Supplementary Material (ESI) for Chemical Communiations This journal is (C) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email loeb@uwindsor.ca _publ_contact_author_name 'Prof Stephen Loeb' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Chemistry & Biochemistry University of Windsor Windsor Ontario N9B 3P4 CANADA ; _publ_contact_author_phone '+ 519 253-3000 ext 3529' _publ_contact_author_fax '+ 519 973-7098 ' _publ_requested_coeditor_name ? _publ_contact_letter ; This structure is part of a study on the synthesis and inclusion properties of a [3]catenane employimg the 1,2-bis(4,4'-bipyridinium)ethane /dibenzo-24-crown-8 ether motif ; _publ_section_title ; Host-guest interactions template the synthesis of a [3]catenane ; loop_ _publ_author_name _publ_author_address S.J.Loeb ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; G.J.E.Davidson ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; R.H.Patel ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; A.L.Hubbard ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; J.A.Wisner ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; data_([3]catenane.(DB24C8.(H2O)2)).2H2O _database_code_depnum_ccdc_archive 'CCDC 221795' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ([3]catenane.(DB24C8.(H2O)2)).2H2O _chemical_formula_sum 'C164 H176 F24 N8 O52 S8' _chemical_formula_weight 3803.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.531(3) _cell_length_b 18.149(4) _cell_length_c 19.061(4) _cell_angle_alpha 63.152(3) _cell_angle_beta 77.773(4) _cell_angle_gamma 89.381(4) _cell_volume 4362.3(15) _cell_formula_units_Z 1 _cell_measurement_temperature 173.5(1) _cell_measurement_reflns_used 'reflections from 120 data frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.116733 _exptl_absorpt_correction_T_max 0.256608 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.5(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 standard frames at start and end' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 13929 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 20.00 _reflns_number_total 8092 _reflns_number_gt 6653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.0817P)^2^+17.8291P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8092 _refine_ls_number_parameters 1155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.2161 _refine_ls_wR_factor_gt 0.2031 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 3.1311(3) -0.7076(3) 1.0734(3) 0.0483(14) Uani 1 1 d . . . O2 O 3.2098(4) -0.6570(3) 0.9024(3) 0.0507(14) Uani 1 1 d . . . O3 O 3.1736(4) -0.7471(6) 0.8190(4) 0.086(2) Uani 1 1 d . . . O4 O 3.0069(5) -0.8320(5) 0.8162(4) 0.085(2) Uani 1 1 d . . . O5 O 2.8477(4) -0.8947(3) 0.9231(4) 0.0543(15) Uani 1 1 d . . . O6 O 2.8139(4) -0.9694(3) 1.1019(3) 0.0527(14) Uani 1 1 d . . . O7 O 2.8077(3) -0.8468(3) 1.1531(3) 0.0453(13) Uani 1 1 d . . . O8 O 2.9816(4) -0.7931(3) 1.1811(3) 0.0467(14) Uani 1 1 d . . . O9 O 2.7115(4) -0.5322(4) 0.9561(4) 0.0635(16) Uani 1 1 d . . . O10 O 2.7146(4) -0.5542(3) 1.1127(3) 0.0615(16) Uani 1 1 d . . . O11 O 2.8887(4) -0.6027(4) 1.1617(4) 0.0701(17) Uani 1 1 d . . . O12 O 2.8697(4) -0.4632(4) 0.8568(3) 0.0631(16) Uani 1 1 d . . . N1 N 2.6597(4) -0.5792(3) 0.6415(4) 0.0323(14) Uani 1 1 d . . . N2 N 2.9238(4) -0.7099(3) 0.9345(3) 0.0310(14) Uani 1 1 d . . . N3 N 3.0607(4) -0.8769(4) 1.0528(4) 0.0329(15) Uani 1 1 d . . . N4 N 3.3384(4) -1.0676(3) 1.3318(4) 0.0360(15) Uani 1 1 d . . . C1 C 2.4364(5) -0.2279(4) 0.5899(4) 0.0347(18) Uani 1 1 d . . . H1A H 2.5005 -0.2296 0.5894 0.042 Uiso 1 1 calc R . . C2 C 2.3897(5) -0.2902(4) 0.5831(4) 0.0324(18) Uani 1 1 d . . . C3 C 2.2949(5) -0.2866(5) 0.5835(4) 0.041(2) Uani 1 1 d . . . H3A H 2.2624 -0.3276 0.5790 0.049 Uiso 1 1 calc R . . C4 C 2.4426(5) -0.3579(5) 0.5765(4) 0.0351(19) Uani 1 1 d . . . C5 C 2.4001(5) -0.4388(4) 0.6141(4) 0.0348(18) Uani 1 1 d . . . H5A H 2.3365 -0.4500 0.6405 0.042 Uiso 1 1 calc R . . C6 C 2.4520(5) -0.5032(5) 0.6127(4) 0.0375(19) Uani 1 1 d . . . H6A H 2.4227 -0.5570 0.6384 0.045 Uiso 1 1 calc R . . C7 C 2.5460(5) -0.4882(5) 0.5736(4) 0.0341(18) Uani 1 1 d . . . C8 C 2.5875(5) -0.4077(5) 0.5337(5) 0.043(2) Uani 1 1 d . . . H8A H 2.6506 -0.3963 0.5058 0.051 Uiso 1 1 calc R . . C9 C 2.5356(5) -0.3435(5) 0.5348(5) 0.042(2) Uani 1 1 d . . . H9A H 2.5643 -0.2894 0.5067 0.051 Uiso 1 1 calc R . . C10 C 2.6045(5) -0.5583(5) 0.5774(4) 0.0391(19) Uani 1 1 d . . . H10A H 2.5636 -0.6066 0.5901 0.047 Uiso 1 1 calc R . . H10B H 2.6477 -0.5422 0.5254 0.047 Uiso 1 1 calc R . . C11 C 2.6152(5) -0.6111(5) 0.7187(5) 0.0397(19) Uani 1 1 d . . . H11A H 2.5496 -0.6207 0.7324 0.048 Uiso 1 1 calc R . . C12 C 2.6617(5) -0.6304(4) 0.7785(4) 0.0335(18) Uani 1 1 d . . . H12A H 2.6281 -0.6525 0.8320 0.040 Uiso 1 1 calc R . . C13 C 2.7599(5) -0.6169(4) 0.7595(4) 0.0296(17) Uani 1 1 d . . . C14 C 2.8046(5) -0.5813(4) 0.6783(5) 0.0368(19) Uani 1 1 d . . . H14A H 2.8701 -0.5702 0.6629 0.044 Uiso 1 1 calc R . . C15 C 2.7542(5) -0.5622(4) 0.6202(4) 0.0389(19) Uani 1 1 d . . . H15A H 2.7854 -0.5374 0.5659 0.047 Uiso 1 1 calc R . . C16 C 2.8158(5) -0.6446(4) 0.8218(4) 0.0295(17) Uani 1 1 d . . . C17 C 2.7759(5) -0.6975(4) 0.9008(4) 0.0353(19) Uani 1 1 d . . . H17A H 2.7108 -0.7117 0.9169 0.042 Uiso 1 1 calc R . . C18 C 2.8294(5) -0.7299(5) 0.9564(4) 0.040(2) Uani 1 1 d . . . H18A H 2.8007 -0.7661 1.0099 0.048 Uiso 1 1 calc R . . C19 C 2.9636(5) -0.6556(5) 0.8594(5) 0.042(2) Uani 1 1 d . . . H19A H 3.0284 -0.6405 0.8453 0.050 Uiso 1 1 calc R . . C20 C 2.9127(5) -0.6212(5) 0.8018(4) 0.042(2) Uani 1 1 d . . . H20A H 2.9422 -0.5824 0.7496 0.051 Uiso 1 1 calc R . . C21 C 2.9824(5) -0.7508(4) 0.9927(4) 0.0378(19) Uani 1 1 d . . . H21A H 2.9489 -0.7600 1.0462 0.045 Uiso 1 1 calc R . . H21B H 3.0407 -0.7161 0.9773 0.045 Uiso 1 1 calc R . . C22 C 3.0038(5) -0.8318(4) 0.9935(5) 0.042(2) Uani 1 1 d . . . H22A H 2.9451 -0.8654 1.0071 0.050 Uiso 1 1 calc R . . H22B H 3.0382 -0.8220 0.9401 0.050 Uiso 1 1 calc R . . C23 C 3.0209(5) -0.9386(5) 1.1262(5) 0.0367(19) Uani 1 1 d . . . H23A H 2.9565 -0.9548 1.1392 0.044 Uiso 1 1 calc R . . C24 C 3.0728(5) -0.9782(4) 1.1823(4) 0.0355(18) Uani 1 1 d . . . H24A H 3.0438 -1.0202 1.2331 0.043 Uiso 1 1 calc R . . C25 C 3.1702(5) -0.9549(4) 1.1624(4) 0.0280(17) Uani 1 1 d . . . C26 C 3.2086(5) -0.8922(4) 1.0875(5) 0.0373(19) Uani 1 1 d . . . H26A H 3.2729 -0.8751 1.0732 0.045 Uiso 1 1 calc R . . C27 C 3.1544(5) -0.8536(4) 1.0327(5) 0.0372(19) Uani 1 1 d . . . H27A H 3.1822 -0.8113 0.9816 0.045 Uiso 1 1 calc R . . C28 C 3.2273(5) -0.9961(4) 1.2221(4) 0.0306(18) Uani 1 1 d . . . C29 C 3.1891(5) -1.0344(5) 1.3037(5) 0.0389(19) Uani 1 1 d . . . H29A H 3.1244 -1.0357 1.3226 0.047 Uiso 1 1 calc R . . C30 C 3.2445(6) -1.0710(4) 1.3580(5) 0.040(2) Uani 1 1 d . . . H30A H 3.2169 -1.0983 1.4131 0.048 Uiso 1 1 calc R . . C31 C 3.3776(5) -1.0324(4) 1.2530(5) 0.0383(19) Uani 1 1 d . . . H31A H 3.4423 -1.0330 1.2355 0.046 Uiso 1 1 calc R . . C32 C 3.3247(5) -0.9955(4) 1.1976(5) 0.0362(19) Uani 1 1 d . . . H32A H 3.3539 -0.9697 1.1428 0.043 Uiso 1 1 calc R . . C33 C 3.3997(6) -1.1011(4) 1.3903(5) 0.045(2) Uani 1 1 d . . . H33A H 3.4432 -1.1356 1.3759 0.054 Uiso 1 1 calc R . . H33B H 3.3610 -1.1352 1.4441 0.054 Uiso 1 1 calc R . . C34 C 3.4552(5) -1.0302(5) 1.3898(4) 0.0378(19) Uani 1 1 d . . . C35 C 3.4139(7) -0.9622(6) 1.3892(7) 0.082(3) Uani 1 1 d . . . H35A H 3.3505 -0.9580 1.3874 0.099 Uiso 1 1 calc R . . C36 C 2.4035(5) -0.0276(5) 0.6022(5) 0.054(2) Uani 1 1 d . . . H36A H 2.3411 -0.0214 0.5973 0.064 Uiso 1 1 calc R . . C37 C 2.4426(5) -0.0968(4) 0.6039(4) 0.0348(19) Uani 1 1 d . . . C38 C 2.5356(6) -0.1007(6) 0.6089(6) 0.073(3) Uani 1 1 d . . . H38A H 2.5655 -0.1469 0.6109 0.087 Uiso 1 1 calc R . . C39 C 3.5472(6) -1.0338(5) 1.3927(5) 0.052(2) Uani 1 1 d . . . H39A H 3.5780 -1.0785 1.3911 0.063 Uiso 1 1 calc R . . C40 C 2.3905(5) -0.1632(4) 0.5973(4) 0.0339(18) Uani 1 1 d . . . C41 C 2.2940(5) -0.1615(5) 0.5970(4) 0.0398(19) Uani 1 1 d . . . H41A H 2.2611 -0.1188 0.6011 0.048 Uiso 1 1 calc R . . C42 C 2.2481(5) -0.2236(5) 0.5904(5) 0.042(2) Uani 1 1 d . . . H42A H 2.1840 -0.2225 0.5907 0.051 Uiso 1 1 calc R . . C43 C 3.0624(6) -0.7984(5) 1.2092(5) 0.039(2) Uani 1 1 d . . . C44 C 3.0679(6) -0.8435(5) 1.2880(5) 0.050(2) Uani 1 1 d . . . H44A H 3.0139 -0.8732 1.3276 0.060 Uiso 1 1 calc R . . C45 C 3.1538(7) -0.8447(6) 1.3088(5) 0.060(2) Uani 1 1 d . . . H45A H 3.1576 -0.8755 1.3623 0.072 Uiso 1 1 calc R . . C46 C 3.2333(7) -0.8005(6) 1.2506(7) 0.064(3) Uani 1 1 d . . . H46A H 3.2908 -0.8018 1.2651 0.077 Uiso 1 1 calc R . . C47 C 3.2290(6) -0.7543(5) 1.1711(6) 0.055(2) Uani 1 1 d . . . H47A H 3.2833 -0.7251 1.1318 0.066 Uiso 1 1 calc R . . C48 C 3.1427(5) -0.7518(5) 1.1502(5) 0.040(2) Uani 1 1 d . . . C49 C 3.1929(6) -0.6349(5) 1.0179(5) 0.058(2) Uani 1 1 d . . . H49A H 3.2276 -0.6182 1.0475 0.069 Uiso 1 1 calc R . . H49B H 3.1555 -0.5903 0.9917 0.069 Uiso 1 1 calc R . . C50 C 3.2600(6) -0.6472(5) 0.9564(6) 0.059(2) Uani 1 1 d . . . H50A H 3.3073 -0.5998 0.9259 0.071 Uiso 1 1 calc R . . H50B H 3.2921 -0.6962 0.9818 0.071 Uiso 1 1 calc R . . C51 C 3.2722(6) -0.6570(6) 0.8342(5) 0.060(2) Uani 1 1 d . . . H51A H 3.3123 -0.7017 0.8524 0.073 Uiso 1 1 calc R . . H51B H 3.3126 -0.6051 0.8045 0.073 Uiso 1 1 calc R . . C52 C 3.2212(7) -0.6672(7) 0.7806(5) 0.074(3) Uani 1 1 d . . . H52A H 3.1760 -0.6262 0.7667 0.088 Uiso 1 1 calc R . . H52B H 3.2653 -0.6588 0.7311 0.088 Uiso 1 1 calc R . . C53 C 3.1589(10) -0.7766(17) 0.7651(12) 0.260(16) Uani 1 1 d . . . H53A H 3.1802 -0.7294 0.7122 0.312 Uiso 1 1 calc R . . H53B H 3.2058 -0.8158 0.7684 0.312 Uiso 1 1 calc R . . C54 C 3.0966(10) -0.8055(11) 0.7603(9) 0.157(8) Uani 1 1 d . . . H54A H 3.1171 -0.8540 0.7548 0.188 Uiso 1 1 calc R . . H54B H 3.0837 -0.7672 0.7088 0.188 Uiso 1 1 calc R . . C55 C 2.9272(7) -0.8181(6) 0.7868(7) 0.065(3) Uani 1 1 d . . . C56 C 2.9249(9) -0.7753(7) 0.7058(8) 0.085(3) Uani 1 1 d . . . H56A H 2.9810 -0.7527 0.6666 0.103 Uiso 1 1 calc R . . C57 C 2.8392(12) -0.7660(6) 0.6830(7) 0.088(4) Uani 1 1 d . . . H57A H 2.8389 -0.7386 0.6284 0.106 Uiso 1 1 calc R . . C58 C 2.7566(8) -0.7958(6) 0.7383(7) 0.068(3) Uani 1 1 d . . . H58A H 2.6998 -0.7887 0.7220 0.082 Uiso 1 1 calc R . . C59 C 2.7566(7) -0.8375(5) 0.8203(6) 0.058(2) Uani 1 1 d . . . H59A H 2.6995 -0.8565 0.8588 0.070 Uiso 1 1 calc R . . C60 C 2.8406(6) -0.8506(5) 0.8444(6) 0.048(2) Uani 1 1 d . . . C61 C 2.7660(6) -0.9466(5) 0.9787(5) 0.054(2) Uani 1 1 d . . . H61A H 2.7392 -0.9773 0.9560 0.064 Uiso 1 1 calc R . . H61B H 2.7185 -0.9137 0.9912 0.064 Uiso 1 1 calc R . . C62 C 2.7962(6) -1.0050(5) 1.0533(6) 0.061(2) Uani 1 1 d . . . H62A H 2.7473 -1.0509 1.0855 0.073 Uiso 1 1 calc R . . H62B H 2.8531 -1.0275 1.0376 0.073 Uiso 1 1 calc R . . C63 C 2.7315(6) -0.9586(5) 1.1498(5) 0.058(2) Uani 1 1 d . . . H63A H 2.6931 -1.0113 1.1829 0.069 Uiso 1 1 calc R . . H63B H 2.6944 -0.9201 1.1152 0.069 Uiso 1 1 calc R . . C64 C 2.7573(6) -0.9265(5) 1.2021(5) 0.052(2) Uani 1 1 d . . . H64A H 2.7007 -0.9228 1.2374 0.062 Uiso 1 1 calc R . . H64B H 2.7964 -0.9639 1.2354 0.062 Uiso 1 1 calc R . . C65 C 2.8151(5) -0.8008(5) 1.1963(5) 0.054(2) Uani 1 1 d . . . H65A H 2.7557 -0.8100 1.2350 0.065 Uiso 1 1 calc R . . H65B H 2.8257 -0.7421 1.1585 0.065 Uiso 1 1 calc R . . C66 C 2.8936(5) -0.8240(5) 1.2405(5) 0.052(2) Uani 1 1 d . . . H66A H 2.8880 -0.7996 1.2770 0.062 Uiso 1 1 calc R . . H66B H 2.8905 -0.8838 1.2719 0.062 Uiso 1 1 calc R . . C67 C 2.7933(7) -0.4490(5) 0.8227(6) 0.056(2) Uani 1 1 d . . . C68 C 2.7961(7) -0.4035(6) 0.7423(6) 0.066(3) Uani 1 1 d . . . H68A H 2.8537 -0.3789 0.7058 0.080 Uiso 1 1 calc R . . C69 C 2.7128(8) -0.3934(6) 0.7143(6) 0.073(3) Uani 1 1 d . . . H69A H 2.7149 -0.3613 0.6597 0.088 Uiso 1 1 calc R . . C70 C 2.6288(7) -0.4309(7) 0.7677(8) 0.081(3) Uani 1 1 d . . . H70A H 2.5738 -0.4259 0.7490 0.097 Uiso 1 1 calc R . . C71 C 2.6246(7) -0.4766(6) 0.8501(6) 0.071(3) Uani 1 1 d . . . H71A H 2.5668 -0.5004 0.8866 0.085 Uiso 1 1 calc R . . C72 C 2.7061(7) -0.4863(6) 0.8768(6) 0.058(2) Uani 1 1 d . . . C73 C 2.6264(6) -0.5482(6) 1.0184(5) 0.064(3) Uani 1 1 d . . . H73A H 2.5768 -0.5776 1.0111 0.077 Uiso 1 1 calc R . . H73B H 2.6047 -0.4961 1.0148 0.077 Uiso 1 1 calc R . . C74 C 2.6474(6) -0.5991(6) 1.0990(5) 0.063(2) Uani 1 1 d . . . H74A H 2.5896 -0.6139 1.1408 0.076 Uiso 1 1 calc R . . H74B H 2.6720 -0.6499 1.1014 0.076 Uiso 1 1 calc R . . C75 C 2.7236(6) -0.5947(5) 1.1943(5) 0.057(2) Uani 1 1 d . . . H75A H 2.7181 -0.6544 1.2142 0.069 Uiso 1 1 calc R . . H75B H 2.6739 -0.5812 1.2282 0.069 Uiso 1 1 calc R . . C76 C 2.8195(6) -0.5657(6) 1.1969(5) 0.059(2) Uani 1 1 d . . . H76A H 2.8305 -0.5057 1.1669 0.071 Uiso 1 1 calc R . . H76B H 2.8225 -0.5823 1.2524 0.071 Uiso 1 1 calc R . . C77 C 2.9803(6) -0.5590(7) 1.1290(6) 0.078(3) Uani 1 1 d . . . H77A H 2.9740 -0.4999 1.1067 0.093 Uiso 1 1 calc R . . H77B H 3.0126 -0.5699 1.0851 0.093 Uiso 1 1 calc R . . C78 C 2.9608(6) -0.4179(6) 0.8104(6) 0.063(3) Uani 1 1 d . . . H78A H 2.9558 -0.3586 0.7850 0.075 Uiso 1 1 calc R . . H78B H 2.9875 -0.4342 0.7689 0.075 Uiso 1 1 calc R . . S1 S 2.12000(15) 0.08054(14) 1.58436(14) 0.0527(6) Uani 1 1 d . . . S2 S 3.10702(15) -0.49054(15) 0.61178(13) 0.0566(7) Uani 1 1 d . . . S3 S 2.51141(16) -0.78420(16) 1.02695(16) 0.0664(7) Uani 1 1 d . . . S4 S 2.54333(17) -1.21094(15) 1.26781(17) 0.0685(7) Uani 1 1 d . . . O13 O 2.1787(6) 0.0226(6) 1.5864(8) 0.173(5) Uani 1 1 d . . . O14 O 2.0827(9) 0.0763(6) 1.6559(6) 0.209(7) Uani 1 1 d . . . O15 O 2.0585(10) 0.0847(8) 1.5414(10) 0.259(9) Uani 1 1 d . . . O16 O 3.1012(4) -0.4887(4) 0.6862(3) 0.0738(18) Uani 1 1 d . . . O17 O 3.1989(4) -0.4723(5) 0.5617(4) 0.093(2) Uani 1 1 d . . . O18 O 3.0520(4) -0.5603(4) 0.6196(4) 0.0731(18) Uani 1 1 d . . . O19 O 2.5396(4) -0.6993(4) 0.9740(4) 0.083(2) Uani 1 1 d . . . O20 O 2.4139(4) -0.8093(4) 1.0399(4) 0.0770(19) Uani 1 1 d . . . O21 O 2.5793(5) -0.8361(5) 1.0104(6) 0.112(3) Uani 1 1 d . . . O22 O 2.5810(4) -1.2873(4) 1.2805(5) 0.088(2) Uani 1 1 d . . . O23 O 2.4462(4) -1.2228(4) 1.3107(5) 0.092(2) Uani 1 1 d . . . O24 O 2.5985(6) -1.1496(5) 1.2706(6) 0.126(3) Uani 1 1 d . . . F1 F 2.1548(9) 0.2363(5) 1.5276(9) 0.260(9) Uani 1 1 d . . . F2 F 2.2314(12) 0.1902(7) 1.4614(6) 0.273(9) Uani 1 1 d . . . F3 F 2.2593(9) 0.1759(8) 1.5603(10) 0.244(7) Uani 1 1 d . . . F4 F 2.9566(4) -0.4121(4) 0.5945(4) 0.1006(19) Uani 1 1 d . . . F5 F 3.0459(4) -0.3968(4) 0.4847(4) 0.103(2) Uani 1 1 d . . . F6 F 3.0844(5) -0.3331(4) 0.5465(5) 0.122(3) Uani 1 1 d . . . F7 F 2.4744(4) -0.7440(5) 1.1443(4) 0.110(2) Uani 1 1 d . . . F8 F 2.4962(6) -0.8723(5) 1.1801(4) 0.156(4) Uani 1 1 d . . . F9 F 2.6120(4) -0.7808(4) 1.1232(4) 0.101(2) Uani 1 1 d . . . F10 F 2.6235(4) -1.1541(4) 1.1133(4) 0.101(2) Uani 1 1 d . . . F11 F 2.4862(5) -1.2143(5) 1.1485(4) 0.118(2) Uani 1 1 d . . . F12 F 2.5047(6) -1.0931(5) 1.1371(5) 0.145(3) Uani 1 1 d . . . C79 C 2.1896(10) 0.1762(9) 1.5325(8) 0.102(4) Uani 1 1 d . . . C80 C 3.0459(7) -0.4039(7) 0.5574(6) 0.073(3) Uani 1 1 d . . . C81 C 2.5225(7) -0.7964(7) 1.1241(7) 0.080(3) Uani 1 1 d . . . C82 C 2.5382(8) -1.1641(7) 1.1632(8) 0.087(3) Uani 1 1 d . . . O1W O 3.1201(4) -0.3910(4) 0.9839(4) 0.0710(18) Uani 1 1 d . . . H1WA H 3.1188 -0.4379 1.0244 0.35(15) Uiso 1 1 d R . . H1WB H 3.1413 -0.3978 0.9423 0.6(3) Uiso 1 1 d R . . O2W O 2.1037(4) -0.0820(4) 1.5123(4) 0.0799(19) 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 0.043(3) 0.055(3) 0.040(4) -0.019(3) -0.005(3) -0.011(3) O2 0.051(3) 0.050(3) 0.047(3) -0.025(3) 0.001(3) 0.002(3) O3 0.037(4) 0.160(7) 0.095(5) -0.096(6) 0.004(3) -0.014(4) O4 0.053(5) 0.132(6) 0.102(5) -0.093(5) 0.009(4) -0.018(4) O5 0.046(4) 0.061(4) 0.067(4) -0.041(3) -0.009(3) -0.004(3) O6 0.043(4) 0.058(4) 0.064(4) -0.035(3) -0.009(3) 0.000(3) O7 0.038(3) 0.054(3) 0.042(3) -0.023(3) -0.001(2) -0.008(3) O8 0.037(3) 0.061(4) 0.046(3) -0.031(3) -0.004(3) 0.006(3) O9 0.057(4) 0.082(4) 0.062(4) -0.046(4) -0.005(3) 0.000(3) O10 0.068(4) 0.058(4) 0.060(4) -0.030(3) -0.011(3) -0.009(3) O11 0.053(4) 0.086(4) 0.088(5) -0.060(4) -0.002(3) 0.001(4) O12 0.046(4) 0.082(4) 0.064(4) -0.040(3) -0.003(3) 0.000(3) N1 0.031(4) 0.040(4) 0.033(4) -0.022(3) -0.011(3) 0.006(3) N2 0.026(4) 0.034(4) 0.034(4) -0.016(3) -0.008(3) 0.002(3) N3 0.023(4) 0.037(4) 0.049(4) -0.025(4) -0.014(3) 0.003(3) N4 0.041(5) 0.034(4) 0.043(5) -0.022(3) -0.019(4) -0.001(3) C1 0.031(4) 0.042(5) 0.039(5) -0.026(4) -0.010(3) 0.007(4) C2 0.029(5) 0.035(4) 0.036(4) -0.020(4) -0.006(3) 0.003(4) C3 0.033(5) 0.048(5) 0.048(5) -0.028(4) -0.008(4) 0.003(4) C4 0.022(5) 0.050(6) 0.041(5) -0.025(4) -0.013(4) 0.006(4) C5 0.024(4) 0.041(5) 0.043(5) -0.022(4) -0.007(3) -0.001(4) C6 0.042(6) 0.037(5) 0.042(5) -0.022(4) -0.017(4) 0.002(4) C7 0.028(5) 0.048(5) 0.045(5) -0.032(4) -0.020(4) 0.015(4) C8 0.027(4) 0.045(5) 0.057(5) -0.025(4) -0.006(4) -0.003(4) C9 0.038(5) 0.036(5) 0.057(5) -0.025(4) -0.012(4) -0.001(4) C10 0.035(4) 0.049(5) 0.046(5) -0.030(4) -0.014(4) 0.006(4) C11 0.024(4) 0.053(5) 0.047(6) -0.028(4) -0.004(4) 0.000(4) C12 0.023(5) 0.043(5) 0.031(4) -0.016(4) -0.003(4) 0.003(3) C13 0.034(5) 0.032(4) 0.024(5) -0.014(4) -0.006(4) 0.003(3) C14 0.022(4) 0.049(5) 0.049(6) -0.030(4) -0.010(4) 0.000(4) C15 0.030(5) 0.050(5) 0.034(5) -0.021(4) 0.001(4) 0.003(4) C16 0.028(5) 0.029(4) 0.030(5) -0.014(4) -0.004(4) -0.001(3) C17 0.016(4) 0.050(5) 0.041(5) -0.022(4) -0.005(4) 0.000(4) C18 0.036(5) 0.048(5) 0.029(4) -0.015(4) 0.000(4) 0.001(4) C19 0.021(4) 0.053(5) 0.044(6) -0.016(5) -0.005(4) -0.006(4) C20 0.032(5) 0.047(5) 0.032(5) -0.005(4) -0.002(4) -0.006(4) C21 0.036(4) 0.039(5) 0.043(5) -0.020(4) -0.017(4) 0.005(4) C22 0.041(5) 0.047(5) 0.049(5) -0.028(4) -0.023(4) 0.013(4) C23 0.020(4) 0.044(5) 0.050(5) -0.026(5) -0.005(4) 0.000(4) C24 0.034(5) 0.031(4) 0.036(4) -0.011(4) -0.009(4) 0.004(4) C25 0.028(5) 0.024(4) 0.040(5) -0.022(4) -0.007(4) -0.001(3) C26 0.022(4) 0.032(4) 0.057(6) -0.020(5) -0.007(4) -0.001(4) C27 0.040(6) 0.031(4) 0.041(5) -0.018(4) -0.008(4) 0.002(4) C28 0.032(5) 0.028(4) 0.042(5) -0.021(4) -0.016(4) 0.001(3) C29 0.032(4) 0.047(5) 0.051(6) -0.032(4) -0.016(4) 0.010(4) C30 0.048(6) 0.040(5) 0.037(5) -0.025(4) -0.003(4) 0.002(4) C31 0.039(5) 0.042(5) 0.046(6) -0.029(4) -0.015(5) 0.002(4) C32 0.033(5) 0.036(4) 0.041(5) -0.018(4) -0.011(4) 0.004(4) C33 0.058(5) 0.038(5) 0.048(5) -0.020(4) -0.029(4) 0.005(4) C34 0.044(6) 0.045(5) 0.035(5) -0.026(4) -0.012(4) 0.009(4) C35 0.054(6) 0.094(8) 0.162(11) -0.096(8) -0.061(7) 0.030(6) C36 0.028(5) 0.057(6) 0.093(7) -0.049(5) -0.013(4) 0.010(5) C37 0.039(5) 0.046(5) 0.028(4) -0.023(4) -0.011(3) 0.014(4) C38 0.057(6) 0.075(7) 0.146(10) -0.087(7) -0.058(6) 0.040(5) C39 0.037(6) 0.052(6) 0.084(7) -0.047(5) -0.010(4) 0.015(4) C40 0.030(5) 0.045(5) 0.038(4) -0.029(4) -0.008(3) 0.005(4) C41 0.037(5) 0.046(5) 0.052(5) -0.037(4) -0.010(4) 0.014(4) C42 0.025(4) 0.056(5) 0.058(5) -0.036(4) -0.009(4) 0.010(4) C43 0.042(6) 0.039(5) 0.047(6) -0.029(4) -0.011(5) 0.008(4) C44 0.054(6) 0.052(5) 0.045(6) -0.024(5) -0.010(4) -0.006(4) C45 0.076(7) 0.068(6) 0.045(6) -0.030(5) -0.024(6) 0.016(6) C46 0.052(6) 0.073(7) 0.084(8) -0.046(6) -0.028(6) 0.006(5) C47 0.041(6) 0.072(6) 0.065(7) -0.041(6) -0.012(5) 0.011(4) C48 0.039(5) 0.041(5) 0.047(6) -0.028(4) -0.003(5) 0.001(4) C49 0.054(6) 0.060(6) 0.065(6) -0.038(5) -0.003(5) -0.007(5) C50 0.051(6) 0.048(5) 0.083(7) -0.038(5) -0.003(5) -0.011(4) C51 0.055(6) 0.065(6) 0.059(6) -0.036(5) 0.010(5) -0.005(5) C52 0.045(6) 0.127(10) 0.046(6) -0.043(6) 0.001(5) 0.020(6) C53 0.070(10) 0.60(4) 0.27(2) -0.37(3) 0.071(12) -0.117(17) C54 0.082(10) 0.28(2) 0.176(14) -0.203(15) 0.058(10) -0.071(11) C55 0.068(8) 0.064(6) 0.080(8) -0.054(6) -0.001(7) -0.007(5) C56 0.103(10) 0.076(8) 0.085(10) -0.059(7) 0.018(7) -0.034(7) C57 0.150(12) 0.051(7) 0.074(8) -0.042(6) -0.013(10) -0.008(8) C58 0.091(9) 0.048(6) 0.084(8) -0.040(6) -0.034(7) 0.011(6) C59 0.074(7) 0.048(5) 0.070(7) -0.041(5) -0.019(5) 0.011(5) C60 0.049(6) 0.049(5) 0.062(7) -0.040(5) -0.008(5) 0.002(5) C61 0.037(5) 0.054(5) 0.081(7) -0.040(5) -0.012(5) -0.009(4) C62 0.054(6) 0.050(5) 0.083(7) -0.035(6) -0.014(5) -0.005(4) C63 0.043(6) 0.056(6) 0.069(6) -0.028(5) -0.005(5) -0.009(4) C64 0.047(5) 0.061(6) 0.048(5) -0.028(5) -0.002(4) -0.007(5) C65 0.034(5) 0.062(6) 0.069(6) -0.038(5) -0.001(4) 0.009(4) C66 0.042(5) 0.070(6) 0.049(5) -0.036(5) 0.000(4) 0.002(4) C67 0.060(7) 0.056(6) 0.061(7) -0.035(5) -0.014(6) 0.010(5) C68 0.069(7) 0.065(6) 0.073(8) -0.042(6) -0.011(6) 0.014(5) C69 0.083(8) 0.065(6) 0.075(7) -0.032(6) -0.027(7) 0.013(6) C70 0.059(7) 0.092(8) 0.102(9) -0.051(7) -0.023(7) 0.006(6) C71 0.059(7) 0.086(7) 0.070(8) -0.035(6) -0.021(5) 0.007(5) C72 0.055(7) 0.062(6) 0.063(7) -0.035(5) -0.010(6) 0.001(5) C73 0.045(6) 0.083(7) 0.073(7) -0.049(6) 0.003(5) -0.011(5) C74 0.058(6) 0.074(6) 0.059(6) -0.038(5) -0.001(5) -0.016(5) C75 0.061(6) 0.065(6) 0.047(6) -0.029(5) -0.005(4) 0.010(5) C76 0.060(6) 0.066(6) 0.060(6) -0.039(5) -0.008(5) 0.001(5) C77 0.044(6) 0.118(9) 0.081(7) -0.061(7) -0.001(5) -0.013(6) C78 0.048(6) 0.069(6) 0.075(7) -0.045(5) 0.006(5) -0.006(5) S1 0.0368(13) 0.0618(15) 0.0632(16) -0.0330(12) -0.0092(11) 0.0079(11) S2 0.0371(14) 0.0897(18) 0.0502(14) -0.0427(13) 0.0009(11) -0.0132(12) S3 0.0392(15) 0.0757(18) 0.0795(18) -0.0360(15) -0.0029(12) -0.0091(13) S4 0.0598(17) 0.0540(16) 0.105(2) -0.0520(15) -0.0091(14) -0.0021(13) O13 0.078(6) 0.097(6) 0.273(13) -0.049(7) 0.013(7) 0.020(5) O14 0.297(15) 0.138(8) 0.147(9) -0.107(7) 0.142(10) -0.129(9) O15 0.232(14) 0.200(13) 0.325(18) -0.034(12) -0.223(15) -0.034(10) O16 0.078(4) 0.104(5) 0.055(4) -0.054(4) -0.007(3) -0.004(4) O17 0.029(4) 0.176(7) 0.071(4) -0.059(5) 0.003(3) -0.016(4) O18 0.062(4) 0.081(4) 0.094(5) -0.057(4) -0.014(3) -0.008(3) O19 0.071(4) 0.076(5) 0.081(5) -0.030(4) 0.009(4) -0.025(4) O20 0.025(3) 0.108(5) 0.077(4) -0.030(4) 0.002(3) -0.025(3) O21 0.080(5) 0.136(7) 0.173(8) -0.115(7) -0.032(5) 0.037(5) O22 0.064(4) 0.067(4) 0.128(6) -0.053(4) 0.004(4) 0.009(4) O23 0.058(5) 0.110(6) 0.123(6) -0.079(5) 0.006(4) 0.016(4) O24 0.145(7) 0.079(5) 0.157(8) -0.070(5) -0.004(6) -0.050(5) F1 0.206(11) 0.057(5) 0.39(2) -0.055(8) 0.076(11) 0.001(6) F2 0.47(2) 0.169(9) 0.097(7) -0.060(6) 0.106(10) -0.177(12) F3 0.150(9) 0.208(12) 0.35(2) -0.101(12) -0.065(11) -0.079(9) F4 0.063(4) 0.110(5) 0.121(5) -0.052(4) -0.009(4) 0.010(3) F5 0.094(4) 0.139(6) 0.070(4) -0.038(4) -0.031(3) -0.005(4) F6 0.134(6) 0.072(4) 0.156(7) -0.035(4) -0.060(5) -0.028(4) F7 0.070(4) 0.176(7) 0.111(5) -0.097(5) -0.004(3) 0.003(4) F8 0.196(8) 0.113(6) 0.103(5) 0.014(5) -0.064(5) -0.094(6) F9 0.073(4) 0.095(4) 0.159(6) -0.066(4) -0.057(4) 0.006(3) F10 0.070(4) 0.094(4) 0.129(5) -0.056(4) 0.012(4) -0.016(3) F11 0.103(5) 0.142(6) 0.104(5) -0.062(5) -0.002(4) -0.036(5) F12 0.167(8) 0.109(6) 0.136(7) -0.046(5) -0.016(5) 0.061(5) C79 0.077(9) 0.103(11) 0.079(9) -0.022(8) 0.026(7) 0.001(8) C80 0.054(7) 0.103(9) 0.052(6) -0.029(6) -0.006(5) -0.026(6) C81 0.046(7) 0.075(8) 0.097(8) -0.028(7) 0.000(6) -0.022(6) C82 0.068(8) 0.066(7) 0.121(10) -0.046(7) -0.004(7) -0.002(6) O1W 0.076(4) 0.072(4) 0.075(4) -0.046(4) -0.012(3) 0.007(3) O2W 0.059(4) 0.111(5) 0.094(5) -0.069(4) -0.016(3) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C48 1.362(9) . ? O1 C49 1.425(9) . ? O2 C51 1.419(9) . ? O2 C50 1.452(10) . ? O3 C52 1.402(12) . ? O3 C53 1.407(14) . ? O4 C55 1.364(11) . ? O4 C54 1.423(13) . ? O5 C60 1.372(10) . ? O5 C61 1.418(9) . ? O6 C62 1.410(10) . ? O6 C63 1.415(9) . ? O7 C64 1.419(9) . ? O7 C65 1.432(9) . ? O8 C43 1.375(9) . ? O8 C66 1.434(9) . ? O9 C72 1.377(10) . ? O9 C73 1.448(10) . ? O10 C74 1.415(9) . ? O10 C75 1.423(9) . ? O11 C77 1.419(10) . ? O11 C76 1.423(10) . ? O12 C67 1.367(10) . ? O12 C78 1.443(10) . ? N1 C11 1.324(9) . ? N1 C15 1.343(9) . ? N1 C10 1.506(9) . ? N2 C19 1.320(9) . ? N2 C18 1.349(9) . ? N2 C21 1.467(8) . ? N3 C23 1.344(9) . ? N3 C27 1.351(9) . ? N3 C22 1.474(9) . ? N4 C31 1.329(9) . ? N4 C30 1.342(9) . ? N4 C33 1.483(9) . ? C1 C40 1.392(10) . ? C1 C2 1.393(10) . ? C2 C3 1.377(10) . ? C2 C4 1.482(10) . ? C3 C42 1.367(10) . ? C4 C9 1.375(10) . ? C4 C5 1.390(10) . ? C5 C6 1.391(10) . ? C6 C7 1.374(10) . ? C7 C8 1.377(10) . ? C7 C10 1.506(10) . ? C8 C9 1.388(10) . ? C11 C12 1.356(10) . ? C12 C13 1.390(9) . ? C13 C14 1.383(10) . ? C13 C16 1.479(9) . ? C14 C15 1.369(10) . ? C16 C17 1.364(9) . ? C16 C20 1.395(9) . ? C17 C18 1.360(10) . ? C19 C20 1.363(10) . ? C21 C22 1.494(10) . ? C23 C24 1.364(10) . ? C24 C25 1.403(9) . ? C25 C26 1.362(10) . ? C25 C28 1.470(9) . ? C26 C27 1.370(10) . ? C28 C29 1.369(10) . ? C28 C32 1.391(10) . ? C29 C30 1.372(10) . ? C31 C32 1.360(10) . ? C33 C34 1.522(10) . ? C34 C39 1.349(10) . ? C34 C35 1.363(11) . ? C35 C38 1.381(12) 2_;47 ? C36 C37 1.363(10) . ? C36 C39 1.384(11) 2_;47 ? C37 C38 1.373(10) . ? C37 C40 1.495(10) . ? C38 C35 1.381(12) 2_;47 ? C39 C36 1.384(11) 2_;47 ? C40 C41 1.404(10) . ? C41 C42 1.383(10) . ? C43 C44 1.368(10) . ? C43 C48 1.396(10) . ? C44 C45 1.384(11) . ? C45 C46 1.372(12) . ? C46 C47 1.377(12) . ? C47 C48 1.389(11) . ? C49 C50 1.457(11) . ? C51 C52 1.457(12) . ? C53 C54 1.091(14) . ? C55 C56 1.389(14) . ? C55 C60 1.407(12) . ? C56 C57 1.387(16) . ? C57 C58 1.344(15) . ? C58 C59 1.395(13) . ? C59 C60 1.375(11) . ? C61 C62 1.493(11) . ? C63 C64 1.470(11) . ? C65 C66 1.505(11) . ? C67 C68 1.364(12) . ? C67 C72 1.401(12) . ? C68 C69 1.400(13) . ? C69 C70 1.362(14) . ? C70 C71 1.394(13) . ? C71 C72 1.364(12) . ? C73 C74 1.488(12) . ? C75 C76 1.514(11) . ? C77 C78 1.489(12) 2_;47 ? C78 C77 1.489(12) 2_;47 ? S1 O15 1.315(10) . ? S1 O14 1.323(9) . ? S1 O13 1.339(9) . ? S1 C79 1.754(14) . ? S2 O17 1.410(6) . ? S2 O16 1.419(6) . ? S2 O18 1.437(6) . ? S2 C80 1.795(11) . ? S3 O19 1.412(7) . ? S3 O20 1.428(6) . ? S3 O21 1.440(7) . ? S3 C81 1.806(12) . ? S4 O24 1.405(7) . ? S4 O22 1.419(6) . ? S4 O23 1.437(7) . ? S4 C82 1.798(13) . ? F1 C79 1.171(14) . ? F2 C79 1.270(14) . ? F3 C79 1.237(16) . ? F4 C80 1.314(11) . ? F5 C80 1.334(10) . ? F6 C80 1.317(11) . ? F7 C81 1.319(12) . ? F8 C81 1.300(11) . ? F9 C81 1.328(10) . ? F10 C82 1.351(12) . ? F11 C82 1.347(12) . ? F12 C82 1.285(12) . ? 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 O1 C49 119.8(6) . . ? C51 O2 C50 112.3(6) . . ? C52 O3 C53 113.7(12) . . ? C55 O4 C54 118.6(10) . . ? C60 O5 C61 116.1(6) . . ? C62 O6 C63 114.2(6) . . ? C64 O7 C65 113.7(6) . . ? C43 O8 C66 117.0(6) . . ? C72 O9 C73 117.8(7) . . ? C74 O10 C75 111.7(6) . . ? C77 O11 C76 114.9(7) . . ? C67 O12 C78 120.7(7) . . ? C11 N1 C15 119.7(6) . . ? C11 N1 C10 120.3(6) . . ? C15 N1 C10 120.0(6) . . ? C19 N2 C18 119.6(6) . . ? C19 N2 C21 120.1(6) . . ? C18 N2 C21 120.3(6) . . ? C23 N3 C27 119.9(6) . . ? C23 N3 C22 121.5(6) . . ? C27 N3 C22 118.6(6) . . ? C31 N4 C30 120.1(6) . . ? C31 N4 C33 119.4(7) . . ? C30 N4 C33 120.5(7) . . ? C40 C1 C2 122.3(6) . . ? C3 C2 C1 118.2(7) . . ? C3 C2 C4 122.2(7) . . ? C1 C2 C4 119.6(6) . . ? C42 C3 C2 120.7(7) . . ? C9 C4 C5 117.8(7) . . ? C9 C4 C2 121.4(7) . . ? C5 C4 C2 120.8(6) . . ? C4 C5 C6 120.6(7) . . ? C7 C6 C5 120.8(7) . . ? C6 C7 C8 118.8(7) . . ? C6 C7 C10 121.1(7) . . ? C8 C7 C10 120.1(7) . . ? C7 C8 C9 120.3(7) . . ? C4 C9 C8 121.6(7) . . ? N1 C10 C7 109.4(5) . . ? N1 C11 C12 122.5(7) . . ? C11 C12 C13 119.8(7) . . ? C14 C13 C12 116.7(6) . . ? C14 C13 C16 120.5(6) . . ? C12 C13 C16 122.7(6) . . ? C15 C14 C13 121.2(7) . . ? N1 C15 C14 120.1(7) . . ? C17 C16 C20 117.1(6) . . ? C17 C16 C13 121.4(6) . . ? C20 C16 C13 121.4(6) . . ? C18 C17 C16 121.3(6) . . ? N2 C18 C17 120.4(7) . . ? N2 C19 C20 121.9(7) . . ? C19 C20 C16 119.5(7) . . ? N2 C21 C22 108.4(5) . . ? N3 C22 C21 110.8(6) . . ? N3 C23 C24 121.5(6) . . ? C23 C24 C25 119.4(7) . . ? C26 C25 C24 117.8(6) . . ? C26 C25 C28 121.9(6) . . ? C24 C25 C28 120.3(6) . . ? C25 C26 C27 121.4(7) . . ? N3 C27 C26 120.1(7) . . ? C29 C28 C32 116.7(6) . . ? C29 C28 C25 122.5(7) . . ? C32 C28 C25 120.7(7) . . ? C28 C29 C30 121.2(7) . . ? N4 C30 C29 120.1(7) . . ? N4 C31 C32 121.1(7) . . ? C31 C32 C28 120.6(7) . . ? N4 C33 C34 109.9(6) . . ? C39 C34 C35 117.4(7) . . ? C39 C34 C33 120.7(7) . . ? C35 C34 C33 121.9(7) . . ? C34 C35 C38 121.3(8) . 2_;47 ? C37 C36 C39 122.5(7) . 2_;47 ? C36 C37 C38 115.5(7) . . ? C36 C37 C40 123.1(7) . . ? C38 C37 C40 121.3(7) . . ? C37 C38 C35 122.0(8) . 2_;47 ? C34 C39 C36 121.2(7) . 2_;47 ? C1 C40 C41 117.8(6) . . ? C1 C40 C37 121.1(6) . . ? C41 C40 C37 121.1(6) . . ? C42 C41 C40 119.6(7) . . ? C3 C42 C41 121.4(7) . . ? C44 C43 O8 125.2(7) . . ? C44 C43 C48 120.1(7) . . ? O8 C43 C48 114.7(7) . . ? C43 C44 C45 119.9(8) . . ? C46 C45 C44 120.2(8) . . ? C45 C46 C47 120.8(8) . . ? C46 C47 C48 119.3(8) . . ? O1 C48 C47 123.7(7) . . ? O1 C48 C43 116.5(7) . . ? C47 C48 C43 119.7(8) . . ? O1 C49 C50 112.7(7) . . ? O2 C50 C49 109.3(7) . . ? O2 C51 C52 111.9(7) . . ? O3 C52 C51 109.8(8) . . ? C54 C53 O3 132.6(13) . . ? C53 C54 O4 127.0(12) . . ? O4 C55 C56 125.5(10) . . ? O4 C55 C60 116.3(10) . . ? C56 C55 C60 118.1(10) . . ? C57 C56 C55 120.3(10) . . ? C58 C57 C56 121.4(11) . . ? C57 C58 C59 119.6(10) . . ? C60 C59 C58 120.3(9) . . ? O5 C60 C59 124.4(8) . . ? O5 C60 C55 115.4(8) . . ? C59 C60 C55 120.3(9) . . ? O5 C61 C62 107.1(6) . . ? O6 C62 C61 114.8(7) . . ? O6 C63 C64 110.1(7) . . ? O7 C64 C63 109.1(7) . . ? O7 C65 C66 113.4(6) . . ? O8 C66 C65 107.6(6) . . ? C68 C67 O12 125.7(9) . . ? C68 C67 C72 119.1(9) . . ? O12 C67 C72 115.2(8) . . ? C67 C68 C69 120.5(9) . . ? C70 C69 C68 119.6(10) . . ? C69 C70 C71 120.6(10) . . ? C72 C71 C70 119.4(10) . . ? C71 C72 O9 124.8(9) . . ? C71 C72 C67 120.8(9) . . ? O9 C72 C67 114.4(8) . . ? O9 C73 C74 109.1(7) . . ? O10 C74 C73 110.3(7) . . ? O10 C75 C76 108.3(7) . . ? O11 C76 C75 107.5(7) . . ? O11 C77 C78 113.2(8) . 2_;47 ? O12 C78 C77 104.3(7) . 2_;47 ? O15 S1 O14 114.7(11) . . ? O15 S1 O13 110.9(10) . . ? O14 S1 O13 114.3(9) . . ? O15 S1 C79 106.2(8) . . ? O14 S1 C79 103.2(6) . . ? O13 S1 C79 106.5(6) . . ? O17 S2 O16 114.8(4) . . ? O17 S2 O18 115.7(4) . . ? O16 S2 O18 113.6(4) . . ? O17 S2 C80 103.8(5) . . ? O16 S2 C80 103.6(5) . . ? O18 S2 C80 103.3(4) . . ? O19 S3 O20 115.1(4) . . ? O19 S3 O21 111.5(5) . . ? O20 S3 O21 116.9(5) . . ? O19 S3 C81 104.2(5) . . ? O20 S3 C81 103.9(4) . . ? O21 S3 C81 103.4(5) . . ? O24 S4 O22 118.7(5) . . ? O24 S4 O23 113.9(5) . . ? O22 S4 O23 112.2(4) . . ? O24 S4 C82 102.2(5) . . ? O22 S4 C82 103.4(5) . . ? O23 S4 C82 104.1(5) . . ? F1 C79 F3 105.0(17) . . ? F1 C79 F2 107.3(14) . . ? F3 C79 F2 99.5(14) . . ? F1 C79 S1 119.2(10) . . ? F3 C79 S1 112.5(11) . . ? F2 C79 S1 111.4(12) . . ? F4 C80 F6 107.5(10) . . ? F4 C80 F5 106.0(8) . . ? F6 C80 F5 107.5(8) . . ? F4 C80 S2 112.1(7) . . ? F6 C80 S2 112.5(7) . . ? F5 C80 S2 110.9(8) . . ? F8 C81 F7 110.3(10) . . ? F8 C81 F9 106.3(9) . . ? F7 C81 F9 106.1(9) . . ? F8 C81 S3 111.1(8) . . ? F7 C81 S3 111.8(8) . . ? F9 C81 S3 111.0(8) . . ? F12 C82 F11 107.5(11) . . ? F12 C82 F10 106.9(9) . . ? F11 C82 F10 102.7(9) . . ? F12 C82 S4 115.1(9) . . ? F11 C82 S4 111.1(8) . . ? F10 C82 S4 112.6(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.563 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.069 #===END