# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 177 loop_ _publ_author_name 'Jiang, Lasheng' _publ_contact_author_name 'Jiang, Lasheng' _publ_contact_author_email jianglsh@scnu.edu.cn _publ_section_title ; One-Pot Synthesis of Donor-Acceptor [2]Rotaxanes Based on Cryptand/Paraquat Recognition Motif ; data_c _database_code_depnum_ccdc_archive 'CCDC 788120' #TrackingRef '[2]pseudorotaxane 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H60 F12 N2 O10 P2' _chemical_formula_weight 1211.00 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' F F 0.0171 0.0103 '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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.789(3) _cell_length_b 26.622(6) _cell_length_c 20.717(4) _cell_angle_alpha 90.00 _cell_angle_beta 127.862(10) _cell_angle_gamma 90.00 _cell_volume 5569(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.956 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 34002 _diffrn_reflns_av_R_equivalents 0.0878 _diffrn_reflns_av_sigmaI/netI 0.1368 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.78 _reflns_number_total 13155 _reflns_number_gt 4146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13155 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2569 _refine_ls_R_factor_gt 0.0996 _refine_ls_wR_factor_ref 0.3605 _refine_ls_wR_factor_gt 0.2747 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C42 C 0.5864(5) 0.76947(19) 0.4209(3) 0.0473(13) Uani 1 1 d . . . C51 C 0.5093(6) 0.55079(19) 0.2875(4) 0.0567(15) Uani 1 1 d . . . C45 C 0.5606(5) 0.71443(19) 0.4060(3) 0.0468(13) Uani 1 1 d . . . C6 C 0.6373(6) 0.6993(2) 0.2812(4) 0.0583(15) Uani 1 1 d . . . H6 H 0.5785 0.6724 0.2583 0.070 Uiso 1 1 calc R . . C3 C 0.8147(6) 0.7783(2) 0.3451(4) 0.0607(15) Uani 1 1 d . . . C17 C 0.6878(6) 0.7301(2) 0.6236(4) 0.0580(15) Uani 1 1 d . . . C15 C 0.6886(6) 0.8195(2) 0.6335(4) 0.0627(16) Uani 1 1 d . . . C1 C 0.5926(6) 0.7469(2) 0.2577(4) 0.0569(15) Uani 1 1 d . . . C18 C 0.5509(5) 0.7293(2) 0.5651(3) 0.0592(15) Uani 1 1 d . . . H18 H 0.5045 0.6993 0.5435 0.071 Uiso 1 1 calc R . . C4 C 0.8602(6) 0.7302(2) 0.3705(4) 0.0623(16) Uani 1 1 d . . . H4 H 0.9505 0.7240 0.4084 0.075 Uiso 1 1 calc R . . C14 C 0.5521(6) 0.8194(2) 0.5742(4) 0.0678(17) Uani 1 1 d . . . H14 H 0.5052 0.8494 0.5576 0.081 Uiso 1 1 calc R . . C5 C 0.7710(6) 0.6912(2) 0.3394(4) 0.0555(14) Uani 1 1 d . . . C50 C 0.4873(6) 0.56069(19) 0.3491(4) 0.0664(17) Uani 1 1 d . . . H50A H 0.3972 0.5518 0.3266 0.080 Uiso 1 1 calc R . . H50B H 0.5471 0.5402 0.3973 0.080 Uiso 1 1 calc R . . C16 C 0.7559(6) 0.7755(2) 0.6573(4) 0.0601(15) Uani 1 1 d . . . H16 H 0.8476 0.7755 0.6961 0.072 Uiso 1 1 calc R . . C48 C 0.4118(6) 0.6468(2) 0.3325(4) 0.0614(16) Uani 1 1 d . . . H48 H 0.3257 0.6354 0.2936 0.074 Uiso 1 1 calc R . . C13 C 0.4868(6) 0.7751(2) 0.5404(4) 0.0617(16) Uani 1 1 d . . . C47 C 0.6317(6) 0.6298(2) 0.4285(4) 0.0611(16) Uani 1 1 d . . . H47 H 0.7001 0.6065 0.4564 0.073 Uiso 1 1 calc R . . C49 C 0.4354(5) 0.6972(2) 0.3481(4) 0.0572(15) Uani 1 1 d . . . H49 H 0.3654 0.7198 0.3190 0.069 Uiso 1 1 calc R . . C46 C 0.6596(6) 0.6798(2) 0.4472(4) 0.0588(15) Uani 1 1 d . . . H46 H 0.7461 0.6900 0.4880 0.071 Uiso 1 1 calc R . . C20 C 0.8103(6) 0.6014(2) 0.6533(4) 0.0743(18) Uani 1 1 d . . . H20A H 0.8828 0.6057 0.7110 0.089 Uiso 1 1 calc R . . H20B H 0.7735 0.5681 0.6454 0.089 Uiso 1 1 calc R . . C2 C 0.6791(7) 0.7871(2) 0.2874(4) 0.0661(17) Uani 1 1 d . . . H2 H 0.6474 0.8195 0.2691 0.079 Uiso 1 1 calc R . . C10 C 0.0982(6) 0.7904(3) 0.2329(5) 0.084(2) Uani 1 1 d . . . H10A H 0.1184 0.8254 0.2491 0.101 Uiso 1 1 calc R . . H10B H 0.0079 0.7843 0.2125 0.101 Uiso 1 1 calc R . . C37 C 0.6252(7) 0.9329(2) 0.3116(5) 0.0722(18) Uani 1 1 d . . . H37 H 0.5388 0.9214 0.2839 0.087 Uiso 1 1 calc R . . C19 C 0.7056(6) 0.6403(2) 0.6265(4) 0.0683(17) Uani 1 1 d . . . H19A H 0.6389 0.6393 0.5676 0.082 Uiso 1 1 calc R . . H19B H 0.6627 0.6335 0.6513 0.082 Uiso 1 1 calc R . . C41 C 0.7124(6) 0.7884(2) 0.4683(4) 0.0698(17) Uani 1 1 d . . . H41 H 0.7847 0.7668 0.4947 0.084 Uiso 1 1 calc R . . C43 C 0.4846(6) 0.8032(2) 0.3860(4) 0.0695(18) Uani 1 1 d . . . H43 H 0.3977 0.7916 0.3548 0.083 Uiso 1 1 calc R . . C25 C 0.9096(7) 0.8223(2) 0.3803(5) 0.083(2) Uani 1 1 d . . . H25A H 0.9110 0.8374 0.3382 0.100 Uiso 1 1 calc R . . H25B H 0.8804 0.8476 0.3999 0.100 Uiso 1 1 calc R . . C36 C 0.7038(7) 0.9385(2) 0.3943(5) 0.0663(17) Uani 1 1 d . . . C11 C 0.1516(6) 0.7568(3) 0.3557(4) 0.081(2) Uani 1 1 d . . . H11A H 0.0790 0.7335 0.3343 0.098 Uiso 1 1 calc R . . H11B H 0.1245 0.7894 0.3615 0.098 Uiso 1 1 calc R . . C56 C 0.4200(7) 0.5666(2) 0.2081(4) 0.0789(19) Uani 1 1 d . . . H56 H 0.3433 0.5828 0.1927 0.095 Uiso 1 1 calc R . . C32 C 0.7615(7) 0.8681(2) 0.6690(4) 0.0809(19) Uani 1 1 d . . . H32A H 0.7561 0.8870 0.6270 0.097 Uiso 1 1 calc R . . H32B H 0.7195 0.8877 0.6867 0.097 Uiso 1 1 calc R . . C44 C 0.5092(7) 0.8542(2) 0.3965(5) 0.0742(19) Uani 1 1 d . . . H44 H 0.4385 0.8764 0.3733 0.089 Uiso 1 1 calc R . . C39 C 0.6554(7) 0.9264(2) 0.4428(5) 0.083(2) Uani 1 1 d . . . H39A H 0.7216 0.9362 0.4994 0.100 Uiso 1 1 calc R . . H39B H 0.5749 0.9451 0.4212 0.100 Uiso 1 1 calc R . . C24 C 0.9421(6) 0.6309(2) 0.4230(5) 0.081(2) Uani 1 1 d . . . H24A H 0.9817 0.6540 0.4685 0.098 Uiso 1 1 calc R . . H24B H 0.9882 0.6342 0.3996 0.098 Uiso 1 1 calc R . . C54 C 0.5482(10) 0.5348(3) 0.1717(6) 0.096(3) Uani 1 1 d . . . H54 H 0.5609 0.5292 0.1327 0.115 Uiso 1 1 calc R . . C9 C 0.1078(6) 0.7814(3) 0.1676(4) 0.087(2) Uani 1 1 d . . . H9A H 0.0856 0.7467 0.1499 0.105 Uiso 1 1 calc R . . H9B H 0.0456 0.8028 0.1213 0.105 Uiso 1 1 calc R . . C52 C 0.6189(6) 0.5268(2) 0.3071(4) 0.0766(18) Uani 1 1 d . . . H52 H 0.6823 0.5157 0.3604 0.092 Uiso 1 1 calc R . . C21 C 0.9452(7) 0.5668(2) 0.6239(4) 0.084(2) Uani 1 1 d . . . H21A H 0.8989 0.5350 0.6098 0.101 Uiso 1 1 calc R . . H21B H 1.0189 0.5662 0.6818 0.101 Uiso 1 1 calc R . . C8 C 0.2535(7) 0.7923(3) 0.1340(5) 0.107(3) Uani 1 1 d . . . H8A H 0.2051 0.8201 0.0969 0.128 Uiso 1 1 calc R . . H8B H 0.2207 0.7613 0.1027 0.128 Uiso 1 1 calc R . . C40 C 0.7317(6) 0.8396(3) 0.4767(4) 0.0748(18) Uani 1 1 d . . . H40 H 0.8176 0.8522 0.5097 0.090 Uiso 1 1 calc R . . C30 C 1.0203(7) 0.8926(3) 0.6923(5) 0.089(2) Uani 1 1 d . . . C31 C 0.9775(8) 0.9001(3) 0.7447(5) 0.100(2) Uani 1 1 d . . . H31A H 1.0552 0.9019 0.8016 0.120 Uiso 1 1 calc R . . H31B H 0.9307 0.9318 0.7305 0.120 Uiso 1 1 calc R . . C12 C 0.2715(6) 0.7389(3) 0.4371(4) 0.0798(19) Uani 1 1 d . . . H12A H 0.2453 0.7239 0.4679 0.096 Uiso 1 1 calc R . . H12B H 0.3181 0.7138 0.4295 0.096 Uiso 1 1 calc R . . C23 C 0.9544(7) 0.5785(3) 0.4520(5) 0.087(2) Uani 1 1 d . . . H23A H 0.9060 0.5562 0.4051 0.104 Uiso 1 1 calc R . . H23B H 1.0469 0.5687 0.4858 0.104 Uiso 1 1 calc R . . C26 C 1.1241(8) 0.8462(3) 0.4934(5) 0.102(2) Uani 1 1 d . . . H26A H 1.1087 0.8743 0.4587 0.123 Uiso 1 1 calc R . . H26B H 1.2151 0.8352 0.5225 0.123 Uiso 1 1 calc R . . C38 C 0.6716(10) 0.9440(3) 0.2680(5) 0.099(3) Uani 1 1 d . . . H38 H 0.6173 0.9398 0.2115 0.119 Uiso 1 1 calc R . . C28 C 1.0816(7) 0.8725(3) 0.5991(5) 0.090(2) Uani 1 1 d . . . C35 C 0.8319(7) 0.9545(2) 0.4340(5) 0.086(2) Uani 1 1 d . . . H35 H 0.8883 0.9576 0.4906 0.104 Uiso 1 1 calc R . . C55 C 0.4391(10) 0.5596(3) 0.1511(5) 0.101(3) Uani 1 1 d . . . H55 H 0.3777 0.5717 0.0983 0.122 Uiso 1 1 calc R . . C7 C 0.4017(8) 0.7979(3) 0.1766(5) 0.102(2) Uani 1 1 d . . . H7A H 0.4155 0.8104 0.1383 0.123 Uiso 1 1 calc R . . H7B H 0.4409 0.8216 0.2215 0.123 Uiso 1 1 calc R . . C29 C 1.0520(7) 0.8842(3) 0.6511(5) 0.090(2) Uani 1 1 d . . . C22 C 0.9961(8) 0.5728(3) 0.5769(5) 0.106(3) Uani 1 1 d . . . H22A H 1.0441 0.6043 0.5929 0.127 Uiso 1 1 calc R . . H22B H 1.0593 0.5461 0.5927 0.127 Uiso 1 1 calc R . . C53 C 0.6381(8) 0.5185(3) 0.2487(6) 0.094(2) Uani 1 1 d . . . H53 H 0.7133 0.5015 0.2630 0.112 Uiso 1 1 calc R . . C33 C 0.7998(11) 0.9614(3) 0.3096(7) 0.110(3) Uani 1 1 d . . . H33 H 0.8318 0.9699 0.2811 0.132 Uiso 1 1 calc R . . C34 C 0.8768(9) 0.9659(3) 0.3901(7) 0.104(3) Uani 1 1 d . . . H34 H 0.9634 0.9770 0.4177 0.125 Uiso 1 1 calc R . . C27 C 1.1016(7) 0.8620(3) 0.5526(5) 0.091(2) Uani 1 1 d . . . F1 F 0.4678(6) 0.5515(3) 0.5295(5) 0.248(4) Uani 1 1 d . . . F2 F 0.3958(8) 0.6072(3) 0.5640(5) 0.217(3) Uani 1 1 d . . . F3 F 0.2025(6) 0.5956(5) 0.4466(5) 0.284(6) Uani 1 1 d . . . F4 F 0.3005(10) 0.5353(4) 0.5195(6) 0.326(7) Uani 1 1 d . . . F5 F 0.2828(7) 0.5464(3) 0.4060(5) 0.205(3) Uani 1 1 d . . . F6 F 0.3801(8) 0.6143(3) 0.4582(5) 0.219(3) Uani 1 1 d . . . F7 F 0.2631(5) 0.9370(2) 0.3271(3) 0.1362(18) Uani 1 1 d . . . F8 F 0.3508(9) 0.9236(4) 0.4521(4) 0.318(7) Uani 1 1 d . . . F9 F 0.3057(9) 1.0001(2) 0.4129(6) 0.221(4) Uani 1 1 d . . . F10 F 0.1127(8) 0.9761(4) 0.3217(4) 0.244(4) Uani 1 1 d . . . F11 F 0.1491(10) 0.9061(3) 0.3582(5) 0.237(4) Uani 1 1 d . . . F12 F 0.2053(5) 0.9638(2) 0.4494(3) 0.1381(18) Uani 1 1 d . . . N1 N 0.6289(5) 0.87169(16) 0.4380(3) 0.0617(13) Uani 1 1 d . . . N2 N 0.5104(5) 0.61424(16) 0.3721(3) 0.0515(11) Uani 1 1 d . . . O1 O 0.3546(4) 0.78059(17) 0.4798(3) 0.0880(14) Uani 1 1 d . . . O2 O 0.7668(4) 0.68815(15) 0.6512(3) 0.0712(12) Uani 1 1 d . . . O3 O 1.0358(5) 0.80599(18) 0.4444(3) 0.0918(15) Uani 1 1 d . . . O4 O 0.8938(5) 0.86059(18) 0.7349(3) 0.0998(15) Uani 1 1 d . . . O5 O 0.8060(4) 0.64241(14) 0.3632(3) 0.0688(11) Uani 1 1 d . . . O6 O 0.4581(5) 0.75235(17) 0.2048(3) 0.0837(13) Uani 1 1 d . . . O15 O 0.1834(4) 0.76026(15) 0.3013(3) 0.0688(11) Uani 1 1 d . . . O16 O 0.2360(4) 0.7915(2) 0.1951(3) 0.1000(16) Uani 1 1 d . . . O19 O 0.8581(4) 0.60631(14) 0.6075(2) 0.0711(12) Uani 1 1 d . . . O20 O 0.9075(5) 0.57245(19) 0.4962(3) 0.0981(16) Uani 1 1 d . . . P1 P 0.3342(2) 0.57467(8) 0.48634(16) 0.0903(7) Uani 1 1 d . . . P2 P 0.23505(17) 0.95041(6) 0.38856(11) 0.0660(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C42 0.042(3) 0.063(3) 0.044(3) -0.001(3) 0.030(3) 0.000(3) C51 0.066(4) 0.046(3) 0.060(4) -0.005(3) 0.039(3) -0.001(3) C45 0.048(3) 0.062(3) 0.042(3) 0.003(3) 0.034(3) 0.005(3) C6 0.054(4) 0.073(4) 0.057(4) -0.004(3) 0.038(3) 0.002(3) C3 0.070(4) 0.068(4) 0.061(4) -0.003(3) 0.048(4) -0.001(3) C17 0.058(4) 0.068(4) 0.058(4) 0.008(3) 0.041(3) 0.004(3) C15 0.075(4) 0.076(4) 0.052(4) 0.001(3) 0.046(4) 0.011(3) C1 0.052(4) 0.081(4) 0.053(4) 0.007(3) 0.040(3) 0.010(3) C18 0.054(4) 0.079(4) 0.049(4) 0.003(3) 0.034(3) 0.002(3) C4 0.053(4) 0.077(4) 0.063(4) 0.002(3) 0.039(3) 0.000(3) C14 0.071(4) 0.077(4) 0.069(4) 0.010(4) 0.049(4) 0.018(4) C5 0.060(4) 0.062(4) 0.054(4) -0.002(3) 0.040(3) 0.001(3) C50 0.088(5) 0.050(3) 0.078(5) 0.005(3) 0.059(4) 0.004(3) C16 0.044(3) 0.086(4) 0.048(4) -0.004(3) 0.027(3) -0.001(3) C48 0.051(4) 0.065(4) 0.070(4) -0.008(3) 0.038(3) 0.001(3) C13 0.046(4) 0.083(4) 0.053(4) 0.005(3) 0.028(3) 0.014(3) C47 0.070(4) 0.062(4) 0.047(4) 0.013(3) 0.034(4) 0.024(3) C49 0.039(3) 0.066(4) 0.062(4) 0.002(3) 0.029(3) 0.011(3) C46 0.052(3) 0.070(4) 0.046(4) 0.003(3) 0.026(3) 0.006(3) C20 0.087(5) 0.067(4) 0.071(5) 0.013(3) 0.050(4) 0.005(3) C2 0.082(5) 0.065(4) 0.070(4) 0.012(3) 0.057(4) 0.012(3) C10 0.055(4) 0.100(5) 0.099(6) 0.032(5) 0.048(4) 0.024(4) C37 0.081(5) 0.062(4) 0.077(5) -0.006(4) 0.050(4) 0.004(3) C19 0.071(4) 0.070(4) 0.071(4) 0.008(3) 0.047(4) 0.001(3) C41 0.056(4) 0.073(4) 0.066(4) -0.005(3) 0.030(3) -0.006(3) C43 0.046(4) 0.073(4) 0.090(5) -0.001(4) 0.042(4) 0.003(3) C25 0.083(5) 0.080(4) 0.102(6) -0.010(4) 0.064(5) -0.011(4) C36 0.079(5) 0.050(3) 0.085(5) -0.014(3) 0.058(4) -0.009(3) C11 0.055(4) 0.126(6) 0.069(5) 0.004(4) 0.041(4) 0.007(4) C56 0.094(5) 0.072(4) 0.068(5) 0.003(4) 0.049(5) 0.017(4) C32 0.069(5) 0.074(4) 0.077(5) -0.005(4) 0.033(4) 0.002(4) C44 0.066(4) 0.062(4) 0.111(6) 0.009(4) 0.063(4) 0.011(3) C39 0.118(6) 0.059(4) 0.096(6) -0.020(4) 0.078(5) -0.014(4) C24 0.063(4) 0.091(5) 0.102(6) 0.015(4) 0.058(4) 0.013(4) C54 0.142(8) 0.103(6) 0.089(7) -0.030(5) 0.095(7) -0.036(6) C9 0.053(4) 0.126(6) 0.070(5) 0.018(4) 0.032(4) 0.016(4) C52 0.067(4) 0.087(5) 0.068(5) -0.004(4) 0.037(4) 0.005(4) C21 0.082(5) 0.077(4) 0.074(5) 0.022(4) 0.038(4) 0.026(4) C8 0.079(5) 0.167(8) 0.074(5) 0.037(5) 0.047(5) 0.041(5) C40 0.061(4) 0.085(5) 0.067(4) -0.017(4) 0.034(4) -0.022(4) C30 0.082(5) 0.095(5) 0.077(6) -0.025(4) 0.043(5) -0.021(4) C31 0.095(6) 0.104(6) 0.105(6) -0.027(5) 0.063(5) -0.027(5) C12 0.066(4) 0.106(5) 0.069(5) 0.008(4) 0.042(4) 0.007(4) C23 0.073(5) 0.105(5) 0.103(6) 0.021(5) 0.064(5) 0.023(4) C26 0.101(6) 0.118(6) 0.109(6) -0.040(5) 0.075(5) -0.044(5) C38 0.160(9) 0.072(5) 0.073(5) -0.002(4) 0.076(6) 0.025(5) C28 0.071(5) 0.108(6) 0.080(6) -0.020(5) 0.042(5) -0.021(4) C35 0.084(5) 0.079(4) 0.098(6) -0.031(4) 0.057(5) -0.019(4) C55 0.147(8) 0.079(5) 0.076(6) 0.000(4) 0.068(6) 0.006(5) C7 0.103(6) 0.129(7) 0.098(6) 0.020(5) 0.074(6) 0.022(5) C29 0.065(5) 0.108(6) 0.067(5) -0.013(5) 0.026(4) -0.004(4) C22 0.084(6) 0.137(7) 0.079(6) 0.012(5) 0.041(5) 0.043(5) C53 0.083(5) 0.108(6) 0.107(7) -0.033(6) 0.067(6) -0.012(5) C33 0.145(9) 0.087(5) 0.147(10) -0.031(6) 0.115(8) -0.025(6) C34 0.091(6) 0.095(6) 0.146(9) -0.043(6) 0.083(7) -0.029(5) C27 0.067(5) 0.099(5) 0.090(6) -0.023(5) 0.040(5) -0.026(4) F1 0.121(5) 0.197(7) 0.255(9) -0.045(6) 0.028(5) 0.073(5) F2 0.245(8) 0.249(8) 0.178(7) -0.080(6) 0.141(6) -0.022(7) F3 0.108(5) 0.570(17) 0.181(7) 0.108(9) 0.092(5) 0.147(7) F4 0.260(10) 0.304(10) 0.257(10) 0.160(9) 0.079(8) -0.092(8) F5 0.165(6) 0.234(7) 0.203(7) -0.097(6) 0.106(6) -0.050(5) F6 0.323(9) 0.193(6) 0.256(8) 0.021(6) 0.235(8) -0.048(7) F7 0.155(5) 0.185(5) 0.121(4) -0.018(4) 0.112(4) -0.001(4) F8 0.297(10) 0.450(14) 0.088(4) 0.038(6) 0.059(6) 0.293(10) F9 0.343(10) 0.178(6) 0.292(9) -0.117(6) 0.271(9) -0.145(6) F10 0.229(8) 0.277(9) 0.115(5) 0.012(6) 0.050(5) 0.137(7) F11 0.389(11) 0.206(7) 0.224(8) -0.129(6) 0.243(9) -0.193(8) F12 0.159(5) 0.184(5) 0.118(4) -0.037(4) 0.108(4) -0.024(4) N1 0.078(4) 0.056(3) 0.069(3) -0.010(3) 0.054(3) -0.003(3) N2 0.057(3) 0.055(3) 0.056(3) 0.000(2) 0.042(3) 0.002(2) O1 0.060(3) 0.098(3) 0.078(3) -0.005(3) 0.028(3) 0.010(3) O2 0.057(3) 0.072(3) 0.072(3) 0.005(2) 0.033(2) 0.004(2) O3 0.087(4) 0.094(3) 0.103(4) -0.026(3) 0.063(3) -0.027(3) O4 0.090(4) 0.094(3) 0.099(4) -0.009(3) 0.049(3) -0.015(3) O5 0.061(3) 0.072(3) 0.072(3) 0.007(2) 0.041(2) 0.006(2) O6 0.080(3) 0.096(3) 0.087(3) 0.020(3) 0.057(3) 0.027(3) O15 0.050(2) 0.093(3) 0.069(3) 0.016(2) 0.040(2) 0.018(2) O16 0.062(3) 0.177(5) 0.066(3) 0.014(3) 0.043(3) 0.018(3) O19 0.073(3) 0.073(3) 0.063(3) 0.022(2) 0.040(2) 0.025(2) O20 0.071(3) 0.140(4) 0.088(4) 0.037(3) 0.052(3) 0.034(3) P1 0.0816(15) 0.0831(13) 0.1062(18) 0.0160(13) 0.0577(14) -0.0020(11) P2 0.0694(12) 0.0687(10) 0.0606(11) -0.0024(9) 0.0403(10) -0.0030(9) _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 C42 C43 1.366(7) . ? C42 C41 1.368(7) . ? C42 C45 1.492(7) . ? C51 C52 1.357(8) . ? C51 C56 1.372(8) . ? C51 C50 1.489(8) . ? C45 C49 1.362(7) . ? C45 C46 1.363(7) . ? C6 C1 1.353(8) . ? C6 C5 1.376(7) . ? C6 H6 0.9300 . ? C3 C4 1.370(8) . ? C3 C2 1.396(8) . ? C3 C25 1.515(8) . ? C17 O2 1.373(6) . ? C17 C18 1.390(7) . ? C17 C16 1.401(8) . ? C15 C16 1.355(8) . ? C15 C14 1.387(8) . ? C15 C32 1.496(8) . ? C1 O6 1.366(6) . ? C1 C2 1.382(8) . ? C18 C13 1.381(8) . ? C18 H18 0.9300 . ? C4 C5 1.375(7) . ? C4 H4 0.9300 . ? C14 C13 1.363(8) . ? C14 H14 0.9300 . ? C5 O5 1.365(6) . ? C50 N2 1.474(7) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C16 H16 0.9300 . ? C48 N2 1.320(7) . ? C48 C49 1.370(7) . ? C48 H48 0.9300 . ? C13 O1 1.361(7) . ? C47 N2 1.311(7) . ? C47 C46 1.370(7) . ? C47 H47 0.9300 . ? C49 H49 0.9300 . ? C46 H46 0.9300 . ? C20 O19 1.415(7) . ? C20 C19 1.503(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C2 H2 0.9300 . ? C10 O15 1.395(7) . ? C10 C9 1.452(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C37 C36 1.361(9) . ? C37 C38 1.383(10) . ? C37 H37 0.9300 . ? C19 O2 1.417(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C41 C40 1.376(8) . ? C41 H41 0.9300 . ? C43 C44 1.381(8) . ? C43 H43 0.9300 . ? C25 O3 1.387(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C36 C35 1.374(8) . ? C36 C39 1.504(8) . ? C11 O15 1.416(7) . ? C11 C12 1.500(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C56 C55 1.358(10) . ? C56 H56 0.9300 . ? C32 O4 1.390(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C44 N1 1.299(7) . ? C44 H44 0.9300 . ? C39 N1 1.485(7) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C24 O5 1.418(7) . ? C24 C23 1.489(9) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C54 C53 1.344(11) . ? C54 C55 1.353(10) . ? C54 H54 0.9300 . ? C9 O16 1.392(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C52 C53 1.391(10) . ? C52 H52 0.9300 . ? C21 O19 1.414(7) . ? C21 C22 1.475(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C8 O16 1.414(8) . ? C8 C7 1.530(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C40 N1 1.345(7) . ? C40 H40 0.9300 . ? C30 C29 1.169(10) . ? C30 C31 1.500(11) . ? C31 O4 1.424(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C12 O1 1.410(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C23 O20 1.378(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C26 O3 1.429(8) . ? C26 C27 1.484(11) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C38 C33 1.383(11) . ? C38 H38 0.9300 . ? C28 C27 1.172(10) . ? C28 C29 1.379(12) . ? C35 C34 1.375(11) . ? C35 H35 0.9300 . ? C55 H55 0.9300 . ? C7 O6 1.348(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C22 O20 1.324(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C53 H53 0.9300 . ? C33 C34 1.322(12) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? F1 P1 1.491(6) . ? F2 P1 1.551(7) . ? F3 P1 1.457(6) . ? F4 P1 1.455(7) . ? F5 P1 1.558(7) . ? F6 P1 1.489(6) . ? F7 P2 1.563(4) . ? F8 P2 1.429(6) . ? F9 P2 1.504(5) . ? F10 P2 1.475(6) . ? F11 P2 1.465(5) . ? F12 P2 1.565(4) . ? 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 C43 C42 C41 117.2(5) . . ? C43 C42 C45 121.1(5) . . ? C41 C42 C45 121.6(5) . . ? C52 C51 C56 116.7(6) . . ? C52 C51 C50 122.2(6) . . ? C56 C51 C50 121.1(6) . . ? C49 C45 C46 117.4(5) . . ? C49 C45 C42 120.3(5) . . ? C46 C45 C42 122.2(5) . . ? C1 C6 C5 119.0(6) . . ? C1 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C4 C3 C2 119.9(6) . . ? C4 C3 C25 120.8(6) . . ? C2 C3 C25 119.3(6) . . ? O2 C17 C18 124.2(5) . . ? O2 C17 C16 114.9(5) . . ? C18 C17 C16 120.8(5) . . ? C16 C15 C14 119.5(6) . . ? C16 C15 C32 120.2(6) . . ? C14 C15 C32 120.3(6) . . ? C6 C1 O6 115.7(6) . . ? C6 C1 C2 121.3(6) . . ? O6 C1 C2 123.0(6) . . ? C13 C18 C17 117.0(6) . . ? C13 C18 H18 121.5 . . ? C17 C18 H18 121.5 . . ? C3 C4 C5 119.3(6) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C13 C14 C15 119.9(6) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? O5 C5 C4 123.8(5) . . ? O5 C5 C6 114.8(5) . . ? C4 C5 C6 121.4(6) . . ? N2 C50 C51 109.9(4) . . ? N2 C50 H50A 109.7 . . ? C51 C50 H50A 109.7 . . ? N2 C50 H50B 109.7 . . ? C51 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? C15 C16 C17 120.2(6) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? N2 C48 C49 120.5(5) . . ? N2 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? O1 C13 C14 113.8(5) . . ? O1 C13 C18 123.7(6) . . ? C14 C13 C18 122.4(6) . . ? N2 C47 C46 121.3(5) . . ? N2 C47 H47 119.3 . . ? C46 C47 H47 119.3 . . ? C45 C49 C48 120.5(5) . . ? C45 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C45 C46 C47 120.0(5) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? O19 C20 C19 110.1(5) . . ? O19 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? O19 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.2 . . ? C1 C2 C3 119.0(5) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? O15 C10 C9 113.1(5) . . ? O15 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? O15 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C36 C37 C38 121.1(7) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? O2 C19 C20 108.4(5) . . ? 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 . . ? C42 C41 C40 119.8(6) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C42 C43 C44 120.8(5) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? O3 C25 C3 109.6(5) . . ? O3 C25 H25A 109.7 . . ? C3 C25 H25A 109.7 . . ? O3 C25 H25B 109.7 . . ? C3 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C37 C36 C35 118.4(7) . . ? C37 C36 C39 121.9(6) . . ? C35 C36 C39 119.6(7) . . ? O15 C11 C12 108.7(5) . . ? O15 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? O15 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.3 . . ? C55 C56 C51 122.6(7) . . ? C55 C56 H56 118.7 . . ? C51 C56 H56 118.7 . . ? O4 C32 C15 112.0(5) . . ? O4 C32 H32A 109.2 . . ? C15 C32 H32A 109.2 . . ? O4 C32 H32B 109.2 . . ? C15 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? N1 C44 C43 121.3(5) . . ? N1 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? N1 C39 C36 109.6(5) . . ? N1 C39 H39A 109.8 . . ? C36 C39 H39A 109.8 . . ? N1 C39 H39B 109.8 . . ? C36 C39 H39B 109.8 . . ? H39A C39 H39B 108.2 . . ? O5 C24 C23 108.9(5) . . ? O5 C24 H24A 109.9 . . ? C23 C24 H24A 109.9 . . ? O5 C24 H24B 109.9 . . ? C23 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C53 C54 C55 119.9(8) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? O16 C9 C10 109.8(6) . . ? O16 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? O16 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C51 C52 C53 121.2(7) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? O19 C21 C22 111.2(6) . . ? O19 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? O19 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? O16 C8 C7 107.8(6) . . ? O16 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? O16 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.5 . . ? N1 C40 C41 121.3(6) . . ? N1 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C29 C30 C31 176.7(8) . . ? O4 C31 C30 111.9(6) . . ? O4 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? O4 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? O1 C12 C11 108.2(6) . . ? O1 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? O1 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? O20 C23 C24 113.3(6) . . ? O20 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? O20 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? O3 C26 C27 109.2(5) . . ? O3 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? O3 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? C37 C38 C33 119.0(8) . . ? C37 C38 H38 120.5 . . ? C33 C38 H38 120.5 . . ? C27 C28 C29 177.3(8) . . ? C36 C35 C34 120.0(8) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C54 C55 C56 119.6(8) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? O6 C7 C8 107.7(7) . . ? O6 C7 H7A 110.2 . . ? C8 C7 H7A 110.2 . . ? O6 C7 H7B 110.2 . . ? C8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? C30 C29 C28 176.2(8) . . ? O20 C22 C21 116.7(7) . . ? O20 C22 H22A 108.1 . . ? C21 C22 H22A 108.1 . . ? O20 C22 H22B 108.1 . . ? C21 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? C54 C53 C52 120.0(7) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C34 C33 C38 119.8(9) . . ? C34 C33 H33 120.1 . . ? C38 C33 H33 120.1 . . ? C33 C34 C35 121.6(8) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C28 C27 C26 177.2(8) . . ? C44 N1 C40 119.4(5) . . ? C44 N1 C39 121.6(5) . . ? C40 N1 C39 119.0(5) . . ? C47 N2 C48 120.2(5) . . ? C47 N2 C50 119.1(5) . . ? C48 N2 C50 120.5(5) . . ? C13 O1 C12 121.7(5) . . ? C17 O2 C19 118.6(4) . . ? C25 O3 C26 113.1(6) . . ? C32 O4 C31 113.0(6) . . ? C5 O5 C24 118.4(5) . . ? C7 O6 C1 121.2(6) . . ? C10 O15 C11 114.8(5) . . ? C9 O16 C8 115.5(6) . . ? C21 O19 C20 111.8(5) . . ? C22 O20 C23 117.0(6) . . ? F4 P1 F3 88.1(6) . . ? F4 P1 F6 175.4(5) . . ? F3 P1 F6 96.0(5) . . ? F4 P1 F1 88.9(6) . . ? F3 P1 F1 177.0(6) . . ? F6 P1 F1 86.9(5) . . ? F4 P1 F2 91.2(6) . . ? F3 P1 F2 92.7(5) . . ? F6 P1 F2 86.5(5) . . ? F1 P1 F2 86.8(4) . . ? F4 P1 F5 95.9(6) . . ? F3 P1 F5 89.9(5) . . ? F6 P1 F5 86.2(5) . . ? F1 P1 F5 91.0(4) . . ? F2 P1 F5 172.5(5) . . ? F8 P2 F11 94.1(7) . . ? F8 P2 F10 177.6(7) . . ? F11 P2 F10 83.5(5) . . ? F8 P2 F9 93.5(7) . . ? F11 P2 F9 172.0(6) . . ? F10 P2 F9 88.8(5) . . ? F8 P2 F7 90.6(4) . . ? F11 P2 F7 87.4(3) . . ? F10 P2 F7 89.0(4) . . ? F9 P2 F7 94.7(3) . . ? F8 P2 F12 89.9(4) . . ? F11 P2 F12 92.3(3) . . ? F10 P2 F12 90.5(4) . . ? F9 P2 F12 85.6(3) . . ? F7 P2 F12 179.4(3) . . ? 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 C43 C42 C45 C49 9.5(8) . . . . ? C41 C42 C45 C49 -168.9(5) . . . . ? C43 C42 C45 C46 -172.3(5) . . . . ? C41 C42 C45 C46 9.2(8) . . . . ? C5 C6 C1 O6 -174.8(5) . . . . ? C5 C6 C1 C2 3.9(8) . . . . ? O2 C17 C18 C13 -176.2(5) . . . . ? C16 C17 C18 C13 1.9(8) . . . . ? C2 C3 C4 C5 -0.9(9) . . . . ? C25 C3 C4 C5 177.8(5) . . . . ? C16 C15 C14 C13 0.0(9) . . . . ? C32 C15 C14 C13 178.0(6) . . . . ? C3 C4 C5 O5 -177.3(5) . . . . ? C3 C4 C5 C6 2.3(8) . . . . ? C1 C6 C5 O5 175.8(5) . . . . ? C1 C6 C5 C4 -3.8(8) . . . . ? C52 C51 C50 N2 105.4(6) . . . . ? C56 C51 C50 N2 -73.2(7) . . . . ? C14 C15 C16 C17 -1.5(9) . . . . ? C32 C15 C16 C17 -179.5(5) . . . . ? O2 C17 C16 C15 178.7(5) . . . . ? C18 C17 C16 C15 0.5(8) . . . . ? C15 C14 C13 O1 -176.3(5) . . . . ? C15 C14 C13 C18 2.5(9) . . . . ? C17 C18 C13 O1 175.3(5) . . . . ? C17 C18 C13 C14 -3.4(8) . . . . ? C46 C45 C49 C48 -0.3(8) . . . . ? C42 C45 C49 C48 177.9(5) . . . . ? N2 C48 C49 C45 -1.4(8) . . . . ? C49 C45 C46 C47 1.3(8) . . . . ? C42 C45 C46 C47 -176.8(5) . . . . ? N2 C47 C46 C45 -0.9(8) . . . . ? C6 C1 C2 C3 -2.6(8) . . . . ? O6 C1 C2 C3 176.0(5) . . . . ? C4 C3 C2 C1 1.0(8) . . . . ? C25 C3 C2 C1 -177.7(5) . . . . ? O19 C20 C19 O2 -69.0(6) . . . . ? C43 C42 C41 C40 -2.3(9) . . . . ? C45 C42 C41 C40 176.3(5) . . . . ? C41 C42 C43 C44 2.1(9) . . . . ? C45 C42 C43 C44 -176.4(5) . . . . ? C4 C3 C25 O3 -7.3(8) . . . . ? C2 C3 C25 O3 171.4(5) . . . . ? C38 C37 C36 C35 -1.3(9) . . . . ? C38 C37 C36 C39 -179.8(5) . . . . ? C52 C51 C56 C55 -0.8(10) . . . . ? C50 C51 C56 C55 177.9(6) . . . . ? C16 C15 C32 O4 -10.3(9) . . . . ? C14 C15 C32 O4 171.7(5) . . . . ? C42 C43 C44 N1 1.6(10) . . . . ? C37 C36 C39 N1 65.6(8) . . . . ? C35 C36 C39 N1 -112.8(6) . . . . ? O15 C10 C9 O16 -60.5(8) . . . . ? C56 C51 C52 C53 -0.6(9) . . . . ? C50 C51 C52 C53 -179.3(6) . . . . ? C42 C41 C40 N1 -1.1(10) . . . . ? C29 C30 C31 O4 -18(15) . . . . ? O15 C11 C12 O1 82.0(6) . . . . ? O5 C24 C23 O20 -68.1(8) . . . . ? C36 C37 C38 C33 -0.5(10) . . . . ? C37 C36 C35 C34 1.9(9) . . . . ? C39 C36 C35 C34 -179.6(6) . . . . ? C53 C54 C55 C56 -1.6(12) . . . . ? C51 C56 C55 C54 1.9(11) . . . . ? O16 C8 C7 O6 80.0(8) . . . . ? C31 C30 C29 C28 44(25) . . . . ? C27 C28 C29 C30 14(31) . . . . ? O19 C21 C22 O20 -61.4(9) . . . . ? C55 C54 C53 C52 0.2(12) . . . . ? C51 C52 C53 C54 0.9(11) . . . . ? C37 C38 C33 C34 1.8(12) . . . . ? C38 C33 C34 C35 -1.2(13) . . . . ? C36 C35 C34 C33 -0.7(12) . . . . ? C29 C28 C27 C26 -51(34) . . . . ? O3 C26 C27 C28 23(19) . . . . ? C43 C44 N1 C40 -5.0(9) . . . . ? C43 C44 N1 C39 173.9(6) . . . . ? C41 C40 N1 C44 4.8(9) . . . . ? C41 C40 N1 C39 -174.2(6) . . . . ? C36 C39 N1 C44 -109.0(7) . . . . ? C36 C39 N1 C40 70.0(7) . . . . ? C46 C47 N2 C48 -0.8(8) . . . . ? C46 C47 N2 C50 174.6(5) . . . . ? C49 C48 N2 C47 1.9(8) . . . . ? C49 C48 N2 C50 -173.4(5) . . . . ? C51 C50 N2 C47 -83.9(6) . . . . ? C51 C50 N2 C48 91.5(6) . . . . ? C14 C13 O1 C12 179.1(5) . . . . ? C18 C13 O1 C12 0.3(9) . . . . ? C11 C12 O1 C13 -156.7(5) . . . . ? C18 C17 O2 C19 -7.9(8) . . . . ? C16 C17 O2 C19 173.9(5) . . . . ? C20 C19 O2 C17 171.2(5) . . . . ? C3 C25 O3 C26 -165.9(5) . . . . ? C27 C26 O3 C25 81.4(8) . . . . ? C15 C32 O4 C31 151.4(6) . . . . ? C30 C31 O4 C32 -85.2(7) . . . . ? C4 C5 O5 C24 -0.5(8) . . . . ? C6 C5 O5 C24 179.9(5) . . . . ? C23 C24 O5 C5 168.1(5) . . . . ? C8 C7 O6 C1 -168.5(5) . . . . ? C6 C1 O6 C7 -179.5(6) . . . . ? C2 C1 O6 C7 1.8(9) . . . . ? C9 C10 O15 C11 -162.5(6) . . . . ? C12 C11 O15 C10 -161.0(6) . . . . ? C10 C9 O16 C8 -170.0(6) . . . . ? C7 C8 O16 C9 -173.7(6) . . . . ? C22 C21 O19 C20 -179.0(6) . . . . ? C19 C20 O19 C21 -172.9(5) . . . . ? C21 C22 O20 C23 179.5(6) . . . . ? C24 C23 O20 C22 -98.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.78 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.612 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.070 # Attachment '[2]pseudorotaxane 2.cif' data_xuhyxmerbenpara _database_code_depnum_ccdc_archive 'CCDC 788121' #TrackingRef '[2]pseudorotaxane 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H68 F12 N2 O10 P2' _chemical_formula_weight 1219.06 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.672(11) _cell_length_b 14.541(11) _cell_length_c 16.402(12) _cell_angle_alpha 112.152(10) _cell_angle_beta 92.063(12) _cell_angle_gamma 104.255(12) _cell_volume 2897(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15071 _diffrn_reflns_av_R_equivalents 0.1026 _diffrn_reflns_av_sigmaI/netI 0.3330 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.20 _reflns_number_total 10446 _reflns_number_gt 2457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10446 _refine_ls_number_parameters 739 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.3528 _refine_ls_R_factor_gt 0.1022 _refine_ls_wR_factor_ref 0.3432 _refine_ls_wR_factor_gt 0.2318 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.090 _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 O1 O 0.7150(5) 0.4432(5) 0.4642(4) 0.064(2) Uani 1 1 d . . . O2 O 0.5029(5) 0.3461(5) 0.4048(4) 0.064(2) Uani 1 1 d . . . O3 O 0.3878(5) 0.4072(5) 0.3016(4) 0.0584(19) Uani 1 1 d . . . O4 O 0.4428(6) 0.4042(5) 0.1304(4) 0.064(2) Uani 1 1 d . . . O5 O 0.6507(6) 0.7068(7) 0.1148(5) 0.082(2) Uani 1 1 d . . . O6 O 0.8669(7) 0.8007(7) 0.1607(6) 0.103(3) Uani 1 1 d . . . O7 O 0.9928(6) 0.8153(8) 0.3132(7) 0.116(3) Uani 1 1 d . . . O8 O 0.9677(5) 0.6765(6) 0.4033(5) 0.076(2) Uani 1 1 d . . . O9 O 0.8207(7) 0.3999(6) 0.0280(5) 0.095(3) Uani 1 1 d . . . O10 O 0.9802(5) 0.2754(6) 0.2545(5) 0.081(2) Uani 1 1 d . . . C41 C 0.6305(10) 0.6004(11) 0.0879(7) 0.067(3) Uani 1 1 d . . . C30 C 0.9551(9) 0.4128(10) 0.3792(7) 0.061(3) Uani 1 1 d . . . C50 C 1.0385(9) 0.2056(10) 0.2134(8) 0.099(4) Uani 1 1 d . . . H50A H 1.0199 0.1464 0.2294 0.119 Uiso 1 1 calc R . . H50B H 1.1105 0.2400 0.2346 0.119 Uiso 1 1 calc R . . C39 C 0.6635(10) 0.4367(13) 0.0211(7) 0.073(4) Uani 1 1 d . . . C37 C 0.5225(8) 0.4542(10) 0.0991(6) 0.054(3) Uani 1 1 d . . . C35 C 0.3223(8) 0.3997(8) 0.2287(6) 0.065(3) Uani 1 1 d . . . H35A H 0.2651 0.4259 0.2497 0.078 Uiso 1 1 calc R . . H35B H 0.2958 0.3281 0.1873 0.078 Uiso 1 1 calc R . . C36 C 0.3821(7) 0.4618(8) 0.1839(6) 0.059(3) Uani 1 1 d . . . H36A H 0.3365 0.4771 0.1473 0.070 Uiso 1 1 calc R . . H36B H 0.4252 0.5267 0.2279 0.070 Uiso 1 1 calc R . . C28 C 0.8084(8) 0.4613(9) 0.4363(6) 0.056(3) Uani 1 1 d . . . C42 C 0.5457(8) 0.5585(10) 0.1178(6) 0.058(3) Uani 1 1 d . . . H42 H 0.5054 0.5988 0.1494 0.070 Uiso 1 1 calc R . . C27 C 0.8481(7) 0.5579(9) 0.4362(6) 0.054(3) Uani 1 1 d . . . H27 H 0.8140 0.6083 0.4579 0.064 Uiso 1 1 calc R . . C29 C 0.8631(9) 0.3865(8) 0.4086(6) 0.061(3) Uani 1 1 d . . . H29 H 0.8379 0.3217 0.4101 0.073 Uiso 1 1 calc R . . C33 C 0.4054(8) 0.3559(8) 0.4233(6) 0.064(3) Uani 1 1 d . . . H33A H 0.4113 0.4246 0.4674 0.077 Uiso 1 1 calc R . . H33B H 0.3735 0.3060 0.4472 0.077 Uiso 1 1 calc R . . C25 C 0.9927(8) 0.5078(10) 0.3739(6) 0.063(3) Uani 1 1 d . . . H25 H 1.0528 0.5225 0.3506 0.076 Uiso 1 1 calc R . . C31 C 0.6643(8) 0.3407(8) 0.4556(7) 0.064(3) Uani 1 1 d . . . H31A H 0.7000 0.3223 0.4967 0.077 Uiso 1 1 calc R . . H31B H 0.6622 0.2912 0.3956 0.077 Uiso 1 1 calc R . . C56 C 0.7310(10) 0.3749(11) -0.0295(7) 0.103(5) Uani 1 1 d . . . H56A H 0.6967 0.3016 -0.0507 0.123 Uiso 1 1 calc R . . H56B H 0.7469 0.3913 -0.0805 0.123 Uiso 1 1 calc R . . C38 C 0.5820(9) 0.3944(9) 0.0495(6) 0.066(3) Uani 1 1 d . . . H38 H 0.5643 0.3238 0.0361 0.079 Uiso 1 1 calc R . . C40 C 0.6910(9) 0.5420(13) 0.0404(7) 0.077(4) Uani 1 1 d . . . H40 H 0.7489 0.5726 0.0217 0.092 Uiso 1 1 calc R . . C51 C 1.0198(12) 0.1709(11) 0.1169(9) 0.118(5) Uani 1 1 d . . . H51A H 0.9471 0.1390 0.0976 0.142 Uiso 1 1 calc R . . H51B H 1.0538 0.1176 0.0906 0.142 Uiso 1 1 calc R . . C45 C 0.9616(11) 0.8692(10) 0.2000(9) 0.101(4) Uani 1 1 d . . . H45A H 0.9531 0.9309 0.2464 0.121 Uiso 1 1 calc R . . H45B H 0.9953 0.8894 0.1559 0.121 Uiso 1 1 calc R . . C26 C 0.9392(8) 0.5795(10) 0.4038(6) 0.057(3) Uani 1 1 d . . . C47 C 1.0683(10) 0.8112(10) 0.3717(9) 0.104(4) Uani 1 1 d . . . H47A H 1.0650 0.8563 0.4321 0.124 Uiso 1 1 calc R . . H47B H 1.1350 0.8370 0.3573 0.124 Uiso 1 1 calc R . . C34 C 0.3422(7) 0.3379(8) 0.3411(6) 0.062(3) Uani 1 1 d . . . H34A H 0.3324 0.2672 0.2990 0.074 Uiso 1 1 calc R . . H34B H 0.2758 0.3465 0.3546 0.074 Uiso 1 1 calc R . . C49 C 1.0107(8) 0.3317(9) 0.3459(7) 0.071(3) Uani 1 1 d . . . H49A H 1.0836 0.3643 0.3576 0.086 Uiso 1 1 calc R . . H49B H 0.9957 0.2856 0.3766 0.086 Uiso 1 1 calc R . . C48 C 1.0568(8) 0.7050(10) 0.3672(8) 0.090(4) Uani 1 1 d . . . H48A H 1.0511 0.6570 0.3059 0.108 Uiso 1 1 calc R . . H48B H 1.1157 0.7035 0.4009 0.108 Uiso 1 1 calc R . . C43 C 0.7134(10) 0.7604(11) 0.0693(8) 0.100(4) Uani 1 1 d . . . H43A H 0.7391 0.7119 0.0227 0.119 Uiso 1 1 calc R . . H43B H 0.6726 0.7897 0.0417 0.119 Uiso 1 1 calc R . . C55 C 0.8940(13) 0.3572(13) -0.0229(10) 0.145(6) Uani 1 1 d . . . H55A H 0.9129 0.3905 -0.0636 0.174 Uiso 1 1 calc R . . H55B H 0.8635 0.2839 -0.0580 0.174 Uiso 1 1 calc R . . C32 C 0.5597(8) 0.3398(8) 0.4760(6) 0.060(3) Uani 1 1 d . . . H32A H 0.5273 0.2766 0.4833 0.073 Uiso 1 1 calc R . . H32B H 0.5619 0.3980 0.5309 0.073 Uiso 1 1 calc R . . C46 C 1.0269(10) 0.8236(12) 0.2391(9) 0.116(5) Uani 1 1 d . . . H46A H 1.0258 0.7557 0.1959 0.140 Uiso 1 1 calc R . . H46B H 1.0968 0.8670 0.2540 0.140 Uiso 1 1 calc R . . C53 C 0.9799(17) 0.3055(19) 0.0741(15) 0.211(8) Uani 1 1 d U . . H53A H 0.9169 0.2513 0.0457 0.253 Uiso 1 1 calc R . . H53B H 0.9701 0.3422 0.1349 0.253 Uiso 1 1 calc R . . C52 C 1.0545(13) 0.2544(16) 0.0795(11) 0.164(8) Uani 1 1 d . . . H52A H 1.1157 0.3054 0.1170 0.196 Uiso 1 1 calc R . . H52B H 1.0720 0.2224 0.0206 0.196 Uiso 1 1 calc R . . C44 C 0.7972(11) 0.8412(10) 0.1292(8) 0.095(4) Uani 1 1 d . . . H44A H 0.8319 0.8829 0.0989 0.114 Uiso 1 1 calc R . . H44B H 0.7718 0.8856 0.1792 0.114 Uiso 1 1 calc R . . N1 N 0.6491(8) 0.1674(7) 0.1741(5) 0.060(2) Uani 1 1 d . . . N2 N 0.7048(7) 0.6945(7) 0.3212(5) 0.054(2) Uani 1 1 d . . . C1 C 0.7804(15) 0.9198(11) 0.6385(9) 0.102(5) Uani 1 1 d . . . H1 H 0.7951 0.9441 0.7000 0.122 Uiso 1 1 calc R . . C2 C 0.6956(13) 0.9239(10) 0.6033(11) 0.094(5) Uani 1 1 d . . . H2 H 0.6499 0.9493 0.6402 0.113 Uiso 1 1 calc R . . C3 C 0.6715(8) 0.8908(9) 0.5111(9) 0.073(3) Uani 1 1 d . . . H3 H 0.6122 0.8967 0.4865 0.087 Uiso 1 1 calc R . . C4 C 0.7380(10) 0.8496(8) 0.4588(7) 0.057(3) Uani 1 1 d . . . C5 C 0.8266(10) 0.8474(9) 0.4974(9) 0.090(4) Uani 1 1 d . . . H5 H 0.8736 0.8226 0.4619 0.108 Uiso 1 1 calc R . . C6 C 0.8474(12) 0.8811(11) 0.5873(11) 0.114(5) Uani 1 1 d . . . H6 H 0.9072 0.8774 0.6131 0.137 Uiso 1 1 calc R . . C7 C 0.7161(8) 0.8083(8) 0.3586(6) 0.065(3) Uani 1 1 d . . . H7A H 0.6539 0.8211 0.3411 0.077 Uiso 1 1 calc R . . H7B H 0.7715 0.8430 0.3359 0.077 Uiso 1 1 calc R . . C8 C 0.6306(8) 0.6324(9) 0.3448(6) 0.052(3) Uani 1 1 d . . . H8 H 0.5875 0.6613 0.3829 0.062 Uiso 1 1 calc R . . C9 C 0.6179(7) 0.5302(8) 0.3145(6) 0.045(3) Uani 1 1 d . . . H9 H 0.5664 0.4886 0.3311 0.054 Uiso 1 1 calc R . . C10 C 0.6822(7) 0.4873(8) 0.2581(6) 0.044(3) Uani 1 1 d . . . C11 C 0.7561(7) 0.5498(9) 0.2350(6) 0.047(3) Uani 1 1 d . . . H11 H 0.7997 0.5218 0.1970 0.057 Uiso 1 1 calc R . . C12 C 0.7677(8) 0.6544(10) 0.2671(7) 0.062(3) Uani 1 1 d . . . H12 H 0.8190 0.6969 0.2512 0.074 Uiso 1 1 calc R . . C13 C 0.6701(8) 0.3755(8) 0.2258(6) 0.045(3) Uani 1 1 d . . . C14 C 0.5786(8) 0.3069(9) 0.2202(6) 0.054(3) Uani 1 1 d . . . H14 H 0.5218 0.3310 0.2346 0.064 Uiso 1 1 calc R . . C15 C 0.5691(8) 0.2035(9) 0.1937(6) 0.056(3) Uani 1 1 d . . . H15 H 0.5060 0.1582 0.1894 0.067 Uiso 1 1 calc R . . C16 C 0.7374(9) 0.2316(11) 0.1759(7) 0.073(3) Uani 1 1 d . . . H16 H 0.7921 0.2051 0.1582 0.088 Uiso 1 1 calc R . . C17 C 0.7505(8) 0.3345(10) 0.2028(6) 0.060(3) Uani 1 1 d . . . H17 H 0.8144 0.3778 0.2057 0.072 Uiso 1 1 calc R . . C18 C 0.6413(9) 0.0596(8) 0.1609(7) 0.074(3) Uani 1 1 d . . . H18A H 0.6876 0.0331 0.1208 0.089 Uiso 1 1 calc R . . H18B H 0.5724 0.0161 0.1353 0.089 Uiso 1 1 calc R . . C19 C 0.6685(11) 0.0590(8) 0.2501(7) 0.062(3) Uani 1 1 d . . . C20 C 0.7689(11) 0.0861(9) 0.2869(9) 0.084(4) Uani 1 1 d . . . H20 H 0.8207 0.0993 0.2542 0.101 Uiso 1 1 calc R . . C21 C 0.7929(12) 0.0938(10) 0.3719(10) 0.105(5) Uani 1 1 d . . . H21 H 0.8610 0.1135 0.3962 0.126 Uiso 1 1 calc R . . C22 C 0.7207(15) 0.0735(10) 0.4200(9) 0.100(5) Uani 1 1 d . . . H22 H 0.7383 0.0776 0.4768 0.120 Uiso 1 1 calc R . . C23 C 0.6223(13) 0.0472(11) 0.3857(11) 0.100(5) Uani 1 1 d . . . H23 H 0.5717 0.0350 0.4198 0.121 Uiso 1 1 calc R . . C24 C 0.5948(10) 0.0377(8) 0.2983(9) 0.084(4) Uani 1 1 d . . . H24 H 0.5264 0.0169 0.2742 0.101 Uiso 1 1 calc R . . C54 C 0.9863(17) 0.3715(19) 0.0354(15) 0.212(8) Uani 1 1 d U . . H54A H 1.0419 0.3670 0.0004 0.254 Uiso 1 1 calc R . . H54B H 1.0040 0.4409 0.0816 0.254 Uiso 1 1 calc R . . P2 P 0.7218(3) 0.9839(4) 0.9118(2) 0.0888(12) Uani 1 1 d . . . P1 P 0.3645(3) 0.7589(3) 0.3168(2) 0.0853(11) Uani 1 1 d . . . F12 F 0.7849(7) 0.9899(9) 0.9953(5) 0.177(4) Uani 1 1 d . . . F2 F 0.2990(7) 0.7709(9) 0.3914(6) 0.182(4) Uani 1 1 d . . . F7 F 0.6539(6) 0.9703(9) 0.8282(5) 0.183(4) Uani 1 1 d . . . F3 F 0.4213(10) 0.7018(10) 0.3510(6) 0.219(6) Uani 1 1 d . . . F10 F 0.8149(7) 1.0203(11) 0.8770(6) 0.233(6) Uani 1 1 d . . . F8 F 0.6252(7) 0.9474(11) 0.9475(5) 0.231(6) Uani 1 1 d . . . F5 F 0.3066(12) 0.8124(11) 0.2828(7) 0.259(7) Uani 1 1 d . . . F4 F 0.4264(11) 0.7386(12) 0.2435(8) 0.261(7) Uani 1 1 d . . . F11 F 0.7197(12) 1.0906(9) 0.9694(8) 0.247(6) Uani 1 1 d . . . F6 F 0.2944(9) 0.6624(8) 0.2568(9) 0.241(6) Uani 1 1 d . . . F1 F 0.4356(9) 0.8566(9) 0.3813(11) 0.282(8) Uani 1 1 d . . . F9 F 0.7197(13) 0.8753(9) 0.8608(8) 0.278(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.058(5) 0.056(5) 0.075(5) 0.020(4) 0.025(4) 0.017(4) O2 0.054(5) 0.089(6) 0.059(5) 0.040(4) 0.019(4) 0.020(4) O3 0.045(4) 0.073(5) 0.062(5) 0.039(4) 0.005(4) 0.005(4) O4 0.072(5) 0.067(5) 0.056(5) 0.029(4) 0.013(4) 0.019(4) O5 0.074(6) 0.100(7) 0.075(6) 0.044(6) 0.026(5) 0.010(5) O6 0.086(7) 0.097(7) 0.117(7) 0.063(6) -0.020(6) -0.018(6) O7 0.045(5) 0.201(10) 0.136(8) 0.109(8) 0.011(6) 0.025(6) O8 0.049(5) 0.066(6) 0.109(6) 0.037(5) 0.011(4) 0.008(4) O9 0.099(7) 0.126(7) 0.073(6) 0.035(6) 0.021(6) 0.062(6) O10 0.079(6) 0.099(6) 0.060(5) 0.009(5) 0.011(5) 0.052(5) C41 0.067(9) 0.074(10) 0.057(8) 0.034(8) -0.002(7) 0.005(8) C30 0.062(8) 0.067(9) 0.054(7) 0.022(7) 0.006(6) 0.024(7) C50 0.101(10) 0.122(12) 0.085(10) 0.025(9) 0.037(9) 0.073(9) C39 0.080(10) 0.113(12) 0.036(7) 0.029(8) 0.008(7) 0.049(9) C37 0.052(7) 0.069(9) 0.036(6) 0.022(7) -0.009(6) 0.006(7) C35 0.062(8) 0.086(9) 0.055(7) 0.036(7) 0.010(6) 0.018(7) C36 0.059(7) 0.076(8) 0.058(7) 0.039(7) 0.016(6) 0.028(7) C28 0.050(7) 0.066(9) 0.042(6) 0.008(6) -0.006(6) 0.023(7) C42 0.051(7) 0.083(10) 0.048(7) 0.033(7) 0.002(6) 0.020(7) C27 0.043(7) 0.051(8) 0.057(7) 0.011(6) 0.002(6) 0.014(6) C29 0.067(8) 0.063(8) 0.050(7) 0.025(6) -0.003(6) 0.015(7) C33 0.057(8) 0.076(8) 0.059(7) 0.036(7) 0.010(6) 0.006(6) C25 0.047(7) 0.080(9) 0.061(7) 0.026(7) 0.005(6) 0.019(7) C31 0.064(8) 0.066(9) 0.067(8) 0.028(7) 0.006(6) 0.025(7) C56 0.100(11) 0.175(14) 0.048(8) 0.030(9) 0.017(8) 0.088(11) C38 0.080(9) 0.090(10) 0.030(6) 0.021(7) 0.013(6) 0.032(8) C40 0.054(8) 0.146(14) 0.049(8) 0.052(9) 0.010(6) 0.041(10) C51 0.153(15) 0.126(14) 0.069(10) 0.012(10) 0.008(10) 0.073(12) C45 0.096(11) 0.089(11) 0.097(10) 0.043(9) -0.005(9) -0.017(9) C26 0.044(7) 0.080(10) 0.057(7) 0.035(7) 0.014(6) 0.020(7) C47 0.076(10) 0.104(12) 0.142(13) 0.077(11) 0.014(9) 0.001(8) C34 0.047(7) 0.070(8) 0.062(7) 0.024(7) -0.002(6) 0.010(6) C49 0.065(8) 0.085(9) 0.054(8) 0.011(7) -0.002(6) 0.032(7) C48 0.043(8) 0.098(11) 0.147(12) 0.067(10) 0.033(8) 0.018(7) C43 0.074(9) 0.130(13) 0.083(10) 0.050(10) 0.000(8) -0.003(9) C55 0.138(15) 0.184(17) 0.128(14) 0.048(13) 0.033(13) 0.092(14) C32 0.059(8) 0.066(8) 0.059(7) 0.028(6) 0.012(6) 0.018(6) C46 0.075(11) 0.175(16) 0.098(11) 0.065(12) 0.016(9) 0.015(10) C53 0.179(15) 0.29(3) 0.227(19) 0.172(15) 0.029(14) 0.071(18) C52 0.136(16) 0.26(2) 0.171(17) 0.121(17) 0.083(13) 0.116(16) C44 0.111(12) 0.090(11) 0.081(10) 0.038(9) 0.012(9) 0.017(10) N1 0.084(8) 0.048(7) 0.040(5) 0.008(5) 0.013(5) 0.020(6) N2 0.056(6) 0.061(7) 0.044(5) 0.022(5) 0.009(5) 0.012(5) C1 0.143(16) 0.073(11) 0.054(9) 0.008(8) 0.001(11) -0.003(11) C2 0.121(14) 0.067(10) 0.086(13) 0.020(9) 0.040(11) 0.026(10) C3 0.061(8) 0.069(9) 0.090(10) 0.032(8) 0.015(8) 0.020(7) C4 0.070(8) 0.046(7) 0.058(8) 0.024(6) 0.009(7) 0.013(7) C5 0.070(9) 0.107(11) 0.061(9) 0.002(8) 0.013(8) 0.020(8) C6 0.129(14) 0.117(13) 0.080(12) 0.009(10) -0.019(10) 0.058(11) C7 0.095(9) 0.054(8) 0.049(7) 0.025(6) 0.016(6) 0.021(7) C8 0.053(7) 0.061(9) 0.034(6) 0.015(6) 0.004(5) 0.011(6) C9 0.045(6) 0.047(8) 0.039(6) 0.013(6) 0.010(5) 0.012(6) C10 0.036(6) 0.057(8) 0.035(6) 0.018(6) -0.002(5) 0.006(6) C11 0.055(7) 0.059(8) 0.032(6) 0.023(6) 0.007(5) 0.015(6) C12 0.055(7) 0.072(10) 0.049(7) 0.027(7) 0.010(6) -0.004(7) C13 0.037(6) 0.061(8) 0.036(6) 0.020(6) 0.004(5) 0.010(6) C14 0.047(7) 0.068(9) 0.050(7) 0.026(6) 0.006(6) 0.020(6) C15 0.057(8) 0.055(9) 0.060(7) 0.031(7) -0.006(6) 0.012(6) C16 0.072(9) 0.079(10) 0.073(9) 0.028(8) 0.032(7) 0.031(8) C17 0.058(8) 0.075(9) 0.061(7) 0.040(7) 0.029(6) 0.020(7) C18 0.093(9) 0.049(8) 0.072(9) 0.013(7) 0.020(7) 0.023(7) C19 0.087(10) 0.054(8) 0.049(8) 0.019(7) 0.013(8) 0.029(7) C20 0.108(12) 0.070(9) 0.071(10) 0.018(8) 0.031(9) 0.031(9) C21 0.129(14) 0.094(12) 0.082(11) 0.037(10) 0.000(10) 0.013(10) C22 0.155(16) 0.073(10) 0.081(11) 0.043(9) 0.013(12) 0.029(11) C23 0.110(13) 0.124(13) 0.109(13) 0.073(11) 0.043(11) 0.060(11) C24 0.106(11) 0.062(9) 0.094(11) 0.040(8) 0.035(10) 0.023(8) C54 0.174(15) 0.30(3) 0.227(19) 0.161(15) 0.021(14) 0.085(17) P2 0.082(3) 0.097(3) 0.055(2) 0.006(2) 0.006(2) 0.009(2) P1 0.085(3) 0.098(3) 0.069(2) 0.020(3) 0.007(2) 0.041(3) F12 0.133(8) 0.295(13) 0.104(6) 0.076(8) 0.001(6) 0.067(8) F2 0.134(8) 0.283(12) 0.138(8) 0.072(8) 0.070(7) 0.085(8) F7 0.115(7) 0.334(14) 0.117(7) 0.126(8) -0.004(6) 0.035(8) F3 0.329(14) 0.288(14) 0.111(7) 0.071(8) 0.003(8) 0.227(12) F10 0.122(8) 0.387(18) 0.108(7) 0.090(9) 0.037(6) -0.063(9) F8 0.117(8) 0.380(18) 0.082(6) 0.053(9) 0.006(6) -0.063(9) F5 0.44(2) 0.303(15) 0.171(9) 0.125(10) 0.069(11) 0.294(16) F4 0.296(15) 0.44(2) 0.193(10) 0.187(13) 0.192(12) 0.244(16) F11 0.361(19) 0.141(10) 0.233(13) 0.036(10) 0.060(13) 0.117(11) F6 0.192(11) 0.142(10) 0.247(13) -0.040(9) -0.075(11) 0.008(8) F1 0.152(10) 0.157(11) 0.369(19) -0.021(12) 0.003(12) -0.040(8) F9 0.45(2) 0.125(10) 0.190(11) -0.028(9) -0.010(13) 0.118(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C28 1.371(11) . ? O1 C31 1.431(10) . ? O2 C33 1.407(10) . ? O2 C32 1.422(10) . ? O3 C35 1.422(10) . ? O3 C34 1.427(10) . ? O4 C37 1.382(11) . ? O4 C36 1.415(9) . ? O5 C41 1.390(12) . ? O5 C43 1.434(11) . ? O6 C45 1.380(13) . ? O6 C44 1.412(13) . ? O7 C46 1.353(12) . ? O7 C47 1.412(13) . ? O8 C26 1.370(11) . ? O8 C48 1.412(11) . ? O9 C56 1.402(12) . ? O9 C55 1.435(13) . ? O10 C49 1.397(10) . ? O10 C50 1.430(11) . ? C41 C42 1.368(13) . ? C41 C40 1.379(14) . ? C30 C29 1.381(12) . ? C30 C25 1.388(13) . ? C30 C49 1.500(13) . ? C50 C51 1.460(14) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C39 C38 1.324(14) . ? C39 C40 1.389(15) . ? C39 C56 1.500(14) . ? C37 C42 1.379(13) . ? C37 C38 1.394(13) . ? C35 C36 1.485(11) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C28 C27 1.376(12) . ? C28 C29 1.414(12) . ? C42 H42 0.9300 . ? C27 C26 1.383(12) . ? C27 H27 0.9300 . ? C29 H29 0.9300 . ? C33 C34 1.473(12) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C25 C26 1.371(12) . ? C25 H25 0.9300 . ? C31 C32 1.478(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C38 H38 0.9300 . ? C40 H40 0.9300 . ? C51 C52 1.541(18) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C45 C46 1.491(16) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C47 C48 1.486(14) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C43 C44 1.429(14) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C55 C54 1.48(2) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C53 C54 1.32(2) . ? C53 C52 1.42(2) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? N1 C16 1.324(12) . ? N1 C15 1.325(11) . ? N1 C18 1.475(11) . ? N2 C12 1.334(11) . ? N2 C8 1.354(11) . ? N2 C7 1.497(11) . ? C1 C2 1.302(17) . ? C1 C6 1.347(16) . ? C1 H1 0.9300 . ? C2 C3 1.402(15) . ? C2 H2 0.9300 . ? C3 C4 1.364(12) . ? C3 H3 0.9300 . ? C4 C5 1.359(14) . ? C4 C7 1.510(12) . ? C5 C6 1.361(15) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.340(12) . ? C8 H8 0.9300 . ? C9 C10 1.382(11) . ? C9 H9 0.9300 . ? C10 C11 1.352(11) . ? C10 C13 1.469(12) . ? C11 C12 1.373(12) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.370(12) . ? C13 C17 1.376(12) . ? C14 C15 1.369(12) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.353(13) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.500(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.351(13) . ? C19 C20 1.378(15) . ? C20 C21 1.375(15) . ? C20 H20 0.9300 . ? C21 C22 1.331(15) . ? C21 H21 0.9300 . ? C22 C23 1.342(16) . ? C22 H22 0.9300 . ? C23 C24 1.415(16) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? P2 F10 1.474(8) . ? P2 F9 1.475(10) . ? P2 F11 1.490(11) . ? P2 F8 1.521(9) . ? P2 F7 1.546(8) . ? P2 F12 1.556(8) . ? P1 F6 1.444(10) . ? P1 F5 1.464(9) . ? P1 F4 1.476(8) . ? P1 F1 1.481(11) . ? P1 F3 1.498(8) . ? P1 F2 1.524(8) . ? 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 C28 O1 C31 118.9(8) . . ? C33 O2 C32 112.2(7) . . ? C35 O3 C34 112.7(7) . . ? C37 O4 C36 119.1(8) . . ? C41 O5 C43 121.2(10) . . ? C45 O6 C44 115.5(11) . . ? C46 O7 C47 113.3(10) . . ? C26 O8 C48 118.6(9) . . ? C56 O9 C55 108.9(10) . . ? C49 O10 C50 114.1(9) . . ? C42 C41 C40 122.4(12) . . ? C42 C41 O5 112.6(12) . . ? C40 C41 O5 124.8(13) . . ? C29 C30 C25 122.0(10) . . ? C29 C30 C49 117.8(11) . . ? C25 C30 C49 120.0(11) . . ? O10 C50 C51 110.0(10) . . ? O10 C50 H50A 109.7 . . ? C51 C50 H50A 109.6 . . ? O10 C50 H50B 109.7 . . ? C51 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? C38 C39 C40 120.3(12) . . ? C38 C39 C56 122.0(14) . . ? C40 C39 C56 117.8(14) . . ? C42 C37 O4 122.7(11) . . ? C42 C37 C38 120.7(11) . . ? O4 C37 C38 116.6(11) . . ? O3 C35 C36 108.2(8) . . ? O3 C35 H35A 110.1 . . ? C36 C35 H35A 110.1 . . ? O3 C35 H35B 110.1 . . ? C36 C35 H35B 110.1 . . ? H35A C35 H35B 108.4 . . ? O4 C36 C35 108.5(8) . . ? O4 C36 H36A 110.0 . . ? C35 C36 H36A 110.0 . . ? O4 C36 H36B 110.0 . . ? C35 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? O1 C28 C27 116.4(10) . . ? O1 C28 C29 123.2(11) . . ? C27 C28 C29 120.4(10) . . ? C41 C42 C37 117.2(11) . . ? C41 C42 H42 121.4 . . ? C37 C42 H42 121.4 . . ? C28 C27 C26 119.5(10) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C30 C29 C28 117.9(10) . . ? C30 C29 H29 121.1 . . ? C28 C29 H29 121.1 . . ? O2 C33 C34 109.6(8) . . ? O2 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? O2 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C26 C25 C30 118.5(10) . . ? C26 C25 H25 120.8 . . ? C30 C25 H25 120.8 . . ? O1 C31 C32 107.2(8) . . ? O1 C31 H31A 110.3 . . ? C32 C31 H31A 110.3 . . ? O1 C31 H31B 110.3 . . ? C32 C31 H31B 110.3 . . ? H31A C31 H31B 108.5 . . ? O9 C56 C39 108.1(9) . . ? O9 C56 H56A 110.1 . . ? C39 C56 H56A 110.1 . . ? O9 C56 H56B 110.1 . . ? C39 C56 H56B 110.1 . . ? H56A C56 H56B 108.4 . . ? C39 C38 C37 120.9(12) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C41 C40 C39 118.6(12) . . ? C41 C40 H40 120.7 . . ? C39 C40 H40 120.7 . . ? C50 C51 C52 116.4(13) . . ? C50 C51 H51A 108.2 . . ? C52 C51 H51A 108.2 . . ? C50 C51 H51B 108.2 . . ? C52 C51 H51B 108.2 . . ? H51A C51 H51B 107.3 . . ? O6 C45 C46 112.1(11) . . ? O6 C45 H45A 109.2 . . ? C46 C45 H45A 109.2 . . ? O6 C45 H45B 109.2 . . ? C46 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? O8 C26 C25 124.7(10) . . ? O8 C26 C27 113.7(10) . . ? C25 C26 C27 121.5(11) . . ? O7 C47 C48 112.8(11) . . ? O7 C47 H47A 109.0 . . ? C48 C47 H47A 109.0 . . ? O7 C47 H47B 109.0 . . ? C48 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? O3 C34 C33 111.9(8) . . ? O3 C34 H34A 109.2 . . ? C33 C34 H34A 109.2 . . ? O3 C34 H34B 109.2 . . ? C33 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? O10 C49 C30 109.4(8) . . ? O10 C49 H49A 109.8 . . ? C30 C49 H49A 109.8 . . ? O10 C49 H49B 109.8 . . ? C30 C49 H49B 109.8 . . ? H49A C49 H49B 108.2 . . ? O8 C48 C47 107.8(9) . . ? O8 C48 H48A 110.1 . . ? C47 C48 H48A 110.1 . . ? O8 C48 H48B 110.1 . . ? C47 C48 H48B 110.1 . . ? H48A C48 H48B 108.5 . . ? C44 C43 O5 111.2(10) . . ? C44 C43 H43A 109.4 . . ? O5 C43 H43A 109.4 . . ? C44 C43 H43B 109.4 . . ? O5 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? O9 C55 C54 111.3(14) . . ? O9 C55 H55A 109.4 . . ? C54 C55 H55A 109.3 . . ? O9 C55 H55B 109.4 . . ? C54 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? O2 C32 C31 108.9(8) . . ? O2 C32 H32A 109.9 . . ? C31 C32 H32A 109.9 . . ? O2 C32 H32B 109.9 . . ? C31 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? O7 C46 C45 110.2(11) . . ? O7 C46 H46A 109.6 . . ? C45 C46 H46A 109.6 . . ? O7 C46 H46B 109.6 . . ? C45 C46 H46B 109.6 . . ? H46A C46 H46B 108.1 . . ? C54 C53 C52 126(2) . . ? C54 C53 H53A 105.9 . . ? C52 C53 H53A 105.9 . . ? C54 C53 H53B 106.0 . . ? C52 C53 H53B 105.9 . . ? H53A C53 H53B 106.2 . . ? C53 C52 C51 113.8(16) . . ? C53 C52 H52A 108.8 . . ? C51 C52 H52A 108.8 . . ? C53 C52 H52B 108.9 . . ? C51 C52 H52B 108.8 . . ? H52A C52 H52B 107.7 . . ? O6 C44 C43 111.3(11) . . ? O6 C44 H44A 109.4 . . ? C43 C44 H44A 109.4 . . ? O6 C44 H44B 109.4 . . ? C43 C44 H44B 109.4 . . ? H44A C44 H44B 108.0 . . ? C16 N1 C15 119.3(10) . . ? C16 N1 C18 121.0(11) . . ? C15 N1 C18 119.4(10) . . ? C12 N2 C8 120.0(9) . . ? C12 N2 C7 121.1(10) . . ? C8 N2 C7 118.9(9) . . ? C2 C1 C6 121.1(15) . . ? C2 C1 H1 119.5 . . ? C6 C1 H1 119.5 . . ? C1 C2 C3 121.5(14) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 117.7(12) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.2 . . ? C5 C4 C3 119.5(11) . . ? C5 C4 C7 119.3(11) . . ? C3 C4 C7 121.2(12) . . ? C4 C5 C6 120.9(12) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 119.3(14) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? N2 C7 C4 108.7(8) . . ? N2 C7 H7A 110.0 . . ? C4 C7 H7A 110.0 . . ? N2 C7 H7B 110.0 . . ? C4 C7 H7B 110.0 . . ? H7A C7 H7B 108.3 . . ? C9 C8 N2 121.5(10) . . ? C9 C8 H8 119.2 . . ? N2 C8 H8 119.3 . . ? C8 C9 C10 119.2(10) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 118.9(10) . . ? C11 C10 C13 121.5(10) . . ? C9 C10 C13 119.6(10) . . ? C10 C11 C12 120.8(10) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? N2 C12 C11 119.6(10) . . ? N2 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C17 116.3(10) . . ? C14 C13 C10 121.7(10) . . ? C17 C13 C10 122.0(10) . . ? C15 C14 C13 121.2(10) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? N1 C15 C14 120.6(10) . . ? N1 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? N1 C16 C17 122.0(11) . . ? N1 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C13 120.5(10) . . ? C16 C17 H17 119.8 . . ? C13 C17 H17 119.8 . . ? N1 C18 C19 107.7(8) . . ? N1 C18 H18A 110.2 . . ? C19 C18 H18A 110.2 . . ? N1 C18 H18B 110.2 . . ? C19 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C24 C19 C20 118.5(11) . . ? C24 C19 C18 120.4(13) . . ? C20 C19 C18 121.0(12) . . ? C21 C20 C19 120.4(13) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 121.5(15) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 119.4(14) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C24 120.7(14) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.7 . . ? C19 C24 C23 119.5(13) . . ? C19 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C53 C54 C55 116(2) . . ? C53 C54 H54A 108.4 . . ? C55 C54 H54A 108.2 . . ? C53 C54 H54B 108.1 . . ? C55 C54 H54B 108.1 . . ? H54A C54 H54B 107.3 . . ? F10 P2 F9 90.9(8) . . ? F10 P2 F11 93.5(8) . . ? F9 P2 F11 174.9(8) . . ? F10 P2 F8 179.3(9) . . ? F9 P2 F8 89.7(9) . . ? F11 P2 F8 86.0(7) . . ? F10 P2 F7 91.2(5) . . ? F9 P2 F7 84.6(7) . . ? F11 P2 F7 98.0(7) . . ? F8 P2 F7 88.5(5) . . ? F10 P2 F12 91.9(6) . . ? F9 P2 F12 92.5(7) . . ? F11 P2 F12 84.7(6) . . ? F8 P2 F12 88.5(5) . . ? F7 P2 F12 175.8(7) . . ? F6 P1 F5 88.0(8) . . ? F6 P1 F4 83.2(8) . . ? F5 P1 F4 94.6(6) . . ? F6 P1 F1 177.8(9) . . ? F5 P1 F1 93.3(8) . . ? F4 P1 F1 98.5(9) . . ? F6 P1 F3 90.6(7) . . ? F5 P1 F3 178.5(9) . . ? F4 P1 F3 85.9(6) . . ? F1 P1 F3 88.0(8) . . ? F6 P1 F2 93.6(8) . . ? F5 P1 F2 88.4(6) . . ? F4 P1 F2 175.5(8) . . ? F1 P1 F2 84.7(7) . . ? F3 P1 F2 91.1(6) . . ? 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 C43 O5 C41 C42 -159.8(9) . . . . ? C43 O5 C41 C40 23.6(15) . . . . ? C49 O10 C50 C51 -165.4(11) . . . . ? C36 O4 C37 C42 0.0(12) . . . . ? C36 O4 C37 C38 177.7(8) . . . . ? C34 O3 C35 C36 -171.1(8) . . . . ? C37 O4 C36 C35 -164.6(7) . . . . ? O3 C35 C36 O4 78.2(9) . . . . ? C31 O1 C28 C27 172.5(8) . . . . ? C31 O1 C28 C29 -7.5(13) . . . . ? C40 C41 C42 C37 0.5(15) . . . . ? O5 C41 C42 C37 -176.3(8) . . . . ? O4 C37 C42 C41 175.8(8) . . . . ? C38 C37 C42 C41 -1.8(14) . . . . ? O1 C28 C27 C26 -176.1(8) . . . . ? C29 C28 C27 C26 4.0(14) . . . . ? C25 C30 C29 C28 -2.0(15) . . . . ? C49 C30 C29 C28 -177.2(9) . . . . ? O1 C28 C29 C30 178.0(9) . . . . ? C27 C28 C29 C30 -2.0(14) . . . . ? C32 O2 C33 C34 -167.0(8) . . . . ? C29 C30 C25 C26 3.9(15) . . . . ? C49 C30 C25 C26 179.0(9) . . . . ? C28 O1 C31 C32 -170.6(8) . . . . ? C55 O9 C56 C39 -169.2(11) . . . . ? C38 C39 C56 O9 -105.1(13) . . . . ? C40 C39 C56 O9 72.7(13) . . . . ? C40 C39 C38 C37 0.0(16) . . . . ? C56 C39 C38 C37 177.7(9) . . . . ? C42 C37 C38 C39 1.7(15) . . . . ? O4 C37 C38 C39 -176.1(8) . . . . ? C42 C41 C40 C39 1.1(16) . . . . ? O5 C41 C40 C39 177.5(10) . . . . ? C38 C39 C40 C41 -1.3(16) . . . . ? C56 C39 C40 C41 -179.2(9) . . . . ? O10 C50 C51 C52 64.7(16) . . . . ? C44 O6 C45 C46 174.5(10) . . . . ? C48 O8 C26 C25 2.0(15) . . . . ? C48 O8 C26 C27 -176.8(9) . . . . ? C30 C25 C26 O8 179.4(9) . . . . ? C30 C25 C26 C27 -1.9(15) . . . . ? C28 C27 C26 O8 176.8(8) . . . . ? C28 C27 C26 C25 -2.0(15) . . . . ? C46 O7 C47 C48 -103.2(13) . . . . ? C35 O3 C34 C33 -172.6(8) . . . . ? O2 C33 C34 O3 -57.4(11) . . . . ? C50 O10 C49 C30 171.8(10) . . . . ? C29 C30 C49 O10 90.2(11) . . . . ? C25 C30 C49 O10 -85.2(12) . . . . ? C26 O8 C48 C47 178.0(9) . . . . ? O7 C47 C48 O8 -68.9(13) . . . . ? C41 O5 C43 C44 -123.9(12) . . . . ? C56 O9 C55 C54 -174.0(14) . . . . ? C33 O2 C32 C31 -174.2(8) . . . . ? O1 C31 C32 O2 71.6(10) . . . . ? C47 O7 C46 C45 -157.2(11) . . . . ? O6 C45 C46 O7 -72.0(15) . . . . ? C54 C53 C52 C51 -172(2) . . . . ? C50 C51 C52 C53 -88(2) . . . . ? C45 O6 C44 C43 164.2(11) . . . . ? O5 C43 C44 O6 68.0(14) . . . . ? C6 C1 C2 C3 -2(2) . . . . ? C1 C2 C3 C4 2.9(19) . . . . ? C2 C3 C4 C5 -3.6(16) . . . . ? C2 C3 C4 C7 177.7(10) . . . . ? C3 C4 C5 C6 3.2(18) . . . . ? C7 C4 C5 C6 -178.0(11) . . . . ? C2 C1 C6 C5 1(2) . . . . ? C4 C5 C6 C1 -2(2) . . . . ? C12 N2 C7 C4 -118.5(10) . . . . ? C8 N2 C7 C4 60.0(12) . . . . ? C5 C4 C7 N2 65.2(13) . . . . ? C3 C4 C7 N2 -116.1(10) . . . . ? C12 N2 C8 C9 -0.4(14) . . . . ? C7 N2 C8 C9 -179.0(9) . . . . ? N2 C8 C9 C10 0.2(14) . . . . ? C8 C9 C10 C11 -0.1(13) . . . . ? C8 C9 C10 C13 178.9(8) . . . . ? C9 C10 C11 C12 0.2(13) . . . . ? C13 C10 C11 C12 -178.8(9) . . . . ? C8 N2 C12 C11 0.5(14) . . . . ? C7 N2 C12 C11 179.0(9) . . . . ? C10 C11 C12 N2 -0.4(14) . . . . ? C11 C10 C13 C14 -155.7(9) . . . . ? C9 C10 C13 C14 25.2(13) . . . . ? C11 C10 C13 C17 26.8(13) . . . . ? C9 C10 C13 C17 -152.2(9) . . . . ? C17 C13 C14 C15 0.5(14) . . . . ? C10 C13 C14 C15 -177.1(8) . . . . ? C16 N1 C15 C14 -3.5(15) . . . . ? C18 N1 C15 C14 169.5(9) . . . . ? C13 C14 C15 N1 1.0(15) . . . . ? C15 N1 C16 C17 4.4(16) . . . . ? C18 N1 C16 C17 -168.5(10) . . . . ? N1 C16 C17 C13 -2.8(17) . . . . ? C14 C13 C17 C16 0.3(14) . . . . ? C10 C13 C17 C16 177.9(9) . . . . ? C16 N1 C18 C19 85.2(12) . . . . ? C15 N1 C18 C19 -87.6(12) . . . . ? N1 C18 C19 C24 95.5(12) . . . . ? N1 C18 C19 C20 -80.6(13) . . . . ? C24 C19 C20 C21 -1.7(17) . . . . ? C18 C19 C20 C21 174.5(11) . . . . ? C19 C20 C21 C22 1(2) . . . . ? C20 C21 C22 C23 -1(2) . . . . ? C21 C22 C23 C24 2(2) . . . . ? C20 C19 C24 C23 2.2(16) . . . . ? C18 C19 C24 C23 -174.0(11) . . . . ? C22 C23 C24 C19 -2.4(19) . . . . ? C52 C53 C54 C55 135(2) . . . . ? O9 C55 C54 C53 80(3) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.486 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.058 # Attachment '[2]rotaxane.cif' data_x _database_code_depnum_ccdc_archive 'CCDC 788122' #TrackingRef '[2]rotaxane.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H94 F12 N2 O11 P2 ' _chemical_formula_weight 1453.43 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' F F 0.0171 0.0103 '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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.677(3) _cell_length_b 17.347(4) _cell_length_c 34.994(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.807(7) _cell_angle_gamma 90.00 _cell_volume 7948(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 0.137 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.944 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19257 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.1158 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.20 _reflns_number_total 14336 _reflns_number_gt 4164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14336 _refine_ls_number_parameters 904 _refine_ls_number_restraints 384 _refine_ls_R_factor_all 0.2465 _refine_ls_R_factor_gt 0.1151 _refine_ls_wR_factor_ref 0.4038 _refine_ls_wR_factor_gt 0.3135 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 N1 N 0.37718(17) 0.60216(13) 0.97308(6) 0.0606(8) Uani 1 1 d . . . N2 N 0.29027(16) 0.70638(13) 0.77447(7) 0.0628(9) Uani 1 1 d . . . C33 C 0.1968(3) 0.7122(3) 1.11947(12) 0.151(2) Uani 1 1 d U . . H33A H 0.2091 0.6578 1.1186 0.227 Uiso 1 1 calc R . . H33B H 0.1401 0.7208 1.1299 0.227 Uiso 1 1 calc R . . H33C H 0.2565 0.7370 1.1363 0.227 Uiso 1 1 calc R . . C34 C 0.1414(3) 0.8284(3) 1.08039(16) 0.163(2) Uani 1 1 d U . . H34A H 0.0795 0.8302 1.0880 0.244 Uiso 1 1 calc R . . H34B H 0.1306 0.8528 1.0549 0.244 Uiso 1 1 calc R . . H34C H 0.1945 0.8550 1.1000 0.244 Uiso 1 1 calc R . . C35 C 0.1727(2) 0.7452(2) 1.07776(10) 0.0918(11) Uani 1 1 d U . . C36 C 0.0845(3) 0.7017(3) 1.05260(12) 0.1270(17) Uani 1 1 d U . . H36A H 0.1028 0.6484 1.0518 0.190 Uiso 1 1 calc R . . H36B H 0.0653 0.7224 1.0260 0.190 Uiso 1 1 calc R . . H36C H 0.0281 0.7060 1.0636 0.190 Uiso 1 1 calc R . . C37 C 0.2685(2) 0.73756(18) 1.06463(9) 0.0741(9) Uani 1 1 d U . . C38 C 0.3404(2) 0.79574(19) 1.06992(9) 0.0806(10) Uani 1 1 d U . . H38 H 0.3283 0.8417 1.0814 0.097 Uiso 1 1 calc R . . C39 C 0.4291(2) 0.78902(19) 1.05899(10) 0.0798(10) Uani 1 1 d U . . C40 C 0.4484(2) 0.72108(18) 1.04264(9) 0.0733(10) Uani 1 1 d U . . H40 H 0.5086 0.7151 1.0357 0.088 Uiso 1 1 calc R . . C41 C 0.3785(2) 0.66126(17) 1.03645(9) 0.0698(9) Uani 1 1 d U . . C42 C 0.2897(2) 0.66954(18) 1.04771(9) 0.0707(10) Uani 1 1 d U . . H42 H 0.2437 0.6288 1.0439 0.085 Uiso 1 1 calc R . . C43 C 0.4777(5) 0.9177(3) 1.08906(19) 0.232(3) Uani 1 1 d U . . H43A H 0.4481 0.9596 1.0716 0.348 Uiso 1 1 calc R . . H43B H 0.5380 0.9354 1.1088 0.348 Uiso 1 1 calc R . . H43C H 0.4292 0.8992 1.1020 0.348 Uiso 1 1 calc R . . C44 C 0.5933(4) 0.8349(4) 1.10217(19) 0.244(3) Uani 1 1 d U . . H44A H 0.6148 0.8801 1.1182 0.366 Uiso 1 1 calc R . . H44B H 0.6491 0.8154 1.0935 0.366 Uiso 1 1 calc R . . H44C H 0.5718 0.7962 1.1176 0.366 Uiso 1 1 calc R . . C45 C 0.5544(4) 0.8669(3) 1.03633(16) 0.222(3) Uani 1 1 d U . . H45A H 0.5888 0.9157 1.0405 0.333 Uiso 1 1 calc R . . H45B H 0.5051 0.8662 1.0105 0.333 Uiso 1 1 calc R . . H45C H 0.6033 0.8265 1.0379 0.333 Uiso 1 1 calc R . . C46 C 0.5046(3) 0.8554(2) 1.06587(12) 0.1207(13) Uani 1 1 d U . . C47 C 0.3991(3) 0.58890(17) 1.01704(9) 0.0768(11) Uani 1 1 d U . . H47A H 0.3562 0.5476 1.0218 0.092 Uiso 1 1 calc R . . H47B H 0.4699 0.5738 1.0283 0.092 Uiso 1 1 calc R . . C48 C 0.4536(2) 0.60500(17) 0.95718(9) 0.0686(10) Uani 1 1 d U . . H48 H 0.5196 0.5957 0.9733 0.082 Uiso 1 1 calc R . . C49 C 0.4384(2) 0.62113(17) 0.91786(8) 0.0633(9) Uani 1 1 d U . . H49 H 0.4930 0.6205 0.9070 0.076 Uiso 1 1 calc R . . C50 C 0.3406(2) 0.63850(16) 0.89400(8) 0.0574(8) Uani 1 1 d U . . C51 C 0.2626(2) 0.63213(18) 0.91121(9) 0.0712(10) Uani 1 1 d U . . H51 H 0.1955 0.6402 0.8958 0.085 Uiso 1 1 calc R . . C52 C 0.2824(2) 0.61413(18) 0.95054(9) 0.0703(11) Uani 1 1 d U . . H52 H 0.2287 0.6102 0.9618 0.084 Uiso 1 1 calc R . . C53 C 0.3234(2) 0.66238(15) 0.85301(8) 0.0551(8) Uani 1 1 d U . . C54 C 0.2517(2) 0.71877(16) 0.83538(9) 0.0633(9) Uani 1 1 d U . . H54 H 0.2143 0.7426 0.8504 0.076 Uiso 1 1 calc R . . C55 C 0.2358(2) 0.73943(16) 0.79632(9) 0.0646(10) Uani 1 1 d U . . H55 H 0.1870 0.7765 0.7849 0.078 Uiso 1 1 calc R . . C56 C 0.3614(2) 0.65227(17) 0.79060(9) 0.0675(10) Uani 1 1 d U . . H56 H 0.3992 0.6306 0.7751 0.081 Uiso 1 1 calc R . . C57 C 0.3786(2) 0.62912(16) 0.82888(9) 0.0610(9) Uani 1 1 d U . . H57 H 0.4270 0.5912 0.8393 0.073 Uiso 1 1 calc R . . C58 C 0.2709(2) 0.72528(17) 0.73178(8) 0.0716(10) Uani 1 1 d U . . H58A H 0.3353 0.7287 0.7254 0.086 Uiso 1 1 calc R . . H58B H 0.2370 0.7749 0.7262 0.086 Uiso 1 1 calc R . . C59 C 0.2051(2) 0.66429(17) 0.70648(9) 0.0647(9) Uani 1 1 d U . . C60 C 0.1009(2) 0.67114(18) 0.69296(9) 0.0682(9) Uani 1 1 d U . . H60 H 0.0706 0.7148 0.7000 0.082 Uiso 1 1 calc R . . C61 C 0.0398(2) 0.61692(19) 0.66973(9) 0.0786(10) Uani 1 1 d U . . C62 C 0.0885(2) 0.54940(19) 0.66260(9) 0.0841(11) Uani 1 1 d U . . H62 H 0.0486 0.5101 0.6479 0.101 Uiso 1 1 calc R . . C63 C 0.1906(3) 0.53886(19) 0.67608(10) 0.0840(10) Uani 1 1 d U . . C64 C 0.2481(2) 0.59877(17) 0.69672(9) 0.0746(10) Uani 1 1 d U . . H64 H 0.3189 0.5945 0.7043 0.089 Uiso 1 1 calc R . . C65 C 0.2440(3) 0.4666(2) 0.66843(12) 0.1155(13) Uani 1 1 d U . . C66 C 0.3044(4) 0.4310(2) 0.70933(13) 0.150(2) Uani 1 1 d U . . H66A H 0.2618 0.4304 0.7269 0.225 Uiso 1 1 calc R . . H66B H 0.3642 0.4615 0.7210 0.225 Uiso 1 1 calc R . . H66C H 0.3243 0.3793 0.7053 0.225 Uiso 1 1 calc R . . C67 C 0.3113(3) 0.4832(3) 0.64134(13) 0.1530(19) Uani 1 1 d U . . H67A H 0.3754 0.5042 0.6569 0.230 Uiso 1 1 calc R . . H67B H 0.2777 0.5196 0.6212 0.230 Uiso 1 1 calc R . . H67C H 0.3233 0.4362 0.6289 0.230 Uiso 1 1 calc R . . C68 C 0.1680(4) 0.4072(3) 0.64769(17) 0.187(3) Uani 1 1 d U . . H68A H 0.1332 0.4246 0.6212 0.281 Uiso 1 1 calc R . . H68B H 0.1193 0.3993 0.6623 0.281 Uiso 1 1 calc R . . H68C H 0.2027 0.3597 0.6463 0.281 Uiso 1 1 calc R . . C69 C -0.1296(3) 0.5972(3) 0.68030(14) 0.159(2) Uani 1 1 d U . . H69A H -0.1985 0.6162 0.6729 0.239 Uiso 1 1 calc R . . H69B H -0.0949 0.6135 0.7070 0.239 Uiso 1 1 calc R . . H69C H -0.1304 0.5420 0.6791 0.239 Uiso 1 1 calc R . . C70 C -0.1050(3) 0.7094(3) 0.64520(16) 0.164(2) Uani 1 1 d U . . H70A H -0.0652 0.7326 0.6297 0.246 Uiso 1 1 calc R . . H70B H -0.0926 0.7360 0.6702 0.246 Uiso 1 1 calc R . . H70C H -0.1762 0.7128 0.6308 0.246 Uiso 1 1 calc R . . C71 C -0.1123(4) 0.5866(4) 0.61142(15) 0.197(3) Uani 1 1 d U . . H71A H -0.0726 0.6045 0.5946 0.295 Uiso 1 1 calc R . . H71B H -0.1831 0.5979 0.5991 0.295 Uiso 1 1 calc R . . H71C H -0.1034 0.5320 0.6152 0.295 Uiso 1 1 calc R . . C72 C -0.0759(3) 0.6280(2) 0.65258(11) 0.0970(12) Uani 1 1 d U . . O1 O 0.01233(15) 0.65918(12) 0.78718(6) 0.0795(8) Uani 1 1 d . . . O2 O 0.00923(17) 0.81550(13) 0.77087(8) 0.1085(10) Uani 1 1 d . . . O3 O 0.1593(2) 0.90042(15) 0.74426(12) 0.1974(15) Uani 1 1 d . . . O4 O 0.3751(2) 0.89265(15) 0.77876(8) 0.1185(11) Uani 1 1 d . . . O5 O 0.58398(18) 0.73617(14) 0.88202(8) 0.1070(10) Uani 1 1 d . . . O6 O 0.61105(16) 0.57677(13) 0.86236(8) 0.1111(10) Uani 1 1 d . . . O7 O 0.47636(15) 0.45526(12) 0.86228(7) 0.0915(9) Uani 1 1 d . . . O8 O 0.25643(15) 0.46786(12) 0.82537(7) 0.0841(8) Uani 1 1 d . . . O9 O -0.09709(15) 0.51151(15) 0.89689(7) 0.1010(9) Uani 1 1 d . . . O10 O 0.2615(2) 0.84638(17) 0.91389(9) 0.1527(13) Uani 1 1 d . . . C1 C 0.1293(2) 0.55781(16) 0.80696(9) 0.0622(9) Uani 1 1 d U . . H1 H 0.1591 0.5736 0.7875 0.075 Uiso 1 1 calc R . . C2 C 0.0441(2) 0.59572(17) 0.81187(9) 0.0651(9) Uani 1 1 d U . . C3 C -0.0026(2) 0.57026(18) 0.83931(10) 0.0733(10) Uani 1 1 d U . . H3 H -0.0589 0.5960 0.8429 0.088 Uiso 1 1 calc R . . C4 C 0.0361(2) 0.50565(19) 0.86140(10) 0.0776(10) Uani 1 1 d U . . C5 C 0.1225(2) 0.46875(18) 0.85792(9) 0.0726(10) Uani 1 1 d U . . H5 H 0.1487 0.4258 0.8734 0.087 Uiso 1 1 calc R . . C6 C 0.1682(2) 0.49701(17) 0.83128(10) 0.0657(9) Uani 1 1 d U . . C7 C 0.3107(2) 0.40808(19) 0.85365(12) 0.1012(13) Uani 1 1 d U . . H7A H 0.3212 0.4253 0.8809 0.121 Uiso 1 1 calc R . . H7B H 0.2710 0.3609 0.8497 0.121 Uiso 1 1 calc R . . C8 C 0.4091(3) 0.39470(19) 0.84596(12) 0.1043(14) Uani 1 1 d U . . H8A H 0.4378 0.3462 0.8579 0.125 Uiso 1 1 calc R . . H8B H 0.3994 0.3917 0.8174 0.125 Uiso 1 1 calc R . . C9 C 0.5693(2) 0.4453(2) 0.85406(13) 0.1078(14) Uani 1 1 d U . . H9A H 0.5589 0.4485 0.8255 0.129 Uiso 1 1 calc R . . H9B H 0.5965 0.3946 0.8629 0.129 Uiso 1 1 calc R . . C10 C 0.6415(3) 0.5036(2) 0.87405(13) 0.1146(14) Uani 1 1 d U . . H10A H 0.6523 0.4992 0.9026 0.138 Uiso 1 1 calc R . . H10B H 0.7064 0.4939 0.8689 0.138 Uiso 1 1 calc R . . C11 C 0.6855(3) 0.6348(2) 0.86988(13) 0.1144(14) Uani 1 1 d U . . H11A H 0.7363 0.6227 0.8564 0.137 Uiso 1 1 calc R . . H11B H 0.7194 0.6378 0.8983 0.137 Uiso 1 1 calc R . . C12 C 0.6383(3) 0.7080(2) 0.85581(12) 0.1106(14) Uani 1 1 d U . . H12A H 0.6904 0.7449 0.8543 0.133 Uiso 1 1 calc R . . H12B H 0.5917 0.7018 0.8292 0.133 Uiso 1 1 calc R . . C13 C 0.5120(3) 0.79414(19) 0.86910(12) 0.0938(11) Uani 1 1 d U . . C14 C 0.4667(3) 0.82033(19) 0.89608(12) 0.0994(12) Uani 1 1 d U . . H14 H 0.4866 0.8018 0.9221 0.119 Uiso 1 1 calc R . . C15 C 0.3898(3) 0.8754(2) 0.88451(12) 0.1033(11) Uani 1 1 d U . . C16 C 0.3576(3) 0.90151(19) 0.84633(11) 0.0970(12) Uani 1 1 d U . . H16 H 0.3046 0.9370 0.8385 0.116 Uiso 1 1 calc R . . C17 C 0.4044(3) 0.87462(19) 0.82003(12) 0.0922(12) Uani 1 1 d U . . C18 C 0.4827(2) 0.82069(18) 0.82973(12) 0.0880(11) Uani 1 1 d U . . H18 H 0.5139 0.8032 0.8110 0.106 Uiso 1 1 calc R . . C19 C 0.3199(3) 0.9626(2) 0.76466(13) 0.1289(15) Uani 1 1 d U . . H19A H 0.3620 0.9972 0.7544 0.155 Uiso 1 1 calc R . . H19B H 0.3027 0.9882 0.7865 0.155 Uiso 1 1 calc R . . C20 C 0.2277(3) 0.9442(2) 0.73347(14) 0.1352(16) Uani 1 1 d U . . H20A H 0.1947 0.9921 0.7225 0.162 Uiso 1 1 calc R . . H20B H 0.2468 0.9178 0.7122 0.162 Uiso 1 1 calc R . . C21 C 0.0767(3) 0.9203(2) 0.74556(15) 0.1574(17) Uani 1 1 d U . . H21A H 0.0524 0.9529 0.7222 0.189 Uiso 1 1 calc R . . H21B H 0.0916 0.9553 0.7681 0.189 Uiso 1 1 calc R . . C22 C -0.0098(3) 0.8830(2) 0.74776(14) 0.1396(16) Uani 1 1 d U . . H22A H -0.0507 0.8699 0.7209 0.168 Uiso 1 1 calc R . . H22B H -0.0496 0.9180 0.7590 0.168 Uiso 1 1 calc R . . C23 C -0.0774(3) 0.7730(2) 0.76881(12) 0.1031(13) Uani 1 1 d U . . H23A H -0.1050 0.7534 0.7419 0.124 Uiso 1 1 calc R . . H23B H -0.1283 0.8065 0.7744 0.124 Uiso 1 1 calc R . . C24 C -0.0591(2) 0.7097(2) 0.79603(11) 0.0982(13) Uani 1 1 d U . . H24A H -0.0328 0.7284 0.8232 0.118 Uiso 1 1 calc R . . H24B H -0.1225 0.6825 0.7937 0.118 Uiso 1 1 calc R . . C25 C -0.0217(3) 0.4699(2) 0.88760(11) 0.1089(14) Uani 1 1 d U . . H25A H -0.0524 0.4226 0.8748 0.131 Uiso 1 1 calc R . . H25B H 0.0278 0.4554 0.9125 0.131 Uiso 1 1 calc R . . C26 C -0.0708(3) 0.5467(3) 0.93433(12) 0.1204(15) Uani 1 1 d U . . H26A H -0.0300 0.5109 0.9538 0.144 Uiso 1 1 calc R . . H26B H -0.1327 0.5571 0.9416 0.144 Uiso 1 1 calc R . . C27 C -0.0132(3) 0.6194(3) 0.93654(12) 0.1132(13) Uani 1 1 d U . . C28 C 0.0283(3) 0.6782(3) 0.93653(12) 0.1104(12) Uani 1 1 d U . . C29 C 0.0794(3) 0.7430(3) 0.93691(12) 0.1188(13) Uani 1 1 d U . . C30 C 0.1326(3) 0.7981(3) 0.93823(14) 0.1315(14) Uani 1 1 d U . . C31 C 0.2047(4) 0.8621(3) 0.93966(14) 0.1526(18) Uani 1 1 d U . . H31A H 0.1673 0.9099 0.9320 0.183 Uiso 1 1 calc R . . H31B H 0.2495 0.8680 0.9666 0.183 Uiso 1 1 calc R . . C32 C 0.3357(3) 0.9010(2) 0.91428(13) 0.1236(16) Uani 1 1 d U . . H32A H 0.3837 0.9047 0.9407 0.148 Uiso 1 1 calc R . . H32B H 0.3045 0.9512 0.9069 0.148 Uiso 1 1 calc R . . P1 P 0.24743(7) 0.38079(6) 0.98419(3) 0.0904(4) Uani 1 1 d . . . F1 F 0.33058(17) 0.42559(13) 0.96866(6) 0.1239(9) Uani 1 1 d . . . F2 F 0.1932(2) 0.35037(15) 0.94153(7) 0.1472(12) Uani 1 1 d . . . F3 F 0.18124(19) 0.45488(15) 0.97644(10) 0.1738(14) Uani 1 1 d . . . F4 F 0.16930(18) 0.33963(17) 1.00157(8) 0.1655(12) Uani 1 1 d . . . F5 F 0.30440(17) 0.41369(14) 1.02730(6) 0.1226(9) Uani 1 1 d . . . F6 F 0.32158(19) 0.30988(13) 0.99324(8) 0.1420(11) Uani 1 1 d . . . P2 P 0.59784(8) 0.69066(6) 0.72977(4) 0.1075(4) Uani 1 1 d . . . F7 F 0.6616(3) 0.7505(2) 0.71778(14) 0.275(2) Uani 1 1 d . . . F8 F 0.5098(3) 0.7166(2) 0.69283(11) 0.2257(19) Uani 1 1 d . . . F9 F 0.5443(3) 0.74254(19) 0.75187(11) 0.253(2) Uani 1 1 d . . . F10 F 0.6392(3) 0.6340(2) 0.70849(11) 0.3017(18) Uani 1 1 d . . . F11 F 0.6821(2) 0.6660(3) 0.76380(10) 0.298(2) Uani 1 1 d . . . F12 F 0.5340(2) 0.62951(19) 0.74176(13) 0.2672(18) Uani 1 1 d . . . O1W O 0.7962(6) 0.9282(4) 0.98563(17) 0.529(4) Uani 1 1 d . . . H1W H 0.7437 0.8978 0.9709 0.793 Uiso 1 1 d R . . H2W H 0.8487 0.9029 0.9832 0.793 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 N1 0.0677(14) 0.0553(13) 0.0550(14) -0.0065(12) 0.0119(12) 0.0089(12) N2 0.0486(13) 0.0598(14) 0.0676(16) 0.0081(13) -0.0031(12) -0.0050(12) C33 0.142(3) 0.198(4) 0.135(3) -0.041(3) 0.073(2) -0.008(3) C34 0.127(3) 0.125(3) 0.257(4) -0.028(3) 0.087(3) 0.012(3) C35 0.0879(17) 0.092(2) 0.1083(19) -0.0200(17) 0.0491(15) -0.0067(17) C36 0.089(2) 0.155(3) 0.144(3) -0.037(3) 0.046(2) -0.034(2) C37 0.0731(15) 0.0707(15) 0.0784(16) -0.0107(14) 0.0216(13) -0.0093(14) C38 0.0794(17) 0.0782(17) 0.0819(18) -0.0217(16) 0.0198(15) -0.0095(16) C39 0.0769(15) 0.0848(17) 0.0766(16) -0.0142(15) 0.0206(14) -0.0174(15) C40 0.0688(16) 0.0815(18) 0.0633(17) -0.0064(15) 0.0093(14) -0.0015(15) C41 0.0809(16) 0.0650(15) 0.0568(15) -0.0001(13) 0.0095(14) 0.0010(14) C42 0.0758(16) 0.0637(16) 0.0674(17) -0.0052(14) 0.0125(15) -0.0057(15) C43 0.221(4) 0.192(4) 0.307(5) -0.133(4) 0.112(4) -0.094(4) C44 0.185(4) 0.247(5) 0.225(5) 0.027(4) -0.058(4) -0.137(3) C45 0.286(5) 0.191(4) 0.211(4) -0.051(4) 0.106(4) -0.140(3) C46 0.113(2) 0.131(2) 0.131(2) -0.046(2) 0.0562(18) -0.0573(19) C47 0.093(2) 0.0696(18) 0.0615(18) -0.0001(16) 0.0130(16) 0.0107(17) C48 0.0583(16) 0.0740(18) 0.0635(18) 0.0043(16) 0.0020(15) 0.0086(15) C49 0.0490(14) 0.0750(16) 0.0631(16) 0.0001(14) 0.0117(13) 0.0028(13) C50 0.0489(13) 0.0561(14) 0.0620(15) -0.0090(13) 0.0077(12) -0.0013(12) C51 0.0553(15) 0.0797(17) 0.0682(17) -0.0108(15) 0.0014(14) -0.0024(15) C52 0.0562(16) 0.0833(19) 0.0645(18) -0.0041(16) 0.0068(15) -0.0053(16) C53 0.0460(13) 0.0512(13) 0.0620(15) -0.0056(12) 0.0059(12) -0.0022(12) C54 0.0539(14) 0.0560(15) 0.0721(17) -0.0129(14) 0.0055(14) 0.0009(13) C55 0.0576(16) 0.0480(15) 0.0787(19) 0.0016(15) 0.0047(15) 0.0024(14) C56 0.0577(16) 0.0678(17) 0.0745(18) 0.0013(15) 0.0149(14) 0.0044(15) C57 0.0435(14) 0.0610(15) 0.0687(17) 0.0047(14) 0.0006(13) 0.0034(13) C58 0.0799(18) 0.0632(17) 0.0686(18) 0.0142(15) 0.0168(15) -0.0027(15) C59 0.0658(14) 0.0636(15) 0.0659(15) 0.0131(13) 0.0209(13) 0.0019(13) C60 0.0676(15) 0.0665(16) 0.0705(16) -0.0022(14) 0.0201(14) 0.0068(14) C61 0.0747(15) 0.0817(17) 0.0802(16) -0.0053(15) 0.0236(14) -0.0038(14) C62 0.0951(18) 0.0749(17) 0.0818(18) -0.0130(16) 0.0246(16) -0.0079(16) C63 0.0971(17) 0.0671(16) 0.0892(17) 0.0045(15) 0.0294(15) 0.0192(15) C64 0.0798(16) 0.0723(17) 0.0755(17) 0.0177(15) 0.0286(14) 0.0202(15) C65 0.142(2) 0.088(2) 0.117(2) -0.0001(19) 0.039(2) 0.029(2) C66 0.196(4) 0.100(3) 0.155(3) 0.032(3) 0.049(3) 0.069(3) C67 0.196(3) 0.121(3) 0.163(3) 0.005(3) 0.086(3) 0.062(3) C68 0.215(5) 0.107(3) 0.203(5) -0.034(3) 0.004(4) 0.038(3) C69 0.082(2) 0.195(4) 0.202(4) 0.050(3) 0.045(3) 0.006(3) C70 0.103(3) 0.159(4) 0.190(4) 0.025(4) -0.022(3) 0.017(3) C71 0.115(3) 0.259(5) 0.179(4) -0.076(4) -0.016(3) 0.019(4) C72 0.0657(17) 0.110(2) 0.109(2) -0.012(2) 0.0155(17) -0.0043(18) O1 0.0779(13) 0.0759(13) 0.0812(14) 0.0006(12) 0.0175(11) 0.0112(11) O2 0.0872(15) 0.0863(15) 0.147(2) 0.0368(15) 0.0263(15) 0.0237(13) O3 0.0853(17) 0.1134(16) 0.385(4) 0.1540(18) 0.055(2) 0.0219(15) O4 0.1152(19) 0.0917(17) 0.126(2) 0.0173(16) -0.0010(17) 0.0167(15) O5 0.0920(16) 0.0932(16) 0.1261(19) 0.0239(15) 0.0161(15) 0.0053(14) O6 0.0708(13) 0.0908(15) 0.170(2) 0.0525(15) 0.0314(14) 0.0158(12) O7 0.0627(12) 0.0772(14) 0.1275(18) -0.0123(14) 0.0164(13) 0.0071(11) O8 0.0722(12) 0.0650(12) 0.1091(16) 0.0067(12) 0.0165(12) 0.0036(11) O9 0.0679(12) 0.133(2) 0.1038(16) 0.0130(15) 0.0281(12) 0.0113(14) O10 0.175(2) 0.116(2) 0.197(2) -0.0528(19) 0.1011(18) -0.0438(18) C1 0.0501(14) 0.0571(15) 0.0728(17) -0.0013(14) 0.0073(13) -0.0082(13) C2 0.0527(15) 0.0627(16) 0.0725(17) -0.0044(14) 0.0063(14) -0.0110(13) C3 0.0540(15) 0.0709(17) 0.0897(18) -0.0049(16) 0.0123(15) -0.0061(14) C4 0.0697(15) 0.0749(16) 0.0857(17) 0.0069(15) 0.0182(14) -0.0112(14) C5 0.0599(15) 0.0663(16) 0.0831(18) 0.0013(15) 0.0070(15) -0.0099(14) C6 0.0521(14) 0.0575(15) 0.0803(17) -0.0078(14) 0.0077(14) -0.0057(13) C7 0.087(2) 0.0570(18) 0.152(3) 0.011(2) 0.022(2) -0.0026(17) C8 0.096(2) 0.0609(19) 0.147(3) 0.005(2) 0.021(2) 0.0159(18) C9 0.0640(18) 0.107(2) 0.148(3) 0.002(2) 0.0222(19) 0.0248(18) C10 0.0697(19) 0.114(2) 0.158(3) 0.015(2) 0.030(2) 0.0252(19) C11 0.0706(19) 0.106(2) 0.161(3) 0.032(2) 0.025(2) 0.001(2) C12 0.0741(19) 0.102(2) 0.156(3) 0.043(2) 0.0334(19) 0.0035(19) C13 0.0817(17) 0.0742(17) 0.119(2) -0.0007(17) 0.0193(17) -0.0291(16) C14 0.102(2) 0.0737(18) 0.114(2) -0.0170(17) 0.0181(18) -0.0274(17) C15 0.1059(18) 0.0729(17) 0.1212(19) -0.0245(17) 0.0170(17) -0.0206(16) C16 0.0908(19) 0.0646(17) 0.117(2) -0.0199(17) 0.0011(19) -0.0102(17) C17 0.0760(18) 0.0618(17) 0.122(2) -0.0116(17) 0.0011(18) -0.0171(16) C18 0.0714(17) 0.0636(17) 0.119(2) 0.0007(17) 0.0125(17) -0.0215(15) C19 0.120(2) 0.071(2) 0.180(3) 0.054(2) 0.019(2) 0.005(2) C20 0.110(3) 0.090(2) 0.185(3) 0.057(2) 0.009(3) 0.016(2) C21 0.149(3) 0.101(2) 0.216(3) 0.082(2) 0.043(3) 0.044(2) C22 0.124(3) 0.088(2) 0.201(3) 0.066(2) 0.038(3) 0.035(2) C23 0.0741(19) 0.099(2) 0.133(2) 0.014(2) 0.0249(19) 0.0293(18) C24 0.0789(19) 0.097(2) 0.119(2) 0.023(2) 0.0291(18) 0.0298(18) C25 0.100(2) 0.109(2) 0.118(2) 0.016(2) 0.032(2) -0.014(2) C26 0.114(2) 0.141(3) 0.105(2) 0.019(2) 0.030(2) 0.005(2) C27 0.100(2) 0.133(2) 0.105(2) 0.017(2) 0.0292(18) 0.005(2) C28 0.1017(19) 0.132(2) 0.107(2) 0.004(2) 0.0454(17) 0.002(2) C29 0.108(2) 0.141(2) 0.115(2) -0.008(2) 0.0432(18) 0.001(2) C30 0.124(2) 0.144(2) 0.134(2) -0.018(2) 0.0505(19) -0.004(2) C31 0.153(3) 0.157(3) 0.155(3) -0.036(3) 0.057(2) -0.001(3) C32 0.124(3) 0.086(2) 0.144(3) -0.024(2) 0.013(2) -0.020(2) P1 0.0781(6) 0.0938(7) 0.0936(7) 0.0025(6) 0.0159(5) -0.0008(5) F1 0.1395(16) 0.1248(16) 0.1120(15) 0.0120(13) 0.0435(12) -0.0270(14) F2 0.148(2) 0.163(2) 0.1000(17) -0.0323(16) -0.0125(16) -0.0253(18) F3 0.1329(18) 0.1259(18) 0.233(3) -0.005(2) 0.006(2) 0.0528(15) F4 0.1262(15) 0.205(3) 0.178(2) 0.0007(19) 0.0647(14) -0.0606(16) F5 0.1216(15) 0.1543(19) 0.0857(14) -0.0101(14) 0.0202(12) -0.0199(15) F6 0.1445(18) 0.0887(14) 0.185(2) 0.0162(15) 0.0345(17) 0.0249(14) P2 0.0998(6) 0.0914(7) 0.1442(8) 0.0132(7) 0.0559(6) 0.0058(6) F7 0.184(2) 0.178(2) 0.464(5) 0.144(3) 0.096(3) -0.021(2) F8 0.181(3) 0.288(4) 0.186(3) 0.031(3) 0.017(2) 0.053(3) F9 0.367(4) 0.171(3) 0.225(3) -0.037(2) 0.093(3) 0.089(3) F10 0.507(4) 0.148(2) 0.375(3) 0.064(2) 0.324(2) 0.119(3) F11 0.110(2) 0.538(6) 0.195(3) 0.172(3) -0.039(2) 0.000(3) F12 0.224(2) 0.151(2) 0.507(4) 0.033(3) 0.234(2) -0.026(2) O1W 0.571(8) 0.750(9) 0.328(4) 0.370(5) 0.228(5) 0.373(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C48 1.319(4) . ? N1 C52 1.324(3) . ? N1 C47 1.498(4) . ? N2 C55 1.341(4) . ? N2 C56 1.352(3) . ? N2 C58 1.477(4) . ? C33 C35 1.513(5) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.516(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.478(5) . ? C35 C37 1.515(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.384(4) . ? C37 C42 1.388(4) . ? C38 C39 1.379(5) . ? C38 H38 0.9300 . ? C39 C40 1.369(5) . ? C39 C46 1.518(5) . ? C40 C41 1.385(4) . ? C40 H40 0.9300 . ? C41 C42 1.388(5) . ? C41 C47 1.492(4) . ? C42 H42 0.9300 . ? C43 C46 1.462(7) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C46 1.523(6) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.407(7) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 C49 1.360(4) . ? C48 H48 0.9300 . ? C49 C50 1.390(4) . ? C49 H49 0.9300 . ? C50 C51 1.373(5) . ? C50 C53 1.445(4) . ? C51 C52 1.360(4) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.396(4) . ? C53 C57 1.409(4) . ? C54 C55 1.368(4) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C57 1.352(4) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 C59 1.501(4) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C64 1.368(4) . ? C59 C60 1.371(4) . ? C60 C61 1.361(4) . ? C60 H60 0.9300 . ? C61 C62 1.405(5) . ? C61 C72 1.534(4) . ? C62 C63 1.351(5) . ? C62 H62 0.9300 . ? C63 C64 1.376(4) . ? C63 C65 1.513(5) . ? C64 H64 0.9300 . ? C65 C68 1.494(6) . ? C65 C67 1.528(7) . ? C65 C66 1.558(6) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 C72 1.476(6) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 C72 1.469(6) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 C72 1.557(6) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? O1 C2 1.389(3) . ? O1 C24 1.412(4) . ? O2 C23 1.380(4) . ? O2 C22 1.404(5) . ? O3 C21 1.196(5) . ? O3 C20 1.341(5) . ? O4 C17 1.418(5) . ? O4 C19 1.439(4) . ? O5 C13 1.388(4) . ? O5 C12 1.424(5) . ? O6 C10 1.362(4) . ? O6 C11 1.401(4) . ? O7 C9 1.393(4) . ? O7 C8 1.404(4) . ? O8 C6 1.378(4) . ? O8 C7 1.477(4) . ? O9 C25 1.373(5) . ? O9 C26 1.395(5) . ? O10 C31 1.376(6) . ? O10 C32 1.386(5) . ? C1 C6 1.363(4) . ? C1 C2 1.391(4) . ? C1 H1 0.9300 . ? C2 C3 1.371(5) . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.381(4) . ? C4 C25 1.506(5) . ? C5 C6 1.355(5) . ? C5 H5 0.9300 . ? C7 C8 1.465(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.445(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.445(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.350(6) . ? C13 C18 1.397(5) . ? C14 C15 1.392(5) . ? C14 H14 0.9300 . ? C15 C16 1.358(5) . ? C15 C32 1.509(6) . ? C16 C17 1.347(6) . ? C16 H16 0.9300 . ? C17 C18 1.389(5) . ? C18 H18 0.9300 . ? C19 C20 1.444(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.370(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.428(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.478(6) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.167(6) . ? C28 C29 1.321(6) . ? C29 C30 1.195(6) . ? C30 C31 1.477(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? P1 F4 1.549(3) . ? P1 F3 1.550(3) . ? P1 F2 1.555(2) . ? P1 F6 1.567(3) . ? P1 F5 1.590(2) . ? P1 F1 1.597(3) . ? P2 F10 1.443(4) . ? P2 F11 1.462(3) . ? P2 F7 1.492(4) . ? P2 F9 1.507(4) . ? P2 F12 1.508(4) . ? P2 F8 1.557(3) . ? O1W H1W 0.9196 . ? O1W H2W 0.8671 . ? 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 C48 N1 C52 120.1(3) . . ? C48 N1 C47 119.4(2) . . ? C52 N1 C47 120.4(3) . . ? C55 N2 C56 120.7(3) . . ? C55 N2 C58 121.0(2) . . ? C56 N2 C58 118.2(3) . . ? C35 C33 H33A 109.5 . . ? C35 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C35 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C33 107.1(3) . . ? C36 C35 C37 113.8(3) . . ? C33 C35 C37 107.0(3) . . ? C36 C35 C34 109.1(3) . . ? C33 C35 C34 106.8(4) . . ? C37 C35 C34 112.6(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 116.6(3) . . ? C38 C37 C35 122.7(3) . . ? C42 C37 C35 120.7(3) . . ? C39 C38 C37 123.4(3) . . ? C39 C38 H38 118.3 . . ? C37 C38 H38 118.3 . . ? C40 C39 C38 118.7(3) . . ? C40 C39 C46 121.0(3) . . ? C38 C39 C46 120.3(3) . . ? C39 C40 C41 120.2(3) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C40 C41 C42 119.9(3) . . ? C40 C41 C47 119.3(3) . . ? C42 C41 C47 120.8(3) . . ? C37 C42 C41 121.2(3) . . ? C37 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C46 C43 H43A 109.5 . . ? C46 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C46 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 H44A 109.5 . . ? C46 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C46 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C45 C46 C43 123.8(5) . . ? C45 C46 C39 116.3(4) . . ? C43 C46 C39 112.3(4) . . ? C45 C46 C44 102.0(4) . . ? C43 C46 C44 88.7(4) . . ? C39 C46 C44 107.2(4) . . ? C41 C47 N1 109.3(2) . . ? C41 C47 H47A 109.8 . . ? N1 C47 H47A 109.8 . . ? C41 C47 H47B 109.8 . . ? N1 C47 H47B 109.8 . . ? H47A C47 H47B 108.3 . . ? N1 C48 C49 121.8(3) . . ? N1 C48 H48 119.1 . . ? C49 C48 H48 119.1 . . ? C48 C49 C50 119.4(3) . . ? C48 C49 H49 120.3 . . ? C50 C49 H49 120.3 . . ? C51 C50 C49 117.0(3) . . ? C51 C50 C53 122.3(2) . . ? C49 C50 C53 120.7(3) . . ? C52 C51 C50 120.6(3) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? N1 C52 C51 120.9(3) . . ? N1 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C54 C53 C57 116.9(3) . . ? C54 C53 C50 122.1(3) . . ? C57 C53 C50 121.1(2) . . ? C55 C54 C53 120.9(3) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? N2 C55 C54 120.2(3) . . ? N2 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? N2 C56 C57 121.2(3) . . ? N2 C56 H56 119.4 . . ? C57 C56 H56 119.4 . . ? C56 C57 C53 120.2(3) . . ? C56 C57 H57 119.9 . . ? C53 C57 H57 119.9 . . ? N2 C58 C59 110.0(2) . . ? N2 C58 H58A 109.7 . . ? C59 C58 H58A 109.7 . . ? N2 C58 H58B 109.7 . . ? C59 C58 H58B 109.7 . . ? H58A C58 H58B 108.2 . . ? C64 C59 C60 117.7(3) . . ? C64 C59 C58 120.4(3) . . ? C60 C59 C58 121.9(3) . . ? C61 C60 C59 123.0(3) . . ? C61 C60 H60 118.5 . . ? C59 C60 H60 118.5 . . ? C60 C61 C62 116.2(3) . . ? C60 C61 C72 122.2(3) . . ? C62 C61 C72 121.6(3) . . ? C63 C62 C61 123.1(3) . . ? C63 C62 H62 118.4 . . ? C61 C62 H62 118.4 . . ? C62 C63 C64 117.2(3) . . ? C62 C63 C65 123.6(3) . . ? C64 C63 C65 119.1(3) . . ? C59 C64 C63 122.5(3) . . ? C59 C64 H64 118.8 . . ? C63 C64 H64 118.8 . . ? C68 C65 C63 110.7(4) . . ? C68 C65 C67 106.7(4) . . ? C63 C65 C67 111.3(3) . . ? C68 C65 C66 106.4(4) . . ? C63 C65 C66 108.7(3) . . ? C67 C65 C66 113.0(4) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C72 C69 H69A 109.5 . . ? C72 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C72 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C72 C70 H70A 109.5 . . ? C72 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C72 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 C69 107.6(4) . . ? C70 C72 C61 112.7(3) . . ? C69 C72 C61 110.5(3) . . ? C70 C72 C71 106.4(4) . . ? C69 C72 C71 110.8(4) . . ? C61 C72 C71 108.7(3) . . ? C2 O1 C24 117.8(3) . . ? C23 O2 C22 113.7(3) . . ? C21 O3 C20 126.3(3) . . ? C17 O4 C19 120.1(3) . . ? C13 O5 C12 119.5(3) . . ? C10 O6 C11 118.1(3) . . ? C9 O7 C8 110.7(3) . . ? C6 O8 C7 116.7(3) . . ? C25 O9 C26 116.4(3) . . ? C31 O10 C32 114.1(4) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 H1 120.7 . . ? C2 C1 H1 120.7 . . ? C3 C2 O1 124.4(3) . . ? C3 C2 C1 120.7(3) . . ? O1 C2 C1 114.9(3) . . ? C2 C3 C4 118.3(3) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 121.8(3) . . ? C3 C4 C25 119.6(3) . . ? C5 C4 C25 118.4(3) . . ? C6 C5 C4 118.0(3) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C5 C6 C1 122.4(3) . . ? C5 C6 O8 124.6(3) . . ? C1 C6 O8 113.0(3) . . ? C8 C7 O8 107.4(3) . . ? C8 C7 H7A 110.2 . . ? O8 C7 H7A 110.2 . . ? C8 C7 H7B 110.2 . . ? O8 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O7 C8 C7 109.6(3) . . ? O7 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O7 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O7 C9 C10 110.5(3) . . ? O7 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? O7 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? O6 C10 C9 113.6(3) . . ? O6 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? O6 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? O6 C11 C12 109.8(3) . . ? O6 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? O6 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O5 C12 C11 110.3(4) . . ? O5 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? O5 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C14 C13 O5 116.2(3) . . ? C14 C13 C18 121.3(3) . . ? O5 C13 C18 122.3(4) . . ? C13 C14 C15 119.3(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 121.2(4) . . ? C16 C15 C32 119.8(3) . . ? C14 C15 C32 118.8(4) . . ? C17 C16 C15 118.3(3) . . ? C17 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? C16 C17 C18 123.5(4) . . ? C16 C17 O4 124.8(3) . . ? C18 C17 O4 111.6(4) . . ? C17 C18 C13 116.4(4) . . ? C17 C18 H18 121.8 . . ? C13 C18 H18 121.8 . . ? O4 C19 C20 109.3(3) . . ? O4 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? O4 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.3 . . ? O3 C20 C19 116.1(4) . . ? O3 C20 H20A 108.3 . . ? C19 C20 H20A 108.3 . . ? O3 C20 H20B 108.3 . . ? C19 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? O3 C21 C22 135.0(4) . . ? O3 C21 H21A 103.4 . . ? C22 C21 H21A 103.4 . . ? O3 C21 H21B 103.4 . . ? C22 C21 H21B 103.4 . . ? H21A C21 H21B 105.2 . . ? C21 C22 O2 114.0(3) . . ? C21 C22 H22A 108.7 . . ? O2 C22 H22A 108.7 . . ? C21 C22 H22B 108.7 . . ? O2 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? O2 C23 C24 113.2(3) . . ? O2 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? O2 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? O1 C24 C23 109.2(3) . . ? O1 C24 H24A 109.8 . . ? C23 C24 H24A 109.8 . . ? O1 C24 H24B 109.8 . . ? C23 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? O9 C25 C4 119.3(3) . . ? O9 C25 H25A 107.5 . . ? C4 C25 H25A 107.5 . . ? O9 C25 H25B 107.5 . . ? C4 C25 H25B 107.5 . . ? H25A C25 H25B 107.0 . . ? O9 C26 C27 114.3(4) . . ? O9 C26 H26A 108.7 . . ? C27 C26 H26A 108.7 . . ? O9 C26 H26B 108.7 . . ? C27 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C26 176.4(4) . . ? C27 C28 C29 177.2(5) . . ? C30 C29 C28 174.8(5) . . ? C29 C30 C31 175.6(5) . . ? O10 C31 C30 109.0(4) . . ? O10 C31 H31A 109.9 . . ? C30 C31 H31A 109.9 . . ? O10 C31 H31B 109.9 . . ? C30 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? O10 C32 C15 107.2(3) . . ? O10 C32 H32A 110.3 . . ? C15 C32 H32A 110.3 . . ? O10 C32 H32B 110.3 . . ? C15 C32 H32B 110.3 . . ? H32A C32 H32B 108.5 . . ? F4 P1 F3 90.95(17) . . ? F4 P1 F2 91.65(15) . . ? F3 P1 F2 91.21(16) . . ? F4 P1 F6 92.20(16) . . ? F3 P1 F6 175.68(15) . . ? F2 P1 F6 91.65(15) . . ? F4 P1 F5 89.83(15) . . ? F3 P1 F5 88.26(15) . . ? F2 P1 F5 178.43(17) . . ? F6 P1 F5 88.79(14) . . ? F4 P1 F1 176.74(15) . . ? F3 P1 F1 88.53(16) . . ? F2 P1 F1 91.58(14) . . ? F6 P1 F1 88.16(14) . . ? F5 P1 F1 86.93(13) . . ? F10 P2 F11 83.5(2) . . ? F10 P2 F7 88.9(2) . . ? F11 P2 F7 92.6(2) . . ? F10 P2 F9 172.8(2) . . ? F11 P2 F9 98.2(2) . . ? F7 P2 F9 98.0(2) . . ? F10 P2 F12 90.5(2) . . ? F11 P2 F12 87.2(2) . . ? F7 P2 F12 179.4(3) . . ? F9 P2 F12 82.6(2) . . ? F10 P2 F8 95.3(2) . . ? F11 P2 F8 178.6(2) . . ? F7 P2 F8 86.5(2) . . ? F9 P2 F8 83.1(2) . . ? F12 P2 F8 93.7(2) . . ? H1W O1W H2W 100.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C36 C35 C37 C38 149.0(3) . . . . ? C33 C35 C37 C38 -92.9(4) . . . . ? C34 C35 C37 C38 24.2(4) . . . . ? C36 C35 C37 C42 -33.3(4) . . . . ? C33 C35 C37 C42 84.8(4) . . . . ? C34 C35 C37 C42 -158.1(3) . . . . ? C42 C37 C38 C39 0.6(5) . . . . ? C35 C37 C38 C39 178.4(3) . . . . ? C37 C38 C39 C40 -1.1(5) . . . . ? C37 C38 C39 C46 -179.8(3) . . . . ? C38 C39 C40 C41 1.5(4) . . . . ? C46 C39 C40 C41 -179.8(3) . . . . ? C39 C40 C41 C42 -1.5(4) . . . . ? C39 C40 C41 C47 177.5(3) . . . . ? C38 C37 C42 C41 -0.6(4) . . . . ? C35 C37 C42 C41 -178.4(3) . . . . ? C40 C41 C42 C37 1.0(4) . . . . ? C47 C41 C42 C37 -177.9(3) . . . . ? C40 C39 C46 C45 38.0(5) . . . . ? C38 C39 C46 C45 -143.3(4) . . . . ? C40 C39 C46 C43 -171.2(4) . . . . ? C38 C39 C46 C43 7.6(5) . . . . ? C40 C39 C46 C44 -75.3(5) . . . . ? C38 C39 C46 C44 103.4(4) . . . . ? C40 C41 C47 N1 -76.5(3) . . . . ? C42 C41 C47 N1 102.5(3) . . . . ? C48 N1 C47 C41 109.5(3) . . . . ? C52 N1 C47 C41 -67.7(3) . . . . ? C52 N1 C48 C49 0.9(4) . . . . ? C47 N1 C48 C49 -176.3(3) . . . . ? N1 C48 C49 C50 2.9(4) . . . . ? C48 C49 C50 C51 -5.2(4) . . . . ? C48 C49 C50 C53 174.6(3) . . . . ? C49 C50 C51 C52 3.9(4) . . . . ? C53 C50 C51 C52 -175.9(3) . . . . ? C48 N1 C52 C51 -2.3(4) . . . . ? C47 N1 C52 C51 174.9(3) . . . . ? C50 C51 C52 N1 -0.2(5) . . . . ? C51 C50 C53 C54 37.3(4) . . . . ? C49 C50 C53 C54 -142.4(3) . . . . ? C51 C50 C53 C57 -142.4(3) . . . . ? C49 C50 C53 C57 37.9(4) . . . . ? C57 C53 C54 C55 0.8(4) . . . . ? C50 C53 C54 C55 -178.9(3) . . . . ? C56 N2 C55 C54 0.1(4) . . . . ? C58 N2 C55 C54 177.2(3) . . . . ? C53 C54 C55 N2 -1.0(4) . . . . ? C55 N2 C56 C57 1.0(4) . . . . ? C58 N2 C56 C57 -176.1(3) . . . . ? N2 C56 C57 C53 -1.2(4) . . . . ? C54 C53 C57 C56 0.3(4) . . . . ? C50 C53 C57 C56 180.0(3) . . . . ? C55 N2 C58 C59 -98.9(3) . . . . ? C56 N2 C58 C59 78.3(3) . . . . ? N2 C58 C59 C64 -85.1(4) . . . . ? N2 C58 C59 C60 93.7(3) . . . . ? C64 C59 C60 C61 -1.7(5) . . . . ? C58 C59 C60 C61 179.5(3) . . . . ? C59 C60 C61 C62 4.8(5) . . . . ? C59 C60 C61 C72 -175.8(3) . . . . ? C60 C61 C62 C63 -3.0(5) . . . . ? C72 C61 C62 C63 177.6(3) . . . . ? C61 C62 C63 C64 -1.9(5) . . . . ? C61 C62 C63 C65 -179.7(4) . . . . ? C60 C59 C64 C63 -3.7(5) . . . . ? C58 C59 C64 C63 175.2(3) . . . . ? C62 C63 C64 C59 5.3(5) . . . . ? C65 C63 C64 C59 -176.7(3) . . . . ? C62 C63 C65 C68 -5.4(6) . . . . ? C64 C63 C65 C68 176.8(4) . . . . ? C62 C63 C65 C67 113.1(4) . . . . ? C64 C63 C65 C67 -64.7(4) . . . . ? C62 C63 C65 C66 -121.9(4) . . . . ? C64 C63 C65 C66 60.3(5) . . . . ? C60 C61 C72 C70 29.9(5) . . . . ? C62 C61 C72 C70 -150.8(4) . . . . ? C60 C61 C72 C69 -90.5(4) . . . . ? C62 C61 C72 C69 88.8(4) . . . . ? C60 C61 C72 C71 147.7(4) . . . . ? C62 C61 C72 C71 -33.0(5) . . . . ? C24 O1 C2 C3 13.1(4) . . . . ? C24 O1 C2 C1 -167.0(2) . . . . ? C6 C1 C2 C3 -3.0(4) . . . . ? C6 C1 C2 O1 177.1(2) . . . . ? O1 C2 C3 C4 178.9(3) . . . . ? C1 C2 C3 C4 -1.0(4) . . . . ? C2 C3 C4 C5 3.2(4) . . . . ? C2 C3 C4 C25 -171.6(3) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? C25 C4 C5 C6 173.5(3) . . . . ? C4 C5 C6 C1 -2.9(4) . . . . ? C4 C5 C6 O8 177.9(3) . . . . ? C2 C1 C6 C5 5.0(4) . . . . ? C2 C1 C6 O8 -175.7(2) . . . . ? C7 O8 C6 C5 -7.9(4) . . . . ? C7 O8 C6 C1 172.9(2) . . . . ? C6 O8 C7 C8 -171.0(3) . . . . ? C9 O7 C8 C7 -177.8(3) . . . . ? O8 C7 C8 O7 76.5(3) . . . . ? C8 O7 C9 C10 -174.6(3) . . . . ? C11 O6 C10 C9 -160.7(4) . . . . ? O7 C9 C10 O6 -61.3(5) . . . . ? C10 O6 C11 C12 -179.4(4) . . . . ? C13 O5 C12 C11 -163.2(3) . . . . ? O6 C11 C12 O5 74.5(4) . . . . ? C12 O5 C13 C14 -177.3(3) . . . . ? C12 O5 C13 C18 6.9(5) . . . . ? O5 C13 C14 C15 -176.5(3) . . . . ? C18 C13 C14 C15 -0.6(5) . . . . ? C13 C14 C15 C16 2.0(5) . . . . ? C13 C14 C15 C32 176.7(3) . . . . ? C14 C15 C16 C17 -2.2(5) . . . . ? C32 C15 C16 C17 -176.8(3) . . . . ? C15 C16 C17 C18 1.0(5) . . . . ? C15 C16 C17 O4 175.8(3) . . . . ? C19 O4 C17 C16 24.1(5) . . . . ? C19 O4 C17 C18 -160.6(3) . . . . ? C16 C17 C18 C13 0.3(5) . . . . ? O4 C17 C18 C13 -175.1(3) . . . . ? C14 C13 C18 C17 -0.5(5) . . . . ? O5 C13 C18 C17 175.2(3) . . . . ? C17 O4 C19 C20 -126.3(4) . . . . ? C21 O3 C20 C19 112.4(5) . . . . ? O4 C19 C20 O3 63.5(5) . . . . ? C20 O3 C21 C22 164.3(6) . . . . ? O3 C21 C22 O2 35.3(9) . . . . ? C23 O2 C22 C21 -172.1(4) . . . . ? C22 O2 C23 C24 -172.8(4) . . . . ? C2 O1 C24 C23 176.7(2) . . . . ? O2 C23 C24 O1 -60.7(4) . . . . ? C26 O9 C25 C4 -99.9(4) . . . . ? C3 C4 C25 O9 -16.0(5) . . . . ? C5 C4 C25 O9 169.1(3) . . . . ? C25 O9 C26 C27 79.6(4) . . . . ? O9 C26 C27 C28 52(8) . . . . ? C26 C27 C28 C29 -139(8) . . . . ? C27 C28 C29 C30 -5(14) . . . . ? C28 C29 C30 C31 20(11) . . . . ? C32 O10 C31 C30 -176.9(3) . . . . ? C29 C30 C31 O10 39(7) . . . . ? C31 O10 C32 C15 -179.7(3) . . . . ? C16 C15 C32 O10 93.0(4) . . . . ? C14 C15 C32 O10 -81.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.833 _diffrn_reflns_theta_full 25.20 _diffrn_measured_fraction_theta_full 0.833 _refine_diff_density_max 0.831 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.079 # Attachment '- [2]rotaxane 7.cif' data_x _database_code_depnum_ccdc_archive 'CCDC 798399' #TrackingRef '- [2]rotaxane 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H92 F12 N2 O11 P2' _chemical_formula_weight 1451.42 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' F F 0.0171 0.0103 '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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.666(2) _cell_length_b 17.343(3) _cell_length_c 34.900(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.726(5) _cell_angle_gamma 90.00 _cell_volume 7922(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3056 _exptl_absorpt_coefficient_mu 0.137 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 73478 _diffrn_reflns_av_R_equivalents 0.0683 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13959 _reflns_number_gt 6791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13959 _refine_ls_number_parameters 955 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2379 _refine_ls_R_factor_gt 0.1610 _refine_ls_wR_factor_ref 0.5147 _refine_ls_wR_factor_gt 0.4757 _refine_ls_goodness_of_fit_ref 1.717 _refine_ls_restrained_S_all 1.719 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.3781(5) 0.8981(4) 0.97294(19) 0.0649(17) Uani 1 1 d . . . N2 N 0.2902(5) 0.7950(4) 0.7738(2) 0.0648(17) Uani 1 1 d . . . C1 C 0.3226(5) 0.8396(4) 0.8513(2) 0.0572(19) Uani 1 1 d . . . C2 C 0.3408(6) 0.8633(4) 0.8937(2) 0.061(2) Uani 1 1 d . . . C4 C 0.2039(6) 0.8382(5) 0.7056(2) 0.068(2) Uani 1 1 d . . . C6 C 0.2374(6) 0.7634(4) 0.7952(3) 0.064(2) Uani 1 1 d . . . H6 H 0.1885 0.7264 0.7837 0.077 Uiso 1 1 calc R . . C8 C 0.2524(6) 0.7836(4) 0.8344(3) 0.064(2) Uani 1 1 d . . . H8 H 0.2152 0.7594 0.8495 0.077 Uiso 1 1 calc R . . C9 C 0.4552(7) 0.8943(5) 0.9566(3) 0.076(2) Uani 1 1 d . . . H9 H 0.5216 0.9028 0.9726 0.091 Uiso 1 1 calc R . . C10 C 0.3774(6) 0.8725(5) 0.8281(3) 0.064(2) Uani 1 1 d . . . H10 H 0.4257 0.9102 0.8391 0.077 Uiso 1 1 calc R . . C12 C 0.3791(6) 0.8379(5) 1.0355(2) 0.066(2) Uani 1 1 d . . . C13 C 0.3625(6) 0.8514(5) 0.7900(3) 0.069(2) Uani 1 1 d . . . H13 H 0.4000 0.8741 0.7746 0.083 Uiso 1 1 calc R . . C14 C 0.4388(6) 0.8784(5) 0.9171(3) 0.072(2) Uani 1 1 d . . . H14 H 0.4930 0.8777 0.9060 0.086 Uiso 1 1 calc R . . C15 C 0.2501(7) 0.9035(6) 0.6965(3) 0.078(2) Uani 1 1 d . . . H15 H 0.3209 0.9076 0.7044 0.093 Uiso 1 1 calc R . . C17 C 0.0846(8) 0.9521(6) 0.6615(3) 0.087(3) Uani 1 1 d . . . H17 H 0.0440 0.9912 0.6468 0.104 Uiso 1 1 calc R . . C18 C 0.4292(7) 0.7090(5) 1.0583(3) 0.076(2) Uani 1 1 d . A . C19 C 0.0381(7) 0.8843(5) 0.6689(3) 0.078(2) Uani 1 1 d . A . C21 C 0.2686(6) 0.7618(5) 1.0637(3) 0.072(2) Uani 1 1 d . A . C22 C 0.2904(7) 0.8298(5) 1.0468(3) 0.074(2) Uani 1 1 d . . . H22 H 0.2446 0.8707 1.0430 0.088 Uiso 1 1 calc R . . C23 C 0.3394(7) 0.7037(6) 1.0691(3) 0.080(2) Uani 1 1 d . . . H23 H 0.3263 0.6580 1.0806 0.096 Uiso 1 1 calc R . . C24 C 0.1001(6) 0.8288(5) 0.6922(2) 0.069(2) Uani 1 1 d . . . H24 H 0.0708 0.7843 0.6989 0.083 Uiso 1 1 calc R . . C25 C -0.0778(7) 0.8715(7) 0.6510(3) 0.096(3) Uani 1 1 d U . . C26 C 0.2633(6) 0.8699(5) 0.9110(3) 0.073(2) Uani 1 1 d . . . H26 H 0.1962 0.8621 0.8956 0.088 Uiso 1 1 calc R . . C27 C 0.2705(7) 0.7774(5) 0.7306(2) 0.073(2) Uani 1 1 d . . . H27A H 0.2374 0.7275 0.7247 0.088 Uiso 1 1 calc R . . H27B H 0.3349 0.7749 0.7241 0.088 Uiso 1 1 calc R . . C28 C 0.4480(7) 0.7775(6) 1.0420(3) 0.080(2) Uani 1 1 d . . . H28 H 0.5086 0.7834 1.0353 0.096 Uiso 1 1 calc R . . C29 C 0.1730(8) 0.7547(6) 1.0772(4) 0.094(3) Uani 1 1 d . . . C31 C 0.2826(6) 0.8877(5) 0.9500(3) 0.071(2) Uani 1 1 d . . . H31 H 0.2286 0.8929 0.9611 0.085 Uiso 1 1 calc R . . C38 C 0.3963(7) 0.9096(5) 1.0160(2) 0.079(2) Uani 1 1 d . . . H38A H 0.3509 0.9494 1.0204 0.094 Uiso 1 1 calc R . . H38B H 0.4661 0.9268 1.0277 0.094 Uiso 1 1 calc R . . C39 C 0.5046(9) 0.6445(7) 1.0648(4) 0.110(3) Uani 1 1 d U . . C40 C 0.1903(9) 0.9631(6) 0.6755(3) 0.092(3) Uani 1 1 d . . . C46 C 0.0834(8) 0.7981(10) 1.0505(4) 0.148(6) Uani 1 1 d . A . H46A H 0.0249 0.7916 1.0602 0.221 Uiso 1 1 calc R . . H46B H 0.0684 0.7785 1.0237 0.221 Uiso 1 1 calc R . . H46C H 0.1001 0.8519 1.0506 0.221 Uiso 1 1 calc R . . C55 C 0.2385(13) 1.0373(8) 0.6668(4) 0.143(6) Uani 1 1 d . . . C61 C 0.5730(14) 0.6408(12) 1.1078(5) 0.050(5) Uani 0.500(18) 1 d P A 1 H61A H 0.6361 0.6158 1.1084 0.075 Uiso 0.500(18) 1 calc PR A 1 H61B H 0.5391 0.6122 1.1238 0.075 Uiso 0.500(18) 1 calc PR A 1 H61C H 0.5868 0.6921 1.1183 0.075 Uiso 0.500(18) 1 calc PR A 1 C61' C 0.5956(14) 0.6698(11) 1.0950(6) 0.050(4) Uani 0.500(18) 1 d P A 1 H61D H 0.6375 0.6260 1.1057 0.075 Uiso 0.500(18) 1 calc PR A 1 H61E H 0.5764 0.6955 1.1161 0.075 Uiso 0.500(18) 1 calc PR A 1 H61F H 0.6332 0.7048 1.0833 0.075 Uiso 0.500(18) 1 calc PR A 1 C63 C 0.1593(16) 1.0963(8) 0.6450(6) 0.202(9) Uani 1 1 d . . . H63A H 0.1343 1.0826 0.6172 0.303 Uiso 1 1 calc R . . H63B H 0.1901 1.1464 0.6474 0.303 Uiso 1 1 calc R . . H63C H 0.1035 1.0969 0.6566 0.303 Uiso 1 1 calc R . . C64 C -0.1038(10) 0.7904(10) 0.6467(7) 0.193(9) Uani 1 1 d . A . H64A H -0.0868 0.7667 0.6726 0.290 Uiso 1 1 calc R . . H64B H -0.0661 0.7660 0.6307 0.290 Uiso 1 1 calc R . . H64C H -0.1757 0.7849 0.6339 0.290 Uiso 1 1 calc R . . C65 C 0.130(3) 0.670(3) 1.0712(9) 0.050(7) Uani 0.500(18) 1 d P A 1 H65A H 0.1816 0.6349 1.0859 0.075 Uiso 0.500(18) 1 calc PR A 1 H65B H 0.1115 0.6571 1.0433 0.075 Uiso 0.500(18) 1 calc PR A 1 H65C H 0.0710 0.6664 1.0807 0.075 Uiso 0.500(18) 1 calc PR A 1 C65' C 0.155(3) 0.672(2) 1.0866(9) 0.050(7) Uani 0.500(18) 1 d P A 2 H65D H 0.2040 0.6575 1.1113 0.075 Uiso 0.500(18) 1 calc PR A 2 H65E H 0.1628 0.6396 1.0654 0.075 Uiso 0.500(18) 1 calc PR A 2 H65F H 0.0874 0.6668 1.0891 0.075 Uiso 0.500(18) 1 calc PR A 2 C66 C -0.118(2) 0.8960(15) 0.6061(8) 0.050(6) Uani 0.500(18) 1 d P A 1 H66A H -0.1897 0.9068 0.5995 0.075 Uiso 0.500(18) 1 calc PR A 1 H66B H -0.1064 0.8549 0.5895 0.075 Uiso 0.500(18) 1 calc PR A 1 H66C H -0.0822 0.9413 0.6017 0.075 Uiso 0.500(18) 1 calc PR A 1 C66' C -0.112(2) 0.9236(14) 0.6187(8) 0.050(5) Uani 0.500(18) 1 d P A 2 H66D H -0.0684 0.9206 0.6017 0.075 Uiso 0.500(18) 1 calc PR A 2 H66E H -0.1114 0.9751 0.6289 0.075 Uiso 0.500(18) 1 calc PR A 2 H66F H -0.1808 0.9103 0.6036 0.075 Uiso 0.500(18) 1 calc PR A 2 C67 C -0.1286(10) 0.9090(11) 0.6795(6) 0.181(8) Uani 1 1 d . A . H67A H -0.2013 0.9028 0.6694 0.272 Uiso 1 1 calc R . . H67B H -0.1121 0.9629 0.6818 0.272 Uiso 1 1 calc R . . H67C H -0.1046 0.8851 0.7053 0.272 Uiso 1 1 calc R . . C68 C 0.3060(13) 1.0722(8) 0.7092(5) 0.160(6) Uani 1 1 d . . . H68A H 0.2638 1.0779 0.7268 0.241 Uiso 1 1 calc R . . H68B H 0.3327 1.1217 0.7049 0.241 Uiso 1 1 calc R . . H68C H 0.3615 1.0379 0.7211 0.241 Uiso 1 1 calc R . . C69 C 0.5260(16) 0.6242(11) 1.0295(5) 0.050(5) Uani 0.500(18) 1 d P A 1 H69A H 0.5312 0.6699 1.0147 0.075 Uiso 0.500(18) 1 calc PR A 1 H69B H 0.4721 0.5921 1.0137 0.075 Uiso 0.500(18) 1 calc PR A 1 H69C H 0.5895 0.5965 1.0357 0.075 Uiso 0.500(18) 1 calc PR A 1 C69' C 0.5752(16) 0.6476(12) 1.0367(6) 0.050(5) Uani 0.500(18) 1 d P A 2 H69D H 0.6021 0.5971 1.0347 0.075 Uiso 0.500(18) 1 calc PR A 2 H69E H 0.6305 0.6828 1.0475 0.075 Uiso 0.500(18) 1 calc PR A 2 H69F H 0.5364 0.6648 1.0106 0.075 Uiso 0.500(18) 1 calc PR A 2 C70 C 0.3143(14) 1.0183(8) 0.6422(5) 0.163(6) Uani 1 1 d . . . H70A H 0.3523 0.9727 0.6529 0.244 Uiso 1 1 calc R . . H70B H 0.3605 1.0607 0.6440 0.244 Uiso 1 1 calc R . . H70C H 0.2768 1.0098 0.6148 0.244 Uiso 1 1 calc R . . C71 C 0.4410(11) 0.5652(8) 1.0606(4) 0.050(5) Uani 0.500(18) 1 d P A 1 H71A H 0.4153 0.5515 1.0329 0.075 Uiso 0.500(18) 1 calc PR A 1 H71B H 0.3849 0.5719 1.0717 0.075 Uiso 0.500(18) 1 calc PR A 1 H71C H 0.4849 0.5249 1.0748 0.075 Uiso 0.500(18) 1 calc PR A 1 C71' C 0.4912(11) 0.5809(8) 1.0953(4) 0.050(5) Uani 0.500(18) 1 d P A 2 H71D H 0.4198 0.5729 1.0921 0.075 Uiso 0.500(18) 1 calc PR A 2 H71E H 0.5242 0.5977 1.1221 0.075 Uiso 0.500(18) 1 calc PR A 2 H71F H 0.5215 0.5335 1.0902 0.075 Uiso 0.500(18) 1 calc PR A 2 C72 C 0.1960(12) 0.7867(10) 1.1190(4) 0.151(6) Uani 1 1 d . A . H72A H 0.2165 0.8396 1.1190 0.227 Uiso 1 1 calc R . . H72B H 0.2502 0.7575 1.1366 0.227 Uiso 1 1 calc R . . H72C H 0.1360 0.7833 1.1280 0.227 Uiso 1 1 calc R . . O1 O 0.0124(4) 0.8430(4) 0.78702(18) 0.0831(17) Uani 1 1 d . . . O2 O 0.0105(6) 0.6856(4) 0.7706(2) 0.111(2) Uani 1 1 d . . . O3 O 0.1598(8) 0.6039(6) 0.7407(5) 0.184(6) Uani 1 1 d . . . O4 O 0.3741(6) 0.6079(5) 0.7767(3) 0.123(3) Uani 1 1 d . . . O5 O 0.5827(6) 0.7652(4) 0.8802(3) 0.111(2) Uani 1 1 d . . . O6 O 0.6107(5) 0.9256(4) 0.8621(2) 0.111(2) Uani 1 1 d . . . O7 O 0.4760(5) 1.0465(4) 0.8624(2) 0.096(2) Uani 1 1 d . . . O8 O 0.2574(4) 1.0340(3) 0.8257(2) 0.0857(18) Uani 1 1 d . . . O9 O -0.0949(5) 0.9889(5) 0.8972(2) 0.106(2) Uani 1 1 d . . . O10 O 0.2613(8) 0.6535(5) 0.9120(3) 0.147(3) Uani 1 1 d . . . C3 C 0.1696(6) 1.0049(5) 0.8306(3) 0.070(2) Uani 1 1 d . . . C5 C 0.0432(6) 0.9062(5) 0.8113(2) 0.069(2) Uani 1 1 d . . . C7 C 0.1278(6) 0.9438(5) 0.8067(3) 0.067(2) Uani 1 1 d . . . H7 H 0.1570 0.9274 0.7871 0.081 Uiso 1 1 calc R . . C11 C -0.0041(6) 0.9325(6) 0.8387(3) 0.077(2) Uani 1 1 d . . . H11 H -0.0620 0.9078 0.8415 0.092 Uiso 1 1 calc R . . C16 C 0.1226(7) 1.0315(5) 0.8584(3) 0.077(2) Uani 1 1 d . . . H16 H 0.1493 1.0732 0.8748 0.093 Uiso 1 1 calc R . . C20 C 0.0344(6) 0.9944(6) 0.8613(3) 0.078(2) Uani 1 1 d . . . C30 C 0.6868(8) 0.8673(7) 0.8702(4) 0.117(4) Uani 1 1 d . . . H30A H 0.7184 0.8626 0.8988 0.140 Uiso 1 1 calc R . . H30B H 0.7394 0.8798 0.8575 0.140 Uiso 1 1 calc R . . C32 C 0.4674(10) 0.6802(6) 0.8948(4) 0.100(3) Uani 1 1 d . . . H32 H 0.4886 0.6976 0.9211 0.120 Uiso 1 1 calc R . . C33 C 0.4834(7) 0.6816(5) 0.8281(4) 0.089(3) Uani 1 1 d . . . H33 H 0.5148 0.6998 0.8095 0.107 Uiso 1 1 calc R . . C34 C 0.5116(8) 0.7066(6) 0.8676(4) 0.092(3) Uani 1 1 d . . . C35 C 0.3094(7) 1.0931(6) 0.8523(4) 0.100(3) Uani 1 1 d . . . H35A H 0.3202 1.0767 0.8798 0.120 Uiso 1 1 calc R . . H35B H 0.2685 1.1397 0.8480 0.120 Uiso 1 1 calc R . . C36 C 0.3597(9) 0.6002(6) 0.8456(5) 0.107(4) Uani 1 1 d . . . H36 H 0.3080 0.5635 0.8384 0.128 Uiso 1 1 calc R . . C37 C 0.4049(8) 0.6274(6) 0.8184(5) 0.103(3) Uani 1 1 d . . . C41 C 0.4075(8) 1.1084(5) 0.8451(4) 0.102(3) Uani 1 1 d . . . H41A H 0.3990 1.1114 0.8166 0.122 Uiso 1 1 calc R . . H41B H 0.4349 1.1571 0.8572 0.122 Uiso 1 1 calc R . . C42 C -0.0582(7) 0.7907(6) 0.7962(3) 0.091(3) Uani 1 1 d . . . H42A H -0.1212 0.8176 0.7951 0.110 Uiso 1 1 calc R . . H42B H -0.0299 0.7707 0.8230 0.110 Uiso 1 1 calc R . . C43 C 0.3909(10) 0.6271(7) 0.8830(5) 0.107(4) Uani 1 1 d . . . C44 C 0.5713(8) 1.0547(7) 0.8547(4) 0.108(4) Uani 1 1 d . . . H44A H 0.5983 1.1058 0.8628 0.130 Uiso 1 1 calc R . . H44B H 0.5618 1.0499 0.8261 0.130 Uiso 1 1 calc R . . C45 C -0.0794(8) 0.7276(6) 0.7678(4) 0.104(3) Uani 1 1 d . . . H45A H -0.1305 0.6939 0.7732 0.124 Uiso 1 1 calc R . . H45B H -0.1065 0.7478 0.7409 0.124 Uiso 1 1 calc R . . C47 C 0.0278(10) 0.8238(10) 0.9351(4) 0.104(3) Uani 1 1 d . . . C48 C 0.3365(12) 0.6000(8) 0.9131(5) 0.138(5) Uani 1 1 d . . . H48A H 0.3068 0.5493 0.9059 0.166 Uiso 1 1 calc R . . H48B H 0.3841 0.5972 0.9398 0.166 Uiso 1 1 calc R . . C49 C -0.0185(10) 1.0320(8) 0.8896(5) 0.130(4) Uani 1 1 d . . . H49A H 0.0325 1.0426 0.9148 0.156 Uiso 1 1 calc R . . H49B H -0.0469 1.0810 0.8783 0.156 Uiso 1 1 calc R . . C50 C 0.3222(11) 0.5416(6) 0.7626(5) 0.132(5) Uani 1 1 d . . . H50A H 0.3038 0.5159 0.7843 0.159 Uiso 1 1 calc R . . H50B H 0.3660 0.5073 0.7531 0.159 Uiso 1 1 calc R . . C51 C 0.6441(8) 0.9973(6) 0.8757(4) 0.101(3) Uani 1 1 d . . . H51A H 0.7102 1.0069 0.8715 0.122 Uiso 1 1 calc R . . H51B H 0.6521 1.0005 0.9042 0.122 Uiso 1 1 calc R . . C52 C -0.0074(10) 0.6179(8) 0.7482(5) 0.133(5) Uani 1 1 d . . . H52A H -0.0498 0.6299 0.7215 0.159 Uiso 1 1 calc R . . H52B H -0.0456 0.5828 0.7602 0.159 Uiso 1 1 calc R . . C53 C -0.0135(10) 0.8813(10) 0.9356(4) 0.118(4) Uani 1 1 d . . . C54 C 0.2292(10) 0.5576(7) 0.7300(5) 0.132(5) Uani 1 1 d . . . H54A H 0.2485 0.5822 0.7083 0.158 Uiso 1 1 calc R . . H54B H 0.1964 0.5091 0.7201 0.158 Uiso 1 1 calc R . . C56 C 0.0805(19) 0.5806(8) 0.7454(6) 0.182(8) Uani 1 1 d . . . H56A H 0.1019 0.5499 0.7696 0.219 Uiso 1 1 calc R . . H56B H 0.0556 0.5439 0.7238 0.219 Uiso 1 1 calc R . . C57 C 0.6343(9) 0.7932(7) 0.8535(4) 0.110(4) Uani 1 1 d . . . H57A H 0.5862 0.8022 0.8274 0.132 Uiso 1 1 calc R . . H57B H 0.6842 0.7556 0.8505 0.132 Uiso 1 1 calc R . . C58 C 0.1364(13) 0.7006(10) 0.9372(4) 0.133(5) Uani 1 1 d . . . C59 C 0.2066(14) 0.6365(9) 0.9400(5) 0.155(6) Uani 1 1 d . . . H59A H 0.2528 0.6325 0.9668 0.187 Uiso 1 1 calc R . . H59B H 0.1694 0.5884 0.9333 0.187 Uiso 1 1 calc R . . C60 C -0.0671(10) 0.9550(9) 0.9353(4) 0.120(4) Uani 1 1 d . . . H60A H -0.1279 0.9463 0.9437 0.144 Uiso 1 1 calc R . . H60B H -0.0230 0.9901 0.9543 0.144 Uiso 1 1 calc R . . C62 C 0.0798(11) 0.7579(11) 0.9359(4) 0.120(4) Uani 1 1 d . . . P1 P 0.24753(19) 0.11919(16) 0.98461(8) 0.0877(8) Uani 1 1 d . . . F1 F 0.1803(6) 0.0462(5) 0.9777(3) 0.170(3) Uani 1 1 d . . . F2 F 0.1706(6) 0.1605(6) 1.0026(3) 0.164(3) Uani 1 1 d . . . F3 F 0.3308(5) 0.0743(4) 0.96907(18) 0.118(2) Uani 1 1 d . . . F4 F 0.3214(6) 0.1893(4) 0.9932(3) 0.143(3) Uani 1 1 d . . . F5 F 0.3056(5) 0.0864(4) 1.02800(18) 0.120(2) Uani 1 1 d . . . F6 F 0.1924(6) 0.1491(5) 0.9422(2) 0.145(3) Uani 1 1 d . . . P2 P 0.5977(3) 0.81166(19) 0.72854(12) 0.1118(11) Uani 1 1 d . . . F7 F 0.5068(9) 0.7863(8) 0.6908(3) 0.225(5) Uani 1 1 d . . . F8 F 0.6328(14) 0.8707(7) 0.7044(5) 0.267(8) Uani 1 1 d . . . F9 F 0.5302(9) 0.8727(6) 0.7398(5) 0.244(6) Uani 1 1 d . . . F10 F 0.6841(7) 0.8434(10) 0.7601(4) 0.273(8) Uani 1 1 d . . . F11 F 0.5437(12) 0.7580(8) 0.7508(4) 0.254(6) Uani 1 1 d . . . F12 F 0.6611(9) 0.7515(8) 0.7147(5) 0.272(7) Uani 1 1 d . . . O1W O 0.796(4) 0.573(3) 0.9847(10) 0.63(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.059(4) 0.064(4) 0.068(4) 0.006(3) 0.013(4) -0.011(3) N2 0.050(4) 0.057(4) 0.078(5) -0.013(3) 0.004(3) 0.008(3) C1 0.038(4) 0.057(4) 0.069(5) 0.004(4) 0.004(3) 0.005(3) C2 0.050(4) 0.044(4) 0.084(6) 0.003(4) 0.009(4) 0.004(3) C4 0.063(5) 0.068(5) 0.074(5) -0.016(4) 0.020(4) -0.002(4) C6 0.055(5) 0.048(4) 0.086(6) -0.003(4) 0.014(4) -0.002(4) C8 0.051(4) 0.049(4) 0.085(6) 0.006(4) 0.008(4) 0.000(4) C9 0.054(5) 0.081(6) 0.086(7) -0.005(5) 0.007(5) -0.010(4) C10 0.044(4) 0.063(5) 0.074(6) -0.009(4) 0.001(4) -0.005(4) C12 0.065(5) 0.065(5) 0.064(5) 0.003(4) 0.011(4) -0.003(4) C13 0.045(4) 0.078(5) 0.081(6) -0.004(5) 0.012(4) -0.004(4) C14 0.047(5) 0.085(6) 0.081(6) -0.013(5) 0.016(4) -0.012(4) C15 0.066(5) 0.086(6) 0.082(6) -0.010(5) 0.022(5) -0.011(5) C17 0.086(7) 0.079(6) 0.092(7) 0.001(5) 0.020(5) 0.007(5) C18 0.073(6) 0.079(6) 0.070(5) 0.014(5) 0.010(4) 0.015(5) C19 0.069(6) 0.079(6) 0.088(6) -0.007(5) 0.024(5) -0.004(5) C21 0.066(5) 0.064(5) 0.084(6) 0.009(4) 0.020(4) 0.003(4) C22 0.069(5) 0.069(5) 0.080(6) 0.002(4) 0.017(4) 0.008(4) C23 0.069(6) 0.085(6) 0.085(6) 0.025(5) 0.020(5) 0.006(5) C24 0.061(5) 0.068(5) 0.076(5) 0.001(4) 0.017(4) -0.005(4) C25 0.056(5) 0.113(7) 0.113(6) 0.019(6) 0.016(5) 0.008(5) C26 0.044(4) 0.082(6) 0.089(7) 0.009(5) 0.012(4) 0.003(4) C27 0.068(5) 0.066(5) 0.078(6) -0.014(4) 0.010(4) 0.004(4) C28 0.062(5) 0.100(7) 0.077(6) 0.006(5) 0.019(4) 0.001(5) C29 0.085(7) 0.086(7) 0.122(9) 0.021(6) 0.050(6) -0.001(5) C31 0.055(5) 0.083(6) 0.070(6) 0.005(4) 0.012(4) 0.006(4) C38 0.082(6) 0.081(6) 0.068(6) -0.005(4) 0.014(4) -0.017(5) C39 0.095(6) 0.113(7) 0.128(7) 0.034(6) 0.044(6) 0.026(6) C40 0.119(9) 0.079(6) 0.083(6) -0.017(5) 0.039(6) -0.024(6) C46 0.067(7) 0.221(16) 0.157(12) 0.053(11) 0.035(7) 0.023(9) C55 0.183(14) 0.121(10) 0.137(11) -0.021(9) 0.065(11) -0.087(11) C61 0.050(10) 0.050(11) 0.050(11) 0.000(8) 0.014(8) 0.000(8) C61' 0.050(10) 0.050(11) 0.050(11) 0.000(8) 0.014(8) 0.000(8) C63 0.224(19) 0.088(9) 0.25(2) 0.066(11) -0.011(15) -0.019(11) C64 0.077(8) 0.156(14) 0.29(2) -0.049(14) -0.029(11) -0.025(9) C65 0.050(18) 0.050(10) 0.050(18) 0.000(16) 0.014(14) 0.000(12) C65' 0.050(18) 0.050(10) 0.050(19) 0.000(16) 0.014(13) 0.000(12) C66 0.050(10) 0.050(15) 0.050(15) 0.000(9) 0.014(11) 0.000(11) C66' 0.050(10) 0.050(15) 0.050(15) 0.000(9) 0.014(11) 0.000(11) C67 0.079(8) 0.218(18) 0.26(2) -0.079(15) 0.077(11) -0.003(10) C68 0.195(15) 0.121(10) 0.168(13) -0.055(9) 0.057(11) -0.082(11) C69 0.050(12) 0.050(11) 0.050(10) 0.000(8) 0.014(9) 0.000(8) C69' 0.050(12) 0.050(11) 0.050(10) 0.000(8) 0.014(9) 0.000(8) C70 0.232(17) 0.116(10) 0.178(14) -0.027(9) 0.120(14) -0.076(11) C71 0.050(8) 0.050(8) 0.050(10) 0.000(6) 0.014(7) 0.000(6) C71' 0.050(9) 0.050(8) 0.050(10) 0.000(6) 0.014(7) 0.000(7) C72 0.137(11) 0.212(16) 0.127(11) 0.036(11) 0.074(9) 0.014(11) O1 0.071(4) 0.084(4) 0.090(4) -0.006(3) 0.017(3) -0.019(3) O2 0.094(5) 0.088(5) 0.144(6) -0.039(4) 0.022(4) -0.027(4) O3 0.095(6) 0.107(7) 0.345(16) -0.121(9) 0.054(8) -0.029(6) O4 0.116(6) 0.100(6) 0.136(7) -0.014(5) 0.008(5) -0.018(5) O5 0.086(5) 0.104(5) 0.138(6) -0.033(5) 0.027(5) -0.004(4) O6 0.059(4) 0.108(5) 0.161(7) -0.041(5) 0.024(4) -0.006(4) O7 0.070(4) 0.080(4) 0.134(6) 0.008(4) 0.024(4) -0.011(3) O8 0.060(3) 0.069(4) 0.127(5) -0.009(3) 0.025(3) -0.004(3) O9 0.057(4) 0.159(7) 0.102(5) -0.020(5) 0.020(4) -0.001(4) O10 0.177(9) 0.104(6) 0.182(9) 0.040(6) 0.086(8) 0.042(6) C3 0.053(5) 0.054(5) 0.097(6) 0.009(4) 0.014(4) 0.014(4) C5 0.056(5) 0.074(5) 0.070(5) 0.003(4) 0.007(4) 0.003(4) C7 0.057(5) 0.061(5) 0.082(6) 0.010(4) 0.017(4) 0.007(4) C11 0.051(5) 0.088(6) 0.086(6) 0.002(5) 0.013(4) 0.011(5) C16 0.064(5) 0.066(5) 0.093(6) 0.003(5) 0.007(5) 0.015(4) C20 0.055(5) 0.085(6) 0.093(6) -0.006(5) 0.017(5) 0.007(5) C30 0.059(6) 0.121(9) 0.171(11) -0.046(8) 0.034(6) -0.006(6) C32 0.111(9) 0.069(6) 0.113(9) 0.007(6) 0.020(8) 0.030(7) C33 0.064(6) 0.073(6) 0.124(9) -0.014(6) 0.015(5) 0.011(5) C34 0.076(6) 0.061(6) 0.130(10) -0.010(6) 0.014(7) 0.016(5) C35 0.072(6) 0.065(6) 0.149(9) -0.006(6) 0.008(6) 0.004(5) C36 0.093(8) 0.062(6) 0.154(12) 0.024(7) 0.017(8) 0.010(6) C37 0.076(7) 0.068(6) 0.150(11) -0.001(7) 0.005(7) 0.013(6) C41 0.080(7) 0.058(5) 0.155(10) 0.001(6) 0.017(6) -0.001(5) C42 0.065(6) 0.097(7) 0.115(8) -0.009(6) 0.029(5) -0.016(5) C43 0.109(9) 0.076(7) 0.122(10) 0.018(7) 0.009(8) 0.028(7) C44 0.073(7) 0.108(8) 0.144(10) -0.005(7) 0.032(6) -0.042(7) C45 0.072(6) 0.089(7) 0.144(10) -0.007(7) 0.022(6) -0.005(6) C47 0.085(8) 0.125(11) 0.108(9) 0.005(8) 0.035(7) -0.004(8) C48 0.157(12) 0.095(8) 0.160(12) 0.026(8) 0.043(10) 0.034(9) C49 0.097(8) 0.133(10) 0.181(13) -0.031(9) 0.075(9) -0.017(8) C50 0.131(10) 0.063(6) 0.184(13) -0.039(7) 0.017(10) 0.002(7) C51 0.069(6) 0.084(7) 0.151(10) -0.021(7) 0.030(6) -0.019(6) C52 0.102(9) 0.100(9) 0.188(13) -0.064(9) 0.028(9) -0.034(7) C53 0.094(9) 0.149(13) 0.110(9) 0.003(9) 0.027(7) 0.006(9) C54 0.107(9) 0.082(7) 0.180(12) -0.063(8) 0.000(9) -0.003(7) C56 0.22(2) 0.090(10) 0.27(2) -0.098(11) 0.122(18) -0.075(13) C57 0.086(7) 0.102(8) 0.143(10) -0.027(7) 0.034(7) 0.014(6) C58 0.138(12) 0.134(12) 0.133(11) 0.012(9) 0.049(10) -0.027(11) C59 0.193(16) 0.111(10) 0.188(15) 0.036(10) 0.096(13) 0.034(11) C60 0.099(8) 0.152(12) 0.114(10) -0.022(9) 0.036(7) -0.005(8) C62 0.094(9) 0.140(13) 0.127(10) 0.015(9) 0.032(8) -0.013(9) P1 0.0679(15) 0.0948(19) 0.0956(19) -0.0004(14) 0.0159(13) 0.0011(14) F1 0.132(6) 0.137(6) 0.215(8) 0.001(6) 0.011(6) -0.053(5) F2 0.127(6) 0.198(8) 0.180(7) 0.008(6) 0.066(5) 0.070(6) F3 0.124(5) 0.131(5) 0.105(4) -0.002(4) 0.043(4) 0.027(4) F4 0.137(6) 0.104(5) 0.188(7) -0.017(4) 0.047(5) -0.029(4) F5 0.117(4) 0.147(5) 0.094(4) 0.008(4) 0.029(3) 0.016(4) F6 0.149(6) 0.155(6) 0.113(5) 0.020(4) 0.007(4) 0.024(5) P2 0.096(2) 0.100(2) 0.154(3) -0.017(2) 0.057(2) -0.0047(18) F7 0.182(9) 0.273(13) 0.199(10) -0.050(9) 0.023(8) -0.077(10) F8 0.42(2) 0.177(9) 0.288(15) -0.063(9) 0.230(16) -0.121(12) F9 0.180(9) 0.167(8) 0.44(2) -0.060(10) 0.177(12) 0.002(7) F10 0.120(7) 0.381(19) 0.257(13) -0.162(13) -0.041(7) 0.026(9) F11 0.296(15) 0.229(12) 0.229(12) 0.053(10) 0.063(11) -0.097(12) F12 0.185(9) 0.217(11) 0.400(19) -0.135(13) 0.061(11) 0.065(9) O1W 0.66(6) 0.91(10) 0.35(4) -0.37(5) 0.20(4) -0.40(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C31 1.332(10) . ? N1 C9 1.338(10) . ? N1 C38 1.464(10) . ? N2 C6 1.299(10) . ? N2 C13 1.391(10) . ? N2 C27 1.485(10) . ? C1 C10 1.375(11) . ? C1 C8 1.375(10) . ? C1 C2 1.486(11) . ? C2 C26 1.367(11) . ? C2 C14 1.378(11) . ? C4 C24 1.369(11) . ? C4 C15 1.377(12) . ? C4 C27 1.499(11) . ? C6 C8 1.369(11) . ? C6 H6 0.9300 . ? C8 H8 0.9300 . ? C9 C14 1.360(12) . ? C9 H9 0.9300 . ? C10 C13 1.336(11) . ? C10 H10 0.9300 . ? C12 C28 1.383(12) . ? C12 C22 1.385(12) . ? C12 C38 1.469(12) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C40 1.390(14) . ? C15 H15 0.9300 . ? C17 C19 1.395(13) . ? C17 C40 1.399(14) . ? C17 H17 0.9300 . ? C18 C28 1.373(13) . ? C18 C23 1.387(12) . ? C18 C39 1.493(13) . ? C19 C24 1.382(12) . ? C19 C25 1.542(13) . ? C21 C23 1.372(12) . ? C21 C22 1.389(12) . ? C21 C29 1.515(13) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C66' 1.42(3) . ? C25 C64 1.448(19) . ? C25 C67 1.511(17) . ? C25 C66 1.56(3) . ? C26 C31 1.346(12) . ? C26 H26 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28 0.9300 . ? C29 C65' 1.50(5) . ? C29 C72 1.506(18) . ? C29 C46 1.510(15) . ? C29 C65 1.57(4) . ? C31 H31 0.9300 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C69 1.39(2) . ? C39 C61' 1.45(2) . ? C39 C61 1.53(2) . ? C39 C69' 1.56(2) . ? C39 C71' 1.581(17) . ? C39 C71 1.611(18) . ? C40 C55 1.516(15) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C55 C63 1.52(2) . ? C55 C70 1.56(2) . ? C55 C68 1.620(19) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C61' H61D 0.9600 . ? C61' H61E 0.9600 . ? C61' H61F 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C65' H65D 0.9600 . ? C65' H65E 0.9600 . ? C65' H65F 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C66' H66D 0.9600 . ? C66' H66E 0.9600 . ? C66' H66F 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C69' H69D 0.9600 . ? C69' H69E 0.9600 . ? C69' H69F 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C71' H71D 0.9600 . ? C71' H71E 0.9600 . ? C71' H71F 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? O1 C5 1.376(10) . ? O1 C42 1.426(11) . ? O2 C52 1.391(13) . ? O2 C45 1.407(12) . ? O3 C56 1.211(19) . ? O3 C54 1.373(14) . ? O4 C50 1.366(13) . ? O4 C37 1.433(15) . ? O5 C34 1.387(12) . ? O5 C57 1.406(14) . ? O6 C51 1.361(11) . ? O6 C30 1.420(13) . ? O7 C44 1.412(12) . ? O7 C41 1.438(11) . ? O8 C3 1.357(10) . ? O8 C35 1.428(11) . ? O9 C49 1.369(13) . ? O9 C60 1.404(14) . ? O10 C48 1.377(14) . ? O10 C59 1.422(16) . ? C3 C7 1.368(12) . ? C3 C16 1.388(12) . ? C5 C7 1.376(11) . ? C5 C11 1.376(12) . ? C7 H7 0.9300 . ? C11 C20 1.345(12) . ? C11 H11 0.9300 . ? C16 C20 1.395(12) . ? C16 H16 0.9300 . ? C20 C49 1.530(14) . ? C30 C57 1.506(15) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C32 C34 1.344(15) . ? C32 C43 1.365(17) . ? C32 H32 0.9300 . ? C33 C34 1.388(15) . ? C33 C37 1.394(14) . ? C33 H33 0.9300 . ? C35 C41 1.457(14) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C43 1.336(16) . ? C36 C37 1.359(17) . ? C36 H36 0.9300 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C45 1.449(14) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C48 1.526(18) . ? C44 C51 1.451(15) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C47 C53 1.150(19) . ? C47 C62 1.34(2) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C54 1.468(17) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C56 1.39(2) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C60 1.47(2) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C62 1.25(2) . ? C58 C59 1.45(2) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? P1 F1 1.541(8) . ? P1 F6 1.545(7) . ? P1 F2 1.546(7) . ? P1 F4 1.554(7) . ? P1 F3 1.596(6) . ? P1 F5 1.598(7) . ? P2 F10 1.469(10) . ? P2 F8 1.490(11) . ? P2 F12 1.521(10) . ? P2 F9 1.527(10) . ? P2 F11 1.529(11) . ? P2 F7 1.590(11) . ? 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 C31 N1 C9 119.6(7) . . ? C31 N1 C38 118.9(7) . . ? C9 N1 C38 121.5(7) . . ? C6 N2 C13 120.7(7) . . ? C6 N2 C27 121.9(7) . . ? C13 N2 C27 117.2(7) . . ? C10 C1 C8 118.1(8) . . ? C10 C1 C2 120.6(7) . . ? C8 C1 C2 121.3(7) . . ? C26 C2 C14 117.9(8) . . ? C26 C2 C1 122.3(7) . . ? C14 C2 C1 119.8(7) . . ? C24 C4 C15 121.2(8) . . ? C24 C4 C27 120.8(8) . . ? C15 C4 C27 118.0(8) . . ? N2 C6 C8 121.2(7) . . ? N2 C6 H6 119.4 . . ? C8 C6 H6 119.4 . . ? C6 C8 C1 119.7(8) . . ? C6 C8 H8 120.2 . . ? C1 C8 H8 120.2 . . ? N1 C9 C14 121.5(7) . . ? N1 C9 H9 119.3 . . ? C14 C9 H9 119.3 . . ? C13 C10 C1 121.4(7) . . ? C13 C10 H10 119.3 . . ? C1 C10 H10 119.3 . . ? C28 C12 C22 119.1(8) . . ? C28 C12 C38 121.7(8) . . ? C22 C12 C38 119.2(8) . . ? C10 C13 N2 118.9(8) . . ? C10 C13 H13 120.5 . . ? N2 C13 H13 120.5 . . ? C9 C14 C2 119.2(8) . . ? C9 C14 H14 120.4 . . ? C2 C14 H14 120.4 . . ? C4 C15 C40 119.6(8) . . ? C4 C15 H15 120.2 . . ? C40 C15 H15 120.2 . . ? C19 C17 C40 122.0(9) . . ? C19 C17 H17 119.0 . . ? C40 C17 H17 119.0 . . ? C28 C18 C23 117.1(8) . . ? C28 C18 C39 120.5(9) . . ? C23 C18 C39 122.4(9) . . ? C24 C19 C17 117.4(8) . . ? C24 C19 C25 121.5(8) . . ? C17 C19 C25 121.1(9) . . ? C23 C21 C22 116.9(8) . . ? C23 C21 C29 122.3(8) . . ? C22 C21 C29 120.8(8) . . ? C12 C22 C21 121.3(8) . . ? C12 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C21 C23 C18 124.0(8) . . ? C21 C23 H23 118.0 . . ? C18 C23 H23 118.0 . . ? C4 C24 C19 121.2(8) . . ? C4 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? C66' C25 C64 121.4(15) . . ? C66' C25 C67 98.0(15) . . ? C64 C25 C67 109.9(13) . . ? C66' C25 C19 107.4(14) . . ? C64 C25 C19 112.0(9) . . ? C67 C25 C19 106.6(10) . . ? C66' C25 C66 24.1(9) . . ? C64 C25 C66 98.9(14) . . ? C67 C25 C66 116.6(14) . . ? C19 C25 C66 112.9(13) . . ? C31 C26 C2 121.0(8) . . ? C31 C26 H26 119.5 . . ? C2 C26 H26 119.5 . . ? N2 C27 C4 110.4(6) . . ? N2 C27 H27A 109.6 . . ? C4 C27 H27A 109.6 . . ? N2 C27 H27B 109.6 . . ? C4 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C18 C28 C12 121.7(8) . . ? C18 C28 H28 119.2 . . ? C12 C28 H28 119.2 . . ? C65' C29 C72 98.2(15) . . ? C65' C29 C46 117.1(16) . . ? C72 C29 C46 108.7(11) . . ? C65' C29 C21 110.7(19) . . ? C72 C29 C21 108.2(9) . . ? C46 C29 C21 112.7(9) . . ? C65' C29 C65 20.4(13) . . ? C72 C29 C65 116.1(16) . . ? C46 C29 C65 100.3(16) . . ? C21 C29 C65 110.9(18) . . ? N1 C31 C26 120.7(8) . . ? N1 C31 H31 119.6 . . ? C26 C31 H31 119.6 . . ? N1 C38 C12 110.9(7) . . ? N1 C38 H38A 109.5 . . ? C12 C38 H38A 109.5 . . ? N1 C38 H38B 109.5 . . ? C12 C38 H38B 109.5 . . ? H38A C38 H38B 108.0 . . ? C69 C39 C61' 111.5(15) . . ? C69 C39 C18 111.6(11) . . ? C61' C39 C18 107.1(12) . . ? C69 C39 C61 129.5(14) . . ? C61' C39 C61 30.8(7) . . ? C18 C39 C61 112.4(12) . . ? C69 C39 C69' 29.3(7) . . ? C61' C39 C69' 83.7(14) . . ? C18 C39 C69' 113.8(11) . . ? C61 C39 C69' 107.8(13) . . ? C69 C39 C71' 121.0(13) . . ? C61' C39 C71' 87.8(12) . . ? C18 C39 C71' 114.5(9) . . ? C61 C39 C71' 57.6(10) . . ? C69' C39 C71' 131.3(12) . . ? C69 C39 C71 87.1(13) . . ? C61' C39 C71 130.7(12) . . ? C18 C39 C71 107.1(9) . . ? C61 C39 C71 102.4(11) . . ? C69' C39 C71 112.8(13) . . ? C71' C39 C71 45.6(8) . . ? C15 C40 C17 118.4(9) . . ? C15 C40 C55 121.0(12) . . ? C17 C40 C55 120.6(12) . . ? C29 C46 H46A 109.5 . . ? C29 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C29 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C40 C55 C63 112.5(13) . . ? C40 C55 C70 109.1(11) . . ? C63 C55 C70 110.9(14) . . ? C40 C55 C68 107.4(11) . . ? C63 C55 C68 109.9(13) . . ? C70 C55 C68 106.7(13) . . ? C39 C61 H61A 109.5 . . ? C39 C61 H61B 109.5 . . ? C39 C61 H61C 109.5 . . ? C39 C61' H61D 109.5 . . ? C39 C61' H61E 109.5 . . ? C39 C61' H61F 109.5 . . ? C55 C63 H63A 109.5 . . ? C55 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C55 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C25 C64 H64A 109.5 . . ? C25 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C25 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C29 C65 H65A 109.5 . . ? C29 C65 H65B 109.5 . . ? C29 C65 H65C 109.5 . . ? C29 C65' H65D 109.5 . . ? C29 C65' H65E 109.5 . . ? H65D C65' H65E 109.5 . . ? C29 C65' H65F 109.5 . . ? H65D C65' H65F 109.5 . . ? H65E C65' H65F 109.5 . . ? C25 C66 H66A 109.5 . . ? C25 C66 H66B 109.5 . . ? C25 C66 H66C 109.5 . . ? C25 C66' H66D 109.5 . . ? C25 C66' H66E 109.5 . . ? H66D C66' H66E 109.5 . . ? C25 C66' H66F 109.5 . . ? H66D C66' H66F 109.5 . . ? H66E C66' H66F 109.5 . . ? C25 C67 H67A 109.5 . . ? C25 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C25 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C55 C68 H68A 109.5 . . ? C55 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C55 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C39 C69 H69A 109.5 . . ? C39 C69 H69B 109.5 . . ? C39 C69 H69C 109.5 . . ? C39 C69' H69D 109.5 . . ? C39 C69' H69E 109.5 . . ? H69D C69' H69E 109.5 . . ? C39 C69' H69F 109.5 . . ? H69D C69' H69F 109.5 . . ? H69E C69' H69F 109.5 . . ? C55 C70 H70A 109.5 . . ? C55 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C55 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C39 C71 H71A 109.5 . . ? C39 C71 H71B 109.5 . . ? C39 C71 H71C 109.5 . . ? C39 C71' H71D 109.5 . . ? C39 C71' H71E 109.5 . . ? H71D C71' H71E 109.5 . . ? C39 C71' H71F 109.5 . . ? H71D C71' H71F 109.5 . . ? H71E C71' H71F 109.5 . . ? C29 C72 H72A 109.5 . . ? C29 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C29 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C5 O1 C42 118.4(7) . . ? C52 O2 C45 112.9(9) . . ? C56 O3 C54 123.9(12) . . ? C50 O4 C37 122.3(11) . . ? C34 O5 C57 118.8(10) . . ? C51 O6 C30 115.3(8) . . ? C44 O7 C41 111.6(8) . . ? C3 O8 C35 118.5(8) . . ? C49 O9 C60 113.4(9) . . ? C48 O10 C59 112.1(11) . . ? O8 C3 C7 116.1(8) . . ? O8 C3 C16 124.7(8) . . ? C7 C3 C16 119.2(8) . . ? C7 C5 C11 120.2(8) . . ? C7 C5 O1 115.1(8) . . ? C11 C5 O1 124.7(8) . . ? C3 C7 C5 120.9(8) . . ? C3 C7 H7 119.6 . . ? C5 C7 H7 119.6 . . ? C20 C11 C5 119.2(9) . . ? C20 C11 H11 120.4 . . ? C5 C11 H11 120.4 . . ? C3 C16 C20 118.6(9) . . ? C3 C16 H16 120.7 . . ? C20 C16 H16 120.7 . . ? C11 C20 C16 121.8(9) . . ? C11 C20 C49 122.7(9) . . ? C16 C20 C49 115.3(9) . . ? O6 C30 C57 106.9(8) . . ? O6 C30 H30A 110.3 . . ? C57 C30 H30A 110.3 . . ? O6 C30 H30B 110.3 . . ? C57 C30 H30B 110.3 . . ? H30A C30 H30B 108.6 . . ? C34 C32 C43 118.5(13) . . ? C34 C32 H32 120.7 . . ? C43 C32 H32 120.7 . . ? C34 C33 C37 115.3(12) . . ? C34 C33 H33 122.3 . . ? C37 C33 H33 122.3 . . ? C32 C34 O5 116.3(12) . . ? C32 C34 C33 122.8(11) . . ? O5 C34 C33 120.8(12) . . ? O8 C35 C41 109.2(9) . . ? O8 C35 H35A 109.8 . . ? C41 C35 H35A 109.8 . . ? O8 C35 H35B 109.8 . . ? C41 C35 H35B 109.8 . . ? H35A C35 H35B 108.3 . . ? C43 C36 C37 118.7(13) . . ? C43 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C36 C37 C33 122.4(13) . . ? C36 C37 O4 124.7(11) . . ? C33 C37 O4 112.8(13) . . ? O7 C41 C35 108.1(8) . . ? O7 C41 H41A 110.1 . . ? C35 C41 H41A 110.1 . . ? O7 C41 H41B 110.1 . . ? C35 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? O1 C42 C45 110.0(8) . . ? O1 C42 H42A 109.7 . . ? C45 C42 H42A 109.7 . . ? O1 C42 H42B 109.7 . . ? C45 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? C36 C43 C32 122.1(14) . . ? C36 C43 C48 118.9(14) . . ? C32 C43 C48 118.9(14) . . ? O7 C44 C51 111.7(9) . . ? O7 C44 H44A 109.3 . . ? C51 C44 H44A 109.3 . . ? O7 C44 H44B 109.3 . . ? C51 C44 H44B 109.3 . . ? H44A C44 H44B 107.9 . . ? O2 C45 C42 110.2(9) . . ? O2 C45 H45A 109.6 . . ? C42 C45 H45A 109.6 . . ? O2 C45 H45B 109.6 . . ? C42 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? C53 C47 C62 177.3(16) . . ? O10 C48 C43 106.2(10) . . ? O10 C48 H48A 110.5 . . ? C43 C48 H48A 110.5 . . ? O10 C48 H48B 110.5 . . ? C43 C48 H48B 110.5 . . ? H48A C48 H48B 108.7 . . ? O9 C49 C20 114.9(10) . . ? O9 C49 H49A 108.6 . . ? C20 C49 H49A 108.6 . . ? O9 C49 H49B 108.6 . . ? C20 C49 H49B 108.6 . . ? H49A C49 H49B 107.5 . . ? O4 C50 C54 111.4(10) . . ? O4 C50 H50A 109.4 . . ? C54 C50 H50A 109.4 . . ? O4 C50 H50B 109.4 . . ? C54 C50 H50B 109.4 . . ? H50A C50 H50B 108.0 . . ? O6 C51 C44 109.7(9) . . ? O6 C51 H51A 109.7 . . ? C44 C51 H51A 109.7 . . ? O6 C51 H51B 109.7 . . ? C44 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? O2 C52 C56 114.6(11) . . ? O2 C52 H52A 108.6 . . ? C56 C52 H52A 108.6 . . ? O2 C52 H52B 108.6 . . ? C56 C52 H52B 108.6 . . ? H52A C52 H52B 107.6 . . ? C47 C53 C60 178.8(15) . . ? O3 C54 C50 114.2(12) . . ? O3 C54 H54A 108.7 . . ? C50 C54 H54A 108.7 . . ? O3 C54 H54B 108.7 . . ? C50 C54 H54B 108.7 . . ? H54A C54 H54B 107.6 . . ? O3 C56 C52 132.7(14) . . ? O3 C56 H56A 104.0 . . ? C52 C56 H56A 104.0 . . ? O3 C56 H56B 104.0 . . ? C52 C56 H56B 104.0 . . ? H56A C56 H56B 105.5 . . ? O5 C57 C30 108.2(10) . . ? O5 C57 H57A 110.1 . . ? C30 C57 H57A 110.1 . . ? O5 C57 H57B 110.1 . . ? C30 C57 H57B 110.1 . . ? H57A C57 H57B 108.4 . . ? C62 C58 C59 177.0(17) . . ? O10 C59 C58 105.3(11) . . ? O10 C59 H59A 110.7 . . ? C58 C59 H59A 110.7 . . ? O10 C59 H59B 110.7 . . ? C58 C59 H59B 110.7 . . ? H59A C59 H59B 108.8 . . ? O9 C60 C53 111.6(10) . . ? O9 C60 H60A 109.3 . . ? C53 C60 H60A 109.3 . . ? O9 C60 H60B 109.3 . . ? C53 C60 H60B 109.3 . . ? H60A C60 H60B 108.0 . . ? C58 C62 C47 174.1(14) . . ? F1 P1 F6 91.2(5) . . ? F1 P1 F2 90.0(6) . . ? F6 P1 F2 91.8(5) . . ? F1 P1 F4 176.1(5) . . ? F6 P1 F4 91.9(5) . . ? F2 P1 F4 92.3(5) . . ? F1 P1 F3 89.9(5) . . ? F6 P1 F3 92.1(4) . . ? F2 P1 F3 176.1(4) . . ? F4 P1 F3 87.7(4) . . ? F1 P1 F5 88.1(5) . . ? F6 P1 F5 178.6(4) . . ? F2 P1 F5 89.5(4) . . ? F4 P1 F5 88.7(4) . . ? F3 P1 F5 86.6(3) . . ? F10 P2 F8 81.1(10) . . ? F10 P2 F12 94.9(7) . . ? F8 P2 F12 89.2(9) . . ? F10 P2 F9 87.9(7) . . ? F8 P2 F9 89.2(8) . . ? F12 P2 F9 176.5(9) . . ? F10 P2 F11 104.4(10) . . ? F8 P2 F11 170.1(10) . . ? F12 P2 F11 98.4(10) . . ? F9 P2 F11 82.9(8) . . ? F10 P2 F7 172.4(10) . . ? F8 P2 F7 91.3(9) . . ? F12 P2 F7 85.9(8) . . ? F9 P2 F7 91.1(8) . . ? F11 P2 F7 82.9(7) . . ? 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 C10 C1 C2 C26 142.3(8) . . . . ? C8 C1 C2 C26 -38.9(10) . . . . ? C10 C1 C2 C14 -38.5(10) . . . . ? C8 C1 C2 C14 140.3(8) . . . . ? C13 N2 C6 C8 -1.1(11) . . . . ? C27 N2 C6 C8 -176.2(7) . . . . ? N2 C6 C8 C1 1.7(11) . . . . ? C10 C1 C8 C6 -1.4(10) . . . . ? C2 C1 C8 C6 179.8(7) . . . . ? C31 N1 C9 C14 -1.6(12) . . . . ? C38 N1 C9 C14 175.5(8) . . . . ? C8 C1 C10 C13 0.6(11) . . . . ? C2 C1 C10 C13 179.4(7) . . . . ? C1 C10 C13 N2 -0.1(11) . . . . ? C6 N2 C13 C10 0.3(11) . . . . ? C27 N2 C13 C10 175.6(7) . . . . ? N1 C9 C14 C2 -2.1(13) . . . . ? C26 C2 C14 C9 4.1(12) . . . . ? C1 C2 C14 C9 -175.1(7) . . . . ? C24 C4 C15 C40 4.0(13) . . . . ? C27 C4 C15 C40 -176.0(8) . . . . ? C40 C17 C19 C24 2.7(14) . . . . ? C40 C17 C19 C25 -176.4(9) . . . . ? C28 C12 C22 C21 -1.4(12) . . . . ? C38 C12 C22 C21 177.2(8) . . . . ? C23 C21 C22 C12 0.7(13) . . . . ? C29 C21 C22 C12 178.0(9) . . . . ? C22 C21 C23 C18 -0.6(14) . . . . ? C29 C21 C23 C18 -177.9(9) . . . . ? C28 C18 C23 C21 1.3(14) . . . . ? C39 C18 C23 C21 179.8(10) . . . . ? C15 C4 C24 C19 0.5(13) . . . . ? C27 C4 C24 C19 -179.5(8) . . . . ? C17 C19 C24 C4 -3.8(13) . . . . ? C25 C19 C24 C4 175.3(8) . . . . ? C24 C19 C25 C66' -160.0(13) . . . . ? C17 C19 C25 C66' 19.0(16) . . . . ? C24 C19 C25 C64 -24.5(16) . . . . ? C17 C19 C25 C64 154.6(13) . . . . ? C24 C19 C25 C67 95.8(13) . . . . ? C17 C19 C25 C67 -85.2(13) . . . . ? C24 C19 C25 C66 -135.0(13) . . . . ? C17 C19 C25 C66 44.1(16) . . . . ? C14 C2 C26 C31 -2.5(12) . . . . ? C1 C2 C26 C31 176.6(7) . . . . ? C6 N2 C27 C4 97.4(8) . . . . ? C13 N2 C27 C4 -77.8(8) . . . . ? C24 C4 C27 N2 -94.2(9) . . . . ? C15 C4 C27 N2 85.8(9) . . . . ? C23 C18 C28 C12 -2.0(13) . . . . ? C39 C18 C28 C12 179.5(9) . . . . ? C22 C12 C28 C18 2.1(13) . . . . ? C38 C12 C28 C18 -176.4(8) . . . . ? C23 C21 C29 C65' -14.4(17) . . . . ? C22 C21 C29 C65' 168.5(13) . . . . ? C23 C21 C29 C72 92.1(12) . . . . ? C22 C21 C29 C72 -85.0(12) . . . . ? C23 C21 C29 C46 -147.7(11) . . . . ? C22 C21 C29 C46 35.2(14) . . . . ? C23 C21 C29 C65 -36.3(17) . . . . ? C22 C21 C29 C65 146.6(13) . . . . ? C9 N1 C31 C26 3.2(12) . . . . ? C38 N1 C31 C26 -173.9(8) . . . . ? C2 C26 C31 N1 -1.1(13) . . . . ? C31 N1 C38 C12 70.9(10) . . . . ? C9 N1 C38 C12 -106.2(9) . . . . ? C28 C12 C38 N1 74.3(10) . . . . ? C22 C12 C38 N1 -104.2(9) . . . . ? C28 C18 C39 C69 -56.2(16) . . . . ? C23 C18 C39 C69 125.4(13) . . . . ? C28 C18 C39 C61' 66.1(15) . . . . ? C23 C18 C39 C61' -112.3(13) . . . . ? C28 C18 C39 C61 98.4(13) . . . . ? C23 C18 C39 C61 -80.1(15) . . . . ? C28 C18 C39 C69' -24.5(16) . . . . ? C23 C18 C39 C69' 157.1(12) . . . . ? C28 C18 C39 C71' 161.7(10) . . . . ? C23 C18 C39 C71' -16.8(16) . . . . ? C28 C18 C39 C71 -149.9(10) . . . . ? C23 C18 C39 C71 31.6(14) . . . . ? C4 C15 C40 C17 -5.0(13) . . . . ? C4 C15 C40 C55 177.1(9) . . . . ? C19 C17 C40 C15 1.6(14) . . . . ? C19 C17 C40 C55 179.6(10) . . . . ? C15 C40 C55 C63 -177.7(13) . . . . ? C17 C40 C55 C63 4.5(17) . . . . ? C15 C40 C55 C70 58.8(15) . . . . ? C17 C40 C55 C70 -119.1(14) . . . . ? C15 C40 C55 C68 -56.5(15) . . . . ? C17 C40 C55 C68 125.6(12) . . . . ? C35 O8 C3 C7 -174.3(7) . . . . ? C35 O8 C3 C16 4.1(11) . . . . ? C42 O1 C5 C7 165.4(7) . . . . ? C42 O1 C5 C11 -14.6(12) . . . . ? O8 C3 C7 C5 175.1(7) . . . . ? C16 C3 C7 C5 -3.3(11) . . . . ? C11 C5 C7 C3 3.7(12) . . . . ? O1 C5 C7 C3 -176.4(7) . . . . ? C7 C5 C11 C20 -1.1(12) . . . . ? O1 C5 C11 C20 178.9(8) . . . . ? O8 C3 C16 C20 -177.8(7) . . . . ? C7 C3 C16 C20 0.5(12) . . . . ? C5 C11 C20 C16 -1.7(13) . . . . ? C5 C11 C20 C49 174.3(10) . . . . ? C3 C16 C20 C11 2.0(13) . . . . ? C3 C16 C20 C49 -174.3(9) . . . . ? C51 O6 C30 C57 179.1(10) . . . . ? C43 C32 C34 O5 174.6(8) . . . . ? C43 C32 C34 C33 -0.8(14) . . . . ? C57 O5 C34 C32 177.5(9) . . . . ? C57 O5 C34 C33 -7.0(13) . . . . ? C37 C33 C34 C32 0.7(13) . . . . ? C37 C33 C34 O5 -174.5(8) . . . . ? C3 O8 C35 C41 172.5(8) . . . . ? C43 C36 C37 C33 0.8(15) . . . . ? C43 C36 C37 O4 -175.2(9) . . . . ? C34 C33 C37 C36 -0.7(13) . . . . ? C34 C33 C37 O4 175.8(8) . . . . ? C50 O4 C37 C36 -23.5(15) . . . . ? C50 O4 C37 C33 160.1(10) . . . . ? C44 O7 C41 C35 176.5(9) . . . . ? O8 C35 C41 O7 -75.7(11) . . . . ? C5 O1 C42 C45 -178.9(8) . . . . ? C37 C36 C43 C32 -1.0(15) . . . . ? C37 C36 C43 C48 176.8(9) . . . . ? C34 C32 C43 C36 0.9(15) . . . . ? C34 C32 C43 C48 -176.8(9) . . . . ? C41 O7 C44 C51 173.7(9) . . . . ? C52 O2 C45 C42 171.3(11) . . . . ? O1 C42 C45 O2 62.6(12) . . . . ? C59 O10 C48 C43 -177.8(13) . . . . ? C36 C43 C48 O10 -93.2(13) . . . . ? C32 C43 C48 O10 84.6(14) . . . . ? C60 O9 C49 C20 105.3(13) . . . . ? C11 C20 C49 O9 13.8(17) . . . . ? C16 C20 C49 O9 -170.0(10) . . . . ? C37 O4 C50 C54 127.9(13) . . . . ? C30 O6 C51 C44 160.5(10) . . . . ? O7 C44 C51 O6 63.8(13) . . . . ? C45 O2 C52 C56 170.9(14) . . . . ? C62 C47 C53 C60 137(58) . . . . ? C56 O3 C54 C50 -106(2) . . . . ? O4 C50 C54 O3 -61.1(17) . . . . ? C54 O3 C56 C52 -165.2(19) . . . . ? O2 C52 C56 O3 -41(3) . . . . ? C34 O5 C57 C30 166.7(8) . . . . ? O6 C30 C57 O5 -77.7(12) . . . . ? C48 O10 C59 C58 175.8(13) . . . . ? C62 C58 C59 O10 -76(31) . . . . ? C49 O9 C60 C53 -84.9(12) . . . . ? C47 C53 C60 O9 -13(72) . . . . ? C59 C58 C62 C47 22(43) . . . . ? C53 C47 C62 C58 -38(42) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.910 _refine_diff_density_min -1.485 _refine_diff_density_rms 0.100