 0.4946 0.062 Uiso 1 1 calc R . . H32B H 0.0106 0.1018 0.4469 0.062 Uiso 1 1 calc R . . C33 C -0.4838(3) 0.26411(16) 0.6718(2) 0.0464(11) Uani 1 1 d . . . H33A H -0.5317 0.2499 0.6775 0.056 Uiso 1 1 calc R . . C34 C -0.4987(3) 0.30105(15) 0.7883(2) 0.0452(10) Uani 1 1 d . . . H34A H -0.4873 0.3312 0.8077 0.054 Uiso 1 1 calc R . . H34B H -0.5542 0.2992 0.7782 0.054 Uiso 1 1 calc R . . C35 C -0.3713(2) 0.27586(15) 0.6055(2) 0.0419(10) Uani 1 1 d . . . C36 C -0.4103(3) 0.11402(15) 0.9551(2) 0.0450(10) Uani 1 1 d . . . H36A H -0.4630 0.1104 0.9441 0.054 Uiso 1 1 calc R . . C37 C 0.1267(2) 0.11506(15) 0.8042(3) 0.0519(12) Uani 1 1 d . . . H37A H 0.1440 0.1083 0.7571 0.062 Uiso 1 1 calc R . . H37B H 0.1723 0.1176 0.8349 0.062 Uiso 1 1 calc R . . C38 C -0.5045(2) 0.22388(15) 0.8314(2) 0.0421(10) Uani 1 1 d . . . H38A H -0.5444 0.2189 0.7983 0.051 Uiso 1 1 calc R . . C39 C -0.4226(2) 0.27357(15) 0.8886(2) 0.0431(10) Uani 1 1 d . . . H39A H -0.4051 0.3035 0.8960 0.052 Uiso 1 1 calc R . . C40 C -0.2595(2) 0.12284(15) 0.9891(2) 0.0431(10) Uani 1 1 d . . . H40A H -0.2070 0.1257 1.0015 0.052 Uiso 1 1 calc R . . C41 C 0.1007(2) 0.34048(14) 0.6310(2) 0.0405(10) Uani 1 1 d . . . H41A H 0.0718 0.3672 0.6243 0.049 Uiso 1 1 calc R . . C42 C -0.3753(3) 0.21107(17) 0.3379(2) 0.0502(11) Uani 1 1 d . . . H42A H -0.3593 0.1808 0.3223 0.060 Uiso 1 1 calc R . . H42B H -0.3829 0.2303 0.2966 0.060 Uiso 1 1 calc R . . C43 C 0.0658(2) 0.29848(13) 0.62756(19) 0.0349(9) Uani 1 1 d . . . C44 C -0.3114(2) 0.19725(15) 0.7682(2) 0.0382(9) Uani 1 1 d . . . H44A H -0.3409 0.2231 0.7567 0.046 Uiso 1 1 calc R . . C45 C -0.2438(3) 0.04200(14) 1.0063(2) 0.0430(10) Uani 1 1 d . . . H45A H -0.2075 0.0488 1.0447 0.052 Uiso 1 1 calc R . . H45B H -0.2761 0.0164 1.0204 0.052 Uiso 1 1 calc R . . C46 C -0.3446(2) 0.30654(15) 0.6540(2) 0.0450(10) Uani 1 1 d . . . H46A H -0.2973 0.3214 0.6476 0.054 Uiso 1 1 calc R . . C47 C -0.2973(2) 0.11635(15) 0.7729(2) 0.0438(10) Uani 1 1 d . . . H47A H -0.3181 0.0872 0.7650 0.053 Uiso 1 1 calc R . . C48 C 0.1865(2) 0.26180(16) 0.6496(2) 0.0431(10) Uani 1 1 d . . . H48A H 0.2156 0.2350 0.6553 0.052 Uiso 1 1 calc R . . C49 C -0.4778(2) 0.18889(15) 0.8697(2) 0.0417(10) Uani 1 1 d . . . H49A H -0.5001 0.1599 0.8643 0.050 Uiso 1 1 calc R . . C50 C -0.0691(2) 0.07064(14) 0.7010(2) 0.0411(9) Uani 1 1 d . . . H50A H -0.0217 0.0730 0.7255 0.049 Uiso 1 1 calc R . . C51 C -0.3935(2) 0.23951(14) 0.9282(2) 0.0403(9) Uani 1 1 d . . . H51A H -0.3566 0.2460 0.9635 0.048 Uiso 1 1 calc R . . C52 C -0.1393(3) 0.34860(15) 0.7550(2) 0.0470(11) Uani 1 1 d . . . H52A H -0.1458 0.3375 0.8027 0.056 Uiso 1 1 calc R . . H52B H -0.1789 0.3717 0.7456 0.056 Uiso 1 1 calc R . . C53 C -0.1287(2) 0.20409(14) 0.9058(2) 0.0374(9) Uani 1 1 d . . . C54 C 0.1795(2) 0.34241(16) 0.6447(2) 0.0448(10) Uani 1 1 d . . . H54A H 0.2041 0.3708 0.6483 0.054 Uiso 1 1 calc R . . C55 C -0.4041(3) 0.03214(16) 0.5599(2) 0.0489(11) Uani 1 1 d . . . C56 C 0.2214(2) 0.30375(16) 0.6529(2) 0.0461(11) Uani 1 1 d . . . H56A H 0.2749 0.3057 0.6608 0.055 Uiso 1 1 calc R . . C57 C -0.4548(2) 0.29422(14) 0.7221(2) 0.0409(10) Uani 1 1 d . . . C58 C -0.1034(2) 0.19451(15) 0.9728(2) 0.0417(10) Uani 1 1 d . . . H58A H -0.0713 0.1694 0.9821 0.050 Uiso 1 1 calc R . . C59 C -0.3237(2) 0.26405(15) 0.5437(2) 0.0440(10) Uani 1 1 d . . . H59A H -0.3575 0.2589 0.5029 0.053 Uiso 1 1 calc R . . H59B H -0.2892 0.2894 0.5334 0.053 Uiso 1 1 calc R . . C60 C -0.3675(2) 0.07752(16) 0.9770(2) 0.0450(10) Uani 1 1 d . . . H60A H -0.3910 0.0489 0.9815 0.054 Uiso 1 1 calc R . . C61 C -0.2008(3) 0.02925(14) 0.9438(2) 0.0415(10) Uani 1 1 d . . . C62 C -0.2543(2) 0.24660(17) 0.3447(2) 0.0450(10) Uani 1 1 d . . . H62A H -0.2701 0.2732 0.3170 0.054 Uiso 1 1 calc R . . H62B H -0.2361 0.2231 0.3128 0.054 Uiso 1 1 calc R . . C63 C -0.1936(2) 0.27072(15) 0.9445(2) 0.0400(9) Uani 1 1 d . . . H63A H -0.2233 0.2968 0.9348 0.048 Uiso 1 1 calc R . . C64 C -0.3399(2) 0.15449(15) 0.7557(2) 0.0440(10) Uani 1 1 d . . . H64A H -0.3893 0.1511 0.7351 0.053 Uiso 1 1 calc R . . C65 C -0.1661(2) 0.10447(14) 0.6281(2) 0.0384(9) Uani 1 1 d . . . C66 C -0.1244(2) 0.24448(12) 0.77500(18) 0.0295(8) Uani 1 1 d . . . C67 C 0.0099(2) 0.21599(13) 0.57231(17) 0.0302(8) Uani 1 1 d . . . C68 C -0.2585(3) 0.14455(15) 0.5466(2) 0.0458(10) Uani 1 1 d . . . H68A H -0.2714 0.1169 0.5246 0.055 Uiso 1 1 calc R . . C69 C -0.1729(2) 0.24174(13) 0.89127(19) 0.0355(9) Uani 1 1 d . . . C70 C -0.1152(2) 0.17476(13) 0.8422(2) 0.0345(9) Uani 1 1 d . . . H70A H -0.0836 0.1475 0.8524 0.041 Uiso 1 1 calc R . . C71 C -0.1262(3) 0.22235(17) 1.0254(2) 0.0492(11) Uani 1 1 d . . . H71A H -0.1117 0.2153 1.0716 0.059 Uiso 1 1 calc R . . C72 C 0.0846(2) 0.15848(15) 0.8036(2) 0.0463(11) Uani 1 1 d . . . H72A H 0.0663 0.1651 0.8504 0.056 Uiso 1 1 calc R . . H72B H 0.1191 0.1831 0.7899 0.056 Uiso 1 1 calc R . . C73 C -0.0825(2) 0.25912(13) 0.50578(18) 0.0334(8) Uani 1 1 d . . . H73A H -0.1090 0.2865 0.4971 0.040 Uiso 1 1 calc R . . C74 C 0.1081(2) 0.25985(14) 0.63785(18) 0.0339(8) Uani 1 1 d . . . C75 C -0.1917(2) 0.25939(15) 0.3946(2) 0.0407(10) Uani 1 1 d . . . H75A H -0.1594 0.2831 0.3744 0.049 Uiso 1 1 calc R . . H75B H -0.2135 0.2713 0.4376 0.049 Uiso 1 1 calc R . . C76 C -0.3764(2) 0.15609(14) 0.94894(19) 0.0368(9) Uani 1 1 d . . . C77 C -0.3003(2) 0.16028(14) 0.9684(2) 0.0400(9) Uani 1 1 d . . . H77A H -0.2763 0.1889 0.9674 0.048 Uiso 1 1 calc R . . C78 C -0.0955(2) 0.10637(14) 0.6617(2) 0.0412(10) Uani 1 1 d . . . H78A H -0.0650 0.1326 0.6576 0.049 Uiso 1 1 calc R . . C79 C -0.1946(2) 0.16371(13) 0.81237(18) 0.0332(8) Uani 1 1 d . . . C80 C -0.1975(2) 0.24619(13) 0.81584(19) 0.0330(8) Uani 1 1 d . . . H80A H -0.2293 0.2735 0.8059 0.040 Uiso 1 1 calc R . . C81 C -0.0807(2) 0.20582(13) 0.78798(18) 0.0325(8) Uani 1 1 d . . . C82 C -0.1831(2) 0.18734(13) 0.6262(2) 0.0381(9) Uani 1 1 d . . . H82A H -0.1429 0.1896 0.6598 0.046 Uiso 1 1 calc R . . C83 C -0.4172(2) 0.19512(14) 0.91736(19) 0.0368(9) Uani 1 1 d . . . C84 C -0.1238(2) 0.00637(14) 0.8241(2) 0.0409(10) Uani 1 1 d . . . C85 C -0.0016(2) 0.17918(13) 0.53015(19) 0.0332(8) Uani 1 1 d . . . H85A H 0.0267 0.1524 0.5382 0.040 Uiso 1 1 calc R . . C86 C -0.2216(2) 0.22471(15) 0.6060(2) 0.0403(9) Uani 1 1 d . . . H86A H -0.2081 0.2529 0.6259 0.048 Uiso 1 1 calc R . . C87 C -0.2021(2) 0.14551(14) 0.59791(19) 0.0375(9) Uani 1 1 d . . . C88 C -0.0179(2) 0.19622(13) 0.74783(18) 0.0302(8) Uani 1 1 d . . . C89 C -0.0195(2) 0.29036(13) 0.61825(18) 0.0308(8) Uani 1 1 d . . . H89A H -0.0494 0.3186 0.6103 0.037 Uiso 1 1 calc R . . C90 C -0.2245(2) 0.12093(14) 0.8017(2) 0.0396(9) Uani 1 1 d . . . H90A H -0.1954 0.0950 0.8140 0.048 Uiso 1 1 calc R . . C91 C -0.2382(2) 0.20166(13) 0.79811(19) 0.0329(8) Uani 1 1 d . . . C92 C -0.0306(2) 0.25574(13) 0.56124(19) 0.0317(8) Uani 1 1 d . . . C93 C 0.0589(2) 0.21715(13) 0.63893(18) 0.0330(8) Uani 1 1 d . . . H93A H 0.0893 0.1890 0.6467 0.040 Uiso 1 1 calc R . . C94 C -0.0427(2) 0.26464(12) 0.68240(18) 0.0288(8) Uani 1 1 d . . . C95 C 0.0000(2) 0.22533(13) 0.69442(17) 0.0299(8) Uani 1 1 d . . . C96 C -0.1049(2) 0.27447(12) 0.72305(18) 0.0305(8) Uani 1 1 d . . . C97 C -0.0547(2) 0.18121(14) 0.47575(19) 0.0358(9) Uani 1 1 d . . . C98 C -0.0951(2) 0.22229(14) 0.46361(19) 0.0355(9) Uani 1 1 d . . . N5 N -0.6311(4) -0.04376(19) 0.8699(3) 0.101(2) Uani 1 1 d . . . C99 C -0.6473(3) -0.0131(2) 0.8382(3) 0.0635(14) Uani 1 1 d . . . C100 C -0.6683(3) 0.0258(2) 0.7977(3) 0.0741(16) Uani 1 1 d . . . H10B H -0.6324 0.0294 0.7601 0.111 Uiso 1 1 d R . . H10C H -0.6667 0.0527 0.8271 0.111 Uiso 1 1 d R . . H10D H -0.7200 0.0219 0.7784 0.111 Uiso 1 1 d R . . N6 N -0.4109(4) 0.34148(19) 0.4749(3) 0.0875(17) Uani 1 1 d . . . C101 C -0.4015(4) 0.3765(2) 0.4983(3) 0.0789(18) Uani 1 1 d . . . C102 C -0.3897(5) 0.4200(3) 0.5284(5) 0.140(4) Uani 1 1 d . . . H10E H -0.4178 0.4221 0.5713 0.210 Uiso 1 1 d R . . H10F H -0.4079 0.4433 0.4962 0.210 Uiso 1 1 d R . . H10G H -0.3351 0.4244 0.5384 0.210 Uiso 1 1 d R . . N7 N -0.0513(7) -0.0520(4) 0.3970(9) 0.253(8) Uani 1 1 d . . . C103 C -0.1116(7) -0.0675(3) 0.4000(5) 0.121(3) Uani 1 1 d . . . C104 C -0.1870(5) -0.0860(3) 0.4028(4) 0.114(3) Uani 1 1 d . . . H10H H -0.2138 -0.0725 0.4414 0.171 Uiso 1 1 d R . . H10I H -0.1839 -0.1187 0.4092 0.171 Uiso 1 1 d R . . H10J H -0.2150 -0.0793 0.3596 0.171 Uiso 1 1 d 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 P1 0.0672(9) 0.0495(8) 0.0467(7) -0.0012(5) -0.0101(6) 0.0082(6) P2 0.0625(8) 0.0446(7) 0.0466(7) -0.0012(5) 0.0087(6) 0.0017(6) P3 0.0575(8) 0.0435(7) 0.0411(6) 0.0018(5) 0.0041(5) 0.0067(6) P4 0.0644(9) 0.0597(9) 0.0626(9) -0.0081(7) 0.0051(7) -0.0179(7) F1 0.166(5) 0.244(7) 0.321(10) -0.209(7) 0.147(6) -0.142(5) F2 0.393(11) 0.232(7) 0.091(4) -0.040(4) -0.108(5) 0.228(8) F3 0.227(6) 0.115(4) 0.182(6) -0.060(4) 0.133(5) -0.065(4) F4 0.244(7) 0.135(4) 0.134(5) -0.006(3) -0.106(5) 0.059(4) F5 0.108(3) 0.075(2) 0.111(3) -0.045(2) -0.009(2) 0.015(2) F6 0.111(3) 0.074(2) 0.081(2) -0.0237(18) 0.026(2) 0.005(2) F7 0.153(4) 0.0545(19) 0.079(2) 0.0089(17) 0.038(2) -0.005(2) F8 0.084(2) 0.089(2) 0.104(3) -0.010(2) -0.034(2) 0.030(2) F9 0.061(2) 0.109(3) 0.071(2) -0.0096(18) 0.0071(16) -0.0211(18) F10 0.0654(18) 0.0499(16) 0.0584(17) 0.0008(13) 0.0048(14) 0.0013(13) F11 0.090(2) 0.0545(17) 0.0668(19) -0.0127(14) 0.0306(17) -0.0007(16) F12 0.098(3) 0.074(2) 0.0518(17) -0.0072(15) 0.0216(16) 0.0056(18) F13 0.217(5) 0.096(3) 0.0419(19) 0.0165(18) -0.003(2) -0.018(3) F14 0.064(2) 0.072(2) 0.279(7) -0.041(3) 0.068(3) -0.0197(19) F15 0.307(7) 0.080(3) 0.049(2) 0.0058(18) -0.012(3) -0.005(3) F16 0.064(2) 0.094(3) 0.225(6) -0.079(3) -0.021(3) 0.028(2) F17 0.112(3) 0.0461(18) 0.089(2) -0.0057(16) -0.024(2) 0.0108(17) F18 0.0474(16) 0.0476(16) 0.085(2) -0.0016(14) 0.0054(14) 0.0054(12) F19 0.110(3) 0.061(2) 0.222(6) 0.028(3) -0.027(4) -0.006(2) F20 0.119(3) 0.122(3) 0.092(3) -0.030(2) 0.040(3) -0.025(3) F21 0.082(2) 0.117(3) 0.101(3) -0.055(2) 0.007(2) -0.036(2) F22 0.113(3) 0.071(2) 0.105(3) -0.007(2) -0.011(2) 0.010(2) F23 0.083(3) 0.164(4) 0.065(2) -0.013(2) 0.0137(19) -0.047(3) F24 0.075(2) 0.091(2) 0.096(3) -0.015(2) -0.0008(19) -0.0300(19) O1 0.0345(15) 0.0385(16) 0.0365(14) 0.0060(11) 0.0012(11) 0.0034(12) O2 0.059(2) 0.064(2) 0.058(2) -0.0037(17) -0.0063(16) -0.0057(17) O3 0.0316(14) 0.0345(15) 0.0339(14) 0.0036(11) -0.0025(11) 0.0033(11) O4 0.0427(19) 0.046(2) 0.110(3) 0.021(2) 0.0090(19) 0.0040(15) O5 0.0534(19) 0.0490(18) 0.0386(16) -0.0116(13) -0.0044(13) 0.0002(15) O6 0.071(3) 0.116(4) 0.072(3) -0.017(2) 0.001(2) -0.041(2) O7 0.055(2) 0.082(3) 0.093(3) -0.026(2) 0.014(2) -0.002(2) O8 0.069(2) 0.054(2) 0.064(2) -0.0069(17) 0.0118(18) 0.0048(18) O9 0.0406(16) 0.0603(19) 0.0312(14) -0.0042(13) -0.0115(12) 0.0037(14) O10 0.0378(16) 0.068(2) 0.0321(15) 0.0021(13) -0.0023(12) -0.0105(14) O11 0.0347(16) 0.0576(19) 0.0481(17) 0.0096(14) -0.0026(13) -0.0025(14) O12 0.060(2) 0.0491(19) 0.0501(19) -0.0033(14) 0.0113(15) 0.0065(15) N1 0.0368(18) 0.047(2) 0.0319(17) 0.0032(15) 0.0022(13) 0.0035(15) N2 0.050(2) 0.042(2) 0.0358(18) 0.0010(15) 0.0035(15) 0.0005(17) N3 0.046(2) 0.047(2) 0.0334(17) 0.0076(15) 0.0046(14) -0.0084(17) N4 0.0404(19) 0.048(2) 0.0325(17) 0.0001(15) 0.0092(14) 0.0088(16) C1 0.072(4) 0.111(5) 0.075(4) 0.013(4) 0.004(3) -0.001(4) C2 0.068(4) 0.045(3) 0.206(9) 0.037(4) -0.003(5) 0.013(3) C3 0.058(3) 0.079(4) 0.095(5) 0.006(3) -0.003(3) 0.009(3) C4 0.058(3) 0.077(4) 0.079(4) -0.026(3) 0.011(3) -0.011(3) C5 0.081(4) 0.072(4) 0.088(4) -0.035(3) 0.009(3) -0.006(3) C6 0.047(3) 0.064(3) 0.097(4) 0.002(3) -0.011(3) -0.009(3) C7 0.070(4) 0.058(3) 0.071(3) -0.029(3) 0.007(3) 0.005(3) C8 0.045(3) 0.045(3) 0.050(3) 0.001(2) 0.0027(19) -0.003(2) C9 0.055(3) 0.043(3) 0.073(4) 0.004(2) -0.016(3) -0.006(2) C10 0.055(3) 0.066(3) 0.055(3) 0.004(2) -0.005(2) -0.008(3) C11 0.060(3) 0.067(3) 0.035(2) -0.010(2) 0.011(2) -0.022(3) C12 0.050(3) 0.040(3) 0.068(3) -0.007(2) 0.002(2) 0.000(2) C13 0.038(2) 0.058(3) 0.051(3) 0.008(2) -0.0061(19) -0.002(2) C14 0.043(2) 0.052(3) 0.040(2) -0.0009(19) -0.0035(18) -0.005(2) C15 0.049(3) 0.044(3) 0.051(3) -0.007(2) -0.005(2) -0.014(2) C16 0.040(2) 0.054(3) 0.051(3) -0.008(2) 0.0082(19) -0.003(2) C17 0.039(2) 0.058(3) 0.059(3) -0.002(2) 0.007(2) 0.001(2) C18 0.066(3) 0.055(3) 0.056(3) 0.006(2) -0.012(2) -0.011(3) C19 0.037(2) 0.045(3) 0.048(2) -0.0009(19) -0.0008(18) -0.0087(19) C20 0.047(3) 0.053(3) 0.034(2) -0.0036(18) 0.0000(18) 0.000(2) C21 0.057(3) 0.041(2) 0.045(2) 0.0063(19) 0.003(2) 0.006(2) C22 0.059(3) 0.047(3) 0.039(2) -0.0046(19) -0.001(2) -0.006(2) C23 0.040(2) 0.047(3) 0.049(2) 0.006(2) 0.0026(19) -0.005(2) C24 0.041(2) 0.050(3) 0.063(3) -0.007(2) 0.002(2) -0.011(2) C25 0.051(3) 0.056(3) 0.044(2) 0.005(2) -0.001(2) -0.006(2) C26 0.048(3) 0.053(3) 0.046(3) -0.002(2) -0.003(2) -0.006(2) C27 0.056(3) 0.047(3) 0.056(3) -0.003(2) 0.013(2) 0.008(2) C28 0.048(3) 0.051(3) 0.038(2) -0.0030(19) 0.0096(18) 0.003(2) C29 0.075(3) 0.044(3) 0.044(2) -0.007(2) 0.011(2) -0.025(2) C30 0.056(3) 0.050(3) 0.041(2) 0.002(2) -0.014(2) -0.006(2) C31 0.042(2) 0.065(3) 0.028(2) 0.0007(19) -0.0062(16) -0.005(2) C32 0.045(3) 0.051(3) 0.059(3) -0.010(2) 0.003(2) -0.004(2) C33 0.040(2) 0.061(3) 0.038(2) 0.006(2) 0.0046(17) 0.001(2) C34 0.044(2) 0.049(3) 0.043(2) 0.0086(19) 0.0117(19) 0.014(2) C35 0.036(2) 0.056(3) 0.034(2) 0.0029(18) 0.0038(16) 0.0050(19) C36 0.040(2) 0.054(3) 0.041(2) 0.005(2) 0.0055(18) -0.004(2) C37 0.036(2) 0.050(3) 0.069(3) 0.013(2) -0.004(2) 0.001(2) C38 0.033(2) 0.058(3) 0.036(2) 0.0000(19) 0.0039(16) 0.001(2) C39 0.041(2) 0.050(3) 0.039(2) -0.0044(19) 0.0088(17) -0.001(2) C40 0.041(2) 0.054(3) 0.034(2) 0.0045(18) 0.0046(17) -0.009(2) C41 0.046(2) 0.045(2) 0.031(2) 0.0011(17) 0.0076(17) -0.0075(19) C42 0.047(3) 0.069(3) 0.034(2) -0.004(2) -0.0039(18) -0.006(2) C43 0.035(2) 0.045(2) 0.0250(18) -0.0010(16) 0.0057(15) -0.0055(18) C44 0.033(2) 0.049(3) 0.033(2) 0.0038(17) 0.0064(16) 0.0032(18) C45 0.049(3) 0.040(2) 0.039(2) 0.0076(18) 0.0010(18) -0.002(2) C46 0.034(2) 0.059(3) 0.042(2) -0.001(2) 0.0062(17) 0.001(2) C47 0.040(2) 0.047(3) 0.045(2) -0.0045(19) 0.0068(18) -0.009(2) C48 0.041(2) 0.060(3) 0.0283(19) 0.0024(18) 0.0050(16) -0.004(2) C49 0.038(2) 0.052(3) 0.036(2) -0.0045(18) 0.0042(17) -0.0026(19) C50 0.039(2) 0.044(2) 0.041(2) -0.0011(18) 0.0040(17) 0.0006(19) C51 0.035(2) 0.049(3) 0.037(2) 0.0001(18) 0.0045(16) -0.0021(19) C52 0.053(3) 0.043(3) 0.046(2) -0.0050(19) 0.009(2) 0.008(2) C53 0.032(2) 0.046(2) 0.033(2) 0.0042(17) 0.0033(15) -0.0115(18) C54 0.042(2) 0.056(3) 0.037(2) 0.0030(19) 0.0042(18) -0.014(2) C55 0.047(3) 0.053(3) 0.047(3) -0.007(2) 0.013(2) -0.006(2) C56 0.032(2) 0.068(3) 0.038(2) -0.001(2) 0.0021(17) -0.014(2) C57 0.040(2) 0.047(2) 0.036(2) 0.0073(18) 0.0053(17) 0.0100(19) C58 0.038(2) 0.057(3) 0.030(2) 0.0115(18) 0.0014(16) -0.0089(19) C59 0.039(2) 0.058(3) 0.035(2) 0.0060(19) 0.0041(17) 0.008(2) C60 0.043(2) 0.054(3) 0.038(2) 0.0066(19) 0.0018(18) -0.012(2) C61 0.049(2) 0.040(2) 0.035(2) 0.0059(17) 0.0003(17) -0.006(2) C62 0.040(2) 0.067(3) 0.0275(19) 0.0056(19) 0.0001(16) -0.001(2) C63 0.042(2) 0.044(2) 0.034(2) -0.0003(17) 0.0094(16) -0.0062(19) C64 0.035(2) 0.056(3) 0.041(2) -0.0089(19) 0.0025(17) -0.008(2) C65 0.041(2) 0.043(2) 0.0304(19) -0.0027(16) 0.0024(16) -0.0058(19) C66 0.0309(19) 0.033(2) 0.0241(17) 0.0016(14) 0.0038(14) 0.0002(16) C67 0.0268(18) 0.040(2) 0.0238(17) 0.0040(15) 0.0042(13) -0.0006(16) C68 0.055(3) 0.048(3) 0.034(2) -0.0027(18) -0.0039(19) 0.000(2) C69 0.036(2) 0.041(2) 0.0298(19) 0.0032(16) 0.0024(15) -0.0109(17) C70 0.035(2) 0.034(2) 0.034(2) 0.0068(16) 0.0014(15) -0.0009(17) C71 0.048(3) 0.071(3) 0.028(2) 0.004(2) -0.0007(17) -0.019(2) C72 0.039(2) 0.046(3) 0.053(3) 0.012(2) -0.0176(19) 0.0020(19) C73 0.033(2) 0.039(2) 0.0283(18) 0.0026(15) 0.0018(14) 0.0043(17) C74 0.0283(19) 0.047(2) 0.0266(18) 0.0018(16) -0.0015(14) -0.0040(17) C75 0.036(2) 0.055(3) 0.032(2) 0.0078(18) 0.0011(16) 0.0033(19) C76 0.040(2) 0.046(2) 0.0250(18) 0.0021(16) 0.0066(15) -0.0032(18) C77 0.039(2) 0.044(2) 0.037(2) 0.0025(18) 0.0080(17) -0.0053(19) C78 0.040(2) 0.043(2) 0.041(2) 0.0024(18) 0.0055(17) -0.0066(19) C79 0.0293(19) 0.044(2) 0.0265(18) 0.0003(15) 0.0034(14) -0.0043(17) C80 0.033(2) 0.037(2) 0.0295(18) 0.0002(15) 0.0057(15) 0.0012(16) C81 0.0295(19) 0.041(2) 0.0272(18) 0.0063(15) 0.0017(14) -0.0056(16) C82 0.034(2) 0.040(2) 0.040(2) 0.0004(17) -0.0015(16) -0.0025(18) C83 0.033(2) 0.050(3) 0.0276(18) -0.0005(16) 0.0067(15) -0.0030(18) C84 0.042(2) 0.036(2) 0.044(2) 0.0069(18) 0.0000(18) 0.0073(18) C85 0.0314(19) 0.039(2) 0.0293(18) 0.0025(16) 0.0041(14) 0.0032(17) C86 0.035(2) 0.052(3) 0.034(2) -0.0013(18) -0.0028(16) -0.0023(19) C87 0.038(2) 0.046(2) 0.0291(19) 0.0032(17) 0.0041(15) -0.0017(18) C88 0.0276(18) 0.033(2) 0.0298(18) 0.0004(15) -0.0016(14) 0.0013(15) C89 0.0286(19) 0.034(2) 0.0293(18) 0.0038(15) 0.0006(14) -0.0026(16) C90 0.038(2) 0.042(2) 0.040(2) 0.0003(17) 0.0095(17) -0.0069(18) C91 0.0277(19) 0.042(2) 0.0296(18) 0.0032(16) 0.0066(14) -0.0024(16) C92 0.0274(18) 0.038(2) 0.0298(18) 0.0065(15) 0.0019(14) -0.0017(16) C93 0.0313(19) 0.040(2) 0.0277(18) -0.0003(15) 0.0030(14) 0.0025(17) C94 0.0250(18) 0.030(2) 0.0311(18) 0.0017(14) 0.0017(14) -0.0013(15) C95 0.0261(18) 0.039(2) 0.0241(17) 0.0022(14) -0.0013(13) -0.0011(16) C96 0.0307(19) 0.031(2) 0.0297(18) -0.0013(14) -0.0014(14) -0.0035(16) C97 0.037(2) 0.043(2) 0.0264(18) -0.0039(16) -0.0017(15) -0.0008(18) C98 0.0277(19) 0.051(2) 0.0276(18) 0.0052(16) -0.0018(14) -0.0021(17) N5 0.158(6) 0.077(4) 0.070(4) 0.008(3) 0.042(4) 0.000(4) C99 0.081(4) 0.065(4) 0.045(3) -0.002(3) 0.016(3) -0.012(3) C100 0.068(4) 0.095(5) 0.059(3) -0.001(3) -0.006(3) 0.001(3) N6 0.125(5) 0.075(4) 0.061(3) 0.005(3) -0.018(3) -0.004(3) C101 0.094(5) 0.083(4) 0.060(4) -0.008(3) 0.001(3) -0.023(4) C102 0.109(6) 0.114(6) 0.201(10) -0.090(7) 0.081(7) -0.053(5) N7 0.154(10) 0.208(11) 0.40(2) -0.105(12) 0.146(12) 0.005(9) C103 0.151(9) 0.115(7) 0.097(6) -0.007(5) 0.033(6) 0.039(7) C104 0.102(6) 0.151(8) 0.089(6) 0.009(5) -0.007(5) 0.017(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 P1 F2 1.474(4) . ? P1 F1 1.490(5) . ? P1 F4 1.539(4) . ? P1 F3 1.557(5) . ? P1 F5 1.578(3) . ? P1 F6 1.592(3) . ? P2 F8 1.566(4) . ? P2 F10 1.584(3) . ? P2 F7 1.587(3) . ? P2 F12 1.600(3) . ? P2 F11 1.607(3) . ? P2 F9 1.610(3) . ? P3 F13 1.530(4) . ? P3 F14 1.539(4) . ? P3 F16 1.562(4) . ? P3 F15 1.563(4) . ? P3 F17 1.583(3) . ? P3 F18 1.598(3) . ? P4 F19 1.563(4) . ? P4 F24 1.566(3) . ? P4 F23 1.579(4) . ? P4 F20 1.586(4) . ? P4 F21 1.591(3) . ? P4 F22 1.601(4) . ? O1 C96 1.380(4) . ? O1 C52 1.461(5) . ? O2 C29 1.405(5) . ? O2 C6 1.424(6) . ? O3 C88 1.384(4) . ? O3 C72 1.434(5) . ? O4 C37 1.403(5) . ? O4 C2 1.424(6) . ? O5 C97 1.355(5) . ? O5 C32 1.428(5) . ? O6 C1 1.402(7) . ? O6 C5 1.443(7) . ? O7 C3 1.378(7) . ? O7 C4 1.413(6) . ? O8 C55 1.387(5) . ? O8 C7 1.416(6) . ? O9 C98 1.380(4) . ? O9 C75 1.416(5) . ? O10 C42 1.426(5) . ? O10 C62 1.426(5) . ? O11 C13 1.424(5) . ? O11 C17 1.439(5) . ? O12 C8 1.373(5) . ? O12 C27 1.410(5) . ? N1 C86 1.340(5) . ? N1 C31 1.352(5) . ? N1 C59 1.484(5) . ? N2 C50 1.325(5) . ? N2 C15 1.369(5) . ? N2 C21 1.495(5) . ? N3 C60 1.339(5) . ? N3 C40 1.340(5) . ? N3 C45 1.500(5) . ? N4 C39 1.339(5) . ? N4 C38 1.341(5) . ? N4 C34 1.498(5) . ? C1 C3 1.527(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.482(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C32 1.510(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C16 1.352(6) . ? C8 C55 1.458(6) . ? C9 C18 1.338(7) . ? C9 C24 1.412(7) . ? C9 H9A 0.9500 . ? C10 C26 1.376(7) . ? C10 C18 1.388(7) . ? C10 H10A 0.9500 . ? C11 C63 1.391(6) . ? C11 C71 1.402(7) . ? C11 H11A 0.9500 . ? C12 C55 1.338(7) . ? C12 C24 1.425(7) . ? C12 H12A 0.9500 . ? C13 C42 1.490(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C61 1.387(6) . ? C14 C23 1.412(6) . ? C14 H14A 0.9500 . ? C15 C30 1.363(6) . ? C15 H15A 0.9500 . ? C16 C19 1.424(6) . ? C16 H16A 0.9500 . ? C17 C27 1.516(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9500 . ? C19 C26 1.407(6) . ? C19 C24 1.413(6) . ? C20 C33 1.370(6) . ? C20 C35 1.391(6) . ? C20 H20A 0.9500 . ? C21 C84 1.518(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C25 1.379(6) . ? C22 C84 1.388(6) . ? C22 H22A 0.9500 . ? C23 C84 1.374(6) . ? C23 H23A 0.9500 . ? C25 C61 1.391(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C57 1.369(6) . ? C28 C46 1.392(6) . ? C28 H28A 0.9500 . ? C29 C52 1.530(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C65 1.392(6) . ? C30 H30A 0.9500 . ? C31 C68 1.366(6) . ? C31 H31A 0.9500 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C57 1.409(6) . ? C33 H33A 0.9500 . ? C34 C57 1.527(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C46 1.384(6) . ? C35 C59 1.517(5) . ? C36 C60 1.380(6) . ? C36 C76 1.390(6) . ? C36 H36A 0.9500 . ? C37 C72 1.485(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C49 1.355(6) . ? C38 H38A 0.9500 . ? C39 C51 1.362(6) . ? C39 H39A 0.9500 . ? C40 C77 1.378(6) . ? C40 H40A 0.9500 . ? C41 C43 1.390(6) . ? C41 C54 1.403(6) . ? C41 H41A 0.9500 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C74 1.378(6) . ? C43 C89 1.522(5) . ? C44 C64 1.384(6) . ? C44 C91 1.403(5) . ? C44 H44A 0.9500 . ? C45 C61 1.492(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9500 . ? C47 C90 1.389(6) . ? C47 C64 1.393(6) . ? C47 H47A 0.9500 . ? C48 C56 1.389(6) . ? C48 C74 1.390(5) . ? C48 H48A 0.9500 . ? C49 C83 1.402(6) . ? C49 H49A 0.9500 . ? C50 C78 1.380(6) . ? C50 H50A 0.9500 . ? C51 C83 1.397(6) . ? C51 H51A 0.9500 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C69 1.385(6) . ? C53 C58 1.392(5) . ? C53 C70 1.533(6) . ? C54 C56 1.370(6) . ? C54 H54A 0.9500 . ? C56 H56A 0.9500 . ? C58 C71 1.379(6) . ? C58 H58A 0.9500 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9500 . ? C62 C75 1.496(5) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C69 1.399(6) . ? C63 H63A 0.9500 . ? C64 H64A 0.9500 . ? C65 C78 1.386(6) . ? C65 C87 1.487(6) . ? C66 C96 1.394(5) . ? C66 C81 1.400(5) . ? C66 C80 1.524(5) . ? C67 C85 1.377(5) . ? C67 C92 1.392(5) . ? C67 C93 1.535(5) . ? C68 C87 1.386(6) . ? C68 H68A 0.9500 . ? C69 C80 1.521(5) . ? C70 C79 1.530(5) . ? C70 C81 1.534(5) . ? C70 H70A 1.0000 . ? C71 H71A 0.9500 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C98 1.380(5) . ? C73 C92 1.396(5) . ? C73 H73A 0.9500 . ? C74 C93 1.534(5) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.384(6) . ? C76 C83 1.486(6) . ? C77 H77A 0.9500 . ? C78 H78A 0.9500 . ? C79 C91 1.386(5) . ? C79 C90 1.388(5) . ? C80 C91 1.538(5) . ? C80 H80A 1.0000 . ? C81 C88 1.395(5) . ? C82 C86 1.352(6) . ? C82 C87 1.396(6) . ? C82 H82A 0.9500 . ? C85 C97 1.391(5) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C88 C95 1.391(5) . ? C89 C92 1.519(5) . ? C89 C94 1.524(5) . ? C89 H89A 1.0000 . ? C90 H90A 0.9500 . ? C93 C95 1.529(5) . ? C93 H93A 1.0000 . ? C94 C96 1.394(5) . ? C94 C95 1.403(5) . ? C97 C98 1.427(6) . ? N5 C99 1.131(7) . ? C99 C100 1.440(8) . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? N6 C101 1.145(7) . ? C101 C102 1.431(9) . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C102 H10G 0.9800 . ? N7 C103 1.156(14) . ? C103 C104 1.435(13) . ? C104 H10H 0.9800 . ? C104 H10I 0.9800 . ? C104 H10J 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 F2 P1 F1 100.4(6) . . ? F2 P1 F4 168.0(5) . . ? F1 P1 F4 91.6(5) . . ? F2 P1 F3 84.7(5) . . ? F1 P1 F3 174.9(5) . . ? F4 P1 F3 83.3(4) . . ? F2 P1 F5 90.6(3) . . ? F1 P1 F5 90.0(3) . . ? F4 P1 F5 89.5(3) . . ? F3 P1 F5 90.3(2) . . ? F2 P1 F6 90.7(3) . . ? F1 P1 F6 90.5(2) . . ? F4 P1 F6 89.0(3) . . ? F3 P1 F6 89.0(2) . . ? F5 P1 F6 178.4(2) . . ? F8 P2 F10 90.19(19) . . ? F8 P2 F7 92.1(2) . . ? F10 P2 F7 177.6(2) . . ? F8 P2 F12 90.8(2) . . ? F10 P2 F12 89.31(16) . . ? F7 P2 F12 89.81(18) . . ? F8 P2 F11 90.7(2) . . ? F10 P2 F11 89.98(16) . . ? F7 P2 F11 90.84(18) . . ? F12 P2 F11 178.3(2) . . ? F8 P2 F9 179.4(2) . . ? F10 P2 F9 89.28(18) . . ? F7 P2 F9 88.5(2) . . ? F12 P2 F9 89.35(19) . . ? F11 P2 F9 89.09(19) . . ? F13 P3 F14 92.1(3) . . ? F13 P3 F16 89.9(3) . . ? F14 P3 F16 177.7(3) . . ? F13 P3 F15 176.7(3) . . ? F14 P3 F15 91.2(4) . . ? F16 P3 F15 86.8(3) . . ? F13 P3 F17 88.5(2) . . ? F14 P3 F17 90.7(2) . . ? F16 P3 F17 90.5(2) . . ? F15 P3 F17 91.2(2) . . ? F13 P3 F18 91.7(2) . . ? F14 P3 F18 90.24(18) . . ? F16 P3 F18 88.61(18) . . ? F15 P3 F18 88.6(2) . . ? F17 P3 F18 179.1(2) . . ? F19 P4 F24 91.0(2) . . ? F19 P4 F23 93.2(3) . . ? F24 P4 F23 90.5(2) . . ? F19 P4 F20 89.9(3) . . ? F24 P4 F20 90.7(2) . . ? F23 P4 F20 176.7(3) . . ? F19 P4 F21 90.6(2) . . ? F24 P4 F21 178.4(2) . . ? F23 P4 F21 89.0(2) . . ? F20 P4 F21 89.6(2) . . ? F19 P4 F22 177.3(3) . . ? F24 P4 F22 88.5(2) . . ? F23 P4 F22 89.5(2) . . ? F20 P4 F22 87.5(2) . . ? F21 P4 F22 90.0(2) . . ? C96 O1 C52 112.9(3) . . ? C29 O2 C6 112.0(4) . . ? C88 O3 C72 113.6(3) . . ? C37 O4 C2 110.2(4) . . ? C97 O5 C32 117.7(3) . . ? C1 O6 C5 112.9(5) . . ? C3 O7 C4 115.3(5) . . ? C55 O8 C7 115.5(4) . . ? C98 O9 C75 118.4(3) . . ? C42 O10 C62 112.5(3) . . ? C13 O11 C17 111.9(3) . . ? C8 O12 C27 115.4(4) . . ? C86 N1 C31 119.6(4) . . ? C86 N1 C59 119.0(4) . . ? C31 N1 C59 121.2(3) . . ? C50 N2 C15 120.6(4) . . ? C50 N2 C21 119.3(4) . . ? C15 N2 C21 119.6(4) . . ? C60 N3 C40 121.0(4) . . ? C60 N3 C45 120.5(4) . . ? C40 N3 C45 118.2(4) . . ? C39 N4 C38 120.1(4) . . ? C39 N4 C34 121.0(4) . . ? C38 N4 C34 118.6(4) . . ? O6 C1 C3 107.7(5) . . ? O6 C1 H1A 110.2 . . ? C3 C1 H1A 110.2 . . ? O6 C1 H1B 110.2 . . ? C3 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? O4 C2 H2A 109.5 . . ? O4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O7 C3 C1 111.4(5) . . ? O7 C3 H3A 109.4 . . ? C1 C3 H3A 109.4 . . ? O7 C3 H3B 109.3 . . ? C1 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O7 C4 C7 114.2(5) . . ? O7 C4 H4A 108.7 . . ? C7 C4 H4A 108.7 . . ? O7 C4 H4B 108.7 . . ? C7 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? O6 C5 C32 108.8(5) . . ? O6 C5 H5A 109.9 . . ? C32 C5 H5A 109.9 . . ? O6 C5 H5B 109.9 . . ? C32 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? O2 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O8 C7 C4 107.8(5) . . ? O8 C7 H7A 110.2 . . ? C4 C7 H7A 110.2 . . ? O8 C7 H7B 110.2 . . ? C4 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? C16 C8 O12 126.3(4) . . ? C16 C8 C55 119.1(4) . . ? O12 C8 C55 114.5(4) . . ? C18 C9 C24 122.1(5) . . ? C18 C9 H9A 119.0 . . ? C24 C9 H9A 119.0 . . ? C26 C10 C18 120.5(5) . . ? C26 C10 H10A 119.8 . . ? C18 C10 H10A 119.8 . . ? C63 C11 C71 119.8(4) . . ? C63 C11 H11A 120.1 . . ? C71 C11 H11A 120.1 . . ? C55 C12 C24 121.8(4) . . ? C55 C12 H12A 119.1 . . ? C24 C12 H12A 119.1 . . ? O11 C13 C42 110.7(4) . . ? O11 C13 H13A 109.5 . . ? C42 C13 H13A 109.5 . . ? O11 C13 H13B 109.5 . . ? C42 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C61 C14 C23 120.5(4) . . ? C61 C14 H14A 119.8 . . ? C23 C14 H14A 119.8 . . ? C30 C15 N2 120.2(4) . . ? C30 C15 H15A 119.9 . . ? N2 C15 H15A 119.9 . . ? C8 C16 C19 121.3(4) . . ? C8 C16 H16A 119.4 . . ? C19 C16 H16A 119.4 . . ? O11 C17 C27 110.0(4) . . ? O11 C17 H17A 109.6 . . ? C27 C17 H17A 109.6 . . ? O11 C17 H17B 109.7 . . ? C27 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C9 C18 C10 119.9(5) . . ? C9 C18 H18A 120.0 . . ? C10 C18 H18A 120.0 . . ? C26 C19 C24 118.3(4) . . ? C26 C19 C16 122.4(4) . . ? C24 C19 C16 119.3(4) . . ? C33 C20 C35 121.2(4) . . ? C33 C20 H20A 119.4 . . ? C35 C20 H20A 119.4 . . ? N2 C21 C84 109.7(3) . . ? N2 C21 H21A 109.7 . . ? C84 C21 H21A 109.7 . . ? N2 C21 H21B 109.7 . . ? C84 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C25 C22 C84 119.5(4) . . ? C25 C22 H22A 120.3 . . ? C84 C22 H22A 120.3 . . ? C84 C23 C14 119.7(4) . . ? C84 C23 H23A 120.1 . . ? C14 C23 H23A 120.1 . . ? C9 C24 C19 118.5(5) . . ? C9 C24 C12 123.1(5) . . ? C19 C24 C12 118.4(5) . . ? C22 C25 C61 121.9(4) . . ? C22 C25 H25A 119.0 . . ? C61 C25 H25A 119.0 . . ? C10 C26 C19 120.7(5) . . ? C10 C26 H26A 119.7 . . ? C19 C26 H26A 119.7 . . ? O12 C27 C17 109.3(4) . . ? O12 C27 H27A 109.8 . . ? C17 C27 H27A 109.8 . . ? O12 C27 H27B 109.8 . . ? C17 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? C57 C28 C46 120.3(4) . . ? C57 C28 H28A 119.8 . . ? C46 C28 H28A 119.8 . . ? O2 C29 C52 106.6(4) . . ? O2 C29 H29A 110.4 . . ? C52 C29 H29A 110.4 . . ? O2 C29 H29B 110.4 . . ? C52 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C15 C30 C65 120.6(4) . . ? C15 C30 H30A 119.7 . . ? C65 C30 H30A 119.7 . . ? N1 C31 C68 120.9(4) . . ? N1 C31 H31A 119.6 . . ? C68 C31 H31A 119.6 . . ? O5 C32 C5 106.7(4) . . ? O5 C32 H32A 110.4 . . ? C5 C32 H32A 110.4 . . ? O5 C32 H32B 110.4 . . ? C5 C32 H32B 110.4 . . ? H32A C32 H32B 108.6 . . ? C20 C33 C57 119.1(4) . . ? C20 C33 H33A 120.4 . . ? C57 C33 H33A 120.4 . . ? N4 C34 C57 109.3(3) . . ? N4 C34 H34A 109.8 . . ? C57 C34 H34A 109.8 . . ? N4 C34 H34B 109.8 . . ? C57 C34 H34B 109.8 . . ? H34A C34 H34B 108.3 . . ? C46 C35 C20 119.2(4) . . ? C46 C35 C59 120.3(4) . . ? C20 C35 C59 120.5(4) . . ? C60 C36 C76 120.1(4) . . ? C60 C36 H36A 119.9 . . ? C76 C36 H36A 119.9 . . ? O4 C37 C72 111.0(4) . . ? O4 C37 H37A 109.4 . . ? C72 C37 H37A 109.4 . . ? O4 C37 H37B 109.4 . . ? C72 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? N4 C38 C49 121.2(4) . . ? N4 C38 H38A 119.4 . . ? C49 C38 H38A 119.4 . . ? N4 C39 C51 120.8(4) . . ? N4 C39 H39A 119.6 . . ? C51 C39 H39A 119.6 . . ? N3 C40 C77 120.6(4) . . ? N3 C40 H40A 119.7 . . ? C77 C40 H40A 119.7 . . ? C43 C41 C54 118.4(4) . . ? C43 C41 H41A 120.8 . . ? C54 C41 H41A 120.8 . . ? O10 C42 C13 110.0(4) . . ? O10 C42 H42A 109.7 . . ? C13 C42 H42A 109.7 . . ? O10 C42 H42B 109.7 . . ? C13 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C74 C43 C41 120.4(4) . . ? C74 C43 C89 114.1(3) . . ? C41 C43 C89 125.3(4) . . ? C64 C44 C91 118.8(4) . . ? C64 C44 H44A 120.6 . . ? C91 C44 H44A 120.6 . . ? C61 C45 N3 110.6(3) . . ? C61 C45 H45A 109.5 . . ? N3 C45 H45A 109.5 . . ? C61 C45 H45B 109.5 . . ? N3 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C35 C46 C28 120.1(4) . . ? C35 C46 H46A 119.9 . . ? C28 C46 H46A 119.9 . . ? C90 C47 C64 120.0(4) . . ? C90 C47 H47A 120.0 . . ? C64 C47 H47A 120.0 . . ? C56 C48 C74 118.6(4) . . ? C56 C48 H48A 120.7 . . ? C74 C48 H48A 120.7 . . ? C38 C49 C83 120.4(4) . . ? C38 C49 H49A 119.8 . . ? C83 C49 H49A 119.8 . . ? N2 C50 C78 120.3(4) . . ? N2 C50 H50A 119.8 . . ? C78 C50 H50A 119.8 . . ? C39 C51 C83 120.7(4) . . ? C39 C51 H51A 119.7 . . ? C83 C51 H51A 119.7 . . ? O1 C52 C29 111.8(3) . . ? O1 C52 H52A 109.2 . . ? C29 C52 H52A 109.2 . . ? O1 C52 H52B 109.2 . . ? C29 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? C69 C53 C58 121.2(4) . . ? C69 C53 C70 113.1(3) . . ? C58 C53 C70 125.7(4) . . ? C56 C54 C41 120.7(4) . . ? C56 C54 H54A 119.6 . . ? C41 C54 H54A 119.6 . . ? C12 C55 O8 127.9(4) . . ? C12 C55 C8 120.0(4) . . ? O8 C55 C8 112.0(4) . . ? C54 C56 C48 120.8(4) . . ? C54 C56 H56A 119.6 . . ? C48 C56 H56A 119.6 . . ? C28 C57 C33 120.0(4) . . ? C28 C57 C34 120.9(4) . . ? C33 C57 C34 119.1(4) . . ? C71 C58 C53 118.5(4) . . ? C71 C58 H58A 120.8 . . ? C53 C58 H58A 120.8 . . ? N1 C59 C35 110.0(3) . . ? N1 C59 H59A 109.7 . . ? C35 C59 H59A 109.7 . . ? N1 C59 H59B 109.7 . . ? C35 C59 H59B 109.7 . . ? H59A C59 H59B 108.2 . . ? N3 C60 C36 120.2(4) . . ? N3 C60 H60A 119.9 . . ? C36 C60 H60A 119.9 . . ? C14 C61 C25 118.1(4) . . ? C14 C61 C45 121.6(4) . . ? C25 C61 C45 120.3(4) . . ? O10 C62 C75 109.1(3) . . ? O10 C62 H62A 109.9 . . ? C75 C62 H62A 109.9 . . ? O10 C62 H62B 109.9 . . ? C75 C62 H62B 109.9 . . ? H62A C62 H62B 108.3 . . ? C11 C63 C69 119.2(4) . . ? C11 C63 H63A 120.4 . . ? C69 C63 H63A 120.4 . . ? C44 C64 C47 121.0(4) . . ? C44 C64 H64A 119.5 . . ? C47 C64 H64A 119.5 . . ? C78 C65 C30 117.1(4) . . ? C78 C65 C87 121.2(4) . . ? C30 C65 C87 121.2(4) . . ? C96 C66 C81 120.8(3) . . ? C96 C66 C80 125.3(3) . . ? C81 C66 C80 113.4(3) . . ? C85 C67 C92 120.9(3) . . ? C85 C67 C93 126.1(3) . . ? C92 C67 C93 112.6(3) . . ? C31 C68 C87 120.2(4) . . ? C31 C68 H68A 119.9 . . ? C87 C68 H68A 119.9 . . ? C53 C69 C63 120.1(4) . . ? C53 C69 C80 114.2(3) . . ? C63 C69 C80 125.7(4) . . ? C79 C70 C53 105.6(3) . . ? C79 C70 C81 103.9(3) . . ? C53 C70 C81 106.3(3) . . ? C79 C70 H70A 113.4 . . ? C53 C70 H70A 113.4 . . ? C81 C70 H70A 113.4 . . ? C58 C71 C11 121.3(4) . . ? C58 C71 H71A 119.4 . . ? C11 C71 H71A 119.4 . . ? O3 C72 C37 109.8(4) . . ? O3 C72 H72A 109.7 . . ? C37 C72 H72A 109.7 . . ? O3 C72 H72B 109.7 . . ? C37 C72 H72B 109.7 . . ? H72A C72 H72B 108.2 . . ? C98 C73 C92 119.4(4) . . ? C98 C73 H73A 120.3 . . ? C92 C73 H73A 120.3 . . ? C43 C74 C48 121.0(4) . . ? C43 C74 C93 112.9(3) . . ? C48 C74 C93 125.9(4) . . ? O9 C75 C62 108.4(4) . . ? O9 C75 H75A 110.0 . . ? C62 C75 H75A 110.0 . . ? O9 C75 H75B 110.0 . . ? C62 C75 H75B 110.0 . . ? H75A C75 H75B 108.4 . . ? C77 C76 C36 118.0(4) . . ? C77 C76 C83 119.6(4) . . ? C36 C76 C83 122.3(4) . . ? C40 C77 C76 119.9(4) . . ? C40 C77 H77A 120.1 . . ? C76 C77 H77A 120.1 . . ? C50 C78 C65 120.8(4) . . ? C50 C78 H78A 119.6 . . ? C65 C78 H78A 119.6 . . ? C91 C79 C90 120.6(4) . . ? C91 C79 C70 113.2(3) . . ? C90 C79 C70 126.1(4) . . ? C69 C80 C66 105.9(3) . . ? C69 C80 C91 105.1(3) . . ? C66 C80 C91 104.3(3) . . ? C69 C80 H80A 113.6 . . ? C66 C80 H80A 113.6 . . ? C91 C80 H80A 113.6 . . ? C88 C81 C66 120.3(3) . . ? C88 C81 C70 126.2(3) . . ? C66 C81 C70 113.2(3) . . ? C86 C82 C87 120.2(4) . . ? C86 C82 H82A 119.9 . . ? C87 C82 H82A 119.9 . . ? C51 C83 C49 116.2(4) . . ? C51 C83 C76 122.4(4) . . ? C49 C83 C76 121.2(4) . . ? C23 C84 C22 120.3(4) . . ? C23 C84 C21 120.3(4) . . ? C22 C84 C21 119.1(4) . . ? C67 C85 C97 120.1(4) . . ? C67 C85 H85A 119.9 . . ? C97 C85 H85A 119.9 . . ? N1 C86 C82 121.6(4) . . ? N1 C86 H86A 119.2 . . ? C82 C86 H86A 119.2 . . ? C68 C87 C82 117.4(4) . . ? C68 C87 C65 123.7(4) . . ? C82 C87 C65 118.6(4) . . ? O3 C88 C95 120.1(3) . . ? O3 C88 C81 120.5(3) . . ? C95 C88 C81 119.0(3) . . ? C92 C89 C43 107.6(3) . . ? C92 C89 C94 102.9(3) . . ? C43 C89 C94 105.3(3) . . ? C92 C89 H89A 113.4 . . ? C43 C89 H89A 113.4 . . ? C94 C89 H89A 113.4 . . ? C79 C90 C47 119.4(4) . . ? C79 C90 H90A 120.3 . . ? C47 C90 H90A 120.3 . . ? C79 C91 C44 120.1(4) . . ? C79 C91 C80 113.8(3) . . ? C44 C91 C80 126.0(4) . . ? C67 C92 C73 120.1(4) . . ? C67 C92 C89 113.9(3) . . ? C73 C92 C89 125.6(3) . . ? C95 C93 C74 105.5(3) . . ? C95 C93 C67 102.8(3) . . ? C74 C93 C67 108.1(3) . . ? C95 C93 H93A 113.2 . . ? C74 C93 H93A 113.2 . . ? C67 C93 H93A 113.2 . . ? C96 C94 C95 120.2(3) . . ? C96 C94 C89 125.8(3) . . ? C95 C94 C89 113.6(3) . . ? C88 C95 C94 120.8(3) . . ? C88 C95 C93 126.4(3) . . ? C94 C95 C93 112.5(3) . . ? O1 C96 C94 119.2(3) . . ? O1 C96 C66 121.5(3) . . ? C94 C96 C66 119.0(3) . . ? O5 C97 C85 126.1(4) . . ? O5 C97 C98 115.1(3) . . ? C85 C97 C98 118.8(3) . . ? C73 C98 O9 125.1(4) . . ? C73 C98 C97 120.6(3) . . ? O9 C98 C97 114.3(3) . . ? N5 C99 C100 179.7(8) . . ? C99 C100 H10B 109.4 . . ? C99 C100 H10C 109.4 . . ? H10B C100 H10C 109.5 . . ? C99 C100 H10D 109.5 . . ? H10B C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? N6 C101 C102 179.2(9) . . ? C101 C102 H10E 109.5 . . ? C101 C102 H10F 109.6 . . ? H10E C102 H10F 109.5 . . ? C101 C102 H10G 109.4 . . ? H10E C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? N7 C103 C104 178.8(15) . . ? C103 C104 H10H 109.4 . . ? C103 C104 H10I 109.6 . . ? H10H C104 H10I 109.5 . . ? C103 C104 H10J 109.5 . . ? H10H C104 H10J 109.5 . . ? H10I C104 H10J 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 C5 O6 C1 C3 164.0(5) . . . . ? C4 O7 C3 C1 175.2(5) . . . . ? O6 C1 C3 O7 -73.0(7) . . . . ? C3 O7 C4 C7 -87.3(7) . . . . ? C1 O6 C5 C32 138.0(6) . . . . ? C55 O8 C7 C4 176.4(4) . . . . ? O7 C4 C7 O8 82.1(6) . . . . ? C27 O12 C8 C16 3.5(7) . . . . ? C27 O12 C8 C55 -179.5(4) . . . . ? C17 O11 C13 C42 -164.4(4) . . . . ? C50 N2 C15 C30 -3.6(7) . . . . ? C21 N2 C15 C30 168.8(4) . . . . ? O12 C8 C16 C19 178.4(4) . . . . ? C55 C8 C16 C19 1.6(7) . . . . ? C13 O11 C17 C27 -171.1(4) . . . . ? C24 C9 C18 C10 -0.4(8) . . . . ? C26 C10 C18 C9 -2.1(8) . . . . ? C8 C16 C19 C26 -178.1(4) . . . . ? C8 C16 C19 C24 2.2(7) . . . . ? C50 N2 C21 C84 88.9(5) . . . . ? C15 N2 C21 C84 -83.5(5) . . . . ? C61 C14 C23 C84 -1.6(7) . . . . ? C18 C9 C24 C19 2.2(7) . . . . ? C18 C9 C24 C12 -175.4(5) . . . . ? C26 C19 C24 C9 -1.5(6) . . . . ? C16 C19 C24 C9 178.2(4) . . . . ? C26 C19 C24 C12 176.1(4) . . . . ? C16 C19 C24 C12 -4.1(6) . . . . ? C55 C12 C24 C9 179.8(5) . . . . ? C55 C12 C24 C19 2.3(7) . . . . ? C84 C22 C25 C61 -1.2(7) . . . . ? C18 C10 C26 C19 2.7(7) . . . . ? C24 C19 C26 C10 -0.8(7) . . . . ? C16 C19 C26 C10 179.5(4) . . . . ? C8 O12 C27 C17 179.2(4) . . . . ? O11 C17 C27 O12 -64.9(5) . . . . ? C6 O2 C29 C52 178.8(4) . . . . ? N2 C15 C30 C65 1.0(7) . . . . ? C86 N1 C31 C68 3.2(6) . . . . ? C59 N1 C31 C68 -173.3(4) . . . . ? C97 O5 C32 C5 172.8(4) . . . . ? O6 C5 C32 O5 -72.7(6) . . . . ? C35 C20 C33 C57 0.4(7) . . . . ? C39 N4 C34 C57 96.9(4) . . . . ? C38 N4 C34 C57 -77.4(5) . . . . ? C33 C20 C35 C46 -2.6(7) . . . . ? C33 C20 C35 C59 176.5(4) . . . . ? C2 O4 C37 C72 -177.1(5) . . . . ? C39 N4 C38 C49 -3.9(6) . . . . ? C34 N4 C38 C49 170.4(4) . . . . ? C38 N4 C39 C51 4.4(6) . . . . ? C34 N4 C39 C51 -169.9(4) . . . . ? C60 N3 C40 C77 -2.3(6) . . . . ? C45 N3 C40 C77 172.5(4) . . . . ? C62 O10 C42 C13 -162.6(4) . . . . ? O11 C13 C42 O10 -62.0(5) . . . . ? C54 C41 C43 C74 0.4(6) . . . . ? C54 C41 C43 C89 175.5(4) . . . . ? C60 N3 C45 C61 99.1(4) . . . . ? C40 N3 C45 C61 -75.7(5) . . . . ? C20 C35 C46 C28 2.2(7) . . . . ? C59 C35 C46 C28 -176.9(4) . . . . ? C57 C28 C46 C35 0.3(7) . . . . ? N4 C38 C49 C83 -2.1(6) . . . . ? C15 N2 C50 C78 1.6(6) . . . . ? C21 N2 C50 C78 -170.8(4) . . . . ? N4 C39 C51 C83 1.3(6) . . . . ? C96 O1 C52 C29 68.5(4) . . . . ? O2 C29 C52 O1 -158.4(4) . . . . ? C43 C41 C54 C56 1.5(6) . . . . ? C24 C12 C55 O8 -179.0(4) . . . . ? C24 C12 C55 C8 1.5(7) . . . . ? C7 O8 C55 C12 12.1(7) . . . . ? C7 O8 C55 C8 -168.3(4) . . . . ? C16 C8 C55 C12 -3.5(7) . . . . ? O12 C8 C55 C12 179.3(4) . . . . ? C16 C8 C55 O8 176.9(4) . . . . ? O12 C8 C55 O8 -0.3(6) . . . . ? C41 C54 C56 C48 -1.7(6) . . . . ? C74 C48 C56 C54 0.1(6) . . . . ? C46 C28 C57 C33 -2.5(7) . . . . ? C46 C28 C57 C34 175.2(4) . . . . ? C20 C33 C57 C28 2.1(6) . . . . ? C20 C33 C57 C34 -175.6(4) . . . . ? N4 C34 C57 C28 -92.1(5) . . . . ? N4 C34 C57 C33 85.6(5) . . . . ? C69 C53 C58 C71 2.8(6) . . . . ? C70 C53 C58 C71 -174.3(4) . . . . ? C86 N1 C59 C35 -68.3(5) . . . . ? C31 N1 C59 C35 108.2(4) . . . . ? C46 C35 C59 N1 94.7(5) . . . . ? C20 C35 C59 N1 -84.4(5) . . . . ? C40 N3 C60 C36 3.2(6) . . . . ? C45 N3 C60 C36 -171.5(4) . . . . ? C76 C36 C60 N3 -0.5(6) . . . . ? C23 C14 C61 C25 1.3(7) . . . . ? C23 C14 C61 C45 -177.6(4) . . . . ? C22 C25 C61 C14 0.1(7) . . . . ? C22 C25 C61 C45 179.0(4) . . . . ? N3 C45 C61 C14 96.0(5) . . . . ? N3 C45 C61 C25 -82.8(5) . . . . ? C42 O10 C62 C75 -171.5(4) . . . . ? C71 C11 C63 C69 0.2(6) . . . . ? C91 C44 C64 C47 0.5(6) . . . . ? C90 C47 C64 C44 -1.4(6) . . . . ? C15 C30 C65 C78 3.3(7) . . . . ? C15 C30 C65 C87 -169.2(4) . . . . ? N1 C31 C68 C87 -0.3(7) . . . . ? C58 C53 C69 C63 -0.7(6) . . . . ? C70 C53 C69 C63 176.7(3) . . . . ? C58 C53 C69 C80 -178.1(3) . . . . ? C70 C53 C69 C80 -0.7(5) . . . . ? C11 C63 C69 C53 -0.8(6) . . . . ? C11 C63 C69 C80 176.3(4) . . . . ? C69 C53 C70 C79 -55.0(4) . . . . ? C58 C53 C70 C79 122.3(4) . . . . ? C69 C53 C70 C81 55.0(4) . . . . ? C58 C53 C70 C81 -127.7(4) . . . . ? C53 C58 C71 C11 -3.4(6) . . . . ? C63 C11 C71 C58 1.9(7) . . . . ? C88 O3 C72 C37 -175.0(3) . . . . ? O4 C37 C72 O3 -62.6(5) . . . . ? C41 C43 C74 C48 -2.1(6) . . . . ? C89 C43 C74 C48 -177.7(3) . . . . ? C41 C43 C74 C93 174.5(3) . . . . ? C89 C43 C74 C93 -1.1(4) . . . . ? C56 C48 C74 C43 1.9(6) . . . . ? C56 C48 C74 C93 -174.3(4) . . . . ? C98 O9 C75 C62 -168.2(3) . . . . ? O10 C62 C75 O9 86.4(4) . . . . ? C60 C36 C76 C77 -2.9(6) . . . . ? C60 C36 C76 C83 172.1(4) . . . . ? N3 C40 C77 C76 -1.3(6) . . . . ? C36 C76 C77 C40 3.8(6) . . . . ? C83 C76 C77 C40 -171.4(4) . . . . ? N2 C50 C78 C65 2.9(6) . . . . ? C30 C65 C78 C50 -5.3(6) . . . . ? C87 C65 C78 C50 167.2(4) . . . . ? C53 C70 C79 C91 55.4(4) . . . . ? C81 C70 C79 C91 -56.3(4) . . . . ? C53 C70 C79 C90 -122.3(4) . . . . ? C81 C70 C79 C90 126.0(4) . . . . ? C53 C69 C80 C66 -54.7(4) . . . . ? C63 C69 C80 C66 128.1(4) . . . . ? C53 C69 C80 C91 55.3(4) . . . . ? C63 C69 C80 C91 -121.9(4) . . . . ? C96 C66 C80 C69 -131.9(4) . . . . ? C81 C66 C80 C69 55.9(4) . . . . ? C96 C66 C80 C91 117.6(4) . . . . ? C81 C66 C80 C91 -54.7(4) . . . . ? C96 C66 C81 C88 -1.5(5) . . . . ? C80 C66 C81 C88 171.1(3) . . . . ? C96 C66 C81 C70 -174.5(3) . . . . ? C80 C66 C81 C70 -1.9(4) . . . . ? C79 C70 C81 C88 -114.7(4) . . . . ? C53 C70 C81 C88 134.1(4) . . . . ? C79 C70 C81 C66 57.8(4) . . . . ? C53 C70 C81 C66 -53.4(4) . . . . ? C39 C51 C83 C49 -6.9(6) . . . . ? C39 C51 C83 C76 167.3(4) . . . . ? C38 C49 C83 C51 7.3(6) . . . . ? C38 C49 C83 C76 -167.0(4) . . . . ? C77 C76 C83 C51 -23.8(6) . . . . ? C36 C76 C83 C51 161.3(4) . . . . ? C77 C76 C83 C49 150.2(4) . . . . ? C36 C76 C83 C49 -24.8(6) . . . . ? C14 C23 C84 C22 0.4(6) . . . . ? C14 C23 C84 C21 174.5(4) . . . . ? C25 C22 C84 C23 0.9(7) . . . . ? C25 C22 C84 C21 -173.2(4) . . . . ? N2 C21 C84 C23 -90.6(5) . . . . ? N2 C21 C84 C22 83.5(5) . . . . ? C92 C67 C85 C97 -0.3(5) . . . . ? C93 C67 C85 C97 172.2(3) . . . . ? C31 N1 C86 C82 -3.0(6) . . . . ? C59 N1 C86 C82 173.6(4) . . . . ? C87 C82 C86 N1 -0.3(6) . . . . ? C31 C68 C87 C82 -2.9(6) . . . . ? C31 C68 C87 C65 171.7(4) . . . . ? C86 C82 C87 C68 3.2(6) . . . . ? C86 C82 C87 C65 -171.7(4) . . . . ? C78 C65 C87 C68 159.1(4) . . . . ? C30 C65 C87 C68 -28.8(6) . . . . ? C78 C65 C87 C82 -26.4(6) . . . . ? C30 C65 C87 C82 145.8(4) . . . . ? C72 O3 C88 C95 94.4(4) . . . . ? C72 O3 C88 C81 -92.8(4) . . . . ? C66 C81 C88 O3 -173.6(3) . . . . ? C70 C81 C88 O3 -1.6(6) . . . . ? C66 C81 C88 C95 -0.7(5) . . . . ? C70 C81 C88 C95 171.3(3) . . . . ? C74 C43 C89 C92 -53.1(4) . . . . ? C41 C43 C89 C92 131.6(4) . . . . ? C74 C43 C89 C94 56.1(4) . . . . ? C41 C43 C89 C94 -119.2(4) . . . . ? C91 C79 C90 C47 3.5(6) . . . . ? C70 C79 C90 C47 -178.9(4) . . . . ? C64 C47 C90 C79 -0.6(6) . . . . ? C90 C79 C91 C44 -4.4(5) . . . . ? C70 C79 C91 C44 177.7(3) . . . . ? C90 C79 C91 C80 177.5(3) . . . . ? C70 C79 C91 C80 -0.4(4) . . . . ? C64 C44 C91 C79 2.3(5) . . . . ? C64 C44 C91 C80 -179.8(4) . . . . ? C69 C80 C91 C79 -54.7(4) . . . . ? C66 C80 C91 C79 56.4(4) . . . . ? C69 C80 C91 C44 127.3(4) . . . . ? C66 C80 C91 C44 -121.6(4) . . . . ? C85 C67 C92 C73 -1.6(5) . . . . ? C93 C67 C92 C73 -175.1(3) . . . . ? C85 C67 C92 C89 171.5(3) . . . . ? C93 C67 C92 C89 -1.9(4) . . . . ? C98 C73 C92 C67 2.2(5) . . . . ? C98 C73 C92 C89 -170.1(3) . . . . ? C43 C89 C92 C67 54.7(4) . . . . ? C94 C89 C92 C67 -56.2(4) . . . . ? C43 C89 C92 C73 -132.6(4) . . . . ? C94 C89 C92 C73 116.5(4) . . . . ? C43 C74 C93 C95 -55.3(4) . . . . ? C48 C74 C93 C95 121.1(4) . . . . ? C43 C74 C93 C67 54.2(4) . . . . ? C48 C74 C93 C67 -129.4(4) . . . . ? C85 C67 C93 C95 -114.0(4) . . . . ? C92 C67 C93 C95 59.0(4) . . . . ? C85 C67 C93 C74 134.7(4) . . . . ? C92 C67 C93 C74 -52.3(4) . . . . ? C92 C89 C94 C96 -115.0(4) . . . . ? C43 C89 C94 C96 132.4(4) . . . . ? C92 C89 C94 C95 58.1(4) . . . . ? C43 C89 C94 C95 -54.5(4) . . . . ? O3 C88 C95 C94 175.1(3) . . . . ? C81 C88 C95 C94 2.3(5) . . . . ? O3 C88 C95 C93 2.3(5) . . . . ? C81 C88 C95 C93 -170.6(3) . . . . ? C96 C94 C95 C88 -1.5(5) . . . . ? C89 C94 C95 C88 -175.0(3) . . . . ? C96 C94 C95 C93 172.3(3) . . . . ? C89 C94 C95 C93 -1.2(4) . . . . ? C74 C93 C95 C88 -130.3(4) . . . . ? C67 C93 C95 C88 116.5(4) . . . . ? C74 C93 C95 C94 56.3(4) . . . . ? C67 C93 C95 C94 -56.9(4) . . . . ? C52 O1 C96 C94 -107.5(4) . . . . ? C52 O1 C96 C66 78.8(4) . . . . ? C95 C94 C96 O1 -174.6(3) . . . . ? C89 C94 C96 O1 -1.9(5) . . . . ? C95 C94 C96 C66 -0.7(5) . . . . ? C89 C94 C96 C66 171.9(3) . . . . ? C81 C66 C96 O1 175.9(3) . . . . ? C80 C66 C96 O1 4.2(6) . . . . ? C81 C66 C96 C94 2.2(5) . . . . ? C80 C66 C96 C94 -169.5(3) . . . . ? C32 O5 C97 C85 14.2(6) . . . . ? C32 O5 C97 C98 -167.3(4) . . . . ? C67 C85 C97 O5 -179.9(4) . . . . ? C67 C85 C97 C98 1.6(6) . . . . ? C92 C73 C98 O9 176.8(3) . . . . ? C92 C73 C98 C97 -0.9(6) . . . . ? C75 O9 C98 C73 0.4(6) . . . . ? C75 O9 C98 C97 178.2(3) . . . . ? O5 C97 C98 C73 -179.7(3) . . . . ? C85 C97 C98 C73 -1.0(6) . . . . ? O5 C97 C98 O9 2.4(5) . . . . ? C85 C97 C98 O9 -178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.925 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.085