# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 #TrackingRef '- DM14Q.cif' #send to: deposit@ccdc.cam.ac.uk _publ_contact_author ; Stephen J. Loeb Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; _publ_contact_author_phone '+ 519 253-3000 ext 3529' _publ_contact_author_fax '+ 519 973-7098 ' _publ_contact_author_email loeb@uwindsor.ca _publ_requested_coeditor_name ? _publ_contact_letter ; This structure is part of a study on the use of tetra- substituted crown ethers to form [2]pseudorotaxanes, [2]rotaxanes and metal-organic rotaxane framework materials. ; _publ_section_title ; [2]Pseudorotaxanes, [2]rotaxanes and metal-organic rotaxane frameworks containing tetra-substituted dibenzo[24]crown-8 wheels ; loop_ _publ_author_name _publ_author_address D.J.Mercer . J.Yacoub . S.K.Loeb . S.J.Loeb ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; _publ_contact_author_name 'Stephen J. Loeb' # Attachment '- DM3.cif' data_dm3 _database_code_depnum_ccdc_archive 'CCDC 864507' #TrackingRef '- DM3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C107 H119.50 F12 N7.50 O25.50 S4' _chemical_formula_weight 2274.84 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.478(4) _cell_length_b 17.317(4) _cell_length_c 22.065(5) _cell_angle_alpha 78.786(3) _cell_angle_beta 78.864(3) _cell_angle_gamma 65.622(3) _cell_volume 5580(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 468 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2380 _exptl_absorpt_coefficient_mu 0.180 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6796 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53157 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19587 _reflns_number_gt 11458 _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. One triflate anion was restrained to be a rigid group using SADI, SIMU and DELU commands, the others using SAME. One of the appended aromatic rings was disordered and this was modelled with a 50:50 occupancy. AFIX 66 commands were used to restrain these aromatic rings to be idealized hexagons with C-C and C-N bonds equal to 1.39 A. Partial occupancy water and acetontrile molecules were also included. One of the acetontrile molecules was restrained to have C-N bond distances of 1.54 and 1.20 A using DFIX commands. ; _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 19587 _refine_ls_number_parameters 1462 _refine_ls_number_restraints 537 _refine_ls_R_factor_all 0.1636 _refine_ls_R_factor_gt 0.1114 _refine_ls_wR_factor_ref 0.3647 _refine_ls_wR_factor_gt 0.3178 _refine_ls_goodness_of_fit_ref 1.291 _refine_ls_restrained_S_all 1.319 _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 0.2126(3) 0.4278(3) 0.1926(2) 0.0493(11) Uani 1 1 d . . . N2 N 0.4257(2) 0.6651(2) 0.26780(17) 0.0359(9) Uani 1 1 d . . . N3 N 0.5589(2) 0.8017(2) 0.23193(18) 0.0373(9) Uani 1 1 d . . . N4 N 0.7901(3) 1.0251(3) 0.3030(2) 0.0548(12) Uani 1 1 d . . . C1 C -0.0070(5) 0.2371(4) 0.4406(3) 0.0718(18) Uani 1 1 d . . . H1A H -0.0296 0.2981 0.4446 0.108 Uiso 1 1 calc R . . H1B H 0.0577 0.2107 0.4436 0.108 Uiso 1 1 calc R . . H1C H -0.0382 0.2094 0.4741 0.108 Uiso 1 1 calc R . . C2 C 0.0121(4) 0.1287(4) 0.3722(3) 0.0642(16) Uani 1 1 d . . . H2A H 0.0019 0.1211 0.3318 0.096 Uiso 1 1 calc R . . H2B H -0.0197 0.1015 0.4058 0.096 Uiso 1 1 calc R . . H2C H 0.0766 0.1021 0.3757 0.096 Uiso 1 1 calc R . . C3 C -0.1248(4) 0.2641(4) 0.3755(3) 0.0722(18) Uani 1 1 d . . . H3A H -0.1491 0.3254 0.3788 0.108 Uiso 1 1 calc R . . H3B H -0.1535 0.2356 0.4103 0.108 Uiso 1 1 calc R . . H3C H -0.1370 0.2557 0.3360 0.108 Uiso 1 1 calc R . . C4 C -0.0238(4) 0.2264(4) 0.3777(3) 0.0539(14) Uani 1 1 d . . . C5 C 0.0249(4) 0.2680(4) 0.3259(3) 0.0504(13) Uani 1 1 d . . . C6 C -0.0145(5) 0.3389(5) 0.2892(4) 0.110(3) Uani 1 1 d . . . H6A H -0.0781 0.3667 0.2961 0.132 Uiso 1 1 calc R . . C7 C 0.0319(5) 0.3751(5) 0.2408(4) 0.111(3) Uani 1 1 d . . . H7A H -0.0014 0.4265 0.2166 0.133 Uiso 1 1 calc R . . C8 C 0.1179(4) 0.3420(4) 0.2272(3) 0.0533(14) Uani 1 1 d . . . C9 C 0.1592(6) 0.2705(7) 0.2629(6) 0.203(8) Uani 1 1 d . . . H9A H 0.2225 0.2420 0.2544 0.244 Uiso 1 1 calc R . . C10 C 0.1130(6) 0.2355(8) 0.3126(7) 0.208(8) Uani 1 1 d . . . H10A H 0.1467 0.1858 0.3381 0.250 Uiso 1 1 calc R . . C11 C 0.1677(4) 0.3784(4) 0.1723(3) 0.0587(15) Uani 1 1 d . . . H11A H 0.2137 0.3312 0.1502 0.070 Uiso 1 1 calc R . . H11B H 0.1250 0.4166 0.1429 0.070 Uiso 1 1 calc R . . C12 C 0.1707(4) 0.5119(4) 0.1914(4) 0.076(2) Uani 1 1 d . . . H12A H 0.1122 0.5399 0.1791 0.091 Uiso 1 1 calc R . . C13 C 0.2103(4) 0.5580(4) 0.2077(4) 0.0733(19) Uani 1 1 d . . . H13A H 0.1791 0.6182 0.2064 0.088 Uiso 1 1 calc R . . C14 C 0.2948(3) 0.5199(3) 0.2260(2) 0.0375(11) Uani 1 1 d . . . C15 C 0.3361(4) 0.4323(4) 0.2270(3) 0.0675(17) Uani 1 1 d . . . H15A H 0.3944 0.4025 0.2396 0.081 Uiso 1 1 calc R . . C16 C 0.2935(4) 0.3881(4) 0.2099(3) 0.0682(17) Uani 1 1 d . . . H16A H 0.3228 0.3278 0.2105 0.082 Uiso 1 1 calc R . . C17 C 0.3408(3) 0.5705(3) 0.2421(2) 0.0353(10) Uani 1 1 d . . . C18 C 0.2964(3) 0.6582(3) 0.2438(3) 0.0471(12) Uani 1 1 d . . . H18A H 0.2357 0.6863 0.2359 0.056 Uiso 1 1 calc R . . C19 C 0.3403(3) 0.7040(3) 0.2568(2) 0.0445(12) Uani 1 1 d . . . H19A H 0.3097 0.7638 0.2580 0.053 Uiso 1 1 calc R . . C20 C 0.4709(3) 0.5799(3) 0.2666(2) 0.0400(11) Uani 1 1 d . . . H20A H 0.5317 0.5530 0.2746 0.048 Uiso 1 1 calc R . . C21 C 0.4289(3) 0.5329(3) 0.2539(2) 0.0418(11) Uani 1 1 d . . . H21A H 0.4608 0.4732 0.2531 0.050 Uiso 1 1 calc R . . C22 C 0.4724(3) 0.7161(3) 0.2803(2) 0.0388(11) Uani 1 1 d . . . H22A H 0.5222 0.6792 0.3048 0.047 Uiso 1 1 calc R . . H22B H 0.4301 0.7624 0.3046 0.047 Uiso 1 1 calc R . . C23 C 0.5088(3) 0.7537(3) 0.2188(2) 0.0384(11) Uani 1 1 d . . . H23A H 0.5493 0.7075 0.1937 0.046 Uiso 1 1 calc R . . H23B H 0.4588 0.7925 0.1949 0.046 Uiso 1 1 calc R . . C24 C 0.5176(3) 0.8876(3) 0.2309(2) 0.0389(11) Uani 1 1 d . . . H24A H 0.4575 0.9169 0.2215 0.047 Uiso 1 1 calc R . . C25 C 0.5640(3) 0.9318(3) 0.2436(2) 0.0395(11) Uani 1 1 d . . . H25A H 0.5354 0.9921 0.2426 0.047 Uiso 1 1 calc R . . C26 C 0.6513(3) 0.8904(3) 0.2577(2) 0.0382(11) Uani 1 1 d . . . C27 C 0.6909(3) 0.8011(3) 0.2576(2) 0.0453(12) Uani 1 1 d . . . H27A H 0.7508 0.7699 0.2668 0.054 Uiso 1 1 calc R . . C28 C 0.6428(3) 0.7591(3) 0.2440(2) 0.0416(11) Uani 1 1 d . . . H28A H 0.6701 0.6990 0.2434 0.050 Uiso 1 1 calc R . . C29 C 0.7012(3) 0.9365(3) 0.2731(2) 0.0451(12) Uani 1 1 d . . . C30 C 0.6637(4) 1.0236(4) 0.2720(3) 0.0614(16) Uani 1 1 d . . . H30A H 0.6047 1.0551 0.2609 0.074 Uiso 1 1 calc R . . C31 C 0.7101(4) 1.0657(4) 0.2865(3) 0.0612(15) Uani 1 1 d . . . H31A H 0.6832 1.1262 0.2844 0.073 Uiso 1 1 calc R . . C32 C 0.8269(5) 0.9404(4) 0.3079(4) 0.081(2) Uani 1 1 d . . . H32A H 0.8836 0.9103 0.3229 0.098 Uiso 1 1 calc R . . C33 C 0.7840(4) 0.8957(4) 0.2917(4) 0.076(2) Uani 1 1 d . . . H33A H 0.8128 0.8353 0.2935 0.092 Uiso 1 1 calc R . . C34 C 0.8409(4) 1.0724(4) 0.3175(3) 0.0587(15) Uani 1 1 d . . . H34A H 0.7995 1.1196 0.3414 0.070 Uiso 1 1 calc R . . H34B H 0.8881 1.0332 0.3436 0.070 Uiso 1 1 calc R . . C35 C 0.8831(4) 1.1078(3) 0.2588(3) 0.0497(13) Uani 1 1 d . . . C36 C 0.8399(4) 1.1895(4) 0.2306(3) 0.0709(17) Uani 1 1 d . . . H36A H 0.7810 1.2234 0.2478 0.085 Uiso 1 1 calc R . . C37 C 0.8813(5) 1.2234(4) 0.1771(3) 0.0748(18) Uani 1 1 d . . . H37A H 0.8503 1.2802 0.1588 0.090 Uiso 1 1 calc R . . C38 C 0.9655(4) 1.1765(4) 0.1506(3) 0.0617(15) Uani 1 1 d . . . C39 C 1.0070(4) 1.0947(5) 0.1790(3) 0.0746(18) Uani 1 1 d . . . H39A H 1.0653 1.0603 0.1612 0.090 Uiso 1 1 calc R . . C40 C 0.9675(4) 1.0599(4) 0.2326(3) 0.0668(16) Uani 1 1 d . . . H40A H 0.9988 1.0032 0.2510 0.080 Uiso 1 1 calc R . . C41 C 1.0147(5) 1.2118(6) 0.0948(4) 0.092(2) Uani 1 1 d U . . C42 C 1.0499(8) 1.1429(7) 0.0433(5) 0.141(4) Uani 1 1 d U . . H42A H 1.0914 1.0875 0.0611 0.211 Uiso 1 1 calc R . . H42B H 1.0808 1.1643 0.0056 0.211 Uiso 1 1 calc R . . H42C H 0.9983 1.1362 0.0326 0.211 Uiso 1 1 calc R . . C43 C 1.1007(7) 1.2050(7) 0.1056(6) 0.155(4) Uani 1 1 d U . . H43A H 1.0923 1.2444 0.1348 0.233 Uiso 1 1 calc R . . H43B H 1.1336 1.2196 0.0661 0.233 Uiso 1 1 calc R . . H43C H 1.1351 1.1463 0.1231 0.233 Uiso 1 1 calc R . . C44 C 0.9609(8) 1.2873(8) 0.0644(7) 0.264(9) Uani 1 1 d U . . H44A H 0.9376 1.3317 0.0921 0.395 Uiso 1 1 calc R . . H44B H 0.9106 1.2798 0.0523 0.395 Uiso 1 1 calc R . . H44C H 0.9959 1.3043 0.0271 0.395 Uiso 1 1 calc R . . O1 O -0.6723(2) 1.9968(2) 0.55660(18) 0.0578(10) Uani 1 1 d . A . O3 O -0.3831(2) 2.0778(2) 0.65174(17) 0.0489(9) Uani 1 1 d . A . O4 O -0.3018(2) 2.0995(2) 0.74877(16) 0.0474(9) Uani 1 1 d . . . O5 O -0.3260(2) 2.1579(2) 0.86292(16) 0.0526(9) Uani 1 1 d . . . O6 O -0.4620(2) 2.3261(2) 0.89164(17) 0.0560(10) Uani 1 1 d . . . O7 O -0.3430(3) 2.5210(2) 0.9405(2) 0.0685(11) Uani 1 1 d . . . O8 O -0.6755(3) 2.7101(3) 0.9351(3) 0.0998(17) Uani 1 1 d . . . O9 O -0.6154(3) 2.4134(3) 0.85283(19) 0.0659(11) Uani 1 1 d . . . O10 O -0.6848(2) 2.4453(2) 0.73987(16) 0.0466(8) Uani 1 1 d . . . O11 O -0.6536(2) 2.3610(2) 0.63229(16) 0.0510(9) Uani 1 1 d . . . O12 O -0.5353(2) 2.1809(2) 0.61141(16) 0.0495(9) Uani 1 1 d . . . C45 C -0.5104(3) 2.0954(3) 0.6082(2) 0.0441(12) Uani 1 1 d . A . C46 C -0.5596(3) 2.0613(3) 0.5867(2) 0.0462(12) Uani 1 1 d . . . H46A H -0.6153 2.0984 0.5723 0.055 Uiso 1 1 calc R . . C47 C -0.5302(3) 1.9737(3) 0.5853(2) 0.0447(12) Uani 1 1 d . A . C48 C -0.4487(4) 1.9195(3) 0.6061(3) 0.0516(13) Uani 1 1 d . . . C49 C -0.3984(4) 1.9544(3) 0.6283(3) 0.0514(13) Uani 1 1 d . A . H49A H -0.3429 1.9175 0.6430 0.062 Uiso 1 1 calc R . . C50 C -0.4277(3) 2.0397(3) 0.6292(2) 0.0472(12) Uani 1 1 d . . . C51 C -0.5823(3) 1.9361(3) 0.5603(3) 0.0506(13) Uani 1 1 d . . . H51A H -0.5532 1.9201 0.5184 0.061 Uiso 1 1 calc R A . H51B H -0.5827 1.8838 0.5879 0.061 Uiso 1 1 calc R . . C52 C -0.7270(4) 1.9732(3) 0.5316(2) 0.0474(12) Uani 1 1 d . . . C53 C -0.7003(4) 1.8957(4) 0.5083(3) 0.0556(14) Uani 1 1 d . A . H53A H -0.6400 1.8554 0.5084 0.067 Uiso 1 1 calc R . . C54 C -0.7623(4) 1.8779(4) 0.4849(3) 0.0633(16) Uani 1 1 d . . . H54A H -0.7441 1.8255 0.4687 0.076 Uiso 1 1 calc R A . C55 C -0.8500(4) 1.9359(4) 0.4851(3) 0.0677(17) Uani 1 1 d . A . H55A H -0.8925 1.9234 0.4695 0.081 Uiso 1 1 calc R . . C56 C -0.8755(4) 2.0118(4) 0.5080(3) 0.0638(16) Uani 1 1 d . . . H56A H -0.9359 2.0518 0.5081 0.077 Uiso 1 1 calc R A . C57 C -0.8157(4) 2.0312(4) 0.5308(3) 0.0589(14) Uani 1 1 d . A . H57A H -0.8347 2.0844 0.5462 0.071 Uiso 1 1 calc R . . C65 C -0.2942(3) 2.0239(3) 0.6666(3) 0.0510(13) Uani 1 1 d . . . H65A H -0.2557 1.9987 0.6292 0.061 Uiso 1 1 calc R A . H65B H -0.2963 1.9768 0.6996 0.061 Uiso 1 1 calc R . . C66 C -0.2574(4) 2.0759(4) 0.6880(3) 0.0550(14) Uani 1 1 d . A . H66A H -0.1923 2.0434 0.6900 0.066 Uiso 1 1 calc R . . H66B H -0.2652 2.1282 0.6579 0.066 Uiso 1 1 calc R . . C67 C -0.2507(4) 2.0489(3) 0.7975(3) 0.0570(14) Uani 1 1 d . . . H67A H -0.1951 2.0595 0.7934 0.068 Uiso 1 1 calc R . . H67B H -0.2334 1.9876 0.7950 0.068 Uiso 1 1 calc R . . C68 C -0.3046(4) 2.0709(3) 0.8585(3) 0.0581(15) Uani 1 1 d . . . H68A H -0.3606 2.0610 0.8624 0.070 Uiso 1 1 calc R . . H68B H -0.2701 2.0339 0.8927 0.070 Uiso 1 1 calc R . . C69 C -0.3691(4) 2.1810(4) 0.9229(3) 0.0553(14) Uani 1 1 d . . . H69A H -0.3301 2.1443 0.9550 0.066 Uiso 1 1 calc R . . H69B H -0.4263 2.1725 0.9322 0.066 Uiso 1 1 calc R . . C70 C -0.3869(4) 2.2723(4) 0.9240(3) 0.0543(14) Uani 1 1 d . . . H70A H -0.3995 2.2845 0.9676 0.065 Uiso 1 1 calc R . . H70B H -0.3333 2.2841 0.9039 0.065 Uiso 1 1 calc R . . C71 C -0.4925(3) 2.4105(4) 0.8933(2) 0.0510(13) Uani 1 1 d . . . C72 C -0.4484(4) 2.4512(4) 0.9138(2) 0.0529(14) Uani 1 1 d . . . H72A H -0.3926 2.4178 0.9293 0.064 Uiso 1 1 calc R . . C73 C -0.4833(4) 2.5405(4) 0.9124(2) 0.0586(15) Uani 1 1 d . . . C74 C -0.5682(4) 2.5884(4) 0.8906(3) 0.0681(17) Uani 1 1 d . . . C75 C -0.6113(4) 2.5449(5) 0.8724(3) 0.0698(18) Uani 1 1 d . . . H75A H -0.6685 2.5773 0.8587 0.084 Uiso 1 1 calc R . . C76 C -0.5776(4) 2.4589(4) 0.8728(3) 0.0609(15) Uani 1 1 d . . . C77 C -0.4317(4) 2.5819(4) 0.9344(3) 0.0614(15) Uani 1 1 d . . . H77A H -0.4300 2.6316 0.9041 0.074 Uiso 1 1 calc R . . H77B H -0.4616 2.6022 0.9750 0.074 Uiso 1 1 calc R . . C78 C -0.2858(4) 2.5439(4) 0.9633(3) 0.0599(15) Uani 1 1 d . . . C79 C -0.1995(5) 2.4812(4) 0.9669(3) 0.0723(18) Uani 1 1 d . . . H79A H -0.1850 2.4264 0.9556 0.087 Uiso 1 1 calc R . . C80 C -0.1356(5) 2.4982(5) 0.9865(3) 0.082(2) Uani 1 1 d . . . H80A H -0.0770 2.4551 0.9890 0.099 Uiso 1 1 calc R . . C81 C -0.1556(5) 2.5781(5) 1.0030(3) 0.0784(19) Uani 1 1 d . . . H81A H -0.1110 2.5904 1.0161 0.094 Uiso 1 1 calc R . . C82 C -0.2413(5) 2.6391(4) 0.9999(3) 0.0734(18) Uani 1 1 d . . . H82A H -0.2559 2.6937 1.0117 0.088 Uiso 1 1 calc R . . C83 C -0.3065(4) 2.6229(4) 0.9802(3) 0.0623(15) Uani 1 1 d . . . H83A H -0.3652 2.6660 0.9782 0.075 Uiso 1 1 calc R . . C84 C -0.6094(5) 2.6833(4) 0.8851(4) 0.088(2) Uani 1 1 d . . . H84A H -0.5625 2.7054 0.8843 0.106 Uiso 1 1 calc R . . H84B H -0.6361 2.7067 0.8457 0.106 Uiso 1 1 calc R . . C85 C -0.7265(5) 2.7983(6) 0.9332(5) 0.097(3) Uani 1 1 d . . . C86 C -0.7911(6) 2.8163(7) 0.9843(6) 0.129(4) Uani 1 1 d . . . H86A H -0.7998 2.7731 1.0154 0.155 Uiso 1 1 calc R . . C87 C -0.8462(6) 2.9090(8) 0.9866(6) 0.129(4) Uani 1 1 d . . . H87A H -0.8906 2.9267 1.0212 0.155 Uiso 1 1 calc R . . C88 C -0.8339(8) 2.9687(8) 0.9401(6) 0.133(4) Uani 1 1 d . . . H88A H -0.8710 3.0276 0.9405 0.160 Uiso 1 1 calc R . . C89 C -0.7707(8) 2.9429(7) 0.8956(6) 0.154(5) Uani 1 1 d . . . H89A H -0.7606 2.9852 0.8642 0.184 Uiso 1 1 calc R . . C90 C -0.7156(7) 2.8576(6) 0.8896(5) 0.124(4) Uani 1 1 d . . . H90A H -0.6711 2.8428 0.8545 0.149 Uiso 1 1 calc R . . C91 C -0.7105(4) 2.4467(4) 0.8487(3) 0.0659(16) Uani 1 1 d . . . H91A H -0.7433 2.4837 0.8818 0.079 Uiso 1 1 calc R . . H91B H -0.7303 2.3985 0.8562 0.079 Uiso 1 1 calc R . . C92 C -0.7339(4) 2.4959(4) 0.7883(3) 0.0639(16) Uani 1 1 d . . . H92A H -0.7991 2.5146 0.7871 0.077 Uiso 1 1 calc R . . H92B H -0.7201 2.5476 0.7822 0.077 Uiso 1 1 calc R . . C93 C -0.7226(4) 2.4858(3) 0.6831(3) 0.0539(14) Uani 1 1 d . . . H93A H -0.7339 2.5474 0.6776 0.065 Uiso 1 1 calc R . . H93B H -0.7809 2.4808 0.6855 0.065 Uiso 1 1 calc R . . C94 C -0.6624(4) 2.4468(3) 0.6297(3) 0.0549(14) Uani 1 1 d . . . H94A H -0.6863 2.4805 0.5908 0.066 Uiso 1 1 calc R . . H94B H -0.6026 2.4477 0.6294 0.066 Uiso 1 1 calc R . . C95 C -0.6113(4) 2.3284(3) 0.5745(2) 0.0581(15) Uani 1 1 d . . . H95A H -0.5500 2.3282 0.5653 0.070 Uiso 1 1 calc R . . H95B H -0.6459 2.3658 0.5404 0.070 Uiso 1 1 calc R . . C96 C -0.6062(4) 2.2389(3) 0.5776(3) 0.0537(14) Uani 1 1 d . . . H96A H -0.6637 2.2355 0.5983 0.064 Uiso 1 1 calc R . . H96B H -0.5956 2.2237 0.5350 0.064 Uiso 1 1 calc R . . S1 S 0.58816(9) 0.32244(8) 0.32943(6) 0.0491(4) Uani 1 1 d DU . . O13 O 0.6535(3) 0.2371(2) 0.3402(2) 0.0683(11) Uani 1 1 d DU . . O14 O 0.5070(3) 0.3282(2) 0.31118(19) 0.0656(11) Uani 1 1 d DU . . O15 O 0.6211(3) 0.3838(3) 0.2945(2) 0.0715(12) Uani 1 1 d DU . . C97 C 0.5544(4) 0.3546(4) 0.4061(3) 0.0711(16) Uani 1 1 d DU . . F1 F 0.6245(3) 0.3538(3) 0.4282(2) 0.1168(16) Uani 1 1 d DU . . F2 F 0.4909(3) 0.4313(3) 0.4061(2) 0.1184(17) Uani 1 1 d DU . . F3 F 0.5238(3) 0.3010(3) 0.44570(17) 0.0922(12) Uani 1 1 d DU . . S2 S 0.08761(10) 0.81762(10) 0.34767(8) 0.0641(5) Uani 1 1 d D . . O16 O 0.1617(4) 0.7858(4) 0.3802(4) 0.143(3) Uani 1 1 d D . . O17 O 0.1158(5) 0.8278(4) 0.2835(3) 0.137(3) Uani 1 1 d D . . O18 O 0.0129(3) 0.8850(3) 0.3688(3) 0.0994(17) Uani 1 1 d D . . C98 C 0.0524(5) 0.7297(5) 0.3606(4) 0.092(2) Uani 1 1 d D . . F4 F 0.1156(5) 0.6597(3) 0.3388(3) 0.176(3) Uani 1 1 d D . . F5 F -0.0157(5) 0.7470(4) 0.3308(4) 0.179(3) Uani 1 1 d D . . F6 F 0.0341(4) 0.7039(4) 0.4189(2) 0.1276(19) Uani 1 1 d D . . S3 S 0.38828(12) 0.14171(10) 0.15509(9) 0.0775(5) Uani 1 1 d D . . O19 O 0.3159(4) 0.1876(5) 0.1169(4) 0.178(4) Uani 1 1 d D . . O20 O 0.3987(7) 0.1878(7) 0.1909(5) 0.252(7) Uani 1 1 d D . . O21 O 0.3855(3) 0.0653(3) 0.1850(3) 0.113(2) Uani 1 1 d D . . C99 C 0.4832(6) 0.1164(5) 0.0986(4) 0.111(3) Uani 1 1 d D . . F7 F 0.4926(4) 0.1846(4) 0.0678(4) 0.223(5) Uani 1 1 d D . . F8 F 0.4856(4) 0.0682(6) 0.0584(3) 0.213(5) Uani 1 1 d D . . F9 F 0.5600(3) 0.0695(3) 0.1243(3) 0.1204(17) Uani 1 1 d D . . S4 S 0.91286(14) 0.64610(15) 0.17938(15) 0.1100(9) Uani 1 1 d D . . O22 O 0.9520(7) 0.6712(7) 0.2209(3) 0.206(4) Uani 1 1 d D . . O23 O 0.9756(4) 0.5783(5) 0.1446(3) 0.142(3) Uani 1 1 d D . . O24 O 0.8364(4) 0.6364(4) 0.2094(4) 0.135(3) Uani 1 1 d D . . C100 C 0.8852(7) 0.7352(8) 0.1233(4) 0.200(9) Uani 1 1 d D . . F10 F 0.8363(8) 0.8059(4) 0.1492(5) 0.292(8) Uani 1 1 d D . . F11 F 0.9607(6) 0.7474(7) 0.0946(3) 0.229(4) Uani 1 1 d D . . F12 F 0.8491(5) 0.7150(5) 0.0862(5) 0.206(4) Uani 1 1 d D . . N1S N 0.4019(5) 0.6382(4) 0.4090(3) 0.0903(19) Uani 1 1 d D . . C1S C 0.3409(5) 0.6329(4) 0.4370(3) 0.0663(17) Uani 1 1 d D . . C2S C 0.2596(5) 0.6268(6) 0.4758(4) 0.104(3) Uani 1 1 d D . . H2SA H 0.2684 0.6153 0.5198 0.155 Uiso 1 1 d R . . H2SB H 0.2473 0.5807 0.4650 0.155 Uiso 1 1 d R . . H2SC H 0.2087 0.6813 0.4684 0.155 Uiso 1 1 d R . . N2S N 0.5869(6) 0.8421(6) 0.0918(3) 0.121(3) Uani 1 1 d D . . C3S C 0.6307(6) 0.8692(5) 0.0605(4) 0.087(2) Uani 1 1 d D . . C4S C 0.6847(7) 0.9070(7) 0.0136(6) 0.151(5) Uani 1 1 d D . . H4SA H 0.7470 0.8656 0.0089 0.227 Uiso 1 1 d R . . H4SB H 0.6825 0.9586 0.0272 0.227 Uiso 1 1 d R . . H4SC H 0.6608 0.9221 -0.0263 0.227 Uiso 1 1 d R . . N3S N 1.1542(7) 0.7445(11) 0.1278(7) 0.244(9) Uani 1 1 d D . . C5S C 1.0921(10) 0.7929(10) 0.1458(8) 0.175(6) Uani 1 1 d D . . C6S C 1.0113(12) 0.8700(11) 0.1652(10) 0.245(9) Uani 1 1 d D . . H6SA H 1.0269 0.8950 0.1951 0.367 Uiso 1 1 d R . . H6SB H 0.9577 0.8582 0.1831 0.367 Uiso 1 1 d R . . H6SC H 0.9991 0.9102 0.1269 0.367 Uiso 1 1 d R . . C58A C -0.418(2) 1.823(2) 0.6123(15) 0.093(11) Uani 0.50 1 d P A -1 H58A H -0.4057 1.7960 0.6553 0.112 Uiso 0.50 1 calc PR A -1 H58B H -0.4616 1.8060 0.5995 0.112 Uiso 0.50 1 calc PR A -1 O2A O -0.3311(4) 1.8020(4) 0.5665(3) 0.0431(16) Uiso 0.50 1 d P A -1 C59A C -0.2771(4) 1.7173(4) 0.5674(4) 0.041(2) Uani 0.50 1 d PGU A -1 C60A C -0.1963(5) 1.6998(4) 0.5284(4) 0.079(4) Uani 0.50 1 d PGU A -1 H60A H -0.1819 1.7454 0.5045 0.094 Uiso 0.50 1 calc PR A -1 C61A C -0.1366(5) 1.6157(5) 0.5243(5) 0.100(5) Uani 0.50 1 d PGU A -1 H61A H -0.0814 1.6038 0.4976 0.120 Uiso 0.50 1 calc PR A -1 C62A C -0.1577(6) 1.5490(4) 0.5593(5) 0.087(4) Uani 0.50 1 d PGU A -1 H62A H -0.1169 1.4915 0.5565 0.105 Uiso 0.50 1 calc PR A -1 C63A C -0.2385(6) 1.5664(4) 0.5983(5) 0.066(3) Uani 0.50 1 d PGU A -1 H63A H -0.2529 1.5208 0.6222 0.079 Uiso 0.50 1 calc PR A -1 C64A C -0.2982(5) 1.6505(5) 0.6023(4) 0.043(3) Uani 0.50 1 d PGU A -1 H64A H -0.3535 1.6624 0.6290 0.052 Uiso 0.50 1 calc PR A -1 N4S N 0.1307(6) 1.5272(6) 0.5695(5) 0.058(2) Uani 0.50 1 d PD B -1 C7S C 0.0951(10) 1.4963(10) 0.6017(6) 0.100(6) Uani 0.50 1 d PD B -1 C8S C 0.0303(19) 1.4763(19) 0.6547(9) 0.187(13) Uani 0.50 1 d PD B -1 H8SA H 0.0276 1.4220 0.6508 0.280 Uiso 0.50 1 calc PR B -1 H8SB H -0.0296 1.5221 0.6530 0.280 Uiso 0.50 1 calc PR B -1 H8SC H 0.0509 1.4718 0.6945 0.280 Uiso 0.50 1 calc PR B -1 C58B C -0.4068(14) 1.8242(13) 0.6024(11) 0.041(5) Uani 0.50 1 d P A -2 H58C H -0.4444 1.7973 0.6314 0.050 Uiso 0.50 1 calc PR A -2 H58D H -0.4082 1.8149 0.5598 0.050 Uiso 0.50 1 calc PR A -2 O2B O -0.3273(8) 1.7865(7) 0.6149(5) 0.096(3) Uiso 0.50 1 d P A -2 C59B C -0.2824(7) 1.7012(6) 0.6132(7) 0.089(4) Uani 0.50 1 d PGU A -2 C60B C -0.1983(8) 1.6641(7) 0.6336(7) 0.122(5) Uani 0.50 1 d PGU A -2 H60B H -0.1748 1.6983 0.6476 0.147 Uiso 0.50 1 calc PR A -2 C61B C -0.1484(7) 1.5769(7) 0.6335(8) 0.137(6) Uani 0.50 1 d PGU A -2 H61B H -0.0909 1.5515 0.6474 0.164 Uiso 0.50 1 calc PR A -2 C62B C -0.1827(9) 1.5268(6) 0.6130(8) 0.136(6) Uani 0.50 1 d PGU A -2 H62B H -0.1487 1.4672 0.6130 0.163 Uiso 0.50 1 calc PR A -2 C63B C -0.2669(9) 1.5640(8) 0.5927(8) 0.115(6) Uani 0.50 1 d PGU A -2 H63B H -0.2904 1.5297 0.5787 0.137 Uiso 0.50 1 calc PR A -2 C64B C -0.3168(7) 1.6512(8) 0.5928(7) 0.096(6) Uani 0.50 1 d PGU A -2 H64B H -0.3743 1.6766 0.5788 0.115 Uiso 0.50 1 calc PR A -2 O2W O 0.1449(16) 1.330(2) 0.6239(15) 0.305(13) Uani 0.50 1 d PU C -2 O1W O 0.5312(5) 0.2062(5) 0.2338(4) 0.165(3) Uani 1 1 d U D -3 H1WA H 0.5263 0.2422 0.2570 0.248 Uiso 1 1 d R D -3 H1WB H 0.5020 0.1832 0.2212 0.248 Uiso 1 1 d R D -3 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 0.056(3) 0.057(3) 0.048(3) -0.009(2) -0.001(2) -0.036(2) N2 0.034(2) 0.038(2) 0.038(2) -0.0037(17) -0.0049(17) -0.0174(17) N3 0.038(2) 0.037(2) 0.042(2) -0.0028(17) -0.0074(17) -0.0194(18) N4 0.063(3) 0.061(3) 0.056(3) -0.007(2) -0.008(2) -0.039(3) C1 0.100(5) 0.070(4) 0.058(4) -0.003(3) -0.008(3) -0.049(4) C2 0.067(4) 0.065(4) 0.074(4) -0.008(3) -0.015(3) -0.036(3) C3 0.056(4) 0.083(5) 0.078(4) 0.007(3) -0.006(3) -0.035(3) C4 0.054(3) 0.055(3) 0.059(3) 0.000(3) -0.009(3) -0.030(3) C5 0.049(3) 0.058(3) 0.057(3) -0.002(3) -0.011(3) -0.033(3) C6 0.071(5) 0.071(5) 0.121(7) 0.036(5) 0.032(4) -0.003(4) C7 0.067(5) 0.068(5) 0.142(7) 0.047(5) 0.015(5) -0.011(4) C8 0.057(3) 0.066(4) 0.054(3) -0.003(3) -0.008(3) -0.043(3) C9 0.063(5) 0.164(10) 0.254(14) 0.136(10) 0.033(7) -0.012(6) C10 0.065(6) 0.166(10) 0.265(15) 0.146(11) 0.020(7) -0.011(6) C11 0.070(4) 0.072(4) 0.059(3) -0.005(3) -0.010(3) -0.054(3) C12 0.047(3) 0.065(4) 0.127(6) -0.014(4) -0.019(4) -0.029(3) C13 0.051(4) 0.051(4) 0.128(6) -0.010(4) -0.023(4) -0.026(3) C14 0.038(3) 0.046(3) 0.035(2) -0.001(2) -0.003(2) -0.024(2) C15 0.062(4) 0.046(3) 0.104(5) -0.016(3) -0.037(4) -0.017(3) C16 0.062(4) 0.048(3) 0.104(5) -0.019(3) -0.026(4) -0.020(3) C17 0.033(2) 0.040(3) 0.036(3) -0.005(2) -0.0029(19) -0.018(2) C18 0.034(3) 0.046(3) 0.064(3) -0.011(2) -0.010(2) -0.015(2) C19 0.039(3) 0.034(3) 0.060(3) -0.005(2) -0.014(2) -0.011(2) C20 0.036(3) 0.035(3) 0.046(3) -0.001(2) -0.005(2) -0.013(2) C21 0.041(3) 0.036(3) 0.052(3) -0.008(2) -0.004(2) -0.018(2) C22 0.042(3) 0.033(2) 0.048(3) -0.002(2) -0.010(2) -0.020(2) C23 0.043(3) 0.041(3) 0.041(3) -0.004(2) -0.009(2) -0.025(2) C24 0.037(3) 0.036(3) 0.045(3) 0.001(2) -0.007(2) -0.016(2) C25 0.044(3) 0.029(2) 0.047(3) 0.001(2) -0.011(2) -0.016(2) C26 0.040(3) 0.041(3) 0.039(3) -0.005(2) 0.000(2) -0.023(2) C27 0.037(3) 0.039(3) 0.061(3) -0.006(2) -0.012(2) -0.015(2) C28 0.042(3) 0.034(3) 0.051(3) -0.006(2) -0.009(2) -0.016(2) C29 0.047(3) 0.048(3) 0.049(3) -0.003(2) -0.002(2) -0.030(2) C30 0.045(3) 0.055(3) 0.095(5) -0.023(3) -0.008(3) -0.024(3) C31 0.057(4) 0.053(3) 0.086(4) -0.017(3) -0.009(3) -0.029(3) C32 0.074(4) 0.052(4) 0.132(6) 0.000(4) -0.050(4) -0.027(3) C33 0.071(4) 0.049(3) 0.126(6) 0.000(4) -0.044(4) -0.031(3) C34 0.074(4) 0.063(4) 0.062(4) -0.002(3) -0.016(3) -0.050(3) C35 0.053(3) 0.049(3) 0.063(3) -0.006(3) -0.017(3) -0.032(3) C36 0.058(4) 0.066(4) 0.080(4) -0.003(3) 0.005(3) -0.024(3) C37 0.073(4) 0.058(4) 0.083(5) 0.005(3) -0.009(4) -0.021(3) C38 0.064(4) 0.078(4) 0.055(3) -0.003(3) -0.009(3) -0.041(3) C39 0.049(4) 0.083(5) 0.082(5) -0.001(4) -0.007(3) -0.020(3) C40 0.067(4) 0.059(4) 0.078(4) 0.003(3) -0.016(3) -0.029(3) C41 0.092(5) 0.126(7) 0.075(5) 0.006(5) -0.014(4) -0.065(5) C42 0.161(9) 0.132(8) 0.116(7) -0.024(6) 0.024(7) -0.057(7) C43 0.107(7) 0.139(8) 0.205(11) 0.031(8) 0.017(7) -0.072(6) C44 0.147(9) 0.151(9) 0.269(13) 0.145(10) 0.103(9) 0.032(7) O1 0.053(2) 0.052(2) 0.068(2) -0.0143(19) -0.0135(19) -0.0136(18) O3 0.046(2) 0.044(2) 0.059(2) -0.0141(17) -0.0063(17) -0.0170(17) O4 0.045(2) 0.0402(19) 0.056(2) -0.0126(16) -0.0156(17) -0.0097(16) O5 0.062(2) 0.051(2) 0.050(2) -0.0057(17) -0.0097(18) -0.0264(18) O6 0.050(2) 0.062(3) 0.056(2) -0.0114(19) -0.0177(18) -0.0153(19) O7 0.068(3) 0.050(2) 0.087(3) -0.010(2) -0.024(2) -0.017(2) O8 0.082(3) 0.097(4) 0.109(4) -0.054(3) -0.034(3) 0.004(3) O9 0.052(2) 0.084(3) 0.062(3) -0.017(2) -0.0160(19) -0.019(2) O10 0.0392(18) 0.0432(19) 0.056(2) -0.0146(16) -0.0099(16) -0.0094(15) O11 0.062(2) 0.0410(19) 0.047(2) -0.0021(16) -0.0094(17) -0.0170(17) O12 0.049(2) 0.044(2) 0.054(2) -0.0042(16) -0.0122(17) -0.0157(17) C45 0.044(3) 0.049(3) 0.038(3) -0.008(2) 0.000(2) -0.018(2) C46 0.044(3) 0.053(3) 0.040(3) -0.005(2) -0.003(2) -0.019(2) C47 0.042(3) 0.046(3) 0.045(3) -0.008(2) 0.000(2) -0.019(2) C48 0.046(3) 0.051(3) 0.061(3) -0.013(3) -0.001(3) -0.023(3) C49 0.043(3) 0.046(3) 0.062(3) -0.011(3) -0.007(3) -0.013(2) C50 0.050(3) 0.051(3) 0.044(3) -0.010(2) -0.002(2) -0.024(3) C51 0.042(3) 0.051(3) 0.058(3) -0.013(3) -0.002(2) -0.016(2) C52 0.050(3) 0.053(3) 0.041(3) 0.004(2) -0.011(2) -0.024(3) C53 0.050(3) 0.057(3) 0.060(3) -0.002(3) -0.011(3) -0.023(3) C54 0.073(4) 0.061(4) 0.064(4) 0.004(3) -0.011(3) -0.037(3) C55 0.065(4) 0.080(5) 0.068(4) 0.019(3) -0.021(3) -0.044(4) C56 0.045(3) 0.072(4) 0.063(4) 0.006(3) -0.012(3) -0.016(3) C57 0.060(4) 0.056(3) 0.058(4) -0.003(3) -0.010(3) -0.021(3) C65 0.048(3) 0.047(3) 0.060(3) -0.013(3) -0.007(3) -0.018(3) C66 0.043(3) 0.052(3) 0.071(4) -0.018(3) -0.003(3) -0.017(3) C67 0.052(3) 0.045(3) 0.070(4) -0.008(3) -0.024(3) -0.007(3) C68 0.066(4) 0.043(3) 0.067(4) 0.011(3) -0.031(3) -0.021(3) C69 0.057(3) 0.059(3) 0.051(3) -0.002(3) -0.016(3) -0.022(3) C70 0.049(3) 0.071(4) 0.044(3) -0.008(3) -0.014(2) -0.021(3) C71 0.039(3) 0.076(4) 0.036(3) -0.009(3) -0.005(2) -0.020(3) C72 0.047(3) 0.059(3) 0.038(3) -0.004(2) -0.005(2) -0.008(3) C73 0.061(4) 0.068(4) 0.039(3) -0.013(3) -0.005(3) -0.015(3) C74 0.068(4) 0.062(4) 0.052(3) -0.013(3) -0.006(3) -0.001(3) C75 0.061(4) 0.084(5) 0.056(4) -0.020(3) -0.014(3) -0.012(3) C76 0.061(4) 0.066(4) 0.042(3) -0.014(3) 0.001(3) -0.011(3) C77 0.065(4) 0.054(3) 0.047(3) -0.013(3) 0.000(3) -0.006(3) C78 0.071(4) 0.050(3) 0.052(3) 0.009(3) -0.009(3) -0.023(3) C79 0.076(4) 0.051(4) 0.087(5) 0.004(3) -0.020(4) -0.024(3) C80 0.084(5) 0.063(4) 0.092(5) 0.012(4) -0.013(4) -0.031(4) C81 0.077(5) 0.082(5) 0.086(5) 0.009(4) -0.018(4) -0.046(4) C82 0.089(5) 0.063(4) 0.072(4) -0.010(3) -0.009(4) -0.033(4) C83 0.068(4) 0.055(4) 0.065(4) -0.008(3) -0.010(3) -0.025(3) C84 0.090(5) 0.069(4) 0.082(5) -0.028(4) -0.027(4) 0.007(4) C85 0.063(5) 0.112(7) 0.109(7) -0.068(6) -0.042(5) 0.008(5) C86 0.079(6) 0.130(8) 0.180(10) -0.091(8) -0.033(6) -0.006(5) C87 0.076(6) 0.148(10) 0.155(10) -0.087(8) -0.030(6) 0.001(6) C88 0.125(9) 0.104(8) 0.134(9) -0.035(7) -0.033(8) 0.008(7) C89 0.156(10) 0.097(7) 0.150(10) -0.046(7) -0.006(8) 0.016(7) C90 0.131(8) 0.081(6) 0.111(7) -0.021(6) -0.041(6) 0.023(6) C91 0.053(4) 0.079(4) 0.063(4) -0.015(3) 0.003(3) -0.025(3) C92 0.039(3) 0.070(4) 0.075(4) -0.032(3) -0.005(3) -0.005(3) C93 0.055(3) 0.037(3) 0.066(4) -0.003(3) -0.025(3) -0.009(2) C94 0.068(4) 0.041(3) 0.055(3) 0.006(2) -0.020(3) -0.021(3) C95 0.069(4) 0.053(3) 0.043(3) 0.000(3) -0.009(3) -0.016(3) C96 0.056(3) 0.050(3) 0.048(3) -0.002(2) -0.016(3) -0.012(3) S1 0.0525(8) 0.0413(7) 0.0555(8) -0.0016(6) -0.0086(6) -0.0216(6) O13 0.065(3) 0.050(2) 0.081(3) -0.014(2) -0.012(2) -0.0114(19) O14 0.071(3) 0.064(3) 0.076(3) -0.002(2) -0.025(2) -0.037(2) O15 0.076(3) 0.069(3) 0.077(3) 0.011(2) -0.011(2) -0.044(2) C97 0.086(5) 0.058(4) 0.070(4) -0.013(3) -0.016(3) -0.025(3) F1 0.142(4) 0.147(4) 0.097(3) -0.033(3) -0.044(3) -0.071(3) F2 0.151(4) 0.064(3) 0.108(3) -0.038(2) -0.006(3) -0.004(3) F3 0.104(3) 0.096(3) 0.060(2) 0.000(2) 0.008(2) -0.034(2) S2 0.0554(9) 0.0601(10) 0.0760(11) -0.0076(8) -0.0076(8) -0.0227(8) O16 0.092(4) 0.111(4) 0.239(8) 0.063(5) -0.093(5) -0.058(4) O17 0.208(7) 0.091(4) 0.107(5) -0.016(3) 0.023(5) -0.072(5) O18 0.069(3) 0.082(3) 0.143(5) -0.045(3) 0.001(3) -0.017(3) C98 0.117(7) 0.094(6) 0.088(6) -0.017(5) -0.021(5) -0.059(5) F4 0.262(8) 0.082(4) 0.165(6) -0.042(4) 0.067(5) -0.078(5) F5 0.248(8) 0.157(5) 0.219(7) 0.023(5) -0.136(6) -0.140(6) F6 0.183(5) 0.158(5) 0.089(3) -0.018(3) 0.018(3) -0.128(4) S3 0.0786(12) 0.0388(8) 0.0978(13) -0.0001(8) 0.0004(10) -0.0146(8) O19 0.101(5) 0.161(7) 0.168(7) 0.072(6) -0.027(5) 0.016(4) O20 0.275(11) 0.275(12) 0.319(13) -0.212(11) 0.131(10) -0.218(10) O21 0.082(3) 0.077(3) 0.165(5) 0.046(3) -0.026(3) -0.038(3) C99 0.117(7) 0.063(5) 0.122(8) 0.016(5) -0.013(6) -0.016(5) F7 0.143(5) 0.150(6) 0.221(8) 0.106(6) 0.059(5) 0.005(4) F8 0.131(5) 0.315(11) 0.150(6) -0.130(7) -0.024(4) 0.001(6) F9 0.088(3) 0.111(4) 0.140(4) 0.011(3) -0.010(3) -0.030(3) S4 0.0619(12) 0.0979(16) 0.172(3) -0.0404(16) 0.0095(14) -0.0338(11) O22 0.274(11) 0.316(13) 0.096(5) -0.036(7) -0.054(6) -0.165(10) O23 0.062(3) 0.153(6) 0.175(7) -0.073(5) 0.003(4) 0.009(4) O24 0.075(4) 0.081(4) 0.215(7) -0.017(4) 0.039(4) -0.021(3) C100 0.163(12) 0.44(3) 0.083(7) -0.070(12) 0.018(8) -0.204(17) F10 0.376(15) 0.102(5) 0.256(11) -0.002(6) 0.158(10) -0.047(7) F11 0.238(9) 0.326(12) 0.129(6) 0.018(6) 0.041(6) -0.164(9) F12 0.191(7) 0.166(6) 0.299(11) -0.051(7) -0.120(7) -0.057(5) N1S 0.094(5) 0.115(5) 0.062(4) -0.018(3) 0.013(3) -0.047(4) C1S 0.088(5) 0.065(4) 0.053(4) -0.001(3) -0.019(4) -0.034(4) C2S 0.095(6) 0.141(8) 0.082(5) 0.024(5) -0.024(4) -0.065(6) N2S 0.190(8) 0.163(7) 0.058(4) -0.010(4) 0.007(4) -0.128(7) C3S 0.100(6) 0.076(5) 0.090(6) -0.011(4) -0.003(5) -0.043(4) C4S 0.132(8) 0.134(8) 0.200(12) -0.066(8) 0.071(8) -0.083(7) N3S 0.098(8) 0.321(19) 0.218(13) 0.110(13) -0.010(9) -0.056(10) C5S 0.103(9) 0.213(17) 0.220(16) -0.028(13) -0.058(11) -0.055(11) C6S 0.200(17) 0.224(19) 0.29(2) -0.067(17) -0.038(16) -0.050(15) C58A 0.062(15) 0.078(17) 0.087(14) 0.000(11) 0.029(11) 0.003(11) C59A 0.035(5) 0.044(5) 0.044(5) -0.006(4) -0.005(4) -0.015(4) C60A 0.062(7) 0.052(6) 0.099(9) -0.022(6) 0.035(6) -0.015(5) C61A 0.068(8) 0.060(6) 0.130(11) -0.015(7) 0.019(7) 0.005(6) C62A 0.082(8) 0.056(6) 0.085(9) -0.012(6) 0.014(7) 0.002(6) C63A 0.070(8) 0.046(6) 0.073(8) -0.017(6) -0.012(6) -0.008(6) C64A 0.053(6) 0.040(6) 0.032(5) -0.005(5) -0.005(5) -0.014(5) N4S 0.059(6) 0.055(6) 0.066(6) 0.010(5) -0.025(5) -0.030(5) C7S 0.148(14) 0.120(12) 0.096(11) 0.063(9) -0.099(11) -0.112(12) C8S 0.30(3) 0.27(3) 0.093(14) -0.020(17) 0.002(18) -0.23(3) C58B 0.024(8) 0.034(9) 0.079(13) -0.020(8) -0.010(8) -0.017(7) C59B 0.079(8) 0.055(7) 0.140(13) -0.029(8) -0.037(9) -0.016(6) C60B 0.096(9) 0.097(8) 0.180(14) -0.044(10) -0.062(10) -0.013(8) C61B 0.103(10) 0.102(9) 0.201(15) -0.064(11) -0.064(10) 0.002(7) C62B 0.113(11) 0.102(10) 0.187(15) -0.067(11) -0.064(11) 0.004(8) C63B 0.108(11) 0.081(8) 0.164(15) -0.054(10) -0.051(10) -0.015(8) C64B 0.100(10) 0.073(8) 0.123(13) -0.039(9) -0.054(9) -0.014(7) O2W 0.178(16) 0.41(3) 0.35(3) -0.01(2) 0.027(18) -0.182(19) O1W 0.124(5) 0.196(8) 0.190(7) -0.109(6) -0.043(5) -0.029(5) _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 C16 1.317(7) . ? N1 C12 1.326(7) . ? N1 C11 1.510(6) . ? N2 C19 1.334(6) . ? N2 C20 1.355(6) . ? N2 C22 1.477(6) . ? N3 C28 1.323(6) . ? N3 C24 1.354(6) . ? N3 C23 1.486(5) . ? N4 C31 1.298(7) . ? N4 C32 1.327(7) . ? N4 C34 1.500(6) . ? C1 C4 1.528(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.566(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.524(8) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.508(7) . ? C5 C10 1.316(10) . ? C5 C6 1.320(8) . ? C6 C7 1.392(9) . ? C6 H6A 0.9500 . ? C7 C8 1.288(9) . ? C7 H7A 0.9500 . ? C8 C9 1.322(10) . ? C8 C11 1.512(7) . ? C9 C10 1.397(11) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.352(8) . ? C12 H12A 0.9500 . ? C13 C14 1.376(7) . ? C13 H13A 0.9500 . ? C14 C15 1.380(7) . ? C14 C17 1.497(6) . ? C15 C16 1.373(8) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C21 1.378(6) . ? C17 C18 1.391(7) . ? C18 C19 1.369(7) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.359(6) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.514(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.379(6) . ? C24 H24A 0.9500 . ? C25 C26 1.384(6) . ? C25 H25A 0.9500 . ? C26 C27 1.409(6) . ? C26 C29 1.477(6) . ? C27 C28 1.378(6) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C33 1.355(8) . ? C29 C30 1.371(7) . ? C30 C31 1.365(7) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.373(8) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C35 1.495(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C40 1.371(8) . ? C35 C36 1.375(8) . ? C36 C37 1.397(9) . ? C36 H36A 0.9500 . ? C37 C38 1.366(9) . ? C37 H37A 0.9500 . ? C38 C39 1.373(9) . ? C38 C41 1.510(9) . ? C39 C40 1.392(9) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C44 1.369(12) . ? C41 C43 1.436(12) . ? C41 C42 1.660(13) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O1 C52 1.367(6) . ? O1 C51 1.428(6) . ? O3 C50 1.375(6) . ? O3 C65 1.437(6) . ? O4 C67 1.417(6) . ? O4 C66 1.445(6) . ? O5 C68 1.418(6) . ? O5 C69 1.423(7) . ? O6 C71 1.341(7) . ? O6 C70 1.429(6) . ? O7 C78 1.368(7) . ? O7 C77 1.419(7) . ? O8 C84 1.392(9) . ? O8 C85 1.402(10) . ? O9 C76 1.361(7) . ? O9 C91 1.444(7) . ? O10 C92 1.418(6) . ? O10 C93 1.431(6) . ? O11 C94 1.424(6) . ? O11 C95 1.430(6) . ? O12 C45 1.376(6) . ? O12 C96 1.416(6) . ? C45 C46 1.374(7) . ? C45 C50 1.410(7) . ? C46 C47 1.394(7) . ? C46 H46A 0.9500 . ? C47 C48 1.386(7) . ? C47 C51 1.499(7) . ? C48 C49 1.407(7) . ? C48 C58B 1.52(2) . ? C48 C58A 1.52(3) . ? C49 C50 1.354(7) . ? C49 H49A 0.9500 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C57 1.391(8) . ? C52 C53 1.396(8) . ? C53 C54 1.391(8) . ? C53 H53A 0.9500 . ? C54 C55 1.377(9) . ? C54 H54A 0.9500 . ? C55 C56 1.373(9) . ? C55 H55A 0.9500 . ? C56 C57 1.366(8) . ? C56 H56A 0.9500 . ? C57 H57A 0.9500 . ? C65 C66 1.459(7) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.484(8) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.489(8) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.380(8) . ? C71 C76 1.414(8) . ? C72 C73 1.407(8) . ? C72 H72A 0.9500 . ? C73 C74 1.423(8) . ? C73 C77 1.505(9) . ? C74 C75 1.380(9) . ? C74 C84 1.486(9) . ? C75 C76 1.356(9) . ? C75 H75A 0.9500 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 C83 1.375(8) . ? C78 C79 1.394(9) . ? C79 C80 1.365(9) . ? C79 H79A 0.9500 . ? C80 C81 1.388(10) . ? C80 H80A 0.9500 . ? C81 C82 1.376(9) . ? C81 H81A 0.9500 . ? C82 C83 1.378(9) . ? C82 H82A 0.9500 . ? C83 H83A 0.9500 . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 C90 1.309(13) . ? C85 C86 1.379(13) . ? C86 C87 1.489(13) . ? C86 H86A 0.9500 . ? C87 C88 1.358(16) . ? C87 H87A 0.9500 . ? C88 C89 1.280(15) . ? C88 H88A 0.9500 . ? C89 C90 1.396(12) . ? C89 H89A 0.9500 . ? C90 H90A 0.9500 . ? C91 C92 1.462(9) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? C93 C94 1.460(8) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 H94A 0.9900 . ? C94 H94B 0.9900 . ? C95 C96 1.506(8) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? S1 O15 1.418(4) . ? S1 O14 1.429(4) . ? S1 O13 1.431(4) . ? S1 C97 1.796(6) . ? C97 F2 1.308(6) . ? C97 F1 1.332(7) . ? C97 F3 1.335(7) . ? S2 O18 1.378(4) . ? S2 O16 1.392(5) . ? S2 O17 1.403(6) . ? S2 C98 1.797(7) . ? C98 F6 1.298(8) . ? C98 F5 1.308(8) . ? C98 F4 1.334(8) . ? S3 O20 1.305(7) . ? S3 O21 1.374(5) . ? S3 O19 1.452(6) . ? S3 C99 1.756(8) . ? C99 F7 1.297(8) . ? C99 F8 1.317(9) . ? C99 F9 1.353(8) . ? S4 O24 1.366(5) . ? S4 O22 1.435(7) . ? S4 O23 1.441(6) . ? S4 C100 1.736(11) . ? C100 F12 1.271(9) . ? C100 F10 1.325(11) . ? C100 F11 1.362(9) . ? N1S C1S 1.102(7) . ? C1S C2S 1.476(9) . ? C2S H2SA 0.9796 . ? C2S H2SB 0.9799 . ? C2S H2SC 0.9801 . ? N2S C3S 1.086(8) . ? C3S C4S 1.467(11) . ? C4S H4SA 0.9799 . ? C4S H4SB 0.9801 . ? C4S H4SC 0.9798 . ? N3S C5S 1.081(13) . ? C5S C6S 1.508(14) . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9799 . ? C58A O2A 1.53(3) . ? C58A H58A 0.9900 . ? C58A H58B 0.9900 . ? O2A C59A 1.365(8) . ? C59A C60A 1.3900 . ? C59A C64A 1.3900 . ? C60A C61A 1.3900 . ? C60A H60A 0.9500 . ? C61A C62A 1.3900 . ? C61A H61A 0.9500 . ? C62A C63A 1.3900 . ? C62A H62A 0.9500 . ? C63A C64A 1.3900 . ? C63A H63A 0.9500 . ? C64A H64A 0.9500 . ? N4S C7S 1.041(11) . ? C7S C8S 1.515(15) . ? C8S H8SA 0.9800 . ? C8S H8SB 0.9800 . ? C8S H8SC 0.9800 . ? C58B O2B 1.26(2) . ? C58B H58C 0.9900 . ? C58B H58D 0.9900 . ? O2B C59B 1.356(13) . ? C59B C60B 1.3900 . ? C59B C64B 1.3900 . ? C60B C61B 1.3900 . ? C60B H60B 0.9500 . ? C61B C62B 1.3900 . ? C61B H61B 0.9500 . ? C62B C63B 1.3900 . ? C62B H62B 0.9500 . ? C63B C64B 1.3900 . ? C63B H63B 0.9500 . ? C64B H64B 0.9500 . ? O1W H1WA 0.8503 . ? O1W H1WB 0.8499 . ? 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 C16 N1 C12 120.3(5) . . ? C16 N1 C11 120.3(5) . . ? C12 N1 C11 119.4(5) . . ? C19 N2 C20 121.0(4) . . ? C19 N2 C22 119.6(4) . . ? C20 N2 C22 119.4(4) . . ? C28 N3 C24 122.0(4) . . ? C28 N3 C23 118.9(4) . . ? C24 N3 C23 119.1(4) . . ? C31 N4 C32 119.5(5) . . ? C31 N4 C34 121.0(5) . . ? C32 N4 C34 119.5(5) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C1 109.8(4) . . ? C5 C4 C3 112.6(5) . . ? C1 C4 C3 108.4(5) . . ? C5 C4 C2 109.4(5) . . ? C1 C4 C2 108.9(5) . . ? C3 C4 C2 107.8(5) . . ? C10 C5 C6 113.2(6) . . ? C10 C5 C4 122.1(6) . . ? C6 C5 C4 124.7(5) . . ? C5 C6 C7 123.6(7) . . ? C5 C6 H6A 118.2 . . ? C7 C6 H6A 118.2 . . ? C8 C7 C6 123.0(7) . . ? C8 C7 H7A 118.5 . . ? C6 C7 H7A 118.5 . . ? C7 C8 C9 114.8(6) . . ? C7 C8 C11 122.9(6) . . ? C9 C8 C11 122.2(6) . . ? C8 C9 C10 122.3(8) . . ? C8 C9 H9A 118.9 . . ? C10 C9 H9A 118.9 . . ? C5 C10 C9 123.1(8) . . ? C5 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? N1 C11 C8 111.5(4) . . ? N1 C11 H11A 109.3 . . ? C8 C11 H11A 109.3 . . ? N1 C11 H11B 109.3 . . ? C8 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N1 C12 C13 120.7(6) . . ? N1 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C12 C13 C14 121.6(6) . . ? C12 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? C13 C14 C15 116.2(5) . . ? C13 C14 C17 122.2(5) . . ? C15 C14 C17 121.7(4) . . ? C16 C15 C14 120.3(5) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? N1 C16 C15 121.0(5) . . ? N1 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C21 C17 C18 117.6(4) . . ? C21 C17 C14 121.6(4) . . ? C18 C17 C14 120.8(4) . . ? C19 C18 C17 120.1(4) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? N2 C19 C18 120.5(4) . . ? N2 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? N2 C20 C21 119.7(4) . . ? N2 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? C20 C21 C17 121.1(4) . . ? C20 C21 H21A 119.4 . . ? C17 C21 H21A 119.4 . . ? N2 C22 C23 108.8(4) . . ? N2 C22 H22A 109.9 . . ? C23 C22 H22A 109.9 . . ? N2 C22 H22B 109.9 . . ? C23 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? N3 C23 C22 108.3(4) . . ? N3 C23 H23A 110.0 . . ? C22 C23 H23A 110.0 . . ? N3 C23 H23B 110.0 . . ? C22 C23 H23B 110.0 . . ? H23A C23 H23B 108.4 . . ? N3 C24 C25 118.9(4) . . ? N3 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? C24 C25 C26 121.5(4) . . ? C24 C25 H25A 119.2 . . ? C26 C25 H25A 119.2 . . ? C25 C26 C27 116.8(4) . . ? C25 C26 C29 122.3(4) . . ? C27 C26 C29 120.9(4) . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? N3 C28 C27 120.6(4) . . ? N3 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C33 C29 C30 116.3(5) . . ? C33 C29 C26 122.6(5) . . ? C30 C29 C26 121.1(5) . . ? C31 C30 C29 120.7(5) . . ? C31 C30 H30A 119.6 . . ? C29 C30 H30A 119.6 . . ? N4 C31 C30 121.7(5) . . ? N4 C31 H31A 119.2 . . ? C30 C31 H31A 119.2 . . ? N4 C32 C33 120.7(6) . . ? N4 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C29 C33 C32 121.0(6) . . ? C29 C33 H33A 119.5 . . ? C32 C33 H33A 119.5 . . ? C35 C34 N4 110.4(4) . . ? C35 C34 H34A 109.6 . . ? N4 C34 H34A 109.6 . . ? C35 C34 H34B 109.6 . . ? N4 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C40 C35 C36 118.4(6) . . ? C40 C35 C34 120.3(5) . . ? C36 C35 C34 121.3(5) . . ? C35 C36 C37 120.9(6) . . ? C35 C36 H36A 119.5 . . ? C37 C36 H36A 119.5 . . ? C38 C37 C36 121.4(6) . . ? C38 C37 H37A 119.3 . . ? C36 C37 H37A 119.3 . . ? C37 C38 C39 116.8(6) . . ? C37 C38 C41 123.2(6) . . ? C39 C38 C41 119.9(6) . . ? C38 C39 C40 122.8(6) . . ? C38 C39 H39A 118.6 . . ? C40 C39 H39A 118.6 . . ? C35 C40 C39 119.7(6) . . ? C35 C40 H40A 120.2 . . ? C39 C40 H40A 120.2 . . ? C44 C41 C43 117.7(10) . . ? C44 C41 C38 113.8(7) . . ? C43 C41 C38 113.3(7) . . ? C44 C41 C42 104.7(11) . . ? C43 C41 C42 98.3(8) . . ? C38 C41 C42 106.7(7) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C52 O1 C51 116.8(4) . . ? C50 O3 C65 116.4(4) . . ? C67 O4 C66 112.9(4) . . ? C68 O5 C69 112.6(4) . . ? C71 O6 C70 117.4(4) . . ? C78 O7 C77 118.7(5) . . ? C84 O8 C85 116.9(7) . . ? C76 O9 C91 121.7(5) . . ? C92 O10 C93 109.5(4) . . ? C94 O11 C95 111.4(4) . . ? C45 O12 C96 116.6(4) . . ? C46 C45 O12 125.2(5) . . ? C46 C45 C50 118.6(5) . . ? O12 C45 C50 116.2(4) . . ? C45 C46 C47 121.9(5) . . ? C45 C46 H46A 119.1 . . ? C47 C46 H46A 119.1 . . ? C48 C47 C46 119.0(5) . . ? C48 C47 C51 118.8(5) . . ? C46 C47 C51 122.2(5) . . ? C47 C48 C49 119.1(5) . . ? C47 C48 C58B 123.6(7) . . ? C49 C48 C58B 117.1(8) . . ? C47 C48 C58A 121.5(14) . . ? C49 C48 C58A 119.0(14) . . ? C58B C48 C58A 9.8(19) . . ? C50 C49 C48 121.3(5) . . ? C50 C49 H49A 119.4 . . ? C48 C49 H49A 119.4 . . ? C49 C50 O3 124.2(5) . . ? C49 C50 C45 120.2(5) . . ? O3 C50 C45 115.5(4) . . ? O1 C51 C47 110.0(4) . . ? O1 C51 H51A 109.7 . . ? C47 C51 H51A 109.7 . . ? O1 C51 H51B 109.7 . . ? C47 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? O1 C52 C57 116.2(5) . . ? O1 C52 C53 124.7(5) . . ? C57 C52 C53 119.1(5) . . ? C54 C53 C52 119.7(5) . . ? C54 C53 H53A 120.2 . . ? C52 C53 H53A 120.2 . . ? C55 C54 C53 120.4(6) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C56 C55 C54 119.4(6) . . ? C56 C55 H55A 120.3 . . ? C54 C55 H55A 120.3 . . ? C57 C56 C55 121.4(6) . . ? C57 C56 H56A 119.3 . . ? C55 C56 H56A 119.3 . . ? C56 C57 C52 120.1(6) . . ? C56 C57 H57A 120.0 . . ? C52 C57 H57A 120.0 . . ? O3 C65 C66 108.3(4) . . ? O3 C65 H65A 110.0 . . ? C66 C65 H65A 110.0 . . ? O3 C65 H65B 110.0 . . ? C66 C65 H65B 110.0 . . ? H65A C65 H65B 108.4 . . ? O4 C66 C65 110.9(4) . . ? O4 C66 H66A 109.5 . . ? C65 C66 H66A 109.5 . . ? O4 C66 H66B 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 108.0 . . ? O4 C67 C68 109.6(4) . . ? O4 C67 H67A 109.8 . . ? C68 C67 H67A 109.8 . . ? O4 C67 H67B 109.8 . . ? C68 C67 H67B 109.8 . . ? H67A C67 H67B 108.2 . . ? O5 C68 C67 109.5(5) . . ? O5 C68 H68A 109.8 . . ? C67 C68 H68A 109.8 . . ? O5 C68 H68B 109.8 . . ? C67 C68 H68B 109.8 . . ? H68A C68 H68B 108.2 . . ? O5 C69 C70 109.0(5) . . ? O5 C69 H69A 109.9 . . ? C70 C69 H69A 109.9 . . ? O5 C69 H69B 109.9 . . ? C70 C69 H69B 109.9 . . ? H69A C69 H69B 108.3 . . ? O6 C70 C69 109.7(4) . . ? O6 C70 H70A 109.7 . . ? C69 C70 H70A 109.7 . . ? O6 C70 H70B 109.7 . . ? C69 C70 H70B 109.7 . . ? H70A C70 H70B 108.2 . . ? O6 C71 C72 125.3(5) . . ? O6 C71 C76 115.1(5) . . ? C72 C71 C76 119.6(6) . . ? C71 C72 C73 122.2(5) . . ? C71 C72 H72A 118.9 . . ? C73 C72 H72A 118.9 . . ? C72 C73 C74 117.4(6) . . ? C72 C73 C77 120.1(5) . . ? C74 C73 C77 122.5(6) . . ? C75 C74 C73 118.4(6) . . ? C75 C74 C84 119.9(6) . . ? C73 C74 C84 121.7(7) . . ? C76 C75 C74 124.4(6) . . ? C76 C75 H75A 117.8 . . ? C74 C75 H75A 117.8 . . ? C75 C76 O9 126.7(6) . . ? C75 C76 C71 117.9(6) . . ? O9 C76 C71 115.4(5) . . ? O7 C77 C73 108.9(5) . . ? O7 C77 H77A 109.9 . . ? C73 C77 H77A 109.9 . . ? O7 C77 H77B 109.9 . . ? C73 C77 H77B 109.9 . . ? H77A C77 H77B 108.3 . . ? O7 C78 C83 125.1(6) . . ? O7 C78 C79 115.3(5) . . ? C83 C78 C79 119.6(6) . . ? C80 C79 C78 120.3(6) . . ? C80 C79 H79A 119.8 . . ? C78 C79 H79A 119.8 . . ? C79 C80 C81 120.5(7) . . ? C79 C80 H80A 119.7 . . ? C81 C80 H80A 119.7 . . ? C82 C81 C80 118.5(7) . . ? C82 C81 H81A 120.7 . . ? C80 C81 H81A 120.7 . . ? C83 C82 C81 121.6(6) . . ? C83 C82 H82A 119.2 . . ? C81 C82 H82A 119.2 . . ? C78 C83 C82 119.4(6) . . ? C78 C83 H83A 120.3 . . ? C82 C83 H83A 120.3 . . ? O8 C84 C74 110.5(7) . . ? O8 C84 H84A 109.6 . . ? C74 C84 H84A 109.6 . . ? O8 C84 H84B 109.6 . . ? C74 C84 H84B 109.6 . . ? H84A C84 H84B 108.1 . . ? C90 C85 C86 122.9(9) . . ? C90 C85 O8 125.9(8) . . ? C86 C85 O8 111.2(10) . . ? C85 C86 C87 114.4(12) . . ? C85 C86 H86A 122.8 . . ? C87 C86 H86A 122.8 . . ? C88 C87 C86 121.0(11) . . ? C88 C87 H87A 119.5 . . ? C86 C87 H87A 119.5 . . ? C89 C88 C87 117.9(11) . . ? C89 C88 H88A 121.1 . . ? C87 C88 H88A 121.1 . . ? C88 C89 C90 125.1(13) . . ? C88 C89 H89A 117.4 . . ? C90 C89 H89A 117.4 . . ? C85 C90 C89 118.6(11) . . ? C85 C90 H90A 120.7 . . ? C89 C90 H90A 120.7 . . ? O9 C91 C92 112.9(5) . . ? O9 C91 H91A 109.0 . . ? C92 C91 H91A 109.0 . . ? O9 C91 H91B 109.0 . . ? C92 C91 H91B 109.0 . . ? H91A C91 H91B 107.8 . . ? O10 C92 C91 110.0(5) . . ? O10 C92 H92A 109.7 . . ? C91 C92 H92A 109.7 . . ? O10 C92 H92B 109.7 . . ? C91 C92 H92B 109.7 . . ? H92A C92 H92B 108.2 . . ? O10 C93 C94 111.0(4) . . ? O10 C93 H93A 109.4 . . ? C94 C93 H93A 109.4 . . ? O10 C93 H93B 109.4 . . ? C94 C93 H93B 109.4 . . ? H93A C93 H93B 108.0 . . ? O11 C94 C93 111.0(4) . . ? O11 C94 H94A 109.4 . . ? C93 C94 H94A 109.4 . . ? O11 C94 H94B 109.4 . . ? C93 C94 H94B 109.4 . . ? H94A C94 H94B 108.0 . . ? O11 C95 C96 110.2(4) . . ? O11 C95 H95A 109.6 . . ? C96 C95 H95A 109.6 . . ? O11 C95 H95B 109.6 . . ? C96 C95 H95B 109.6 . . ? H95A C95 H95B 108.1 . . ? O12 C96 C95 109.5(4) . . ? O12 C96 H96A 109.8 . . ? C95 C96 H96A 109.8 . . ? O12 C96 H96B 109.8 . . ? C95 C96 H96B 109.8 . . ? H96A C96 H96B 108.2 . . ? O15 S1 O14 113.7(2) . . ? O15 S1 O13 116.1(3) . . ? O14 S1 O13 114.4(2) . . ? O15 S1 C97 103.7(3) . . ? O14 S1 C97 103.9(3) . . ? O13 S1 C97 102.8(3) . . ? F2 C97 F1 108.8(5) . . ? F2 C97 F3 107.7(5) . . ? F1 C97 F3 107.2(5) . . ? F2 C97 S1 111.8(4) . . ? F1 C97 S1 110.0(5) . . ? F3 C97 S1 111.3(4) . . ? O18 S2 O16 117.7(4) . . ? O18 S2 O17 115.1(4) . . ? O16 S2 O17 109.6(5) . . ? O18 S2 C98 104.6(4) . . ? O16 S2 C98 102.9(3) . . ? O17 S2 C98 105.2(4) . . ? F6 C98 F5 110.1(7) . . ? F6 C98 F4 103.6(7) . . ? F5 C98 F4 104.1(7) . . ? F6 C98 S2 114.1(5) . . ? F5 C98 S2 111.5(5) . . ? F4 C98 S2 112.7(6) . . ? O20 S3 O21 114.3(7) . . ? O20 S3 O19 114.7(7) . . ? O21 S3 O19 111.9(4) . . ? O20 S3 C99 106.3(5) . . ? O21 S3 C99 106.5(4) . . ? O19 S3 C99 101.8(4) . . ? F7 C99 F8 108.2(9) . . ? F7 C99 F9 106.4(7) . . ? F8 C99 F9 102.6(6) . . ? F7 C99 S3 111.5(6) . . ? F8 C99 S3 115.3(7) . . ? F9 C99 S3 112.0(6) . . ? O24 S4 O22 109.7(6) . . ? O24 S4 O23 116.6(4) . . ? O22 S4 O23 114.6(5) . . ? O24 S4 C100 109.6(5) . . ? O22 S4 C100 101.5(5) . . ? O23 S4 C100 103.4(5) . . ? F12 C100 F10 117.3(12) . . ? F12 C100 F11 111.8(9) . . ? F10 C100 F11 104.0(10) . . ? F12 C100 S4 102.7(8) . . ? F10 C100 S4 111.0(7) . . ? F11 C100 S4 110.1(8) . . ? N1S C1S C2S 178.5(8) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 110.3 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 108.7 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? N2S C3S C4S 174.6(10) . . ? C3S C4S H4SA 109.2 . . ? C3S C4S H4SB 109.4 . . ? H4SA C4S H4SB 109.5 . . ? C3S C4S H4SC 109.8 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? N3S C5S C6S 171(2) . . ? C5S C6S H6SA 109.0 . . ? C5S C6S H6SB 114.3 . . ? H6SA C6S H6SB 109.5 . . ? C5S C6S H6SC 105.0 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? O2A C58A C48 99.8(19) . . ? O2A C58A H58A 111.8 . . ? C48 C58A H58A 111.8 . . ? O2A C58A H58B 111.8 . . ? C48 C58A H58B 111.8 . . ? H58A C58A H58B 109.5 . . ? C59A O2A C58A 115.7(14) . . ? O2A C59A C60A 114.8(5) . . ? O2A C59A C64A 125.2(5) . . ? C60A C59A C64A 120.0 . . ? C59A C60A C61A 120.0 . . ? C59A C60A H60A 120.0 . . ? C61A C60A H60A 120.0 . . ? C60A C61A C62A 120.0 . . ? C60A C61A H61A 120.0 . . ? C62A C61A H61A 120.0 . . ? C61A C62A C63A 120.0 . . ? C61A C62A H62A 120.0 . . ? C63A C62A H62A 120.0 . . ? C64A C63A C62A 120.0 . . ? C64A C63A H63A 120.0 . . ? C62A C63A H63A 120.0 . . ? C63A C64A C59A 120.0 . . ? C63A C64A H64A 120.0 . . ? C59A C64A H64A 120.0 . . ? N4S C7S C8S 164(2) . . ? O2B C58B C48 115.4(10) . . ? O2B C58B H58C 108.4 . . ? C48 C58B H58C 108.4 . . ? O2B C58B H58D 108.4 . . ? C48 C58B H58D 108.4 . . ? H58C C58B H58D 107.5 . . ? C58B O2B C59B 121.1(12) . . ? O2B C59B C60B 116.7(9) . . ? O2B C59B C64B 123.3(9) . . ? C60B C59B C64B 120.0 . . ? C59B C60B C61B 120.0 . . ? C59B C60B H60B 120.0 . . ? C61B C60B H60B 120.0 . . ? C62B C61B C60B 120.0 . . ? C62B C61B H61B 120.0 . . ? C60B C61B H61B 120.0 . . ? C61B C62B C63B 120.0 . . ? C61B C62B H62B 120.0 . . ? C63B C62B H62B 120.0 . . ? C62B C63B C64B 120.0 . . ? C62B C63B H63B 120.0 . . ? C64B C63B H63B 120.0 . . ? C63B C64B C59B 120.0 . . ? C63B C64B H64B 120.0 . . ? C59B C64B H64B 120.0 . . ? H1WA O1W H1WB 143.3 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.171 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.110 data_dm14q _database_code_depnum_ccdc_archive 'CCDC 864508' #TrackingRef '- DM14Q.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C119 H169 B6 Cd F24 N31 O60' _chemical_formula_weight 3627.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 20.057(3) _cell_length_b 22.223(3) _cell_length_c 18.474(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.497(2) _cell_angle_gamma 90.00 _cell_volume 7763(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 332 _cell_measurement_theta_min 1.08 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3748 _exptl_absorpt_coefficient_mu 0.270 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9333 _exptl_absorpt_correction_T_max 0.9709 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 73748 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 27335 _reflns_number_gt 15867 _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. All tetrafluorborate anions were refined as rigid groups using a combination of DFIX, SADI, SIMU and DELU restraints. AFIX 66 commands were used to restrain all the aromatic rings in the crown ether to be idealized hexagons with C-C and C-N bonds equal to 1.39 A. Some of the geometry of the polyether portions of the crown ether were restrained to have chemcially reasonable bond distances and angles using DFIX, DANG, and SIMU restraints. The unit cell contains 46 molecules of nitromethane which were treated as diffuse contributions to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.318 0.540 -0.160 3267 1486 ' ' _platon_squeeze_details ; ; _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^)+(0.1662P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.19(3) _refine_ls_number_reflns 27335 _refine_ls_number_parameters 1174 _refine_ls_number_restraints 534 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.2405 _refine_ls_wR_factor_gt 0.2214 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.001 _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 Cd1 Cd -1.72548(3) 0.208906(18) 0.43953(3) 0.06087(16) Uani 1 1 d . . . O1W O -1.6623(4) 0.2140(3) 0.3555(4) 0.093(2) Uani 1 1 d . . . H1WA H -1.6280 0.1821 0.3663 0.139 Uiso 1 1 d R . . H1WB H -1.6945 0.2098 0.3040 0.139 Uiso 1 1 d R . . O2W O -1.7984(4) 0.20221(19) 0.5176(4) 0.0774(18) Uani 1 1 d . . . H2WA H -1.7901 0.2366 0.5509 0.116 Uiso 1 1 d R . . H2WB H -1.8471 0.2013 0.4855 0.116 Uiso 1 1 d R . . N1 N -1.7312(4) -0.68488(14) 0.4366(4) 0.0710(14) Uani 1 1 d G . . C1 C -1.7057(4) -0.6530(3) 0.3867(4) 0.147(5) Uani 1 1 d G . . H1A H -1.6884 -0.6734 0.3528 0.176 Uiso 1 1 calc R . . C2 C -1.7062(5) -0.5904(3) 0.3873(4) 0.126(4) Uani 1 1 d G . . H2A H -1.6891 -0.5691 0.3538 0.151 Uiso 1 1 calc R . . C3 C -1.7322(5) -0.55980(14) 0.4379(5) 0.081(2) Uani 1 1 d G . . C4 C -1.7576(4) -0.5917(3) 0.4878(4) 0.151(6) Uani 1 1 d G . . H4A H -1.7750 -0.5712 0.5217 0.181 Uiso 1 1 calc R . . C5 C -1.7572(4) -0.6543(3) 0.4872(4) 0.100(3) Uani 1 1 d G . . H5A H -1.7742 -0.6756 0.5206 0.121 Uiso 1 1 calc R . . C6 C -1.7315(5) -0.49555(15) 0.4385(4) 0.099(3) Uani 1 1 d G . . C7 C -1.7326(6) -0.4661(3) 0.5045(4) 0.162(6) Uani 1 1 d G . . H7A H -1.7270 -0.4878 0.5491 0.195 Uiso 1 1 calc R . . C8 C -1.7421(5) -0.4041(3) 0.5037(3) 0.119(4) Uani 1 1 d G . . H8A H -1.7428 -0.3844 0.5478 0.142 Uiso 1 1 calc R . . N2 N -1.7505(4) -0.37158(15) 0.4369(4) 0.118(3) Uani 1 1 d G . . C9 C -1.7494(5) -0.4011(3) 0.3710(3) 0.113(4) Uani 1 1 d G . . H9A H -1.7551 -0.3793 0.3263 0.136 Uiso 1 1 calc R . . C10 C -1.7400(5) -0.4631(3) 0.3717(3) 0.105(3) Uani 1 1 d G . . H10A H -1.7392 -0.4828 0.3276 0.127 Uiso 1 1 calc R . . C11 C -1.7552(8) -0.3055(5) 0.4378(7) 0.111(4) Uani 1 1 d . . . H11A H -1.7882 -0.2917 0.3892 0.134 Uiso 1 1 calc R . . H11B H -1.7732 -0.2932 0.4781 0.134 Uiso 1 1 calc R . . C12 C -1.6892(11) -0.2787(5) 0.4500(9) 0.142(6) Uani 1 1 d . . . H12A H -1.6713 -0.2891 0.4089 0.170 Uiso 1 1 calc R . . H12B H -1.6554 -0.2922 0.4983 0.170 Uiso 1 1 calc R . . N3 N -1.7004(4) -0.21279(17) 0.4516(4) 0.109(3) Uani 1 1 d G . . C13 C -1.7227(5) -0.1829(3) 0.3815(3) 0.166(7) Uani 1 1 d G . . H13A H -1.7351 -0.2047 0.3360 0.199 Uiso 1 1 calc R . . C14 C -1.7266(4) -0.1205(3) 0.3794(3) 0.112(4) Uani 1 1 d G . . H14A H -1.7416 -0.1005 0.3325 0.134 Uiso 1 1 calc R . . C15 C -1.7082(3) -0.08788(17) 0.4475(4) 0.084(3) Uani 1 1 d G . . C16 C -1.6858(4) -0.1177(2) 0.5176(3) 0.090(3) Uani 1 1 d G . . H16A H -1.6735 -0.0959 0.5631 0.109 Uiso 1 1 calc R . . C17 C -1.6819(4) -0.1802(2) 0.5197(3) 0.110(3) Uani 1 1 d G . . H17A H -1.6670 -0.2002 0.5666 0.132 Uiso 1 1 calc R . . C18 C -1.7080(3) -0.02012(13) 0.4462(3) 0.070(2) Uani 1 1 d G . . C19 C -1.6881(3) 0.0108(2) 0.3912(3) 0.069(2) Uani 1 1 d G . . H19A H -1.6715 -0.0102 0.3572 0.083 Uiso 1 1 calc R . . C20 C -1.6932(3) 0.0732(2) 0.3871(3) 0.076(2) Uani 1 1 d G . . H20A H -1.6799 0.0939 0.3503 0.091 Uiso 1 1 calc R . . N4 N -1.7181(3) 0.10462(13) 0.4379(4) 0.0650(14) Uani 1 1 d G . . C21 C -1.7379(3) 0.0737(2) 0.4929(3) 0.081(3) Uani 1 1 d G . . H21A H -1.7546 0.0947 0.5268 0.097 Uiso 1 1 calc R . . C22 C -1.7329(3) 0.0113(2) 0.4970(3) 0.078(2) Uani 1 1 d G . . H22A H -1.7462 -0.0094 0.5338 0.093 Uiso 1 1 calc R . . N5 N -2.6238(3) 0.2097(2) -0.4515(2) 0.071(2) Uani 1 1 d G . . C23 C -2.6270(3) 0.2204(4) -0.3786(3) 0.146(5) Uani 1 1 d G . . H23A H -2.6702 0.2290 -0.3725 0.175 Uiso 1 1 calc R . . C24 C -2.5657(4) 0.2185(4) -0.3149(2) 0.135(4) Uani 1 1 d G . . H24A H -2.5679 0.2257 -0.2662 0.162 Uiso 1 1 calc R . . C25 C -2.5012(3) 0.2057(3) -0.3241(4) 0.091(4) Uani 1 1 d G . . C26 C -2.4979(3) 0.1950(5) -0.3970(5) 0.190(7) Uani 1 1 d G . . H26A H -2.4547 0.1864 -0.4031 0.228 Uiso 1 1 calc R . . C27 C -2.5592(4) 0.1969(4) -0.4607(3) 0.242(10) Uani 1 1 d G . . H27A H -2.5570 0.1897 -0.5094 0.290 Uiso 1 1 calc R . . C28 C -2.4356(4) 0.1981(4) -0.2547(4) 0.140(6) Uani 1 1 d G . . C29 C -2.3835(5) 0.1590(4) -0.2604(4) 0.152(5) Uani 1 1 d G . . H29A H -2.3875 0.1414 -0.3073 0.182 Uiso 1 1 calc R . . C30 C -2.3253(4) 0.1463(4) -0.1959(6) 0.168(6) Uani 1 1 d G . . H30A H -2.2904 0.1201 -0.1997 0.202 Uiso 1 1 calc R . . N6 N -2.3193(4) 0.1726(5) -0.1258(4) 0.225(7) Uani 1 1 d G . . C31 C -2.3714(5) 0.2117(5) -0.1201(4) 0.163(7) Uani 1 1 d G . . H31A H -2.3673 0.2293 -0.0731 0.196 Uiso 1 1 calc R . . C32 C -2.4295(4) 0.2245(4) -0.1845(5) 0.133(4) Uani 1 1 d G . . H32A H -2.4644 0.2506 -0.1807 0.159 Uiso 1 1 calc R . . C33 C -2.2025(5) 0.2086(6) -0.0551(5) 0.114(4) Uani 1 1 d . . . H33A H -2.2243 0.2475 -0.0544 0.136 Uiso 1 1 calc R . . H33B H -2.1901 0.2065 -0.1015 0.136 Uiso 1 1 calc R . . C34 C -2.2506(6) 0.1641(6) -0.0570(7) 0.137(4) Uani 1 1 d . . . H34A H -2.2616 0.1649 -0.0097 0.164 Uiso 1 1 calc R . . H34B H -2.2302 0.1252 -0.0609 0.164 Uiso 1 1 calc R . . N7 N -2.13909(18) 0.2041(3) 0.0106(2) 0.083(2) Uani 1 1 d G . . C35 C -2.14199(18) 0.2173(3) 0.0830(2) 0.098(3) Uani 1 1 d G . . H35A H -2.1853 0.2252 0.0893 0.118 Uiso 1 1 calc R . . C36 C -2.0802(2) 0.2187(3) 0.14615(19) 0.089(2) Uani 1 1 d G . . H36A H -2.0821 0.2275 0.1946 0.106 Uiso 1 1 calc R . . C37 C -2.01549(19) 0.2068(2) 0.1368(2) 0.075(2) Uani 1 1 d G . . C38 C -2.01259(18) 0.1936(3) 0.0644(3) 0.070(2) Uani 1 1 d G . . H38A H -1.9693 0.1857 0.0582 0.083 Uiso 1 1 calc R . . C39 C -2.0744(2) 0.1923(3) 0.00129(19) 0.068(2) Uani 1 1 d G . . H39A H -2.0724 0.1834 -0.0472 0.082 Uiso 1 1 calc R . . C40 C -1.95038(18) 0.20627(19) 0.20491(19) 0.065(3) Uani 1 1 d G . . C41 C -1.94139(18) 0.24942(17) 0.2618(2) 0.0603(16) Uani 1 1 d G . . H41A H -1.9765 0.2779 0.2574 0.072 Uiso 1 1 calc R . . C42 C -1.8800(2) 0.24997(16) 0.3254(2) 0.0548(15) Uani 1 1 d G . . H42A H -1.8739 0.2788 0.3635 0.066 Uiso 1 1 calc R . . N8 N -1.82749(16) 0.20738(17) 0.3321(2) 0.066(2) Uani 1 1 d G . . C43 C -1.83647(19) 0.16423(18) 0.2751(2) 0.0700(19) Uani 1 1 d G . . H43A H -1.8014 0.1357 0.2795 0.084 Uiso 1 1 calc R . . C44 C -1.8979(2) 0.16367(19) 0.2115(2) 0.0741(19) Uani 1 1 d G . . H44A H -1.9039 0.1348 0.1734 0.089 Uiso 1 1 calc R . . O1 O -0.9645(11) 0.4752(18) 1.2525(10) 0.342(15) Uani 1 1 d . . . O2 O -0.8724(4) 0.4611(3) 1.1498(4) 0.1141(19) Uani 1 1 d . . . O3 O -1.1730(7) 0.3524(6) 1.0357(7) 0.196(4) Uani 1 1 d D . . O4 O -1.2976(4) 0.2748(4) 1.0490(5) 0.129(3) Uani 1 1 d D . . O5 O -1.2625(8) 0.1678(7) 1.1214(10) 0.241(6) Uani 1 1 d D . . O6 O -1.1677(5) 0.0816(4) 1.0858(7) 0.160(3) Uani 1 1 d D . . O7 O -0.9565(4) -0.0687(3) 1.2792(4) 0.1102(19) Uani 1 1 d . . . O8 O -0.8480(3) 0.0225(2) 1.1641(3) 0.0799(15) Uani 1 1 d . . . O9 O -1.1183(4) 0.0570(3) 0.9737(5) 0.127(2) Uani 1 1 d D . . O10 O -1.1622(4) 0.1135(5) 0.8312(4) 0.146(3) Uani 1 1 d D . . O11 O -1.1007(6) 0.2310(7) 0.8319(6) 0.192(4) Uani 1 1 d D . . O12 O -1.0947(5) 0.3254(4) 0.9571(5) 0.153(3) Uani 1 1 d D . . C45 C -1.0623(5) 0.3521(3) 1.0268(4) 0.125(3) Uani 1 1 d G . . C46 C -0.9897(4) 0.3623(3) 1.0551(4) 0.109(3) Uani 1 1 d G . . H46A H -0.9617 0.3519 1.0258 0.130 Uiso 1 1 calc R . . C47 C -0.9591(3) 0.3878(3) 1.1273(4) 0.107(3) Uani 1 1 d G . . C48 C -1.0009(5) 0.4033(4) 1.1712(4) 0.127(4) Uani 1 1 d G . . C49 C -1.0734(5) 0.3931(4) 1.1428(6) 0.155(5) Uani 1 1 d G . . H49A H -1.1014 0.4034 1.1722 0.186 Uiso 1 1 calc R . . C50 C -1.1041(3) 0.3676(4) 1.0706(6) 0.143(4) Uani 1 1 d G . . C51 C -0.8773(6) 0.3990(5) 1.1521(6) 0.114(3) Uani 1 1 d . . . H51A H -0.8532 0.3838 1.2035 0.136 Uiso 1 1 calc R . . H51B H -0.8573 0.3801 1.1167 0.136 Uiso 1 1 calc R . . C52 C -0.8006(4) 0.4815(4) 1.1716(4) 0.129(5) Uani 1 1 d G . . C53 C -0.7918(6) 0.5436(4) 1.1714(4) 0.128(4) Uani 1 1 d G . . H53A H -0.8311 0.5687 1.1577 0.153 Uiso 1 1 calc R . . C54 C -0.7243(8) 0.5680(4) 1.1918(5) 0.220(12) Uani 1 1 d G . . H54A H -0.7184 0.6095 1.1916 0.265 Uiso 1 1 calc R . . C55 C -0.6655(6) 0.5305(6) 1.2123(5) 0.168(8) Uani 1 1 d G . . H55A H -0.6203 0.5468 1.2259 0.202 Uiso 1 1 calc R . . C56 C -0.6743(4) 0.4684(5) 1.2125(4) 0.171(7) Uani 1 1 d G . . H56A H -0.6350 0.4433 1.2262 0.206 Uiso 1 1 calc R . . C57 C -0.7418(5) 0.4440(3) 1.1921(3) 0.087(2) Uani 1 1 d G . . H57A H -0.7477 0.4025 1.1922 0.104 Uiso 1 1 calc R . . C58 C -0.9751(13) 0.4208(13) 1.267(2) 0.32(3) Uani 1 1 d . . . H58A H -1.0124 0.4160 1.2890 0.389 Uiso 1 1 calc R . . H58B H -0.9325 0.4001 1.2976 0.389 Uiso 1 1 calc R . . C59 C -0.9521(9) 0.5380(8) 1.2984(10) 0.33(2) Uani 1 1 d G . . C60 C -0.9250(9) 0.5158(6) 1.3729(13) 0.232(10) Uani 1 1 d G . . H60A H -0.9287 0.4751 1.3822 0.278 Uiso 1 1 calc R . . C61 C -0.8922(8) 0.5546(10) 1.4334(8) 0.225(10) Uani 1 1 d G . . H61A H -0.8740 0.5397 1.4832 0.270 Uiso 1 1 calc R . . C62 C -0.8866(7) 0.6155(9) 1.4195(10) 0.200(8) Uani 1 1 d G . . H62A H -0.8647 0.6414 1.4600 0.240 Uiso 1 1 calc R . . C63 C -0.9138(8) 0.6377(6) 1.3450(13) 0.184(6) Uani 1 1 d G . . H63A H -0.9101 0.6785 1.3357 0.221 Uiso 1 1 calc R . . C64 C -0.9465(8) 0.5990(9) 1.2845(8) 0.201(7) Uani 1 1 d G . . H64A H -0.9647 0.6138 1.2347 0.242 Uiso 1 1 calc R . . C65 C -1.2255(9) 0.3671(8) 1.0737(12) 0.215(8) Uani 1 1 d DU . . H65A H -1.2057 0.3558 1.1274 0.258 Uiso 1 1 calc R . . H65B H -1.2324 0.4104 1.0717 0.258 Uiso 1 1 calc R . . C66 C -1.2953(9) 0.3382(8) 1.0412(13) 0.217(8) Uani 1 1 d DU . . H66A H -1.3268 0.3560 1.0651 0.260 Uiso 1 1 calc R . . H66B H -1.3138 0.3478 0.9869 0.260 Uiso 1 1 calc R . . C67 C -1.3293(8) 0.2568(6) 1.1033(6) 0.144(5) Uani 1 1 d DU . . H67A H -1.3775 0.2715 1.0878 0.173 Uiso 1 1 calc R . . H67B H -1.3034 0.2740 1.1530 0.173 Uiso 1 1 calc R . . C68 C -1.3291(8) 0.1909(6) 1.1092(8) 0.140(5) Uani 1 1 d DU . . H68A H -1.3451 0.1793 1.1512 0.168 Uiso 1 1 calc R . . H68B H -1.3617 0.1742 1.0622 0.168 Uiso 1 1 calc R . . C69 C -1.2648(8) 0.1023(7) 1.1337(10) 0.175(5) Uani 1 1 d DU . . H69A H -1.2998 0.0839 1.0897 0.210 Uiso 1 1 calc R . . H69B H -1.2782 0.0946 1.1786 0.210 Uiso 1 1 calc R . . C70 C -1.1935(9) 0.0758(7) 1.1447(11) 0.207(7) Uani 1 1 d DU . . H70A H -1.1600 0.0941 1.1899 0.248 Uiso 1 1 calc R . . H70B H -1.1956 0.0332 1.1555 0.248 Uiso 1 1 calc R . . C71 C -1.1011(3) 0.0553(3) 1.1026(5) 0.123(3) Uani 1 1 d G . . C72 C -1.0613(4) 0.0406(3) 1.1778(4) 0.136(4) Uani 1 1 d G . . H72A H -1.0792 0.0481 1.2173 0.163 Uiso 1 1 calc R . . C73 C -0.9949(3) 0.0147(3) 1.1938(3) 0.102(3) Uani 1 1 d G . . C74 C -0.9681(3) 0.0035(3) 1.1347(3) 0.080(2) Uani 1 1 d G . . C75 C -1.0079(3) 0.0182(3) 1.0596(3) 0.092(2) Uani 1 1 d G . . H75A H -0.9900 0.0107 1.0200 0.111 Uiso 1 1 calc R . . C76 C -1.0743(3) 0.0441(3) 1.0435(3) 0.114(3) Uani 1 1 d G . . C77 C -0.9563(6) -0.0030(4) 1.2774(5) 0.107(3) Uani 1 1 d . . . H77A H -0.9082 0.0121 1.2943 0.128 Uiso 1 1 calc R . . H77B H -0.9805 0.0132 1.3105 0.128 Uiso 1 1 calc R . . C78 C -0.9233(4) -0.0931(3) 1.3510(3) 0.101(3) Uani 1 1 d G . . C79 C -0.8959(3) -0.0608(3) 1.4189(4) 0.101(3) Uani 1 1 d G . . H79A H -0.8954 -0.0189 1.4177 0.121 Uiso 1 1 calc R . . C80 C -0.8694(4) -0.0909(4) 1.4886(3) 0.119(3) Uani 1 1 d G . . H80A H -0.8512 -0.0693 1.5340 0.143 Uiso 1 1 calc R . . C81 C -0.8703(4) -0.1535(4) 1.4903(4) 0.141(4) Uani 1 1 d G . . H81A H -0.8526 -0.1737 1.5369 0.169 Uiso 1 1 calc R . . C82 C -0.8976(4) -0.1858(3) 1.4224(5) 0.120(3) Uani 1 1 d G . . H82A H -0.8982 -0.2276 1.4236 0.144 Uiso 1 1 calc R . . C83 C -0.9241(4) -0.1556(3) 1.3527(4) 0.119(3) Uani 1 1 d G . . H83A H -0.9424 -0.1773 1.3073 0.143 Uiso 1 1 calc R . . C84 C -0.8970(4) -0.0237(4) 1.1452(4) 0.089(2) Uani 1 1 d . . . H84A H -0.8854 -0.0535 1.1858 0.107 Uiso 1 1 calc R . . H84B H -0.8970 -0.0431 1.0981 0.107 Uiso 1 1 calc R . . C85 C -0.7785(2) 0.0071(3) 1.1808(3) 0.084(2) Uani 1 1 d G . . C86 C -0.7548(3) -0.0520(2) 1.1867(3) 0.075(2) Uani 1 1 d G . . H86A H -0.7869 -0.0836 1.1790 0.091 Uiso 1 1 calc R . . C87 C -0.6831(4) -0.0641(3) 1.2040(3) 0.097(3) Uani 1 1 d G . . H87A H -0.6673 -0.1037 1.2080 0.117 Uiso 1 1 calc R . . C88 C -0.6352(2) -0.0169(4) 1.2155(3) 0.100(3) Uani 1 1 d G . . H88A H -0.5872 -0.0250 1.2271 0.120 Uiso 1 1 calc R . . C89 C -0.6588(3) 0.0422(3) 1.2096(3) 0.101(3) Uani 1 1 d G . . H89A H -0.6268 0.0738 1.2173 0.121 Uiso 1 1 calc R . . C90 C -0.7305(3) 0.0543(2) 1.1922(3) 0.075(2) Uani 1 1 d G . . H90A H -0.7464 0.0939 1.1883 0.090 Uiso 1 1 calc R . . C91 C -1.0996(8) 0.0380(7) 0.9119(8) 0.169(5) Uani 1 1 d DU . . H91A H -1.0886 -0.0046 0.9156 0.203 Uiso 1 1 calc R . . H91B H -1.0589 0.0602 0.9090 0.203 Uiso 1 1 calc R . . C92 C -1.1624(7) 0.0507(7) 0.8449(7) 0.163(5) Uani 1 1 d DU . . H92A H -1.1604 0.0283 0.8005 0.195 Uiso 1 1 calc R . . H92B H -1.2050 0.0392 0.8552 0.195 Uiso 1 1 calc R . . C93 C -1.1206(11) 0.1329(8) 0.7890(13) 0.219(8) Uani 1 1 d DU . . H93A H -1.1290 0.1075 0.7443 0.263 Uiso 1 1 calc R . . H93B H -1.0711 0.1295 0.8201 0.263 Uiso 1 1 calc R . . C94 C -1.1368(8) 0.1970(7) 0.7639(7) 0.158(6) Uani 1 1 d DU . . H94A H -1.1190 0.2068 0.7225 0.190 Uiso 1 1 calc R . . H94B H -1.1874 0.2045 0.7469 0.190 Uiso 1 1 calc R . . C95 C -1.1018(13) 0.2943(8) 0.8251(9) 0.207(8) Uani 1 1 d DU . . H95A H -1.1500 0.3091 0.8113 0.249 Uiso 1 1 calc R . . H95B H -1.0826 0.3065 0.7856 0.249 Uiso 1 1 calc R . . C96 C -1.0569(9) 0.3197(9) 0.9028(9) 0.198(6) Uani 1 1 d DU . . H96A H -1.0163 0.2937 0.9248 0.237 Uiso 1 1 calc R . . H96B H -1.0394 0.3590 0.8951 0.237 Uiso 1 1 calc R . . B1 B -0.7640(6) 0.2644(4) 1.1455(5) 0.122(3) Uani 1 1 d DU . . F1 F -0.7189(5) 0.2940(2) 1.1168(3) 0.154(3) Uani 1 1 d DU . . F2 F -0.7447(3) 0.2058(2) 1.1545(3) 0.1133(17) Uani 1 1 d DU . . F3 F -0.7612(5) 0.2887(3) 1.2148(4) 0.159(3) Uani 1 1 d DU . . F4 F -0.8322(5) 0.2680(4) 1.0939(6) 0.241(5) Uani 1 1 d DU . . B2 B -0.9535(7) 0.1265(5) 1.4074(7) 0.186(5) Uani 1 1 d DU . . F5 F -0.9413(4) 0.1781(4) 1.4468(4) 0.167(2) Uani 1 1 d DU . . F6 F -0.8921(6) 0.1080(4) 1.3986(6) 0.225(4) Uani 1 1 d DU . . F7 F -0.9806(8) 0.0844(5) 1.4404(8) 0.302(6) Uani 1 1 d DU . . F8 F -0.9998(6) 0.1380(6) 1.3364(6) 0.265(5) Uani 1 1 d DU . . B3 B -0.5185(9) -0.2333(8) 1.4637(10) 0.355(12) Uani 1 1 d DU . . F9 F -0.4894(10) -0.1749(8) 1.4741(12) 0.389(9) Uani 1 1 d DU . . F10 F -0.4666(9) -0.2779(8) 1.4689(12) 0.380(10) Uani 1 1 d DU . . F11 F -0.5700(10) -0.2372(9) 1.3901(10) 0.406(11) Uani 1 1 d DU . . F12 F -0.5511(11) -0.2446(11) 1.5190(12) 0.451(12) Uani 1 1 d DU . . B4 B -0.7957(8) 0.2546(6) 1.6958(8) 0.284(4) Uani 1 1 d DU . . F13 F -0.7937(9) 0.2830(5) 1.6351(7) 0.268(4) Uani 1 1 d DU . . F14 F -0.8640(7) 0.2440(7) 1.6861(8) 0.305(4) Uani 1 1 d DU . . F15 F -0.7663(8) 0.2846(5) 1.7581(7) 0.271(4) Uani 1 1 d DU . . F16 F -0.7633(9) 0.2023(5) 1.6985(8) 0.293(4) Uani 1 1 d DU . . B5 B -1.4898(15) 0.1385(12) 0.3784(16) 0.714(17) Uani 1 1 d DU . . F17 F -1.504(2) 0.1976(12) 0.384(2) 0.717(17) Uani 1 1 d DU . . F18 F -1.4306(18) 0.1237(17) 0.437(2) 0.714(17) Uani 1 1 d DU . . F19 F -1.479(2) 0.1296(18) 0.311(2) 0.715(17) Uani 1 1 d DU . . F20 F -1.5454(18) 0.1052(15) 0.381(3) 0.710(17) Uani 1 1 d DU . . B6 B -1.3277(11) 0.0815(10) 0.5881(11) 0.518(9) Uani 1 1 d DU . . F21 F -1.3277(15) 0.0359(11) 0.5355(12) 0.521(9) Uani 1 1 d DU . . F22 F -1.3946(11) 0.1073(13) 0.5645(15) 0.515(9) Uani 1 1 d DU . . F23 F -1.2775(13) 0.1246(12) 0.5888(14) 0.517(9) Uani 1 1 d DU . . F24 F -1.3139(15) 0.0564(12) 0.6602(11) 0.518(9) Uani 1 1 d DU . . 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 Cd1 0.0545(2) 0.0700(3) 0.03386(18) 0.0075(3) -0.01755(13) -0.0009(3) O1W 0.077(4) 0.142(6) 0.076(4) 0.043(3) 0.050(3) 0.029(3) O2W 0.098(4) 0.040(3) 0.073(4) -0.001(2) 0.000(3) -0.008(2) N1 0.063(3) 0.093(3) 0.038(2) 0.022(5) -0.007(2) 0.023(4) C1 0.252(17) 0.114(10) 0.098(9) 0.013(8) 0.091(11) 0.002(11) C2 0.176(11) 0.108(9) 0.132(9) -0.059(7) 0.101(9) -0.016(8) C3 0.111(6) 0.078(5) 0.049(3) 0.002(6) 0.020(4) 0.031(6) C4 0.245(15) 0.073(7) 0.108(9) -0.049(7) 0.026(9) 0.032(9) C5 0.141(8) 0.103(8) 0.070(6) 0.045(6) 0.052(6) 0.023(7) C6 0.150(7) 0.080(5) 0.063(4) -0.031(7) 0.030(4) -0.024(7) C7 0.32(2) 0.086(8) 0.097(9) 0.000(7) 0.089(11) 0.021(10) C8 0.194(12) 0.083(7) 0.081(6) 0.005(5) 0.048(7) -0.004(7) N2 0.207(11) 0.066(4) 0.094(5) 0.025(5) 0.068(7) 0.009(5) C9 0.218(12) 0.071(6) 0.052(5) 0.004(4) 0.046(6) 0.017(6) C10 0.204(11) 0.072(6) 0.043(5) -0.001(4) 0.044(6) 0.009(6) C11 0.136(10) 0.114(8) 0.081(7) 0.001(6) 0.033(8) -0.024(7) C12 0.223(17) 0.101(8) 0.093(9) -0.010(7) 0.042(10) -0.016(9) N3 0.152(9) 0.104(5) 0.075(6) -0.018(4) 0.043(6) -0.033(4) C13 0.33(2) 0.092(8) 0.073(7) 0.002(6) 0.063(10) -0.046(10) C14 0.183(11) 0.082(6) 0.070(5) 0.011(5) 0.041(6) -0.014(6) C15 0.111(8) 0.089(5) 0.045(4) 0.011(4) 0.015(5) -0.006(4) C16 0.107(7) 0.107(7) 0.062(5) -0.005(5) 0.035(5) -0.006(5) C17 0.143(9) 0.098(7) 0.084(6) 0.000(5) 0.031(6) -0.036(6) C18 0.071(6) 0.083(5) 0.045(4) -0.001(4) 0.005(4) -0.003(3) C19 0.097(6) 0.062(5) 0.056(4) 0.005(3) 0.037(4) -0.007(4) C20 0.069(5) 0.083(6) 0.070(6) 0.015(5) 0.015(4) 0.010(4) N4 0.078(4) 0.064(3) 0.048(2) 0.005(4) 0.015(2) -0.021(4) C21 0.124(7) 0.071(5) 0.057(5) 0.028(4) 0.042(5) 0.006(5) C22 0.106(6) 0.082(6) 0.053(4) 0.014(4) 0.038(4) -0.010(4) N5 0.086(6) 0.061(4) 0.036(4) 0.010(3) -0.021(4) -0.004(3) C23 0.112(8) 0.189(12) 0.095(8) 0.032(7) -0.020(6) -0.034(7) C24 0.093(8) 0.214(13) 0.069(6) 0.005(6) -0.012(5) -0.030(7) C25 0.064(7) 0.108(9) 0.067(8) -0.013(5) -0.023(6) 0.015(5) C26 0.096(9) 0.28(2) 0.154(14) 0.011(13) -0.008(9) 0.018(10) C27 0.149(16) 0.36(3) 0.157(16) 0.015(15) -0.032(13) 0.035(15) C28 0.057(7) 0.222(14) 0.113(12) -0.062(9) -0.007(7) 0.017(7) C29 0.140(11) 0.186(12) 0.124(10) -0.028(9) 0.036(9) -0.019(10) C30 0.101(8) 0.257(18) 0.111(9) -0.052(10) -0.012(7) -0.007(9) N6 0.185(15) 0.32(2) 0.141(12) -0.057(13) 0.024(11) 0.009(14) C31 0.127(12) 0.203(16) 0.103(10) -0.024(8) -0.038(9) -0.013(9) C32 0.069(6) 0.203(12) 0.092(8) -0.021(8) -0.021(5) 0.012(7) C33 0.074(6) 0.186(11) 0.061(5) -0.008(6) -0.004(5) -0.018(6) C34 0.114(9) 0.164(11) 0.110(8) 0.010(8) 0.006(8) 0.028(8) N7 0.029(3) 0.158(6) 0.044(3) 0.007(3) -0.012(2) -0.020(3) C35 0.078(5) 0.123(7) 0.085(6) 0.011(5) 0.016(5) 0.012(5) C36 0.056(4) 0.141(7) 0.052(4) -0.007(4) -0.005(3) 0.016(4) C37 0.047(5) 0.104(6) 0.047(5) -0.014(4) -0.018(4) 0.008(4) C38 0.056(4) 0.095(5) 0.041(4) 0.001(3) -0.006(3) 0.008(3) C39 0.065(5) 0.092(5) 0.036(4) 0.000(3) 0.002(3) 0.002(4) C40 0.048(6) 0.100(7) 0.040(5) -0.001(4) 0.006(5) 0.011(4) C41 0.058(4) 0.050(4) 0.059(4) -0.012(3) 0.002(3) 0.008(3) C42 0.048(3) 0.053(4) 0.049(3) -0.001(3) -0.003(3) 0.012(3) N8 0.025(3) 0.103(6) 0.060(5) 0.005(3) 0.001(3) -0.007(3) C43 0.061(4) 0.070(4) 0.058(4) -0.012(3) -0.009(3) 0.018(3) C44 0.082(5) 0.081(5) 0.044(3) -0.006(3) 0.002(3) 0.009(4) O1 0.243(18) 0.60(5) 0.164(13) -0.04(2) 0.046(12) 0.00(3) O2 0.120(5) 0.101(5) 0.118(5) 0.009(4) 0.035(4) -0.004(4) O3 0.173(9) 0.221(11) 0.182(10) 0.009(8) 0.043(8) 0.046(9) O4 0.105(5) 0.148(7) 0.128(7) -0.014(5) 0.029(5) 0.014(5) O5 0.209(13) 0.226(14) 0.334(19) 0.015(13) 0.151(13) 0.028(11) O6 0.102(5) 0.153(7) 0.245(10) 0.022(7) 0.086(6) 0.005(5) O7 0.126(5) 0.110(5) 0.082(4) 0.003(3) 0.018(3) -0.009(4) O8 0.080(4) 0.076(3) 0.074(3) 0.002(3) 0.012(3) -0.008(3) O9 0.128(6) 0.129(6) 0.113(5) -0.015(4) 0.024(5) -0.001(4) O10 0.120(6) 0.204(9) 0.101(5) -0.005(6) 0.021(4) 0.023(6) O11 0.141(8) 0.293(15) 0.128(8) -0.040(9) 0.027(6) -0.005(9) O12 0.145(7) 0.163(7) 0.124(7) 0.024(6) 0.010(6) 0.023(6) C45 0.131(10) 0.118(8) 0.122(10) 0.011(7) 0.038(9) 0.008(7) C46 0.110(8) 0.101(7) 0.103(7) 0.003(5) 0.019(6) 0.006(5) C47 0.114(8) 0.103(7) 0.106(7) -0.001(6) 0.042(6) 0.007(6) C48 0.118(9) 0.123(9) 0.127(9) 0.001(7) 0.023(7) 0.005(7) C49 0.116(10) 0.177(13) 0.175(13) 0.028(11) 0.053(9) 0.027(9) C50 0.108(9) 0.135(10) 0.162(12) 0.018(9) 0.012(10) 0.002(8) C51 0.116(8) 0.123(9) 0.082(6) 0.006(5) 0.009(5) 0.026(6) C52 0.228(16) 0.092(8) 0.070(7) 0.002(6) 0.053(8) -0.002(9) C53 0.181(12) 0.095(8) 0.084(7) 0.012(6) 0.013(7) -0.009(8) C54 0.31(3) 0.202(19) 0.132(14) 0.018(13) 0.053(17) 0.09(2) C55 0.24(2) 0.168(14) 0.115(11) -0.033(11) 0.088(13) -0.090(16) C56 0.168(13) 0.29(2) 0.080(8) -0.031(11) 0.068(9) -0.077(14) C57 0.121(7) 0.082(6) 0.056(5) -0.002(4) 0.027(5) -0.012(5) C58 0.127(14) 0.27(3) 0.53(6) -0.22(4) 0.05(2) 0.010(17) C59 0.57(6) 0.142(18) 0.28(3) 0.01(2) 0.16(4) -0.06(2) C60 0.21(2) 0.21(2) 0.29(3) 0.06(2) 0.09(2) 0.036(17) C61 0.24(2) 0.30(3) 0.158(17) -0.011(19) 0.089(16) -0.02(2) C62 0.26(2) 0.173(16) 0.176(19) -0.004(13) 0.078(16) -0.060(15) C63 0.170(14) 0.201(17) 0.210(19) -0.017(18) 0.100(15) -0.003(13) C64 0.219(18) 0.23(2) 0.172(17) -0.019(17) 0.085(15) -0.007(15) C65 0.167(14) 0.195(16) 0.27(2) -0.053(14) 0.055(15) 0.045(13) C66 0.164(15) 0.24(2) 0.241(19) -0.028(16) 0.058(14) 0.031(15) C67 0.177(12) 0.160(11) 0.072(6) -0.004(7) 0.009(7) 0.043(9) C68 0.134(11) 0.203(14) 0.094(9) -0.026(9) 0.052(8) -0.011(10) C69 0.148(12) 0.194(15) 0.175(13) -0.005(11) 0.043(10) 0.015(11) C70 0.166(14) 0.151(12) 0.34(2) 0.014(13) 0.129(15) -0.002(10) C71 0.126(9) 0.101(7) 0.151(10) 0.007(7) 0.059(9) -0.005(6) C72 0.150(11) 0.128(9) 0.117(9) 0.013(7) 0.026(8) -0.027(8) C73 0.069(5) 0.118(7) 0.114(7) 0.016(6) 0.024(5) 0.001(5) C74 0.082(5) 0.079(5) 0.078(5) -0.002(4) 0.023(4) -0.009(4) C75 0.077(5) 0.110(6) 0.085(6) 0.011(5) 0.022(4) 0.002(5) C76 0.123(8) 0.120(8) 0.094(7) -0.004(6) 0.029(7) 0.007(6) C77 0.121(7) 0.093(7) 0.090(6) -0.001(5) 0.012(5) -0.011(5) C78 0.127(7) 0.082(6) 0.085(6) -0.003(5) 0.024(5) -0.005(5) C79 0.089(6) 0.131(8) 0.080(6) 0.002(5) 0.025(5) -0.009(5) C80 0.125(8) 0.124(8) 0.094(7) 0.011(6) 0.019(6) -0.008(6) C81 0.141(10) 0.169(12) 0.117(9) 0.003(9) 0.048(8) -0.004(9) C82 0.118(8) 0.117(7) 0.126(9) 0.017(7) 0.040(7) 0.003(6) C83 0.115(7) 0.151(10) 0.091(7) 0.009(6) 0.032(6) -0.007(7) C84 0.081(5) 0.111(6) 0.062(4) 0.009(4) 0.005(4) -0.004(5) C85 0.104(7) 0.100(6) 0.043(4) 0.007(4) 0.017(4) -0.017(6) C86 0.115(7) 0.059(5) 0.049(4) 0.004(3) 0.023(4) 0.009(4) C87 0.085(6) 0.126(8) 0.081(6) 0.009(5) 0.029(5) -0.003(6) C88 0.100(8) 0.135(9) 0.059(5) 0.008(5) 0.018(5) -0.002(8) C89 0.098(7) 0.152(10) 0.053(5) 0.007(5) 0.026(5) -0.006(6) C90 0.096(7) 0.084(6) 0.048(4) -0.007(4) 0.028(4) -0.011(5) C91 0.174(13) 0.166(12) 0.157(12) 0.017(10) 0.044(11) 0.040(10) C92 0.161(12) 0.185(14) 0.124(10) -0.018(10) 0.025(8) 0.058(11) C93 0.202(16) 0.220(18) 0.26(2) 0.069(16) 0.104(16) 0.006(14) C94 0.105(9) 0.28(2) 0.077(8) -0.006(10) 0.017(7) -0.002(10) C95 0.25(2) 0.217(18) 0.105(11) -0.001(12) -0.010(12) 0.042(15) C96 0.181(15) 0.261(18) 0.149(13) 0.064(13) 0.052(12) 0.021(13) B1 0.210(10) 0.094(6) 0.063(6) 0.006(5) 0.047(6) 0.022(8) F1 0.317(9) 0.075(3) 0.082(4) 0.000(2) 0.083(5) -0.009(4) F2 0.159(5) 0.088(3) 0.102(4) 0.010(3) 0.055(4) 0.011(3) F3 0.271(10) 0.119(4) 0.109(4) -0.004(3) 0.094(5) 0.020(5) F4 0.258(8) 0.188(8) 0.218(9) -0.012(7) -0.001(7) 0.058(7) B2 0.187(15) 0.121(11) 0.220(16) -0.001(9) 0.028(11) 0.011(11) F5 0.157(6) 0.153(5) 0.174(6) -0.001(5) 0.034(5) 0.000(5) F6 0.233(9) 0.205(9) 0.232(10) 0.001(7) 0.071(7) 0.041(7) F7 0.369(17) 0.217(10) 0.335(14) 0.001(10) 0.139(13) -0.083(11) F8 0.246(10) 0.319(14) 0.186(8) -0.048(7) 0.013(7) 0.008(9) B3 0.26(3) 0.47(3) 0.32(2) 0.09(3) 0.068(15) 0.043(17) F9 0.32(2) 0.47(2) 0.39(2) -0.02(2) 0.152(18) 0.011(16) F10 0.276(17) 0.45(2) 0.42(3) 0.178(18) 0.124(16) 0.054(14) F11 0.39(2) 0.39(2) 0.346(19) 0.128(18) -0.010(16) 0.054(17) F12 0.48(3) 0.50(3) 0.43(2) 0.08(3) 0.24(2) 0.06(2) B4 0.372(12) 0.269(9) 0.220(8) -0.003(6) 0.111(9) -0.003(8) F13 0.368(11) 0.260(8) 0.194(7) -0.004(5) 0.117(8) -0.003(7) F14 0.378(11) 0.297(8) 0.246(7) -0.005(6) 0.110(8) -0.005(7) F15 0.372(11) 0.257(8) 0.198(7) -0.006(5) 0.113(8) -0.001(7) F16 0.379(11) 0.264(8) 0.233(7) -0.010(5) 0.096(8) 0.009(7) B5 0.78(4) 0.61(3) 0.90(4) 0.06(3) 0.48(4) 0.26(3) F17 0.78(4) 0.61(3) 0.90(4) 0.06(3) 0.48(4) 0.26(3) F18 0.78(4) 0.61(3) 0.90(4) 0.06(3) 0.48(4) 0.26(3) F19 0.78(4) 0.61(3) 0.90(4) 0.06(3) 0.48(4) 0.26(3) F20 0.77(4) 0.61(3) 0.90(4) 0.05(3) 0.48(4) 0.26(3) B6 0.49(2) 0.60(3) 0.395(16) -0.100(15) 0.052(16) -0.023(16) F21 0.49(2) 0.60(3) 0.399(16) -0.098(15) 0.051(16) -0.020(16) F22 0.49(2) 0.60(3) 0.394(16) -0.102(15) 0.057(16) -0.022(16) F23 0.48(2) 0.60(3) 0.394(16) -0.100(15) 0.050(16) -0.024(16) F24 0.49(2) 0.60(3) 0.395(16) -0.099(15) 0.052(16) -0.025(16) _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 Cd1 O1W 2.312(5) . ? Cd1 N4 2.323(3) . ? Cd1 N8 2.328(3) . ? Cd1 N5 2.340(4) 1_656 ? Cd1 N1 2.363(3) 1_565 ? Cd1 O2W 2.376(7) . ? O1W H1WA 0.9603 . ? O1W H1WB 0.9598 . ? O2W H2WA 0.9601 . ? O2W H2WB 0.9600 . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? N1 Cd1 2.363(3) 1_545 ? C1 C2 1.3900 . ? C1 H1A 0.9300 . ? C2 C3 1.3900 . ? C2 H2A 0.9300 . ? C3 C4 1.3900 . ? C3 C6 1.428(5) . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.3900 . ? C6 C10 1.3900 . ? C7 C8 1.3900 . ? C7 H7A 0.9300 . ? C8 N2 1.3900 . ? C8 H8A 0.9300 . ? N2 C9 1.3900 . ? N2 C11 1.472(12) . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.400(16) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.484(13) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N3 C13 1.3900 . ? N3 C17 1.3900 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 C16 1.3900 . ? C15 C18 1.506(5) . ? C16 C17 1.3900 . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.3900 . ? C18 C22 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9300 . ? C20 N4 1.3900 . ? C20 H20A 0.9300 . ? N4 C21 1.3900 . ? C21 C22 1.3900 . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? N5 C23 1.3900 . ? N5 C27 1.3900 . ? N5 Cd1 2.340(4) 1_454 ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 C28 1.509(7) . ? C26 C27 1.3900 . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C29 1.3900 . ? C28 C32 1.3900 . ? C29 C30 1.3900 . ? C29 H29A 0.9300 . ? C30 N6 1.3900 . ? C30 H30A 0.9300 . ? N6 C31 1.3900 . ? N6 C34 1.541(12) . ? C31 C32 1.3900 . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.375(14) . ? C33 N7 1.439(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? N7 C35 1.3900 . ? N7 C39 1.3900 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 C37 1.3900 . ? C36 H36A 0.9300 . ? C37 C38 1.3900 . ? C37 C40 1.480(4) . ? C38 C39 1.3900 . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C41 1.3900 . ? C40 C44 1.3900 . ? C41 C42 1.3900 . ? C41 H41A 0.9300 . ? C42 N8 1.3900 . ? C42 H42A 0.9300 . ? N8 C43 1.3900 . ? C43 C44 1.3900 . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? O1 C58 1.27(4) . ? O1 C59 1.61(3) . ? O2 C51 1.384(12) . ? O2 C52 1.434(10) . ? O3 C50 1.359(14) . ? O3 C65 1.484(15) . ? O4 C67 1.411(12) . ? O4 C66 1.419(14) . ? O5 C68 1.377(13) . ? O5 C69 1.476(14) . ? O6 C70 1.360(14) . ? O6 C71 1.395(9) . ? O7 C78 1.381(8) . ? O7 C77 1.460(11) . ? O8 C85 1.368(7) . ? O8 C84 1.382(10) . ? O9 C76 1.329(8) . ? O9 C91 1.381(12) . ? O10 C93 1.385(14) . ? O10 C92 1.420(13) . ? O11 C95 1.411(14) . ? O11 C94 1.439(13) . ? O12 C45 1.369(11) . ? O12 C96 1.450(14) . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C46 C47 1.3900 . ? C46 H46A 0.9300 . ? C47 C48 1.3900 . ? C47 C51 1.569(12) . ? C48 C49 1.3900 . ? C48 C58 1.71(4) . ? C49 C50 1.3900 . ? C49 H49A 0.9300 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C53 H53A 0.9300 . ? C54 C55 1.3900 . ? C54 H54A 0.9300 . ? C55 C56 1.3900 . ? C55 H55A 0.9300 . ? C56 C57 1.3900 . ? C56 H56A 0.9300 . ? C57 H57A 0.9300 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C60 H60A 0.9300 . ? C61 C62 1.3900 . ? C61 H61A 0.9300 . ? C62 C63 1.3900 . ? C62 H62A 0.9300 . ? C63 C64 1.3900 . ? C63 H63A 0.9300 . ? C64 H64A 0.9300 . ? C65 C66 1.473(15) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 C68 1.467(14) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 C70 1.496(14) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C72 H72A 0.9300 . ? C73 C74 1.3900 . ? C73 C77 1.529(10) . ? C74 C75 1.3900 . ? C74 C84 1.502(10) . ? C75 C76 1.3900 . ? C75 H75A 0.9300 . ? C77 H77A 0.9700 . ? C77 H77B 0.9700 . ? C78 C79 1.3900 . ? C78 C83 1.3900 . ? C79 C80 1.3900 . ? C79 H79A 0.9300 . ? C80 C81 1.3900 . ? C80 H80A 0.9300 . ? C81 C82 1.3900 . ? C81 H81A 0.9300 . ? C82 C83 1.3900 . ? C82 H82A 0.9300 . ? C83 H83A 0.9300 . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C85 C86 1.3900 . ? C85 C90 1.3900 . ? C86 C87 1.3900 . ? C86 H86A 0.9300 . ? C87 C88 1.3900 . ? C87 H87A 0.9300 . ? C88 C89 1.3900 . ? C88 H88A 0.9300 . ? C89 C90 1.3900 . ? C89 H89A 0.9300 . ? C90 H90A 0.9300 . ? C91 C92 1.469(13) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C93 C94 1.498(15) . ? C93 H93A 0.9700 . ? C93 H93B 0.9700 . ? C94 H94A 0.9700 . ? C94 H94B 0.9700 . ? C95 C96 1.526(15) . ? C95 H95A 0.9700 . ? C95 H95B 0.9700 . ? C96 H96A 0.9700 . ? C96 H96B 0.9700 . ? B1 F2 1.353(9) . ? B1 F1 1.361(9) . ? B1 F3 1.373(9) . ? B1 F4 1.385(9) . ? B2 F7 1.328(11) . ? B2 F5 1.336(10) . ? B2 F8 1.354(11) . ? B2 F6 1.359(11) . ? B3 F12 1.409(13) . ? B3 F11 1.409(13) . ? B3 F9 1.410(12) . ? B3 F10 1.416(12) . ? B4 F15 1.290(11) . ? B4 F13 1.299(12) . ? B4 F16 1.326(12) . ? B4 F14 1.342(12) . ? B5 F20 1.352(13) . ? B5 F18 1.355(14) . ? B5 F19 1.356(13) . ? B5 F17 1.358(13) . ? B6 F24 1.383(13) . ? B6 F22 1.389(13) . ? B6 F23 1.389(13) . ? B6 F21 1.403(13) . ? 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 O1W Cd1 N4 89.3(2) . . ? O1W Cd1 N8 87.2(2) . . ? N4 Cd1 N8 90.93(19) . . ? O1W Cd1 N5 93.5(3) . 1_656 ? N4 Cd1 N5 88.7(2) . 1_656 ? N8 Cd1 N5 179.2(2) . 1_656 ? O1W Cd1 N1 88.3(3) . 1_565 ? N4 Cd1 N1 177.5(3) . 1_565 ? N8 Cd1 N1 88.4(2) . 1_565 ? N5 Cd1 N1 92.0(2) 1_656 1_565 ? O1W Cd1 O2W 175.6(3) . . ? N4 Cd1 O2W 90.02(18) . . ? N8 Cd1 O2W 88.47(19) . . ? N5 Cd1 O2W 90.8(2) 1_656 . ? N1 Cd1 O2W 92.4(2) 1_565 . ? Cd1 O1W H1WA 109.8 . . ? Cd1 O1W H1WB 108.9 . . ? H1WA O1W H1WB 109.5 . . ? Cd1 O2W H2WA 109.2 . . ? Cd1 O2W H2WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? C1 N1 C5 120.0 . . ? C1 N1 Cd1 119.9(4) . 1_545 ? C5 N1 Cd1 120.0(4) . 1_545 ? N1 C1 C2 120.0 . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 C6 119.4(6) . . ? C4 C3 C6 120.6(6) . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 H5A 120.0 . . ? N1 C5 H5A 120.0 . . ? C7 C6 C10 120.0 . . ? C7 C6 C3 118.4(6) . . ? C10 C6 C3 120.9(6) . . ? C6 C7 C8 120.0 . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? N2 C8 C7 120.0 . . ? N2 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 N2 C9 120.0 . . ? C8 N2 C11 119.9(6) . . ? C9 N2 C11 120.0(6) . . ? C10 C9 N2 120.0 . . ? C10 C9 H9A 120.0 . . ? N2 C9 H9A 120.0 . . ? C9 C10 C6 120.0 . . ? C9 C10 H10A 120.0 . . ? C6 C10 H10A 120.0 . . ? C12 C11 N2 111.4(9) . . ? C12 C11 H11A 109.3 . . ? N2 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? N2 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 N3 106.3(13) . . ? C11 C12 H12A 110.5 . . ? N3 C12 H12A 110.5 . . ? C11 C12 H12B 110.5 . . ? N3 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C13 N3 C17 120.0 . . ? C13 N3 C12 117.2(7) . . ? C17 N3 C12 122.4(7) . . ? C14 C13 N3 120.0 . . ? C14 C13 H13A 120.0 . . ? N3 C13 H13A 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 C18 119.3(5) . . ? C14 C15 C18 120.6(5) . . ? C15 C16 C17 120.0 . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 N3 120.0 . . ? C16 C17 H17A 120.0 . . ? N3 C17 H17A 120.0 . . ? C19 C18 C22 120.0 . . ? C19 C18 C15 120.6(5) . . ? C22 C18 C15 119.3(5) . . ? C18 C19 C20 120.0 . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? N4 C20 C19 120.0 . . ? N4 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 N4 C21 120.0 . . ? C20 N4 Cd1 123.3(3) . . ? C21 N4 Cd1 116.7(3) . . ? C22 C21 N4 120.0 . . ? C22 C21 H21A 120.0 . . ? N4 C21 H21A 120.0 . . ? C21 C22 C18 120.0 . . ? C21 C22 H22A 120.0 . . ? C18 C22 H22A 120.0 . . ? C23 N5 C27 120.0 . . ? C23 N5 Cd1 121.7(4) . 1_454 ? C27 N5 Cd1 118.3(4) . 1_454 ? N5 C23 C24 120.0 . . ? N5 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 C28 120.1(6) . . ? C26 C25 C28 119.6(6) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 N5 120.0 . . ? C26 C27 H27A 120.0 . . ? N5 C27 H27A 120.0 . . ? C29 C28 C32 120.0 . . ? C29 C28 C25 118.0(6) . . ? C32 C28 C25 121.7(7) . . ? C30 C29 C28 120.0 . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? N6 C30 C29 120.0 . . ? N6 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C31 N6 C30 120.0 . . ? C31 N6 C34 120.1(8) . . ? C30 N6 C34 119.5(8) . . ? N6 C31 C32 120.0 . . ? N6 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C28 120.0 . . ? C31 C32 H32A 120.0 . . ? C28 C32 H32A 120.0 . . ? C34 C33 N7 112.8(9) . . ? C34 C33 H33A 109.0 . . ? N7 C33 H33A 109.0 . . ? C34 C33 H33B 109.0 . . ? N7 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 N6 111.1(10) . . ? C33 C34 H34A 109.4 . . ? N6 C34 H34A 109.4 . . ? C33 C34 H34B 109.4 . . ? N6 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? C35 N7 C39 120.0 . . ? C35 N7 C33 119.2(5) . . ? C39 N7 C33 120.5(5) . . ? C36 C35 N7 120.0 . . ? C36 C35 H35A 120.0 . . ? N7 C35 H35A 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 C40 119.5(3) . . ? C38 C37 C40 120.5(3) . . ? C37 C38 C39 120.0 . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C38 C39 N7 120.0 . . ? C38 C39 H39A 120.0 . . ? N7 C39 H39A 120.0 . . ? C41 C40 C44 120.0 . . ? C41 C40 C37 119.5(3) . . ? C44 C40 C37 120.5(3) . . ? C40 C41 C42 120.0 . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 N8 120.0 . . ? C41 C42 H42A 120.0 . . ? N8 C42 H42A 120.0 . . ? C42 N8 C43 120.0 . . ? C42 N8 Cd1 119.29(18) . . ? C43 N8 Cd1 120.70(18) . . ? C44 C43 N8 120.0 . . ? C44 C43 H43A 120.0 . . ? N8 C43 H43A 120.0 . . ? C43 C44 C40 120.0 . . ? C43 C44 H44A 120.0 . . ? C40 C44 H44A 120.0 . . ? C58 O1 C59 136(3) . . ? C51 O2 C52 112.4(7) . . ? C50 O3 C65 119.4(12) . . ? C67 O4 C66 113.1(11) . . ? C68 O5 C69 108.3(12) . . ? C70 O6 C71 112.1(11) . . ? C78 O7 C77 114.2(6) . . ? C85 O8 C84 117.1(6) . . ? C76 O9 C91 117.4(9) . . ? C93 O10 C92 116.4(11) . . ? C95 O11 C94 117.3(13) . . ? C45 O12 C96 119.6(11) . . ? O12 C45 C46 122.2(8) . . ? O12 C45 C50 117.8(8) . . ? C46 C45 C50 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46A 120.0 . . ? C47 C46 H46A 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 C51 124.5(7) . . ? C46 C47 C51 115.5(7) . . ? C49 C48 C47 120.0 . . ? C49 C48 C58 110.1(11) . . ? C47 C48 C58 128.7(10) . . ? C48 C49 C50 120.0 . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? O3 C50 C49 127.7(9) . . ? O3 C50 C45 112.3(9) . . ? C49 C50 C45 120.0 . . ? O2 C51 C47 103.1(7) . . ? O2 C51 H51A 111.1 . . ? C47 C51 H51A 111.1 . . ? O2 C51 H51B 111.1 . . ? C47 C51 H51B 111.1 . . ? H51A C51 H51B 109.1 . . ? C53 C52 C57 120.0 . . ? C53 C52 O2 115.4(7) . . ? C57 C52 O2 124.6(7) . . ? C52 C53 C54 120.0 . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55A 120.0 . . ? C54 C55 H55A 120.0 . . ? C55 C56 C57 120.0 . . ? C55 C56 H56A 120.0 . . ? C57 C56 H56A 120.0 . . ? C56 C57 C52 120.0 . . ? C56 C57 H57A 120.0 . . ? C52 C57 H57A 120.0 . . ? O1 C58 C48 91(3) . . ? O1 C58 H58A 113.5 . . ? C48 C58 H58A 113.5 . . ? O1 C58 H58B 113.5 . . ? C48 C58 H58B 113.5 . . ? H58A C58 H58B 110.8 . . ? C60 C59 C64 120.0 . . ? C60 C59 O1 98.9(18) . . ? C64 C59 O1 139.1(18) . . ? C59 C60 C61 120.0 . . ? C59 C60 H60A 120.0 . . ? C61 C60 H60A 120.0 . . ? C62 C61 C60 120.0 . . ? C62 C61 H61A 120.0 . . ? C60 C61 H61A 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62A 120.0 . . ? C63 C62 H62A 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63A 120.0 . . ? C64 C63 H63A 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 H64A 120.0 . . ? C59 C64 H64A 120.0 . . ? C66 C65 O3 116.0(14) . . ? C66 C65 H65A 108.3 . . ? O3 C65 H65A 108.3 . . ? C66 C65 H65B 108.3 . . ? O3 C65 H65B 108.3 . . ? H65A C65 H65B 107.4 . . ? O4 C66 C65 116.8(14) . . ? O4 C66 H66A 108.1 . . ? C65 C66 H66A 108.1 . . ? O4 C66 H66B 108.1 . . ? C65 C66 H66B 108.1 . . ? H66A C66 H66B 107.3 . . ? O4 C67 C68 110.2(10) . . ? O4 C67 H67A 109.6 . . ? C68 C67 H67A 109.6 . . ? O4 C67 H67B 109.6 . . ? C68 C67 H67B 109.6 . . ? H67A C67 H67B 108.1 . . ? O5 C68 C67 111.3(12) . . ? O5 C68 H68A 109.4 . . ? C67 C68 H68A 109.4 . . ? O5 C68 H68B 109.4 . . ? C67 C68 H68B 109.4 . . ? H68A C68 H68B 108.0 . . ? O5 C69 C70 109.4(13) . . ? O5 C69 H69A 109.8 . . ? C70 C69 H69A 109.8 . . ? O5 C69 H69B 109.8 . . ? C70 C69 H69B 109.8 . . ? H69A C69 H69B 108.2 . . ? O6 C70 C69 117.1(14) . . ? O6 C70 H70A 108.0 . . ? C69 C70 H70A 108.0 . . ? O6 C70 H70B 108.0 . . ? C69 C70 H70B 108.0 . . ? H70A C70 H70B 107.3 . . ? C72 C71 C76 120.0 . . ? C72 C71 O6 120.5(7) . . ? C76 C71 O6 119.5(7) . . ? C71 C72 C73 120.0 . . ? C71 C72 H72A 120.0 . . ? C73 C72 H72A 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 C77 123.3(6) . . ? C72 C73 C77 116.6(6) . . ? C73 C74 C75 120.0 . . ? C73 C74 C84 124.8(5) . . ? C75 C74 C84 115.2(5) . . ? C76 C75 C74 120.0 . . ? C76 C75 H75A 120.0 . . ? C74 C75 H75A 120.0 . . ? O9 C76 C75 125.2(6) . . ? O9 C76 C71 114.8(6) . . ? C75 C76 C71 120.0 . . ? O7 C77 C73 106.0(7) . . ? O7 C77 H77A 110.5 . . ? C73 C77 H77A 110.5 . . ? O7 C77 H77B 110.5 . . ? C73 C77 H77B 110.5 . . ? H77A C77 H77B 108.7 . . ? O7 C78 C79 125.6(5) . . ? O7 C78 C83 114.2(5) . . ? C79 C78 C83 120.0 . . ? C78 C79 C80 120.0 . . ? C78 C79 H79A 120.0 . . ? C80 C79 H79A 120.0 . . ? C81 C80 C79 120.0 . . ? C81 C80 H80A 120.0 . . ? C79 C80 H80A 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81A 120.0 . . ? C82 C81 H81A 120.0 . . ? C81 C82 C83 120.0 . . ? C81 C82 H82A 120.0 . . ? C83 C82 H82A 120.0 . . ? C82 C83 C78 120.0 . . ? C82 C83 H83A 120.0 . . ? C78 C83 H83A 120.0 . . ? O8 C84 C74 107.3(7) . . ? O8 C84 H84A 110.2 . . ? C74 C84 H84A 110.2 . . ? O8 C84 H84B 110.2 . . ? C74 C84 H84B 110.2 . . ? H84A C84 H84B 108.5 . . ? O8 C85 C86 123.4(5) . . ? O8 C85 C90 116.6(5) . . ? C86 C85 C90 120.0 . . ? C87 C86 C85 120.0 . . ? C87 C86 H86A 120.0 . . ? C85 C86 H86A 120.0 . . ? C86 C87 C88 120.0 . . ? C86 C87 H87A 120.0 . . ? C88 C87 H87A 120.0 . . ? C89 C88 C87 120.0 . . ? C89 C88 H88A 120.0 . . ? C87 C88 H88A 120.0 . . ? C88 C89 C90 120.0 . . ? C88 C89 H89A 120.0 . . ? C90 C89 H89A 120.0 . . ? C89 C90 C85 120.0 . . ? C89 C90 H90A 120.0 . . ? C85 C90 H90A 120.0 . . ? O9 C91 C92 104.1(10) . . ? O9 C91 H91A 110.9 . . ? C92 C91 H91A 110.9 . . ? O9 C91 H91B 110.9 . . ? C92 C91 H91B 110.9 . . ? H91A C91 H91B 108.9 . . ? O10 C92 C91 106.6(12) . . ? O10 C92 H92A 110.4 . . ? C91 C92 H92A 110.4 . . ? O10 C92 H92B 110.4 . . ? C91 C92 H92B 110.4 . . ? H92A C92 H92B 108.6 . . ? O10 C93 C94 111.2(15) . . ? O10 C93 H93A 109.4 . . ? C94 C93 H93A 109.4 . . ? O10 C93 H93B 109.4 . . ? C94 C93 H93B 109.4 . . ? H93A C93 H93B 108.0 . . ? O11 C94 C93 103.6(13) . . ? O11 C94 H94A 111.0 . . ? C93 C94 H94A 111.0 . . ? O11 C94 H94B 111.0 . . ? C93 C94 H94B 111.0 . . ? H94A C94 H94B 109.0 . . ? O11 C95 C96 107.3(13) . . ? O11 C95 H95A 110.3 . . ? C96 C95 H95A 110.3 . . ? O11 C95 H95B 110.3 . . ? C96 C95 H95B 110.3 . . ? H95A C95 H95B 108.5 . . ? O12 C96 C95 113.7(15) . . ? O12 C96 H96A 108.8 . . ? C95 C96 H96A 108.8 . . ? O12 C96 H96B 108.8 . . ? C95 C96 H96B 108.8 . . ? H96A C96 H96B 107.7 . . ? F2 B1 F1 108.3(7) . . ? F2 B1 F3 110.1(7) . . ? F1 B1 F3 110.3(7) . . ? F2 B1 F4 108.5(8) . . ? F1 B1 F4 109.6(8) . . ? F3 B1 F4 110.0(8) . . ? F7 B2 F5 112.5(10) . . ? F7 B2 F8 108.9(10) . . ? F5 B2 F8 108.0(9) . . ? F7 B2 F6 111.5(10) . . ? F5 B2 F6 108.4(9) . . ? F8 B2 F6 107.3(10) . . ? F12 B3 F11 108.6(11) . . ? F12 B3 F9 109.7(11) . . ? F11 B3 F9 109.0(11) . . ? F12 B3 F10 109.6(11) . . ? F11 B3 F10 107.9(11) . . ? F9 B3 F10 112.0(11) . . ? F15 B4 F13 112.4(11) . . ? F15 B4 F16 110.3(11) . . ? F13 B4 F16 107.7(11) . . ? F15 B4 F14 110.7(11) . . ? F13 B4 F14 107.1(11) . . ? F16 B4 F14 108.5(11) . . ? F20 B5 F18 110.6(12) . . ? F20 B5 F19 110.1(12) . . ? F18 B5 F19 109.5(12) . . ? F20 B5 F17 109.3(12) . . ? F18 B5 F17 108.7(12) . . ? F19 B5 F17 108.6(12) . . ? F24 B6 F22 109.3(11) . . ? F24 B6 F23 111.0(11) . . ? F22 B6 F23 109.8(11) . . ? F24 B6 F21 109.3(11) . . ? F22 B6 F21 107.7(11) . . ? F23 B6 F21 109.7(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.361 _refine_diff_density_min -0.516 _refine_diff_density_rms 0.077 # Attachment '- DM62.cif' data_dm62 _database_code_depnum_ccdc_archive 'CCDC 864509' #TrackingRef '- DM62.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C172 H158 F24 N18 O47 Ru2 S8' _chemical_formula_weight 4143.78 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.248(9) _cell_length_b 20.018(10) _cell_length_c 28.528(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.355(8) _cell_angle_gamma 90.00 _cell_volume 10412(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 65 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 20.82 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4248 _exptl_absorpt_coefficient_mu 0.321 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5432 _exptl_absorpt_correction_T_max 0.8618 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 61239 _diffrn_reflns_av_R_equivalents 0.5423 _diffrn_reflns_av_sigmaI/netI 0.3550 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 20.82 _reflns_number_total 10811 _reflns_number_gt 3255 _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. Crystals were very weakly diffracting and of poor quality. Only non-carbon hetero-atoms were refined anisotropically. One triflate anion was restrained as a rigid group using SADI, SIMU, DELU and DFIX commands, the other 3 triflate ions were restrained using the SAME command. One of the triflate anions was modelled for a 50:50 disorder. AFIX 66 commands were used to restrain all the aromatic rings in the complex to be idealized hexagons with C-C and C-N bonds equal to 1.39 A. One of the EtCOO-Ph-O-CH2 groups on the crown ether was disordered over two sites and modelled as 50% occupancy for both sites. Various DFIX DANG SIMU and DELU restraints were necessary to achieve a chemically reasonable geomtery for the disorder model. ; _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 10811 _refine_ls_number_parameters 709 _refine_ls_number_restraints 596 _refine_ls_R_factor_all 0.4242 _refine_ls_R_factor_gt 0.2267 _refine_ls_wR_factor_ref 0.5573 _refine_ls_wR_factor_gt 0.4545 _refine_ls_goodness_of_fit_ref 1.292 _refine_ls_restrained_S_all 1.280 _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 Ru1 Ru 0.58123(17) 2.74553(12) 0.60143(9) 0.0698(11) Uani 1 1 d . . . N1 N 0.6585(9) 2.6762(8) 0.6240(6) 0.048(6) Uiso 1 1 d G . . C1 C 0.7264(10) 2.6904(7) 0.6456(6) 0.047(8) Uiso 1 1 d G . . H1A H 0.7396 2.7353 0.6526 0.056 Uiso 1 1 calc R . . C2 C 0.7750(8) 2.6389(10) 0.6570(7) 0.091(12) Uiso 1 1 d G . . H2A H 0.8214 2.6486 0.6717 0.109 Uiso 1 1 calc R . . C3 C 0.7556(10) 2.5731(9) 0.6467(7) 0.073(10) Uiso 1 1 d G . . H3A H 0.7888 2.5379 0.6545 0.087 Uiso 1 1 calc R . . C4 C 0.6877(12) 2.5590(6) 0.6252(7) 0.096(12) Uiso 1 1 d G . . H4A H 0.6745 2.5140 0.6182 0.116 Uiso 1 1 calc R . . C5 C 0.6391(8) 2.6105(9) 0.6138(6) 0.047(8) Uiso 1 1 d G . . C6 C 0.5715(9) 2.6034(10) 0.5898(6) 0.054(9) Uiso 1 1 d G . . C7 C 0.5410(11) 2.5435(7) 0.5739(7) 0.073(10) Uiso 1 1 d G . . H7A H 0.5658 2.5025 0.5804 0.088 Uiso 1 1 calc R . . C8 C 0.4743(12) 2.5435(8) 0.5485(7) 0.094(12) Uiso 1 1 d G . . H8A H 0.4535 2.5025 0.5377 0.112 Uiso 1 1 calc R . . C9 C 0.4382(9) 2.6033(11) 0.5390(7) 0.094(12) Uiso 1 1 d G . . H9A H 0.3926 2.6033 0.5217 0.113 Uiso 1 1 calc R . . C10 C 0.4687(11) 2.6633(8) 0.5549(7) 0.069(10) Uiso 1 1 d G . . N2 N 0.5353(11) 2.6633(7) 0.5803(6) 0.065(7) Uiso 1 1 d G . . C11 C 0.4412(14) 2.7268(9) 0.5511(8) 0.098(13) Uiso 1 1 d G . . C12 C 0.3724(13) 2.7425(13) 0.5316(9) 0.116(13) Uiso 1 1 d G . . H12A H 0.3423 2.7084 0.5179 0.139 Uiso 1 1 calc R . . C13 C 0.3476(11) 2.8082(15) 0.5320(9) 0.156(19) Uiso 1 1 d G . . H13A H 0.3005 2.8189 0.5186 0.187 Uiso 1 1 calc R . . C14 C 0.3917(15) 2.8581(10) 0.5519(9) 0.124(15) Uiso 1 1 d G . . H14A H 0.3747 2.9029 0.5522 0.149 Uiso 1 1 calc R . . C15 C 0.4605(14) 2.8423(10) 0.5715(8) 0.119(15) Uiso 1 1 d G . . H15A H 0.4906 2.8764 0.5852 0.143 Uiso 1 1 calc R . . N3 N 0.4853(10) 2.7767(12) 0.5711(7) 0.078(9) Uiso 1 1 d G . . N4 N 0.6466(9) 2.7688(10) 0.5463(6) 0.075(8) Uiso 1 1 d G . . C16 C 0.6498(9) 2.7338(8) 0.5043(7) 0.084(11) Uiso 1 1 d G . . H16A H 0.6194 2.6959 0.4988 0.101 Uiso 1 1 calc R . . C17 C 0.6976(11) 2.7544(10) 0.4704(6) 0.077(10) Uiso 1 1 d G . . H17A H 0.6998 2.7305 0.4417 0.093 Uiso 1 1 calc R . . C18 C 0.7420(9) 2.8099(10) 0.4785(6) 0.069(10) Uiso 1 1 d G . . H18A H 0.7746 2.8240 0.4553 0.083 Uiso 1 1 calc R . . C19 C 0.7388(10) 2.8449(8) 0.5204(7) 0.067(10) Uiso 1 1 d G . . H19A H 0.7692 2.8829 0.5260 0.080 Uiso 1 1 calc R . . C20 C 0.6911(11) 2.8243(9) 0.5543(6) 0.072(10) Uiso 1 1 d G . . C21 C 0.6822(11) 2.8572(10) 0.5989(5) 0.065(9) Uiso 1 1 d G . . C22 C 0.7193(9) 2.9132(10) 0.6163(7) 0.070(10) Uiso 1 1 d G . . H22A H 0.7582 2.9319 0.5994 0.085 Uiso 1 1 calc R . . C23 C 0.6994(10) 2.9419(8) 0.6582(7) 0.069(10) Uiso 1 1 d G . . C24 C 0.6424(11) 2.9146(9) 0.6829(6) 0.060(9) Uiso 1 1 d G . . H24A H 0.6288 2.9342 0.7116 0.072 Uiso 1 1 calc R . . C25 C 0.6053(9) 2.8586(10) 0.6655(7) 0.080(11) Uiso 1 1 d G . . N5 N 0.6252(10) 2.8299(8) 0.6235(7) 0.084(9) Uiso 1 1 d G . . C26 C 0.5504(8) 2.8219(8) 0.6861(6) 0.051(8) Uiso 1 1 d G . . C27 C 0.5115(10) 2.8457(7) 0.7235(6) 0.054(9) Uiso 1 1 d G . . H27A H 0.5246 2.8871 0.7378 0.065 Uiso 1 1 calc R . . C28 C 0.4534(10) 2.8089(10) 0.7401(5) 0.078(11) Uiso 1 1 d G . . H28A H 0.4268 2.8252 0.7656 0.094 Uiso 1 1 calc R . . C29 C 0.4342(9) 2.7483(9) 0.7192(6) 0.070(9) Uiso 1 1 d G . . H29A H 0.3944 2.7231 0.7305 0.083 Uiso 1 1 calc R . . C30 C 0.4730(10) 2.7245(7) 0.6818(6) 0.076(11) Uiso 1 1 d G . . H30A H 0.4599 2.6831 0.6675 0.092 Uiso 1 1 calc R . . N6 N 0.5312(9) 2.7613(8) 0.6652(5) 0.052(7) Uiso 1 1 d G . . C31 C 0.7427(12) 2.9994(8) 0.6771(7) 0.062(9) Uiso 1 1 d G . . C32 C 0.7072(9) 3.0466(11) 0.7038(7) 0.085(11) Uiso 1 1 d G . . H32A H 0.6557 3.0439 0.7071 0.102 Uiso 1 1 calc R . . C33 C 0.7471(12) 3.0978(9) 0.7256(7) 0.082(11) Uiso 1 1 d G . . H33A H 0.7229 3.1300 0.7439 0.098 Uiso 1 1 calc R . . C34 C 0.8225(12) 3.1018(9) 0.7208(7) 0.063(9) Uiso 1 1 d G . . C35 C 0.8580(9) 3.0546(11) 0.6941(7) 0.090(12) Uiso 1 1 d G . . H35A H 0.9095 3.0573 0.6908 0.108 Uiso 1 1 calc R . . C36 C 0.8181(12) 3.0034(9) 0.6722(6) 0.069(10) Uiso 1 1 d G . . H36A H 0.8423 2.9712 0.6540 0.083 Uiso 1 1 calc R . . C37 C 0.8693(17) 3.1540(15) 0.7469(11) 0.077(10) Uiso 1 1 d . . . H37A H 0.8410 3.1731 0.7726 0.092 Uiso 1 1 calc R . . H37B H 0.9134 3.1321 0.7612 0.092 Uiso 1 1 calc R . . N7 N 0.8923(10) 3.2087(8) 0.7158(5) 0.055(7) Uiso 1 1 d G . . C38 C 0.8458(8) 3.2625(9) 0.7064(6) 0.062(9) Uiso 1 1 d G . . H38A H 0.8011 3.2663 0.7221 0.075 Uiso 1 1 calc R . . C39 C 0.8647(10) 3.3106(8) 0.6739(7) 0.086(11) Uiso 1 1 d G . . H39A H 0.8330 3.3474 0.6675 0.103 Uiso 1 1 calc R . . C40 C 0.9301(11) 3.3050(8) 0.6509(6) 0.062(9) Uiso 1 1 d G . . C41 C 0.9766(9) 3.2512(10) 0.6604(6) 0.060(8) Uiso 1 1 d G . . H41A H 1.0213 3.2474 0.6446 0.072 Uiso 1 1 calc R . . C42 C 0.9577(9) 3.2031(8) 0.6928(6) 0.073(10) Uiso 1 1 d G . . H42A H 0.9894 3.1663 0.6993 0.087 Uiso 1 1 calc R . . C43 C 0.9462(12) 3.3583(8) 0.6169(6) 0.052(8) Uiso 1 1 d G . . C44 C 0.8922(8) 3.3982(10) 0.5954(7) 0.077(10) Uiso 1 1 d G . . H44A H 0.8421 3.3910 0.6017 0.092 Uiso 1 1 calc R . . C45 C 0.9116(10) 3.4485(9) 0.5647(6) 0.072(10) Uiso 1 1 d G . . H45A H 0.8747 3.4757 0.5500 0.086 Uiso 1 1 calc R . . N8 N 0.9849(11) 3.4590(8) 0.5555(6) 0.066(8) Uiso 1 1 d G . . C46 C 1.0389(8) 3.4191(10) 0.5769(7) 0.080(11) Uiso 1 1 d G . . H46A H 1.0890 3.4263 0.5706 0.096 Uiso 1 1 calc R . . C47 C 1.0195(10) 3.3688(9) 0.6076(6) 0.074(10) Uiso 1 1 d G . . H47A H 1.0564 3.3415 0.6223 0.089 Uiso 1 1 calc R . . C48 C 1.0059(18) 3.5121(15) 0.5238(9) 0.076(11) Uiso 1 1 d . . . H48A H 0.9758 3.5524 0.5287 0.091 Uiso 1 1 calc R . . H48B H 1.0582 3.5238 0.5297 0.091 Uiso 1 1 calc R . . O7 O 1.0389(14) 3.3266(10) 0.4831(8) 0.097(8) Uani 1 1 d . . . O8 O 1.1660(13) 3.4225(10) 0.4801(8) 0.085(7) Uani 1 1 d . . . O9 O 1.1741(14) 3.5192(11) 0.5471(9) 0.110(9) Uani 1 1 d . . . O10 O 0.8998(12) 3.3525(9) 0.4754(8) 0.078(7) Uani 1 1 d . . . C49 C 0.9218(12) 3.2971(8) 0.5001(6) 0.057(9) Uiso 1 1 d G . . C50 C 0.8708(9) 3.2552(11) 0.5199(7) 0.094(11) Uiso 1 1 d G A . H50A H 0.8199 3.2649 0.5163 0.113 Uiso 1 1 calc R . . C51 C 0.8942(12) 3.1991(10) 0.5450(7) 0.086(11) Uiso 1 1 d G . . C52 C 0.9687(13) 3.1849(8) 0.5503(7) 0.070(10) Uiso 1 1 d GDU A . C53 C 1.0197(9) 3.2269(11) 0.5305(7) 0.078(11) Uiso 1 1 d G . . H53A H 1.0706 3.2172 0.5341 0.093 Uiso 1 1 calc R A . C54 C 0.9962(11) 3.2830(10) 0.5054(7) 0.068(10) Uiso 1 1 d G A . C65 C 0.9994(17) 3.1248(10) 0.5781(10) 0.084(11) Uiso 1 1 d DU . . H65A H 1.0537 3.1257 0.5795 0.100 Uiso 1 1 calc R A . H65B H 0.9820 3.1254 0.6105 0.100 Uiso 1 1 calc R . . O4 O 0.9724(13) 3.0654(9) 0.5531(7) 0.103(8) Uiso 1 1 d DU A . C66 C 0.9692(12) 3.0053(8) 0.5757(7) 0.082(11) Uiso 1 1 d GD . . C67 C 0.9995(11) 2.9935(10) 0.6205(7) 0.082(11) Uiso 1 1 d GD A . H67A H 1.0276 3.0273 0.6362 0.098 Uiso 1 1 calc R . . C68 C 0.9887(12) 2.9323(12) 0.6421(6) 0.119(15) Uiso 1 1 d GD A . H68A H 1.0094 2.9242 0.6727 0.143 Uiso 1 1 calc R . . C69 C 0.9477(13) 2.8829(9) 0.6191(8) 0.111(14) Uiso 1 1 d GD A . C70 C 0.9174(11) 2.8947(9) 0.5743(8) 0.091(12) Uiso 1 1 d GD A . H70A H 0.8893 2.8609 0.5586 0.109 Uiso 1 1 calc R . . C71 C 0.9282(12) 2.9559(11) 0.5527(6) 0.103(13) Uiso 1 1 d GD A . H71A H 0.9075 2.9639 0.5221 0.123 Uiso 1 1 calc R . . C72 C 0.928(2) 2.8179(14) 0.6399(11) 0.117(17) Uiso 1 1 d DU . . O5 O 0.8880(15) 2.7760(11) 0.6222(9) 0.133(10) Uani 1 1 d DU A . O6 O 0.9611(16) 2.8121(11) 0.6814(9) 0.140(11) Uani 1 1 d DU A . C73 C 0.952(2) 2.7468(13) 0.7033(13) 0.147(16) Uiso 1 1 d DU . . H73A H 0.8998 2.7383 0.7091 0.176 Uiso 1 1 calc R A . H73B H 0.9700 2.7109 0.6828 0.176 Uiso 1 1 calc R . . C74 C 0.994(3) 2.749(2) 0.7463(12) 0.19(2) Uiso 1 1 d DU A . H74A H 0.9892 2.7062 0.7628 0.287 Uiso 1 1 calc R . . H74B H 0.9765 2.7852 0.7658 0.287 Uiso 1 1 calc R . . H74C H 1.0459 2.7563 0.7399 0.287 Uiso 1 1 calc R . . C75 C 1.1164(19) 3.3082(16) 0.4856(12) 0.077(11) Uiso 1 1 d . . . H75A H 1.1233 3.2628 0.4729 0.092 Uiso 1 1 calc R . . H75B H 1.1361 3.3095 0.5184 0.092 Uiso 1 1 calc R . . C76 C 1.155(2) 3.3612(17) 0.4551(12) 0.093(12) Uiso 1 1 d . . . H76A H 1.2033 3.3436 0.4460 0.111 Uiso 1 1 calc R . . H76B H 1.1250 3.3696 0.4261 0.111 Uiso 1 1 calc R . . C77 C 1.2260(19) 3.4244(16) 0.5100(12) 0.072(11) Uiso 1 1 d . . . H77A H 1.2694 3.4075 0.4940 0.086 Uiso 1 1 calc R . . H77B H 1.2180 3.3958 0.5376 0.086 Uiso 1 1 calc R . . C78 C 1.239(2) 3.4960(18) 0.5256(14) 0.106(14) Uiso 1 1 d . . . H78A H 1.2814 3.4983 0.5483 0.127 Uiso 1 1 calc R . . H78B H 1.2496 3.5244 0.4983 0.127 Uiso 1 1 calc R . . C79 C 0.809(2) 3.4208(19) 0.4294(13) 0.105(13) Uiso 1 1 d . . . H79A H 0.8388 3.4167 0.4013 0.126 Uiso 1 1 calc R . . H79B H 0.7566 3.4202 0.4192 0.126 Uiso 1 1 calc R . . C80 C 0.826(2) 3.3624(17) 0.4631(13) 0.092(12) Uiso 1 1 d . . . H80A H 0.7991 3.3699 0.4922 0.111 Uiso 1 1 calc R . . H80B H 0.8063 3.3209 0.4485 0.111 Uiso 1 1 calc R . . C55A C 0.845(3) 3.162(3) 0.581(2) 0.012(18) Uiso 0.33 1 d PD A -1 H55A H 0.8749 3.1323 0.6014 0.014 Uiso 0.33 1 calc PR A -1 H55B H 0.8191 3.1947 0.6002 0.014 Uiso 0.33 1 calc PR A -1 O3A O 0.793(3) 3.124(3) 0.5514(18) 0.10(3) Uiso 0.33 1 d PD A -1 C56A C 0.733(2) 3.092(2) 0.5686(17) 0.04(2) Uiso 0.33 1 d PGD A -1 C57A C 0.699(3) 3.042(3) 0.5417(18) 0.05(3) Uiso 0.33 1 d PGD A -1 H57A H 0.7253 3.0210 0.5177 0.064 Uiso 0.33 1 calc PR A -1 C58A C 0.628(3) 3.024(3) 0.5499(19) 0.05(3) Uiso 0.33 1 d PGD A -1 H58A H 0.6046 2.9895 0.5315 0.065 Uiso 0.33 1 calc PR A -1 C59A C 0.590(2) 3.055(3) 0.5851(18) 0.09(3) Uiso 0.33 1 d PGD A -1 C60A C 0.623(2) 3.105(2) 0.6120(16) 0.04(2) Uiso 0.33 1 d PGD A -1 H60A H 0.5976 3.1263 0.6360 0.054 Uiso 0.33 1 calc PR A -1 C61A C 0.695(2) 3.124(2) 0.6038(14) 0.05(3) Uiso 0.33 1 d PGD A -1 H61A H 0.7182 3.1578 0.6222 0.061 Uiso 0.33 1 calc PR A -1 C62A C 0.521(3) 3.027(3) 0.602(2) 0.15(5) Uiso 0.33 1 d PD A -1 O1A O 0.485(4) 2.986(4) 0.580(4) 0.24(6) Uiso 0.33 1 d PD A -1 O2A O 0.485(4) 3.075(4) 0.622(3) 0.19(4) Uiso 0.33 1 d PD A -1 C63A C 0.407(4) 3.059(8) 0.626(9) 0.39(16) Uiso 0.33 1 d PD A -1 H63A H 0.3870 3.0797 0.6539 0.470 Uiso 0.33 1 calc PR A -1 H63B H 0.3787 3.0753 0.5977 0.470 Uiso 0.33 1 calc PR A -1 C64A C 0.403(10) 2.988(9) 0.629(14) 0.6(3) Uiso 0.33 1 d PD A -1 H64A H 0.3521 2.9748 0.6328 0.845 Uiso 0.33 1 calc PR A -1 H64B H 0.4339 2.9726 0.6553 0.845 Uiso 0.33 1 calc PR A -1 H64C H 0.4203 2.9685 0.5996 0.845 Uiso 0.33 1 calc PR A -1 C55B C 0.830(3) 3.147(3) 0.558(2) 0.11(2) Uiso 0.67 1 d PD A -2 H55C H 0.8449 3.1200 0.5861 0.133 Uiso 0.67 1 calc PR A -2 H55D H 0.7837 3.1705 0.5639 0.133 Uiso 0.67 1 calc PR A -2 O3B O 0.824(2) 3.106(2) 0.5156(16) 0.19(2) Uiso 0.67 1 d PD A -2 C56B C 0.768(2) 3.062(2) 0.5082(16) 0.25(5) Uiso 0.67 1 d PGD A -2 C57B C 0.766(2) 3.016(2) 0.4713(15) 0.18(3) Uiso 0.67 1 d PGD A -2 H57B H 0.8058 3.0144 0.4509 0.218 Uiso 0.67 1 calc PR A -2 C58B C 0.706(2) 2.974(2) 0.4644(14) 0.17(3) Uiso 0.67 1 d PGD A -2 H58B H 0.7052 2.9430 0.4392 0.207 Uiso 0.67 1 calc PR A -2 C59B C 0.648(2) 2.977(2) 0.4943(16) 0.17(3) Uiso 0.67 1 d PGD A -2 C60B C 0.650(2) 3.023(3) 0.5312(17) 0.19(4) Uiso 0.67 1 d PGD A -2 H60B H 0.6101 3.0248 0.5516 0.233 Uiso 0.67 1 calc PR A -2 C61B C 0.710(3) 3.065(2) 0.5381(16) 0.18(4) Uiso 0.67 1 d PGD A -2 H61B H 0.7108 3.0961 0.5633 0.211 Uiso 0.67 1 calc PR A -2 C62B C 0.586(3) 2.930(3) 0.491(2) 0.23(4) Uiso 0.67 1 d PD A -2 O1B O 0.532(3) 2.930(3) 0.5142(19) 0.25(3) Uiso 0.67 1 d PD A -2 O2B O 0.584(3) 2.902(3) 0.4496(17) 0.23(3) Uiso 0.67 1 d PD A -2 C63B C 0.534(4) 2.845(4) 0.448(2) 0.23(4) Uiso 0.67 1 d PD A -2 H63C H 0.5477 2.8127 0.4731 0.281 Uiso 0.67 1 calc PR A -2 H63D H 0.4829 2.8600 0.4525 0.281 Uiso 0.67 1 calc PR A -2 C64B C 0.540(5) 2.816(4) 0.403(3) 0.31(6) Uiso 0.67 1 d PD A -2 H64D H 0.5029 2.7805 0.3990 0.471 Uiso 0.67 1 calc PR A -2 H64E H 0.5890 2.7961 0.4011 0.471 Uiso 0.67 1 calc PR A -2 H64F H 0.5325 2.8498 0.3790 0.471 Uiso 0.67 1 calc PR A -2 S1 S 1.0380(7) 3.0381(5) 0.7786(4) 0.132(4) Uani 1 1 d DU . . O11 O 1.0350(15) 2.9683(6) 0.7681(8) 0.148(7) Uani 1 1 d DU . . O12 O 0.9875(13) 3.0592(10) 0.8120(7) 0.147(7) Uani 1 1 d DU . . O13 O 1.0439(15) 3.0805(9) 0.7389(6) 0.142(7) Uani 1 1 d DU . . C81 C 1.1230(10) 3.0453(10) 0.8104(7) 0.190(8) Uani 1 1 d DU . . F1 F 1.1785(13) 3.0248(12) 0.7848(9) 0.203(8) Uani 1 1 d DU . . F2 F 1.1372(14) 3.1089(9) 0.8228(9) 0.197(8) Uani 1 1 d DU . . F3 F 1.1265(15) 3.0092(11) 0.8503(8) 0.198(8) Uani 1 1 d DU . . S2 S 0.8154(7) 2.8610(5) 0.9101(5) 0.131(4) Uani 1 1 d DU . . O14 O 0.7745(15) 2.8085(12) 0.9304(10) 0.188(8) Uani 1 1 d DU . . O15 O 0.8537(17) 2.9003(12) 0.9424(9) 0.190(8) Uani 1 1 d DU . . O16 O 0.7793(13) 2.8931(10) 0.8717(7) 0.122(7) Uani 1 1 d DU . . C82 C 0.8883(14) 2.8139(13) 0.8880(10) 0.252(11) Uani 1 1 d DU . . F4 F 0.8726(18) 2.7799(13) 0.8494(10) 0.254(12) Uani 1 1 d DU . . F5 F 0.9137(19) 2.7701(15) 0.9207(11) 0.279(12) Uani 1 1 d DU . . F6 F 0.9402(16) 2.8617(15) 0.8793(13) 0.281(12) Uani 1 1 d DU . . S3 S 0.9500(7) 2.5301(5) 0.6968(4) 0.134(4) Uani 1 1 d DU . . O17 O 0.9510(16) 2.5463(12) 0.6471(7) 0.159(7) Uani 1 1 d DU . . O18 O 0.9227(15) 2.4675(9) 0.7053(9) 0.146(7) Uani 1 1 d DU . . O19 O 0.9236(15) 2.5855(10) 0.7223(8) 0.146(7) Uani 1 1 d DU . . C83 C 1.0454(12) 2.5278(14) 0.7084(11) 0.250(11) Uani 1 1 d DU . . F7 F 1.0625(17) 2.5097(17) 0.7523(11) 0.273(11) Uani 1 1 d DU . . F8 F 1.0782(15) 2.4838(16) 0.6804(13) 0.271(11) Uani 1 1 d DU . . F9 F 1.0760(15) 2.5895(14) 0.7012(13) 0.245(11) Uani 1 1 d DU . . S4A S 1.2089(18) 3.2811(13) 0.6459(14) 0.178(14) Uani 0.50 1 d PDU B -1 O20A O 1.167(3) 3.260(2) 0.6847(18) 0.182(15) Uani 0.50 1 d PDU B -1 O21A O 1.278(2) 3.251(2) 0.645(3) 0.185(15) Uani 0.50 1 d PDU B -1 O22A O 1.168(3) 3.288(3) 0.6032(16) 0.183(16) Uani 0.50 1 d PDU B -1 C84A C 1.233(2) 3.3633(15) 0.6636(15) 0.228(16) Uani 0.50 1 d PDU B -1 F10A F 1.176(2) 3.402(2) 0.673(2) 0.232(17) Uani 0.50 1 d PDU B -1 F11A F 1.277(3) 3.362(2) 0.7028(17) 0.231(16) Uani 0.50 1 d PDU B -1 F12A F 1.270(3) 3.395(2) 0.6295(17) 0.231(16) Uani 0.50 1 d PDU B -1 S4B S 1.1879(17) 3.2521(12) 0.6445(8) 0.135(9) Uani 0.50 1 d PDU C -2 O20B O 1.152(3) 3.289(2) 0.6804(14) 0.147(12) Uani 0.50 1 d PDU C -2 O21B O 1.2625(19) 3.265(2) 0.6435(19) 0.146(11) Uani 0.50 1 d PDU C -2 O22B O 1.147(3) 3.248(2) 0.6016(12) 0.141(12) Uani 0.50 1 d PDU C -2 C84B C 1.184(2) 3.1701(14) 0.6679(13) 0.202(14) Uani 0.50 1 d PDU C -2 F10B F 1.222(3) 3.162(2) 0.7080(13) 0.209(15) Uani 0.50 1 d PDU C -2 F11B F 1.208(3) 3.1222(18) 0.6389(15) 0.205(15) Uani 0.50 1 d PDU C -2 F12B F 1.112(2) 3.154(2) 0.6760(17) 0.209(15) Uani 0.50 1 d PDU C -2 N1S N 0.784(2) 2.820(2) 0.7314(15) 0.155(17) Uiso 1 1 d . . . C1S C 0.810(3) 2.858(3) 0.751(2) 0.18(2) Uiso 1 1 d . . . C2S C 0.853(3) 2.916(3) 0.7750(18) 0.19(2) Uiso 1 1 d . . . H2SA H 0.8891 2.9332 0.7539 0.284 Uiso 1 1 calc R . . H2SB H 0.8776 2.8990 0.8037 0.284 Uiso 1 1 calc R . . H2SC H 0.8186 2.9515 0.7829 0.284 Uiso 1 1 calc R . . O1W O 0.792(3) 3.172(2) 0.3495(18) 0.118(18) Uiso 0.50 1 d P . . O2W O 1.0929(18) 2.8861(15) 0.9215(12) 0.172(13) Uiso 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 Ru1 0.113(2) 0.0393(15) 0.0599(18) 0.0000(16) 0.0397(15) -0.0023(19) O7 0.13(2) 0.067(15) 0.10(2) 0.035(13) 0.061(16) 0.004(15) O8 0.11(2) 0.076(16) 0.071(18) 0.033(13) 0.035(16) -0.021(15) O9 0.11(2) 0.067(17) 0.15(2) 0.004(16) 0.017(19) -0.015(16) O10 0.083(19) 0.041(13) 0.110(19) 0.013(12) 0.033(14) 0.007(12) O5 0.17(3) 0.069(17) 0.16(3) -0.001(16) 0.040(19) -0.040(17) O6 0.22(3) 0.070(18) 0.14(3) 0.012(16) 0.04(2) -0.046(19) S1 0.200(10) 0.075(6) 0.124(10) 0.010(6) 0.061(7) 0.012(8) O11 0.230(18) 0.077(9) 0.141(16) 0.020(10) 0.051(14) 0.025(13) O12 0.210(14) 0.109(14) 0.127(16) -0.004(12) 0.064(12) 0.014(14) O13 0.212(18) 0.077(12) 0.142(14) 0.020(10) 0.067(12) 0.015(14) C81 0.206(13) 0.153(17) 0.21(2) 0.010(15) 0.018(12) 0.020(15) F1 0.209(13) 0.172(18) 0.23(2) 0.012(16) 0.033(15) 0.031(17) F2 0.207(18) 0.151(16) 0.23(2) 0.000(14) -0.012(16) 0.027(15) F3 0.215(19) 0.176(18) 0.204(19) 0.017(16) 0.004(13) 0.001(17) S2 0.201(12) 0.051(7) 0.141(12) 0.009(6) 0.020(9) 0.001(7) O14 0.227(18) 0.139(16) 0.198(19) 0.081(13) 0.010(14) -0.017(13) O15 0.27(2) 0.108(16) 0.190(19) 0.005(11) -0.044(15) 0.002(13) O16 0.184(17) 0.056(13) 0.129(16) 0.006(10) 0.033(13) -0.024(11) C82 0.31(2) 0.18(2) 0.27(3) 0.037(16) 0.11(2) 0.103(15) F4 0.35(3) 0.16(2) 0.26(2) 0.019(16) 0.14(2) 0.106(18) F5 0.35(3) 0.21(2) 0.29(3) 0.045(19) 0.10(2) 0.152(17) F6 0.29(2) 0.25(2) 0.31(3) 0.032(19) 0.12(2) 0.063(18) S3 0.193(10) 0.070(7) 0.143(10) 0.014(7) 0.050(9) 0.007(8) O17 0.227(18) 0.111(14) 0.145(12) 0.022(12) 0.080(14) 0.006(15) O18 0.226(16) 0.070(10) 0.145(16) 0.024(12) 0.042(15) 0.017(12) O19 0.210(16) 0.088(12) 0.143(15) -0.013(12) 0.042(15) -0.011(13) C83 0.188(12) 0.25(3) 0.31(3) -0.02(2) 0.009(17) 0.015(13) F7 0.231(19) 0.26(3) 0.32(3) 0.00(2) -0.040(18) 0.002(19) F8 0.181(16) 0.28(3) 0.36(3) -0.03(3) 0.03(2) 0.039(17) F9 0.164(16) 0.27(3) 0.30(3) -0.02(2) 0.02(2) -0.011(15) S4A 0.10(3) 0.23(2) 0.21(4) -0.08(2) 0.08(2) -0.003(19) O20A 0.11(3) 0.24(3) 0.21(4) -0.08(3) 0.08(2) 0.00(2) O21A 0.10(3) 0.24(3) 0.22(4) -0.07(3) 0.07(2) -0.01(2) O22A 0.11(3) 0.23(3) 0.21(4) -0.07(3) 0.07(2) 0.01(2) C84A 0.21(4) 0.21(3) 0.26(4) -0.07(3) 0.03(3) -0.02(2) F10A 0.22(4) 0.21(3) 0.27(5) -0.08(3) 0.03(3) -0.02(2) F11A 0.21(4) 0.22(3) 0.26(4) -0.07(3) 0.03(3) -0.03(3) F12A 0.22(4) 0.22(3) 0.26(5) -0.07(3) 0.03(3) -0.03(2) S4B 0.13(2) 0.208(19) 0.066(15) 0.017(16) 0.051(16) 0.07(2) O20B 0.14(3) 0.23(2) 0.07(2) 0.01(2) 0.05(2) 0.07(2) O21B 0.14(2) 0.22(2) 0.08(2) 0.00(2) 0.04(2) 0.07(2) O22B 0.14(3) 0.21(3) 0.075(18) 0.01(2) 0.043(19) 0.07(3) C84B 0.25(4) 0.22(2) 0.14(3) 0.06(2) 0.07(3) 0.07(3) F10B 0.27(4) 0.23(3) 0.13(3) 0.07(2) 0.07(3) 0.08(3) F11B 0.26(4) 0.20(2) 0.15(3) 0.06(2) 0.07(3) 0.07(3) F12B 0.26(4) 0.22(3) 0.15(3) 0.06(2) 0.08(3) 0.06(3) _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 Ru1 N2 1.933(14) . ? Ru1 N5 1.962(14) . ? Ru1 N3 2.019(18) . ? Ru1 N1 2.062(13) . ? Ru1 N4 2.066(14) . ? Ru1 N6 2.093(13) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C1 H1A 0.9500 . ? C2 C3 1.3900 . ? C2 H2A 0.9500 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.394(19) . ? C6 C7 1.3900 . ? C6 N2 1.3900 . ? C7 C8 1.3900 . ? C7 H7A 0.9500 . ? C8 C9 1.3900 . ? C8 H8A 0.9500 . ? C9 C10 1.3900 . ? C9 H9A 0.9500 . ? C10 C11 1.37(2) . ? C10 N2 1.3900 . ? C11 C12 1.3900 . ? C11 N3 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9500 . ? C13 C14 1.3900 . ? C13 H13A 0.9500 . ? C14 C15 1.3900 . ? C14 H14A 0.9500 . ? C15 N3 1.3900 . ? C15 H15A 0.9500 . ? N4 C16 1.3900 . ? N4 C20 1.3900 . ? C16 C17 1.3900 . ? C16 H16A 0.9500 . ? C17 C18 1.3900 . ? C17 H17A 0.9500 . ? C18 C19 1.3900 . ? C18 H18A 0.9500 . ? C19 C20 1.3900 . ? C19 H19A 0.9500 . ? C20 C21 1.446(19) . ? C21 C22 1.3900 . ? C21 N5 1.3900 . ? C22 C23 1.3900 . ? C22 H22A 0.9500 . ? C23 C24 1.3900 . ? C23 C31 1.485(19) . ? C24 C25 1.3900 . ? C24 H24A 0.9500 . ? C25 N5 1.3900 . ? C25 C26 1.392(19) . ? C26 C27 1.3900 . ? C26 N6 1.3900 . ? C27 C28 1.3900 . ? C27 H27A 0.9500 . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 N6 1.3900 . ? C30 H30A 0.9500 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 H32A 0.9500 . ? C33 C34 1.3900 . ? C33 H33A 0.9500 . ? C34 C35 1.3900 . ? C34 C37 1.52(3) . ? C35 C36 1.3900 . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 N7 1.48(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N7 C38 1.3900 . ? N7 C42 1.3900 . ? C38 C39 1.3900 . ? C38 H38A 0.9500 . ? C39 C40 1.3900 . ? C39 H39A 0.9500 . ? C40 C41 1.3900 . ? C40 C43 1.480(18) . ? C41 C42 1.3900 . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C44 1.3900 . ? C43 C47 1.3900 . ? C44 C45 1.3900 . ? C44 H44A 0.9500 . ? C45 N8 1.3900 . ? C45 H45A 0.9500 . ? N8 C46 1.3900 . ? N8 C48 1.46(3) . ? C46 C47 1.3900 . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 C48 1.45(5) 3_7<6 ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? O7 C54 1.35(2) . ? O7 C75 1.46(3) . ? O8 C77 1.36(3) . ? O8 C76 1.43(3) . ? O9 C79 1.40(4) 3_7<6 ? O9 C78 1.43(4) . ? O10 C49 1.36(2) . ? O10 C80 1.39(4) . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C50 H50A 0.9500 . ? C51 C52 1.3900 . ? C51 C55A 1.57(6) . ? C51 C55B 1.62(6) . ? C52 C53 1.3900 . ? C52 C65 1.534(17) . ? C53 C54 1.3900 . ? C53 H53A 0.9500 . ? C65 O4 1.463(17) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? O4 C66 1.368(15) . ? C66 C67 1.3900 . ? C66 C71 1.3900 . ? C67 C68 1.3900 . ? C67 H67A 0.9500 . ? C68 C69 1.3900 . ? C68 H68A 0.9500 . ? C69 C70 1.3900 . ? C69 C72 1.481(18) . ? C70 C71 1.3900 . ? C70 H70A 0.9500 . ? C71 H71A 0.9500 . ? C72 O5 1.208(17) . ? C72 O6 1.311(17) . ? O6 C73 1.461(10) . ? C73 C74 1.421(10) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.56(4) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.52(4) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 O9 1.40(4) 3_7<6 ? C79 C80 1.54(4) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C55A O3A 1.46(3) . ? C55A H55A 0.9900 . ? C55A H55B 0.9900 . ? O3A C56A 1.37(2) . ? C56A C57A 1.3900 . ? C56A C61A 1.3900 . ? C57A C58A 1.3900 . ? C57A H57A 0.9500 . ? C58A C59A 1.3900 . ? C58A H58A 0.9500 . ? C59A C60A 1.3900 . ? C59A C62A 1.48(3) . ? C60A C61A 1.3900 . ? C60A H60A 0.9500 . ? C61A H61A 0.9500 . ? C62A O1A 1.22(3) . ? C62A O2A 1.32(3) . ? O2A C63A 1.47(2) . ? C63A C64A 1.42(2) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A H64A 0.9800 . ? C64A H64B 0.9800 . ? C64A H64C 0.9800 . ? C55B O3B 1.47(2) . ? C55B H55C 0.9900 . ? C55B H55D 0.9900 . ? O3B C56B 1.37(2) . ? C56B C57B 1.3900 . ? C56B C61B 1.3900 . ? C57B C58B 1.3900 . ? C57B H57B 0.9500 . ? C58B C59B 1.3900 . ? C58B H58B 0.9500 . ? C59B C60B 1.3900 . ? C59B C62B 1.48(2) . ? C60B C61B 1.3900 . ? C60B H60B 0.9500 . ? C61B H61B 0.9500 . ? C62B O1B 1.21(2) . ? C62B O2B 1.31(3) . ? O2B C63B 1.47(2) . ? C63B C64B 1.41(2) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C64B H64D 0.9800 . ? C64B H64E 0.9800 . ? C64B H64F 0.9800 . ? S1 O12 1.419(9) . ? S1 O13 1.422(9) . ? S1 O11 1.429(9) . ? S1 C81 1.771(10) . ? C81 F1 1.337(10) . ? C81 F2 1.344(10) . ? C81 F3 1.349(10) . ? S2 O15 1.380(16) . ? S2 O16 1.409(15) . ? S2 O14 1.424(16) . ? S2 C82 1.767(19) . ? C82 F4 1.316(19) . ? C82 F5 1.348(19) . ? C82 F6 1.38(2) . ? S3 O18 1.375(15) . ? S3 O19 1.421(15) . ? S3 O17 1.455(16) . ? S3 C83 1.759(19) . ? C83 F7 1.328(19) . ? C83 F8 1.35(2) . ? C83 F9 1.37(2) . ? S4A O21A 1.397(18) . ? S4A O22A 1.408(17) . ? S4A O20A 1.433(18) . ? S4A C84A 1.77(2) . ? C84A F10A 1.32(2) . ? C84A F11A 1.35(2) . ? C84A F12A 1.37(2) . ? S4B O21B 1.385(18) . ? S4B O22B 1.413(17) . ? S4B O20B 1.439(17) . ? S4B C84B 1.78(2) . ? C84B F10B 1.33(2) . ? C84B F11B 1.35(2) . ? C84B F12B 1.37(2) . ? N1S C1S 1.04(7) . ? C1S C2S 1.54(7) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N5 178.4(9) . . ? N2 Ru1 N3 76.8(9) . . ? N5 Ru1 N3 102.0(9) . . ? N2 Ru1 N1 78.8(8) . . ? N5 Ru1 N1 102.3(8) . . ? N3 Ru1 N1 155.7(9) . . ? N2 Ru1 N4 102.2(8) . . ? N5 Ru1 N4 79.0(9) . . ? N3 Ru1 N4 97.0(8) . . ? N1 Ru1 N4 88.9(7) . . ? N2 Ru1 N6 101.6(7) . . ? N5 Ru1 N6 77.2(8) . . ? N3 Ru1 N6 85.6(8) . . ? N1 Ru1 N6 98.5(6) . . ? N4 Ru1 N6 156.1(8) . . ? C1 N1 C5 120.0 . . ? C1 N1 Ru1 125.9(10) . . ? C5 N1 Ru1 114.0(10) . . ? N1 C1 C2 120.0 . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C1 C2 C3 120.0 . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 C6 125.6(16) . . ? N1 C5 C6 114.3(16) . . ? C7 C6 N2 120.0 . . ? C7 C6 C5 125.7(16) . . ? N2 C6 C5 114.3(16) . . ? C8 C7 C6 120.0 . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 N2 110.5(19) . . ? C11 C10 C9 129.5(19) . . ? N2 C10 C9 120.0 . . ? C10 N2 C6 120.0 . . ? C10 N2 Ru1 121.4(12) . . ? C6 N2 Ru1 118.5(12) . . ? C10 C11 C12 124(2) . . ? C10 C11 N3 116(2) . . ? C12 C11 N3 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 N3 120.0 . . ? C14 C15 H15A 120.0 . . ? N3 C15 H15A 120.0 . . ? C15 N3 C11 120.0 . . ? C15 N3 Ru1 124.4(15) . . ? C11 N3 Ru1 115.5(15) . . ? C16 N4 C20 120.0 . . ? C16 N4 Ru1 126.0(12) . . ? C20 N4 Ru1 113.9(12) . . ? C17 C16 N4 120.0 . . ? C17 C16 H16A 120.0 . . ? N4 C16 H16A 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C20 C19 C18 120.0 . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 N4 120.0 . . ? C19 C20 C21 125.0(17) . . ? N4 C20 C21 115.0(17) . . ? C22 C21 N5 120.0 . . ? C22 C21 C20 127.6(17) . . ? N5 C21 C20 112.2(17) . . ? C23 C22 C21 120.0 . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 C31 118.5(17) . . ? C24 C23 C31 121.4(17) . . ? C23 C24 C25 120.0 . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? N5 C25 C24 120.0 . . ? N5 C25 C26 111.3(17) . . ? C24 C25 C26 128.5(17) . . ? C25 N5 C21 120.0 . . ? C25 N5 Ru1 120.9(13) . . ? C21 N5 Ru1 118.8(13) . . ? C27 C26 N6 120.0 . . ? C27 C26 C25 122.9(16) . . ? N6 C26 C25 116.9(16) . . ? C28 C27 C26 120.0 . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? N6 C30 C29 120.0 . . ? N6 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 N6 C26 120.0 . . ? C30 N6 Ru1 125.6(10) . . ? C26 N6 Ru1 113.1(10) . . ? C32 C31 C36 120.0 . . ? C32 C31 C23 118.2(17) . . ? C36 C31 C23 121.5(17) . . ? C31 C32 C33 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 C37 118(2) . . ? C33 C34 C37 121.8(19) . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36A 120.0 . . ? C31 C36 H36A 120.0 . . ? N7 C37 C34 112(2) . . ? N7 C37 H37A 109.1 . . ? C34 C37 H37A 109.1 . . ? N7 C37 H37B 109.1 . . ? C34 C37 H37B 109.1 . . ? H37A C37 H37B 107.9 . . ? C38 N7 C42 120.0 . . ? C38 N7 C37 120.2(19) . . ? C42 N7 C37 119.5(18) . . ? C39 C38 N7 120.0 . . ? C39 C38 H38A 120.0 . . ? N7 C38 H38A 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39A 120.0 . . ? C38 C39 H39A 120.0 . . ? C39 C40 C41 120.0 . . ? C39 C40 C43 116.7(16) . . ? C41 C40 C43 123.3(17) . . ? C40 C41 C42 120.0 . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 N7 120.0 . . ? C41 C42 H42A 120.0 . . ? N7 C42 H42A 120.0 . . ? C44 C43 C47 120.0 . . ? C44 C43 C40 123.1(17) . . ? C47 C43 C40 116.9(17) . . ? C43 C44 C45 120.0 . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C44 C45 N8 120.0 . . ? C44 C45 H45A 120.0 . . ? N8 C45 H45A 120.0 . . ? C46 N8 C45 120.0 . . ? C46 N8 C48 119(2) . . ? C45 N8 C48 121(2) . . ? C47 C46 N8 120.0 . . ? C47 C46 H46A 120.0 . . ? N8 C46 H46A 120.0 . . ? C46 C47 C43 120.0 . . ? C46 C47 H47A 120.0 . . ? C43 C47 H47A 120.0 . . ? C48 C48 N8 108(3) 3_7<6 . ? C48 C48 H48A 110.2 3_7<6 . ? N8 C48 H48A 110.2 . . ? C48 C48 H48B 110.2 3_7<6 . ? N8 C48 H48B 110.2 . . ? H48A C48 H48B 108.5 . . ? C54 O7 C75 113(2) . . ? C77 O8 C76 115(3) . . ? C79 O9 C78 108(3) 3_7<6 . ? C49 O10 C80 120(2) . . ? O10 C49 C50 120.8(19) . . ? O10 C49 C54 119.2(19) . . ? C50 C49 C54 120.0 . . ? C51 C50 C49 120.0 . . ? C51 C50 H50A 120.0 . . ? C49 C50 H50A 120.0 . . ? C50 C51 C52 120.0 . . ? C50 C51 C55A 123(3) . . ? C52 C51 C55A 115(3) . . ? C50 C51 C55B 115(3) . . ? C52 C51 C55B 124(3) . . ? C55A C51 C55B 27(2) . . ? C51 C52 C53 120.0 . . ? C51 C52 C65 123(2) . . ? C53 C52 C65 117(2) . . ? C54 C53 C52 120.0 . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? O7 C54 C53 127(2) . . ? O7 C54 C49 113(2) . . ? C53 C54 C49 120.0 . . ? O4 C65 C52 106.1(18) . . ? O4 C65 H65A 110.5 . . ? C52 C65 H65A 110.5 . . ? O4 C65 H65B 110.5 . . ? C52 C65 H65B 110.5 . . ? H65A C65 H65B 108.7 . . ? C66 O4 C65 120.3(17) . . ? O4 C66 C67 124.1(16) . . ? O4 C66 C71 115.8(16) . . ? C67 C66 C71 120.0 . . ? C66 C67 C68 120.0 . . ? C66 C67 H67A 120.0 . . ? C68 C67 H67A 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68A 120.0 . . ? C69 C68 H68A 120.0 . . ? C70 C69 C68 120.0 . . ? C70 C69 C72 115.1(18) . . ? C68 C69 C72 124.8(18) . . ? C69 C70 C71 120.0 . . ? C69 C70 H70A 120.0 . . ? C71 C70 H70A 120.0 . . ? C70 C71 C66 120.0 . . ? C70 C71 H71A 120.0 . . ? C66 C71 H71A 120.0 . . ? O5 C72 O6 124(2) . . ? O5 C72 C69 126(2) . . ? O6 C72 C69 109(2) . . ? C72 O6 C73 114(2) . . ? C74 C73 O6 106.1(14) . . ? C74 C73 H73A 110.5 . . ? O6 C73 H73A 110.5 . . ? C74 C73 H73B 110.5 . . ? O6 C73 H73B 110.5 . . ? H73A C73 H73B 108.7 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O7 C75 C76 105(3) . . ? O7 C75 H75A 110.7 . . ? C76 C75 H75A 110.7 . . ? O7 C75 H75B 110.7 . . ? C76 C75 H75B 110.7 . . ? H75A C75 H75B 108.8 . . ? O8 C76 C75 111(3) . . ? O8 C76 H76A 109.4 . . ? C75 C76 H76A 109.4 . . ? O8 C76 H76B 109.4 . . ? C75 C76 H76B 109.4 . . ? H76A C76 H76B 108.0 . . ? O8 C77 C78 109(3) . . ? O8 C77 H77A 109.9 . . ? C78 C77 H77A 109.9 . . ? O8 C77 H77B 109.9 . . ? C78 C77 H77B 109.9 . . ? H77A C77 H77B 108.3 . . ? O9 C78 C77 108(3) . . ? O9 C78 H78A 110.1 . . ? C77 C78 H78A 110.1 . . ? O9 C78 H78B 110.1 . . ? C77 C78 H78B 110.1 . . ? H78A C78 H78B 108.4 . . ? O9 C79 C80 109(3) 3_7<6 . ? O9 C79 H79A 110.0 3_7<6 . ? C80 C79 H79A 110.0 . . ? O9 C79 H79B 110.0 3_7<6 . ? C80 C79 H79B 110.0 . . ? H79A C79 H79B 108.3 . . ? O10 C80 C79 116(3) . . ? O10 C80 H80A 108.4 . . ? C79 C80 H80A 108.4 . . ? O10 C80 H80B 108.4 . . ? C79 C80 H80B 108.4 . . ? H80A C80 H80B 107.5 . . ? O3A C55A C51 105(4) . . ? O3A C55A H55A 110.8 . . ? C51 C55A H55A 110.8 . . ? O3A C55A H55B 110.8 . . ? C51 C55A H55B 110.8 . . ? H55A C55A H55B 108.9 . . ? C56A O3A C55A 123(3) . . ? O3A C56A C57A 118(2) . . ? O3A C56A C61A 119(2) . . ? C57A C56A C61A 120.00(7) . . ? C58A C57A C56A 120.0 . . ? C58A C57A H57A 120.0 . . ? C56A C57A H57A 120.0 . . ? C57A C58A C59A 120.0 . . ? C57A C58A H58A 120.0 . . ? C59A C58A H58A 120.0 . . ? C60A C59A C58A 120.00(6) . . ? C60A C59A C62A 117(2) . . ? C58A C59A C62A 122(2) . . ? C59A C60A C61A 120.0 . . ? C59A C60A H60A 120.0 . . ? C61A C60A H60A 120.0 . . ? C60A C61A C56A 120.0 . . ? C60A C61A H61A 120.0 . . ? C56A C61A H61A 120.0 . . ? O1A C62A O2A 118(4) . . ? O1A C62A C59A 122(4) . . ? O2A C62A C59A 108(3) . . ? C62A O2A C63A 111(4) . . ? C64A C63A O2A 106(3) . . ? C64A C63A H63A 110.5 . . ? O2A C63A H63A 110.5 . . ? C64A C63A H63B 110.5 . . ? O2A C63A H63B 110.5 . . ? H63A C63A H63B 108.7 . . ? C63A C64A H64A 109.5 . . ? C63A C64A H64B 109.5 . . ? H64A C64A H64B 109.5 . . ? C63A C64A H64C 109.5 . . ? H64A C64A H64C 109.5 . . ? H64B C64A H64C 109.5 . . ? O3B C55B C51 101(4) . . ? O3B C55B H55C 111.5 . . ? C51 C55B H55C 111.5 . . ? O3B C55B H55D 111.5 . . ? C51 C55B H55D 111.5 . . ? H55C C55B H55D 109.3 . . ? C56B O3B C55B 121(3) . . ? O3B C56B C57B 122(2) . . ? O3B C56B C61B 118(2) . . ? C57B C56B C61B 120.00(7) . . ? C56B C57B C58B 120.00(7) . . ? C56B C57B H57B 120.0 . . ? C58B C57B H57B 120.0 . . ? C59B C58B C57B 120.0 . . ? C59B C58B H58B 120.0 . . ? C57B C58B H58B 120.0 . . ? C58B C59B C60B 120.00(6) . . ? C58B C59B C62B 123(2) . . ? C60B C59B C62B 117(2) . . ? C59B C60B C61B 120.00(7) . . ? C59B C60B H60B 120.0 . . ? C61B C60B H60B 120.0 . . ? C60B C61B C56B 120.0 . . ? C60B C61B H61B 120.0 . . ? C56B C61B H61B 120.0 . . ? O1B C62B O2B 120(4) . . ? O1B C62B C59B 128(4) . . ? O2B C62B C59B 108(3) . . ? C62B O2B C63B 111(3) . . ? C64B C63B O2B 106(3) . . ? C64B C63B H63C 110.5 . . ? O2B C63B H63C 110.5 . . ? C64B C63B H63D 110.5 . . ? O2B C63B H63D 110.5 . . ? H63C C63B H63D 108.7 . . ? C63B C64B H64D 109.5 . . ? C63B C64B H64E 109.5 . . ? H64D C64B H64E 109.5 . . ? C63B C64B H64F 109.5 . . ? H64D C64B H64F 109.5 . . ? H64E C64B H64F 109.5 . . ? O12 S1 O13 115.4(10) . . ? O12 S1 O11 114.4(10) . . ? O13 S1 O11 114.9(10) . . ? O12 S1 C81 102.1(14) . . ? O13 S1 C81 105.4(14) . . ? O11 S1 C81 102.3(13) . . ? F1 C81 F2 107.1(13) . . ? F1 C81 F3 106.6(13) . . ? F2 C81 F3 106.5(13) . . ? F1 C81 S1 111.2(17) . . ? F2 C81 S1 111.6(16) . . ? F3 C81 S1 113.5(16) . . ? O15 S2 O16 117.8(15) . . ? O15 S2 O14 114.1(18) . . ? O16 S2 O14 114.7(16) . . ? O15 S2 C82 100.0(16) . . ? O16 S2 C82 107.4(14) . . ? O14 S2 C82 99.6(14) . . ? F4 C82 F5 107(2) . . ? F4 C82 F6 110(2) . . ? F5 C82 F6 111(2) . . ? F4 C82 S2 116(2) . . ? F5 C82 S2 110.0(19) . . ? F6 C82 S2 103.2(18) . . ? O18 S3 O19 119.3(16) . . ? O18 S3 O17 113.2(16) . . ? O19 S3 O17 110.1(15) . . ? O18 S3 C83 107.8(15) . . ? O19 S3 C83 106.1(15) . . ? O17 S3 C83 97.9(14) . . ? F7 C83 F8 107(2) . . ? F7 C83 F9 108(2) . . ? F8 C83 F9 108(2) . . ? F7 C83 S3 112(2) . . ? F8 C83 S3 111(2) . . ? F9 C83 S3 110.7(19) . . ? O21A S4A O22A 118(2) . . ? O21A S4A O20A 113(2) . . ? O22A S4A O20A 115(2) . . ? O21A S4A C84A 102(2) . . ? O22A S4A C84A 106(2) . . ? O20A S4A C84A 100.6(19) . . ? F10A C84A F11A 106(3) . . ? F10A C84A F12A 107(3) . . ? F11A C84A F12A 107(3) . . ? F10A C84A S4A 115(2) . . ? F11A C84A S4A 111(2) . . ? F12A C84A S4A 111(2) . . ? O21B S4B O22B 119(2) . . ? O21B S4B O20B 113(2) . . ? O22B S4B O20B 114(2) . . ? O21B S4B C84B 104(2) . . ? O22B S4B C84B 103.9(19) . . ? O20B S4B C84B 100.0(18) . . ? F10B C84B F11B 106(3) . . ? F10B C84B F12B 107(3) . . ? F11B C84B F12B 106(3) . . ? F10B C84B S4B 114(2) . . ? F11B C84B S4B 114(2) . . ? F12B C84B S4B 110(2) . . ? N1S C1S C2S 175(7) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.359 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.168 # Attachment '- DM65Q.cif' data_dm65q _database_code_depnum_ccdc_archive 'CCDC 864510' #TrackingRef '- DM65Q.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C138 H144 F12 N12 O39 S4' _chemical_formula_weight 2950.90 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.417(3) _cell_length_b 25.553(3) _cell_length_c 13.838(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.228(2) _cell_angle_gamma 90.00 _cell_volume 7372.1(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 241 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3080 _exptl_absorpt_coefficient_mu 0.161 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6208 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 65405 _diffrn_reflns_av_R_equivalents 0.1602 _diffrn_reflns_av_sigmaI/netI 0.1309 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12927 _reflns_number_gt 6234 _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. A cluster of 3 water molecules required a 50:50 disorder model; the O-atoms were restrained with SIMU to have appoximately equivalent displacement parameters. ; _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^)+(0.1065P)^2^+24.1041P] 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 12927 _refine_ls_number_parameters 920 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2414 _refine_ls_R_factor_gt 0.1361 _refine_ls_wR_factor_ref 0.3449 _refine_ls_wR_factor_gt 0.2818 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.5507(4) 0.0872(4) 0.6908(7) 0.089(3) Uani 1 1 d . . . N2 N 0.5493(4) 0.1568(3) 0.9120(6) 0.067(2) Uani 1 1 d . . . N3 N 0.5039(4) 0.2455(4) 1.0808(9) 0.121(4) Uani 1 1 d . . . N4 N 0.1184(3) 0.0890(3) 0.6254(4) 0.0407(15) Uani 1 1 d . . . N5 N -0.0013(3) 0.0246(2) 0.1269(4) 0.0357(14) Uani 1 1 d . . . C1 C 0.5927(6) 0.0601(6) 0.6505(9) 0.119(5) Uani 1 1 d . . . H1A H 0.5799 0.0506 0.5825 0.143 Uiso 1 1 calc R . . C2 C 0.6534(6) 0.0455(6) 0.7028(12) 0.118(5) Uani 1 1 d . . . H2A H 0.6807 0.0253 0.6720 0.141 Uiso 1 1 calc R . . C3 C 0.6726(6) 0.0605(6) 0.7977(10) 0.122(5) Uani 1 1 d . . . H3A H 0.7144 0.0520 0.8350 0.146 Uiso 1 1 calc R . . C4 C 0.6312(6) 0.0880(5) 0.8398(9) 0.105(4) Uani 1 1 d . . . H4A H 0.6444 0.0989 0.9070 0.126 Uiso 1 1 calc R . . C5 C 0.5706(5) 0.1003(4) 0.7867(8) 0.074(3) Uani 1 1 d . . . C6 C 0.5243(5) 0.1280(4) 0.8312(7) 0.065(3) Uani 1 1 d . . . C7 C 0.4589(4) 0.1210(4) 0.7962(7) 0.061(2) Uani 1 1 d . . . H7A H 0.4434 0.0992 0.7402 0.073 Uiso 1 1 calc R . . C8 C 0.4156(4) 0.1458(4) 0.8430(7) 0.060(2) Uani 1 1 d . . . C9 C 0.4422(4) 0.1770(4) 0.9243(7) 0.066(3) Uani 1 1 d . . . H9A H 0.4148 0.1956 0.9574 0.079 Uiso 1 1 calc R . . C10 C 0.5087(5) 0.1815(4) 0.9582(7) 0.070(3) Uani 1 1 d . . . C11 C 0.5384(5) 0.2093(4) 1.0502(9) 0.082(3) Uani 1 1 d . . . C12 C 0.5999(6) 0.1984(5) 1.1000(9) 0.104(4) Uani 1 1 d . . . H12A H 0.6246 0.1732 1.0745 0.125 Uiso 1 1 calc R . . C13 C 0.6260(7) 0.2244(6) 1.1880(11) 0.137(6) Uani 1 1 d . . . H13A H 0.6684 0.2170 1.2241 0.165 Uiso 1 1 calc R . . C14 C 0.5897(7) 0.2606(6) 1.2213(11) 0.138(6) Uani 1 1 d . . . H14A H 0.6058 0.2786 1.2819 0.166 Uiso 1 1 calc R . . C15 C 0.5297(6) 0.2707(6) 1.1661(12) 0.147(7) Uani 1 1 d . . . H15A H 0.5048 0.2967 1.1888 0.177 Uiso 1 1 calc R . . C16 C 0.3465(4) 0.1366(4) 0.8117(6) 0.051(2) Uani 1 1 d . . . C17 C 0.3018(4) 0.1746(3) 0.8161(6) 0.057(2) Uani 1 1 d . . . H17A H 0.3162 0.2084 0.8395 0.068 Uiso 1 1 calc R . . C18 C 0.2368(4) 0.1651(3) 0.7873(6) 0.052(2) Uani 1 1 d . . . H18A H 0.2070 0.1924 0.7889 0.063 Uiso 1 1 calc R . . C19 C 0.2154(4) 0.1157(3) 0.7564(5) 0.048(2) Uani 1 1 d . . . C20 C 0.2591(4) 0.0766(3) 0.7518(5) 0.050(2) Uani 1 1 d . . . H20A H 0.2448 0.0424 0.7304 0.061 Uiso 1 1 calc R . . C21 C 0.3239(4) 0.0877(4) 0.7786(5) 0.051(2) Uani 1 1 d . . . H21A H 0.3539 0.0609 0.7740 0.061 Uiso 1 1 calc R . . C22 C 0.1439(4) 0.1033(3) 0.7322(5) 0.047(2) Uani 1 1 d . . . H22A H 0.1360 0.0738 0.7745 0.057 Uiso 1 1 calc R . . H22B H 0.1201 0.1341 0.7484 0.057 Uiso 1 1 calc R . . C23 C 0.1031(4) 0.1273(3) 0.5590(5) 0.047(2) Uani 1 1 d . . . H23A H 0.1082 0.1629 0.5794 0.057 Uiso 1 1 calc R . . C24 C 0.0795(4) 0.1150(3) 0.4602(5) 0.0421(19) Uani 1 1 d . . . H24A H 0.0689 0.1424 0.4127 0.050 Uiso 1 1 calc R . . C25 C 0.0713(3) 0.0639(3) 0.4296(5) 0.0378(18) Uani 1 1 d . . . C26 C 0.0880(3) 0.0251(3) 0.5014(5) 0.0381(18) Uani 1 1 d . . . H26A H 0.0831 -0.0107 0.4833 0.046 Uiso 1 1 calc R . . C27 C 0.1113(4) 0.0389(3) 0.5975(5) 0.0431(19) Uani 1 1 d . . . H27A H 0.1229 0.0123 0.6462 0.052 Uiso 1 1 calc R . . C28 C 0.0453(3) 0.0502(3) 0.3233(5) 0.0341(17) Uani 1 1 d . . . C29 C 0.0410(3) 0.0872(3) 0.2488(5) 0.0405(18) Uani 1 1 d . . . H29A H 0.0547 0.1221 0.2654 0.049 Uiso 1 1 calc R . . C30 C 0.0171(4) 0.0738(3) 0.1515(5) 0.045(2) Uani 1 1 d . . . H30A H 0.0136 0.0996 0.1011 0.054 Uiso 1 1 calc R . . C31 C 0.0022(3) -0.0121(3) 0.1970(5) 0.0371(18) Uani 1 1 d . . . H31A H -0.0115 -0.0468 0.1784 0.045 Uiso 1 1 calc R . . C32 C 0.0252(3) -0.0001(3) 0.2950(5) 0.0365(17) Uani 1 1 d . . . H32A H 0.0275 -0.0265 0.3440 0.044 Uiso 1 1 calc R . . C33 C -0.0264(3) 0.0107(3) 0.0211(5) 0.0428(19) Uani 1 1 d . . . H33A H -0.0448 0.0421 -0.0166 0.051 Uiso 1 1 calc R . . H33B H -0.0608 -0.0158 0.0154 0.051 Uiso 1 1 calc R . . O1 O -0.5530(3) 0.0402(3) -0.8892(5) 0.091(2) Uani 1 1 d . . . O2 O -0.4768(3) 0.0623(3) -0.9696(5) 0.102(3) Uani 1 1 d . . . O3 O -0.3195(3) 0.0195(3) -0.5287(4) 0.0698(18) Uani 1 1 d . . . O4 O -0.2309(3) -0.1346(3) -0.4527(4) 0.0688(17) Uani 1 1 d . . . O5 O -0.2931(5) -0.3413(4) -0.7129(9) 0.153(4) Uani 1 1 d . . . O6 O -0.3884(4) -0.3058(3) -0.7283(7) 0.130(3) Uani 1 1 d . . . O7 O -0.1538(2) -0.0404(2) -0.1204(3) 0.0488(14) Uani 1 1 d . . . O8 O -0.0928(2) -0.1000(2) 0.0642(3) 0.0454(13) Uani 1 1 d . . . O9 O -0.0338(2) 0.1284(2) -0.0705(4) 0.0485(14) Uani 1 1 d . . . O10 O -0.1345(2) 0.0558(2) -0.1737(3) 0.0467(13) Uani 1 1 d . . . C34 C -0.1658(3) 0.0235(4) -0.2459(5) 0.046(2) Uani 1 1 d . . . C35 C -0.1892(3) 0.0378(4) -0.3443(5) 0.049(2) Uani 1 1 d . . . H35A H -0.1831 0.0727 -0.3639 0.059 Uiso 1 1 calc R . . C36 C -0.2215(4) 0.0026(4) -0.4151(5) 0.050(2) Uani 1 1 d . . . C37 C -0.2303(3) -0.0477(4) -0.3881(6) 0.051(2) Uani 1 1 d . . . C38 C -0.2072(4) -0.0628(3) -0.2904(6) 0.050(2) Uani 1 1 d . . . H38A H -0.2125 -0.0980 -0.2718 0.060 Uiso 1 1 calc R . . C39 C -0.1764(3) -0.0275(4) -0.2190(5) 0.045(2) Uani 1 1 d . . . C40 C -0.2508(4) 0.0226(4) -0.5192(6) 0.061(2) Uani 1 1 d . . . H40A H -0.2375 0.0592 -0.5271 0.073 Uiso 1 1 calc R . . H40B H -0.2375 0.0006 -0.5698 0.073 Uiso 1 1 calc R . . C41 C -0.3579(4) 0.0280(3) -0.6190(6) 0.053(2) Uani 1 1 d . . . C42 C -0.4212(4) 0.0134(4) -0.6299(6) 0.065(3) Uani 1 1 d . . . H42A H -0.4342 -0.0019 -0.5751 0.078 Uiso 1 1 calc R . . C43 C -0.4664(4) 0.0206(4) -0.7181(6) 0.068(3) Uani 1 1 d . . . H43A H -0.5097 0.0103 -0.7240 0.082 Uiso 1 1 calc R . . C44 C -0.4469(4) 0.0430(4) -0.7976(6) 0.059(2) Uani 1 1 d . . . C45 C -0.3837(5) 0.0564(4) -0.7881(6) 0.069(3) Uani 1 1 d . . . H45A H -0.3702 0.0702 -0.8437 0.083 Uiso 1 1 calc R . . C46 C -0.3392(4) 0.0500(4) -0.6979(6) 0.059(2) Uani 1 1 d . . . H46A H -0.2960 0.0608 -0.6914 0.071 Uiso 1 1 calc R . . C47 C -0.4931(5) 0.0489(4) -0.8949(7) 0.074(3) Uani 1 1 d . . . C48 C -0.6033(5) 0.0438(6) -0.9796(8) 0.102(4) Uani 1 1 d . . . H48A H -0.5874 0.0629 -1.0314 0.122 Uiso 1 1 calc R . . H48B H -0.6168 0.0083 -1.0049 0.122 Uiso 1 1 calc R . . C49 C -0.6560(6) 0.0709(7) -0.9568(8) 0.135(6) Uani 1 1 d . . . H49A H -0.6907 0.0735 -1.0166 0.202 Uiso 1 1 calc R . . H49B H -0.6424 0.1060 -0.9327 0.202 Uiso 1 1 calc R . . H49C H -0.6713 0.0517 -0.9053 0.202 Uiso 1 1 calc R . . C50 C -0.2675(4) -0.0885(4) -0.4580(6) 0.067(3) Uani 1 1 d . . . H50A H -0.3085 -0.0962 -0.4394 0.080 Uiso 1 1 calc R . . H50B H -0.2774 -0.0749 -0.5268 0.080 Uiso 1 1 calc R . . C51 C -0.2583(4) -0.1771(4) -0.5061(6) 0.058(2) Uani 1 1 d . . . C52 C -0.2182(5) -0.2188(4) -0.5131(9) 0.090(4) Uani 1 1 d . . . H52A H -0.1748 -0.2182 -0.4770 0.108 Uiso 1 1 calc R . . C53 C -0.2410(5) -0.2609(5) -0.5717(10) 0.105(4) Uani 1 1 d . . . H53A H -0.2125 -0.2884 -0.5790 0.126 Uiso 1 1 calc R . . C54 C -0.3051(5) -0.2640(4) -0.6207(8) 0.078(3) Uani 1 1 d . . . C55 C -0.3448(5) -0.2231(4) -0.6111(7) 0.074(3) Uani 1 1 d . . . H55A H -0.3890 -0.2251 -0.6430 0.088 Uiso 1 1 calc R . . C56 C -0.3223(4) -0.1788(4) -0.5564(7) 0.072(3) Uani 1 1 d . . . H56A H -0.3501 -0.1502 -0.5533 0.087 Uiso 1 1 calc R . . C57 C -0.3274(7) -0.3078(5) -0.6893(11) 0.104(4) Uani 1 1 d . . . C58 C -0.4137(9) -0.3482(7) -0.7984(18) 0.219(12) Uani 1 1 d . . . H58A H -0.3887 -0.3502 -0.8503 0.263 Uiso 1 1 calc R . . H58B H -0.4094 -0.3821 -0.7628 0.263 Uiso 1 1 calc R . . C59 C -0.4731(15) -0.3395(8) -0.839(2) 0.37(2) Uani 1 1 d . . . H59A H -0.4896 -0.3677 -0.8861 0.552 Uiso 1 1 calc R . . H59B H -0.4771 -0.3060 -0.8745 0.552 Uiso 1 1 calc R . . H59C H -0.4979 -0.3382 -0.7877 0.552 Uiso 1 1 calc R . . C60 C -0.1755(4) -0.0897(3) -0.0903(5) 0.048(2) Uani 1 1 d . . . H60A H -0.1543 -0.1188 -0.1174 0.058 Uiso 1 1 calc R . . H60B H -0.2225 -0.0931 -0.1161 0.058 Uiso 1 1 calc R . . C61 C -0.1596(4) -0.0921(3) 0.0205(5) 0.052(2) Uani 1 1 d . . . H61A H -0.1735 -0.0590 0.0464 0.062 Uiso 1 1 calc R . . H61B H -0.1844 -0.1209 0.0416 0.062 Uiso 1 1 calc R . . C62 C -0.0738(4) -0.1525(3) 0.0616(5) 0.048(2) Uani 1 1 d . . . H62A H -0.0778 -0.1637 -0.0081 0.058 Uiso 1 1 calc R . . H62B H -0.1018 -0.1752 0.0915 0.058 Uiso 1 1 calc R . . C63 C 0.0057(4) 0.1580(3) -0.1180(5) 0.051(2) Uani 1 1 d . . . H63A H -0.0072 0.1953 -0.1204 0.061 Uiso 1 1 calc R . . H63B H 0.0013 0.1454 -0.1869 0.061 Uiso 1 1 calc R . . C64 C -0.1008(4) 0.1391(4) -0.1036(6) 0.062(2) Uani 1 1 d . . . H64A H -0.1067 0.1772 -0.1159 0.074 Uiso 1 1 calc R . . H64B H -0.1226 0.1297 -0.0502 0.074 Uiso 1 1 calc R . . C65 C -0.1321(4) 0.1100(4) -0.1969(6) 0.062(2) Uani 1 1 d . . . H65A H -0.1761 0.1234 -0.2232 0.074 Uiso 1 1 calc R . . H65B H -0.1072 0.1150 -0.2483 0.074 Uiso 1 1 calc R . . S1 S 0.06342(12) 0.26690(9) 0.72206(16) 0.0586(6) Uani 1 1 d . . . O11 O 0.0478(3) 0.2813(2) 0.8144(4) 0.0718(18) Uani 1 1 d . . . O12 O 0.0943(3) 0.3075(2) 0.6799(4) 0.0691(17) Uani 1 1 d . . . O13 O 0.0887(3) 0.2160(2) 0.7223(5) 0.080(2) Uani 1 1 d . . . C66 C -0.0147(6) 0.2618(5) 0.6419(8) 0.089(3) Uani 1 1 d . . . F1 F -0.0459(3) 0.3060(3) 0.6274(5) 0.113(2) Uani 1 1 d . . . F2 F -0.0512(3) 0.2256(3) 0.6688(5) 0.109(2) Uani 1 1 d . . . F3 F -0.0091(4) 0.2472(3) 0.5491(5) 0.133(3) Uani 1 1 d . . . S2 S -0.15872(11) 0.06344(10) 0.18987(19) 0.0614(7) Uani 1 1 d . . . O14 O -0.1225(3) 0.1070(3) 0.1755(7) 0.107(3) Uani 1 1 d . . . O15 O -0.1825(3) 0.0634(3) 0.2793(5) 0.082(2) Uani 1 1 d . . . O16 O -0.1336(3) 0.0144(3) 0.1709(5) 0.0773(19) Uani 1 1 d . . . C67 C -0.2295(6) 0.0692(6) 0.0932(9) 0.093(4) Uani 1 1 d . . . F4 F -0.2155(4) 0.0700(4) 0.0045(5) 0.163(4) Uani 1 1 d . . . F5 F -0.2645(3) 0.1091(4) 0.1001(7) 0.146(3) Uani 1 1 d . . . F6 F -0.2680(3) 0.0273(3) 0.0917(5) 0.125(3) Uani 1 1 d . . . N1S N 0.0600(5) -0.1046(4) 0.4548(9) 0.106(4) Uani 1 1 d . . . C1S C 0.0824(6) -0.1331(5) 0.5168(10) 0.097(4) Uani 1 1 d . . . C2S C 0.1078(9) -0.1714(5) 0.5992(11) 0.156(7) Uani 1 1 d . . . O1WA O -0.3013(19) 0.3362(12) 0.019(2) 0.214(12) Uiso 0.50 1 d P A -1 O2WA O -0.2033(13) 0.2234(11) 0.080(2) 0.205(11) Uiso 0.50 1 d P B -1 O3WA O -0.2435(17) 0.2218(14) -0.124(3) 0.257(15) Uiso 0.50 1 d P C -1 O1WB O -0.2383(14) 0.2199(12) -0.035(3) 0.212(12) Uiso 0.50 1 d P D -2 O2WB O -0.3709(13) 0.3331(10) -0.0237(18) 0.179(9) Uiso 0.50 1 d P E -2 O3WB O -0.2493(17) 0.3412(12) 0.048(2) 0.211(12) Uiso 0.50 1 d P F -2 O4W O 0.462(2) 0.1288(19) 0.532(4) 0.38(3) Uiso 0.50 1 d P . . H4WA H 0.4227 0.1267 0.5337 0.577 Uiso 0.50 1 d PR . . H4WB H 0.4848 0.1147 0.5844 0.462 Uiso 0.50 1 d PR . . 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 0.075(6) 0.128(8) 0.072(6) -0.018(5) 0.032(5) 0.001(5) N2 0.055(5) 0.070(5) 0.077(6) -0.001(4) 0.015(4) 0.000(4) N3 0.065(6) 0.123(9) 0.166(10) -0.093(8) 0.006(6) 0.000(6) N4 0.044(4) 0.053(4) 0.024(3) -0.003(3) 0.006(3) 0.002(3) N5 0.035(3) 0.047(4) 0.025(3) -0.002(3) 0.006(3) 0.001(3) C1 0.083(9) 0.202(15) 0.083(9) -0.050(9) 0.045(8) -0.016(9) C2 0.062(8) 0.170(14) 0.134(13) -0.016(10) 0.048(8) 0.024(8) C3 0.078(9) 0.203(16) 0.083(9) -0.031(10) 0.017(7) 0.028(9) C4 0.075(8) 0.145(11) 0.100(9) -0.021(8) 0.030(7) 0.036(8) C5 0.062(7) 0.099(8) 0.066(7) -0.001(6) 0.028(6) 0.006(6) C6 0.061(6) 0.082(7) 0.053(6) 0.000(5) 0.018(5) 0.009(5) C7 0.055(6) 0.074(7) 0.055(6) -0.005(5) 0.014(5) 0.005(5) C8 0.042(5) 0.070(6) 0.065(6) -0.007(5) 0.007(4) 0.001(5) C9 0.041(5) 0.073(7) 0.086(7) -0.015(5) 0.018(5) 0.004(5) C10 0.060(6) 0.074(7) 0.081(7) -0.021(5) 0.023(5) 0.006(5) C11 0.054(6) 0.075(7) 0.111(9) -0.042(6) 0.009(6) 0.000(5) C12 0.080(9) 0.118(10) 0.105(10) -0.042(8) 0.001(7) 0.008(7) C13 0.090(10) 0.173(15) 0.133(12) -0.070(11) -0.006(9) 0.016(10) C14 0.085(10) 0.176(15) 0.141(13) -0.099(11) -0.002(9) 0.001(10) C15 0.070(9) 0.170(15) 0.190(16) -0.112(13) 0.008(10) 0.003(9) C16 0.052(5) 0.061(6) 0.041(5) 0.002(4) 0.011(4) 0.009(5) C17 0.053(6) 0.056(6) 0.058(6) -0.007(4) 0.008(4) -0.006(5) C18 0.059(6) 0.048(5) 0.048(5) -0.005(4) 0.009(4) 0.003(4) C19 0.045(5) 0.071(6) 0.026(4) -0.001(4) 0.007(4) 0.002(4) C20 0.059(6) 0.060(6) 0.028(4) -0.004(4) 0.003(4) 0.010(5) C21 0.054(6) 0.069(6) 0.028(4) 0.001(4) 0.006(4) 0.019(5) C22 0.059(5) 0.053(5) 0.034(4) -0.003(4) 0.017(4) 0.005(4) C23 0.062(5) 0.045(5) 0.036(5) -0.009(4) 0.013(4) 0.002(4) C24 0.056(5) 0.047(5) 0.022(4) 0.003(3) 0.007(3) 0.004(4) C25 0.027(4) 0.056(5) 0.031(4) -0.009(4) 0.007(3) -0.006(4) C26 0.047(5) 0.045(5) 0.021(4) -0.001(3) 0.006(3) 0.004(4) C27 0.045(5) 0.048(5) 0.033(4) 0.006(4) 0.004(3) 0.005(4) C28 0.026(4) 0.047(5) 0.028(4) -0.003(3) 0.003(3) 0.007(3) C29 0.047(5) 0.044(5) 0.029(4) -0.005(3) 0.005(3) -0.004(4) C30 0.048(5) 0.055(5) 0.030(4) 0.010(4) 0.006(4) 0.002(4) C31 0.034(4) 0.045(5) 0.033(4) -0.005(4) 0.007(3) -0.005(3) C32 0.041(4) 0.044(5) 0.025(4) 0.001(3) 0.010(3) -0.003(4) C33 0.044(5) 0.061(5) 0.019(4) -0.008(3) -0.001(3) -0.008(4) O1 0.052(4) 0.159(7) 0.056(4) 0.010(4) 0.003(3) 0.007(4) O2 0.070(5) 0.164(8) 0.063(5) 0.039(5) 0.000(4) 0.000(5) O3 0.050(4) 0.116(5) 0.037(3) 0.004(3) -0.001(3) 0.015(3) O4 0.053(4) 0.078(5) 0.068(4) -0.011(3) -0.001(3) 0.005(3) O5 0.123(8) 0.089(7) 0.220(12) -0.046(7) -0.016(7) 0.018(6) O6 0.088(6) 0.101(7) 0.170(9) -0.051(6) -0.034(6) 0.011(5) O7 0.044(3) 0.069(4) 0.028(3) -0.001(3) -0.002(2) -0.006(3) O8 0.051(3) 0.049(4) 0.033(3) -0.002(2) 0.005(2) -0.007(3) O9 0.050(3) 0.057(4) 0.038(3) 0.007(3) 0.009(3) -0.006(3) O10 0.045(3) 0.058(4) 0.033(3) 0.004(3) 0.001(2) -0.001(3) C34 0.029(4) 0.078(6) 0.031(4) -0.006(4) 0.005(3) -0.001(4) C35 0.036(4) 0.076(6) 0.038(5) 0.000(4) 0.012(4) 0.007(4) C36 0.033(4) 0.087(7) 0.030(4) -0.007(4) 0.003(3) 0.008(4) C37 0.030(4) 0.082(7) 0.038(5) -0.020(5) 0.003(4) 0.007(4) C38 0.037(5) 0.069(6) 0.041(5) -0.007(4) 0.004(4) 0.008(4) C39 0.024(4) 0.075(6) 0.035(4) -0.008(4) 0.007(3) -0.006(4) C40 0.036(5) 0.100(7) 0.045(5) -0.003(5) 0.005(4) 0.004(5) C41 0.047(5) 0.072(6) 0.038(5) -0.006(4) 0.006(4) 0.010(4) C42 0.050(6) 0.105(8) 0.039(5) 0.013(5) 0.011(4) 0.014(5) C43 0.052(6) 0.096(8) 0.050(6) 0.008(5) -0.001(5) 0.011(5) C44 0.046(6) 0.082(7) 0.045(5) 0.005(5) 0.000(4) 0.015(5) C45 0.072(7) 0.100(8) 0.036(5) 0.013(5) 0.013(5) 0.014(6) C46 0.042(5) 0.084(7) 0.049(5) 0.002(5) 0.005(4) 0.005(5) C47 0.059(7) 0.113(9) 0.048(6) 0.020(6) 0.004(5) 0.007(6) C48 0.045(6) 0.189(13) 0.062(7) -0.005(7) -0.006(5) 0.009(7) C49 0.070(8) 0.261(19) 0.066(8) -0.001(9) 0.002(6) 0.045(10) C50 0.049(5) 0.102(8) 0.045(5) -0.023(5) 0.000(4) 0.008(5) C51 0.049(6) 0.073(7) 0.048(5) -0.003(5) 0.001(4) -0.010(5) C52 0.060(7) 0.068(7) 0.127(10) 0.011(7) -0.011(6) 0.011(6) C53 0.073(8) 0.071(8) 0.145(11) 0.005(8) -0.025(7) 0.007(6) C54 0.069(7) 0.061(7) 0.092(8) 0.006(6) -0.004(6) 0.005(6) C55 0.055(6) 0.096(8) 0.068(7) -0.003(6) 0.008(5) 0.003(6) C56 0.050(6) 0.099(8) 0.065(6) -0.021(6) 0.009(5) 0.004(5) C57 0.083(9) 0.076(9) 0.138(12) -0.008(8) -0.008(8) 0.011(7) C58 0.137(15) 0.155(17) 0.29(3) -0.110(17) -0.100(16) 0.018(13) C59 0.36(4) 0.139(19) 0.47(5) -0.15(2) -0.19(4) 0.00(2) C60 0.039(5) 0.065(6) 0.040(5) -0.007(4) 0.007(4) -0.003(4) C61 0.057(6) 0.063(6) 0.039(5) -0.003(4) 0.019(4) -0.013(4) C62 0.059(5) 0.063(6) 0.024(4) 0.000(4) 0.012(4) -0.014(4) C63 0.070(6) 0.051(5) 0.031(4) 0.006(4) 0.010(4) -0.007(4) C64 0.065(6) 0.063(6) 0.058(6) -0.002(5) 0.016(5) 0.004(5) C65 0.047(5) 0.076(7) 0.057(6) 0.005(5) 0.001(4) 0.011(5) S1 0.0777(17) 0.0502(14) 0.0469(13) 0.0026(11) 0.0121(12) 0.0049(12) O11 0.114(5) 0.059(4) 0.045(4) -0.006(3) 0.023(3) -0.017(4) O12 0.084(5) 0.062(4) 0.067(4) 0.006(3) 0.027(4) -0.002(3) O13 0.107(5) 0.060(4) 0.075(5) 0.000(3) 0.025(4) 0.025(4) C66 0.127(10) 0.074(8) 0.061(7) 0.009(6) 0.009(7) -0.015(8) F1 0.093(5) 0.080(5) 0.145(6) 0.035(4) -0.019(4) 0.008(4) F2 0.104(5) 0.103(5) 0.102(5) 0.027(4) -0.011(4) -0.034(4) F3 0.200(8) 0.122(6) 0.055(4) -0.001(4) -0.014(4) -0.039(5) S2 0.0508(14) 0.0651(17) 0.0692(16) 0.0069(12) 0.0156(12) 0.0005(12) O14 0.078(5) 0.083(5) 0.164(8) 0.022(5) 0.033(5) -0.010(4) O15 0.082(5) 0.097(5) 0.070(4) -0.002(4) 0.023(4) 0.006(4) O16 0.079(5) 0.068(4) 0.084(5) 0.002(4) 0.017(4) 0.008(4) C67 0.085(9) 0.107(10) 0.092(9) 0.036(7) 0.028(7) -0.005(8) F4 0.106(6) 0.302(12) 0.082(5) 0.059(6) 0.024(4) 0.002(6) F5 0.093(5) 0.161(8) 0.181(8) 0.066(6) 0.026(5) 0.059(5) F6 0.078(5) 0.171(7) 0.113(6) 0.013(5) -0.005(4) -0.022(5) N1S 0.125(9) 0.057(6) 0.150(10) 0.031(6) 0.063(8) 0.014(6) C1S 0.124(11) 0.054(7) 0.116(11) -0.014(7) 0.036(9) -0.004(7) C2S 0.232(19) 0.080(9) 0.115(11) 0.014(8) -0.047(11) 0.008(10) _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 C5 1.340(12) . ? N1 C1 1.353(13) . ? N2 C6 1.342(11) . ? N2 C10 1.347(11) . ? N3 C11 1.313(12) . ? N3 C15 1.347(15) . ? N4 C23 1.331(9) . ? N4 C27 1.336(9) . ? N4 C22 1.499(9) . ? N5 C30 1.338(9) . ? N5 C31 1.338(9) . ? N5 C33 1.483(8) . ? C1 C2 1.387(16) . ? C1 H1A 0.9500 . ? C2 C3 1.339(16) . ? C2 H2A 0.9500 . ? C3 C4 1.365(15) . ? C3 H3A 0.9500 . ? C4 C5 1.373(14) . ? C4 H4A 0.9500 . ? C5 C6 1.464(13) . ? C6 C7 1.385(12) . ? C7 C8 1.400(11) . ? C7 H7A 0.9500 . ? C8 C9 1.389(12) . ? C8 C16 1.463(11) . ? C9 C10 1.400(12) . ? C9 H9A 0.9500 . ? C10 C11 1.470(13) . ? C11 C12 1.368(14) . ? C12 C13 1.387(15) . ? C12 H12A 0.9500 . ? C13 C14 1.356(16) . ? C13 H13A 0.9500 . ? C14 C15 1.360(17) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.374(11) . ? C16 C21 1.379(11) . ? C17 C18 1.379(11) . ? C17 H17A 0.9500 . ? C18 C19 1.377(11) . ? C18 H18A 0.9500 . ? C19 C20 1.382(11) . ? C19 C22 1.525(11) . ? C20 C21 1.382(11) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.381(10) . ? C23 H23A 0.9500 . ? C24 C25 1.373(10) . ? C24 H24A 0.9500 . ? C25 C26 1.391(10) . ? C25 C28 1.490(9) . ? C26 C27 1.355(9) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C32 1.383(9) . ? C28 C29 1.387(10) . ? C29 C30 1.371(10) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.369(9) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C33 1.490(14) 3 ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? O1 C47 1.321(11) . ? O1 C48 1.456(10) . ? O2 C47 1.213(11) . ? O3 C41 1.347(9) . ? O3 C40 1.449(9) . ? O4 C51 1.370(10) . ? O4 C50 1.406(10) . ? O5 C57 1.219(14) . ? O6 C57 1.296(13) . ? O6 C58 1.471(16) . ? O7 C39 1.379(8) . ? O7 C60 1.439(9) . ? O8 C62 1.405(9) . ? O8 C61 1.435(9) . ? O9 C63 1.405(9) . ? O9 C64 1.429(9) . ? O10 C34 1.349(9) . ? O10 C65 1.424(10) . ? C34 C35 1.388(10) . ? C34 C39 1.388(11) . ? C35 C36 1.392(11) . ? C35 H35A 0.9500 . ? C36 C37 1.364(12) . ? C36 C40 1.522(11) . ? C37 C38 1.384(11) . ? C37 C50 1.517(11) . ? C38 C39 1.388(10) . ? C38 H38A 0.9500 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.367(11) . ? C41 C42 1.380(11) . ? C42 C43 1.385(11) . ? C42 H42A 0.9500 . ? C43 C44 1.387(12) . ? C43 H43A 0.9500 . ? C44 C45 1.371(12) . ? C44 C47 1.486(12) . ? C45 C46 1.397(11) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C48 C49 1.418(14) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.384(13) . ? C51 C56 1.389(12) . ? C52 C53 1.369(14) . ? C52 H52A 0.9500 . ? C53 C54 1.389(14) . ? C53 H53A 0.9500 . ? C54 C55 1.373(13) . ? C54 C57 1.474(16) . ? C55 C56 1.385(13) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C58 C59 1.29(3) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.494(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.494(11) 3 ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C62 1.494(11) 3 ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.509(11) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? S1 O13 1.409(6) . ? S1 O12 1.425(6) . ? S1 O11 1.441(6) . ? S1 C66 1.789(12) . ? C66 F1 1.304(12) . ? C66 F2 1.318(12) . ? C66 F3 1.368(12) . ? S2 O14 1.397(7) . ? S2 O16 1.411(7) . ? S2 O15 1.442(7) . ? S2 C67 1.783(13) . ? C67 F5 1.282(14) . ? C67 F4 1.328(13) . ? C67 F6 1.349(13) . ? N1S C1S 1.144(14) . ? C1S C2S 1.507(18) . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8501 . ? 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 C5 N1 C1 116.4(10) . . ? C6 N2 C10 118.3(8) . . ? C11 N3 C15 118.1(11) . . ? C23 N4 C27 120.8(6) . . ? C23 N4 C22 118.6(6) . . ? C27 N4 C22 120.6(6) . . ? C30 N5 C31 120.7(6) . . ? C30 N5 C33 119.7(6) . . ? C31 N5 C33 119.6(6) . . ? N1 C1 C2 123.8(11) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C3 C2 C1 118.4(12) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.8 . . ? C2 C3 C4 118.8(12) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C3 C4 C5 121.1(12) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? N1 C5 C4 121.4(10) . . ? N1 C5 C6 116.4(9) . . ? C4 C5 C6 122.2(10) . . ? N2 C6 C7 122.7(8) . . ? N2 C6 C5 115.9(9) . . ? C7 C6 C5 121.2(9) . . ? C6 C7 C8 120.3(9) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C9 C8 C7 116.2(8) . . ? C9 C8 C16 122.2(8) . . ? C7 C8 C16 121.5(8) . . ? C8 C9 C10 121.1(8) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? N2 C10 C9 121.3(9) . . ? N2 C10 C11 116.1(9) . . ? C9 C10 C11 122.4(9) . . ? N3 C11 C12 121.9(10) . . ? N3 C11 C10 117.1(10) . . ? C12 C11 C10 120.9(10) . . ? C11 C12 C13 119.5(11) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C14 C13 C12 118.5(13) . . ? C14 C13 H13A 120.7 . . ? C12 C13 H13A 120.7 . . ? C13 C14 C15 118.6(12) . . ? C13 C14 H14A 120.7 . . ? C15 C14 H14A 120.7 . . ? N3 C15 C14 123.2(12) . . ? N3 C15 H15A 118.4 . . ? C14 C15 H15A 118.4 . . ? C17 C16 C21 117.4(8) . . ? C17 C16 C8 122.6(8) . . ? C21 C16 C8 119.9(8) . . ? C16 C17 C18 122.0(8) . . ? C16 C17 H17A 119.0 . . ? C18 C17 H17A 119.0 . . ? C19 C18 C17 119.6(8) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C18 C19 C20 119.7(8) . . ? C18 C19 C22 120.4(7) . . ? C20 C19 C22 119.8(8) . . ? C21 C20 C19 119.2(8) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C16 C21 C20 122.0(8) . . ? C16 C21 H21A 119.0 . . ? C20 C21 H21A 119.0 . . ? N4 C22 C19 112.7(6) . . ? N4 C22 H22A 109.0 . . ? C19 C22 H22A 109.0 . . ? N4 C22 H22B 109.0 . . ? C19 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N4 C23 C24 119.5(7) . . ? N4 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C25 C24 C23 121.0(7) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C24 C25 C26 117.6(6) . . ? C24 C25 C28 121.4(7) . . ? C26 C25 C28 121.0(7) . . ? C27 C26 C25 119.6(7) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? N4 C27 C26 121.6(7) . . ? N4 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? C32 C28 C29 117.5(6) . . ? C32 C28 C25 121.3(6) . . ? C29 C28 C25 121.3(7) . . ? C30 C29 C28 120.3(7) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? N5 C30 C29 120.5(7) . . ? N5 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? N5 C31 C32 120.6(7) . . ? N5 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C31 C32 C28 120.5(7) . . ? C31 C32 H32A 119.8 . . ? C28 C32 H32A 119.8 . . ? N5 C33 C33 109.8(7) . 3 ? N5 C33 H33A 109.7 . . ? C33 C33 H33A 109.7 3 . ? N5 C33 H33B 109.7 . . ? C33 C33 H33B 109.7 3 . ? H33A C33 H33B 108.2 . . ? C47 O1 C48 118.4(8) . . ? C41 O3 C40 117.8(6) . . ? C51 O4 C50 118.2(7) . . ? C57 O6 C58 115.4(11) . . ? C39 O7 C60 115.6(6) . . ? C62 O8 C61 113.1(6) . . ? C63 O9 C64 114.4(6) . . ? C34 O10 C65 117.7(6) . . ? O10 C34 C35 125.0(8) . . ? O10 C34 C39 117.4(7) . . ? C35 C34 C39 117.6(7) . . ? C34 C35 C36 122.1(8) . . ? C34 C35 H35A 118.9 . . ? C36 C35 H35A 118.9 . . ? C37 C36 C35 119.6(7) . . ? C37 C36 C40 121.6(8) . . ? C35 C36 C40 118.7(9) . . ? C36 C37 C38 119.3(7) . . ? C36 C37 C50 123.9(8) . . ? C38 C37 C50 116.7(9) . . ? C37 C38 C39 121.4(8) . . ? C37 C38 H38A 119.3 . . ? C39 C38 H38A 119.3 . . ? O7 C39 C38 123.4(8) . . ? O7 C39 C34 116.6(7) . . ? C38 C39 C34 120.0(7) . . ? O3 C40 C36 104.9(6) . . ? O3 C40 H40A 110.8 . . ? C36 C40 H40A 110.8 . . ? O3 C40 H40B 110.8 . . ? C36 C40 H40B 110.8 . . ? H40A C40 H40B 108.8 . . ? O3 C41 C46 125.4(8) . . ? O3 C41 C42 115.7(8) . . ? C46 C41 C42 119.0(8) . . ? C41 C42 C43 122.1(8) . . ? C41 C42 H42A 119.0 . . ? C43 C42 H42A 119.0 . . ? C42 C43 C44 118.5(9) . . ? C42 C43 H43A 120.8 . . ? C44 C43 H43A 120.8 . . ? C45 C44 C43 119.7(8) . . ? C45 C44 C47 120.0(9) . . ? C43 C44 C47 120.1(9) . . ? C44 C45 C46 120.9(8) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? C41 C46 C45 119.8(8) . . ? C41 C46 H46A 120.1 . . ? C45 C46 H46A 120.1 . . ? O2 C47 O1 124.8(9) . . ? O2 C47 C44 122.6(10) . . ? O1 C47 C44 112.5(8) . . ? C49 C48 O1 108.1(9) . . ? C49 C48 H48A 110.1 . . ? O1 C48 H48A 110.1 . . ? C49 C48 H48B 110.1 . . ? O1 C48 H48B 110.1 . . ? H48A C48 H48B 108.4 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O4 C50 C37 109.7(7) . . ? O4 C50 H50A 109.7 . . ? C37 C50 H50A 109.7 . . ? O4 C50 H50B 109.7 . . ? C37 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? O4 C51 C52 117.0(8) . . ? O4 C51 C56 123.1(9) . . ? C52 C51 C56 119.9(9) . . ? C53 C52 C51 120.3(10) . . ? C53 C52 H52A 119.9 . . ? C51 C52 H52A 119.9 . . ? C52 C53 C54 120.8(11) . . ? C52 C53 H53A 119.6 . . ? C54 C53 H53A 119.6 . . ? C55 C54 C53 118.3(10) . . ? C55 C54 C57 121.7(10) . . ? C53 C54 C57 119.7(11) . . ? C54 C55 C56 122.0(9) . . ? C54 C55 H55A 119.0 . . ? C56 C55 H55A 119.0 . . ? C55 C56 C51 118.6(9) . . ? C55 C56 H56A 120.7 . . ? C51 C56 H56A 120.7 . . ? O5 C57 O6 121.8(13) . . ? O5 C57 C54 125.4(12) . . ? O6 C57 C54 112.6(12) . . ? C59 C58 O6 109.9(17) . . ? C59 C58 H58A 109.7 . . ? O6 C58 H58A 109.7 . . ? C59 C58 H58B 109.7 . . ? O6 C58 H58B 109.7 . . ? H58A C58 H58B 108.2 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O7 C60 C61 108.6(6) . . ? O7 C60 H60A 110.0 . . ? C61 C60 H60A 110.0 . . ? O7 C60 H60B 110.0 . . ? C61 C60 H60B 110.0 . . ? H60A C60 H60B 108.3 . . ? O8 C61 C60 114.2(6) . . ? O8 C61 H61A 108.7 . . ? C60 C61 H61A 108.7 . . ? O8 C61 H61B 108.7 . . ? C60 C61 H61B 108.7 . . ? H61A C61 H61B 107.6 . . ? O8 C62 C63 109.3(6) . 3 ? O8 C62 H62A 109.8 . . ? C63 C62 H62A 109.8 3 . ? O8 C62 H62B 109.8 . . ? C63 C62 H62B 109.8 3 . ? H62A C62 H62B 108.3 . . ? O9 C63 C62 109.0(6) . 3 ? O9 C63 H63A 109.9 . . ? C62 C63 H63A 109.9 3 . ? O9 C63 H63B 109.9 . . ? C62 C63 H63B 109.9 3 . ? H63A C63 H63B 108.3 . . ? O9 C64 C65 113.4(7) . . ? O9 C64 H64A 108.9 . . ? C65 C64 H64A 108.9 . . ? O9 C64 H64B 108.9 . . ? C65 C64 H64B 108.9 . . ? H64A C64 H64B 107.7 . . ? O10 C65 C64 108.6(7) . . ? O10 C65 H65A 110.0 . . ? C64 C65 H65A 110.0 . . ? O10 C65 H65B 110.0 . . ? C64 C65 H65B 110.0 . . ? H65A C65 H65B 108.3 . . ? O13 S1 O12 117.3(4) . . ? O13 S1 O11 113.7(4) . . ? O12 S1 O11 113.6(4) . . ? O13 S1 C66 103.8(5) . . ? O12 S1 C66 104.7(5) . . ? O11 S1 C66 101.2(5) . . ? F1 C66 F2 109.6(11) . . ? F1 C66 F3 104.2(9) . . ? F2 C66 F3 105.0(9) . . ? F1 C66 S1 113.9(8) . . ? F2 C66 S1 114.0(8) . . ? F3 C66 S1 109.3(9) . . ? O14 S2 O16 115.7(5) . . ? O14 S2 O15 116.1(5) . . ? O16 S2 O15 112.5(4) . . ? O14 S2 C67 103.4(5) . . ? O16 S2 C67 103.2(6) . . ? O15 S2 C67 103.8(5) . . ? F5 C67 F4 108.4(11) . . ? F5 C67 F6 105.4(11) . . ? F4 C67 F6 105.3(12) . . ? F5 C67 S2 114.9(10) . . ? F4 C67 S2 111.2(9) . . ? F6 C67 S2 111.0(8) . . ? N1S C1S C2S 176.6(15) . . ? H4WA O4W H4WB 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.579 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.078 # Attachment '- DM75a.cif' data_dm75a _database_code_depnum_ccdc_archive 'CCDC 864511' #TrackingRef '- DM75a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H94 B2 F8 N8 O24' _chemical_formula_weight 1749.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.627(6) _cell_length_b 12.680(2) _cell_length_c 20.775(3) _cell_angle_alpha 90.00 _cell_angle_beta 123.038(2) _cell_angle_gamma 90.00 _cell_volume 8309(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 465 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 26.37 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6293 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43181 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8470 _reflns_number_gt 4758 _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. The tetrafluoroborate anion was treated as a rigid group with equivalent B-F bond lengths and equivalent F-B-F angles using SADI, SIMU and DELU restraints. The unit cell contains 24 molecules of nitromethane which were treated as diffuse contributions to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.183 968 339 ' ' 2 0.000 0.500 0.565 968 339 ' ' _platon_squeeze_details ; ; _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 8470 _refine_ls_number_parameters 451 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1669 _refine_ls_R_factor_gt 0.1216 _refine_ls_wR_factor_ref 0.3818 _refine_ls_wR_factor_gt 0.3558 _refine_ls_goodness_of_fit_ref 1.259 _refine_ls_restrained_S_all 1.296 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.16799(11) 1.3039(3) 0.1414(2) 0.0588(9) Uani 1 1 d . . . O2 O 0.13569(10) 1.1417(3) 0.2081(2) 0.0659(10) Uani 1 1 d . . . O3 O 0.23125(10) 0.8453(2) 0.15013(18) 0.0478(8) Uani 1 1 d . . . O4 O 0.23187(15) 0.6156(3) 0.1358(2) 0.0789(12) Uani 1 1 d . . . O5 O 0.28284(13) 0.9879(3) -0.0088(2) 0.0661(10) Uani 1 1 d . . . O6 O 0.24898(10) 0.9984(2) 0.08840(18) 0.0492(8) Uani 1 1 d . . . N1 N 0.19388(11) 0.2073(3) 0.4563(2) 0.0401(8) Uani 1 1 d . . . C1 C 0.06721(18) 0.1035(5) 0.4719(4) 0.0800(18) Uani 1 1 d . . . H1A H 0.0778 0.1646 0.5034 0.096 Uiso 1 1 calc R . . C2 C 0.03100(18) 0.0472(6) 0.4600(3) 0.0785(18) Uani 1 1 d . . . H2A H 0.0169 0.0753 0.4827 0.094 Uiso 1 1 calc R . . C3 C 0.0160(2) -0.0387(5) 0.4206(5) 0.085(2) Uani 1 1 d . . . C4 C 0.0323(3) -0.0707(7) 0.3836(7) 0.140(4) Uani 1 1 d . . . H4A H 0.0187 -0.1267 0.3479 0.168 Uiso 1 1 calc R . . C5 C 0.0699(3) -0.0263(6) 0.3936(6) 0.115(3) Uani 1 1 d . . . H5A H 0.0835 -0.0597 0.3716 0.138 Uiso 1 1 calc R . . C6 C 0.08604(14) 0.0636(4) 0.4345(3) 0.0500(11) Uani 1 1 d . . . C7 C 0.12419(13) 0.1144(4) 0.4452(3) 0.0472(11) Uani 1 1 d . . . C8 C 0.14714(16) 0.0618(4) 0.4205(3) 0.0625(14) Uani 1 1 d . . . H8A H 0.1389 -0.0068 0.3989 0.075 Uiso 1 1 calc R . . C9 C 0.18192(15) 0.1100(5) 0.4275(3) 0.0610(14) Uani 1 1 d . . . H9A H 0.1978 0.0731 0.4116 0.073 Uiso 1 1 calc R . . C10 C 0.17209(14) 0.2598(4) 0.4795(2) 0.0460(10) Uani 1 1 d . . . H10A H 0.1805 0.3291 0.4996 0.055 Uiso 1 1 calc R . . C11 C 0.13746(14) 0.2139(4) 0.4743(3) 0.0496(11) Uani 1 1 d . . . H11A H 0.1224 0.2523 0.4913 0.060 Uiso 1 1 calc R . . C12 C 0.23115(14) 0.2557(4) 0.4606(3) 0.0489(11) Uani 1 1 d . . . H12A H 0.2362 0.2204 0.4238 0.059 Uiso 1 1 calc R . . H12B H 0.2256 0.3314 0.4468 0.059 Uiso 1 1 calc R . . C13 C 0.21768(14) 1.0186(3) 0.1009(2) 0.0435(10) Uani 1 1 d . . . C14 C 0.19462(16) 1.1105(4) 0.0821(3) 0.0518(12) Uani 1 1 d . . . H14A H 0.1998 1.1645 0.0565 0.062 Uiso 1 1 calc R . . C15 C 0.16457(16) 1.1271(4) 0.0985(3) 0.0526(12) Uani 1 1 d . . . C16 C 0.15598(16) 1.0490(4) 0.1341(3) 0.0517(11) Uani 1 1 d . . . C17 C 0.17750(14) 0.9528(4) 0.1510(3) 0.0510(11) Uani 1 1 d . . . H17A H 0.1708 0.8974 0.1734 0.061 Uiso 1 1 calc R . . C18 C 0.20863(13) 0.9373(3) 0.1353(2) 0.0400(9) Uani 1 1 d . . . C19 C 0.14280(17) 1.2335(4) 0.0794(3) 0.0626(14) Uani 1 1 d . . . H19A H 0.1392 1.2615 0.0317 0.075 Uiso 1 1 calc R . . H19B H 0.1144 1.2262 0.0710 0.075 Uiso 1 1 calc R . . C20 C 0.15049(15) 1.4006(4) 0.1376(3) 0.0528(12) Uani 1 1 d . . . C21 C 0.1724(2) 1.4583(4) 0.2059(3) 0.0637(14) Uani 1 1 d . . . H21A H 0.1965 1.4292 0.2506 0.076 Uiso 1 1 calc R . . C22 C 0.1583(2) 1.5591(4) 0.2072(4) 0.0668(15) Uani 1 1 d . . . H22A H 0.1729 1.5989 0.2534 0.080 Uiso 1 1 calc R . . C23 C 0.1245(2) 1.6013(5) 0.1442(5) 0.089(2) Uani 1 1 d . . . H23A H 0.1153 1.6704 0.1460 0.107 Uiso 1 1 calc R . . C24 C 0.1029(2) 1.5435(6) 0.0764(5) 0.092(2) Uani 1 1 d . . . H24A H 0.0790 1.5735 0.0318 0.110 Uiso 1 1 calc R . . C25 C 0.11586(18) 1.4424(5) 0.0732(4) 0.0706(15) Uani 1 1 d . . . H25A H 0.1009 1.4028 0.0270 0.085 Uiso 1 1 calc R . . C26 C 0.12228(15) 1.0568(4) 0.1525(3) 0.0584(13) Uani 1 1 d . . . H26A H 0.0944 1.0731 0.1055 0.070 Uiso 1 1 calc R . . H26B H 0.1200 0.9897 0.1743 0.070 Uiso 1 1 calc R . . C27 C 0.10831(15) 1.1765(4) 0.2276(3) 0.0577(13) Uani 1 1 d . . . C28 C 0.07209(15) 1.1223(4) 0.2093(3) 0.0580(13) Uani 1 1 d . . . H28A H 0.0645 1.0580 0.1814 0.070 Uiso 1 1 calc R . . C29 C 0.04712(17) 1.1653(5) 0.2331(3) 0.0674(15) Uani 1 1 d . . . H29A H 0.0217 1.1302 0.2200 0.081 Uiso 1 1 calc R . . C30 C 0.05779(18) 1.2549(5) 0.2742(3) 0.0708(16) Uani 1 1 d . . . H30A H 0.0403 1.2822 0.2901 0.085 Uiso 1 1 calc R . . C31 C 0.09419(19) 1.3064(5) 0.2927(3) 0.0682(15) Uani 1 1 d . . . H31A H 0.1023 1.3687 0.3229 0.082 Uiso 1 1 calc R . . C32 C 0.11938(17) 1.2689(5) 0.2679(3) 0.0623(14) Uani 1 1 d . . . H32A H 0.1438 1.3067 0.2787 0.075 Uiso 1 1 calc R . . C33 C 0.22589(16) 0.7684(4) 0.1944(3) 0.0510(11) Uani 1 1 d . . . H33A H 0.1958 0.7466 0.1672 0.061 Uiso 1 1 calc R . . H33B H 0.2342 0.7985 0.2447 0.061 Uiso 1 1 calc R . . C34 C 0.25343(18) 0.6746(4) 0.2058(3) 0.0597(13) Uani 1 1 d . . . H34A H 0.2814 0.6983 0.2175 0.072 Uiso 1 1 calc R . . H34B H 0.2578 0.6306 0.2489 0.072 Uiso 1 1 calc R . . C35 C 0.2448(2) 0.5167(4) 0.1433(3) 0.0777(18) Uani 1 1 d . . . H35A H 0.2411 0.4810 0.1818 0.093 Uiso 1 1 calc R . . H35B H 0.2754 0.5162 0.1630 0.093 Uiso 1 1 calc R . . C36 C 0.27873(16) 1.0442(4) -0.0696(3) 0.0512(11) Uani 1 1 d . . . H36A H 0.3073 1.0624 -0.0579 0.061 Uiso 1 1 calc R . . H36B H 0.2635 1.1109 -0.0759 0.061 Uiso 1 1 calc R . . C37 C 0.29969(18) 1.0491(4) 0.0608(3) 0.0593(13) Uani 1 1 d . . . H37A H 0.3165 1.1089 0.0604 0.071 Uiso 1 1 calc R . . H37B H 0.3187 1.0045 0.1060 0.071 Uiso 1 1 calc R . . C38 C 0.26430(17) 1.0900(4) 0.0665(3) 0.0537(12) Uani 1 1 d . . . H38A H 0.2746 1.1461 0.1059 0.064 Uiso 1 1 calc R . . H38B H 0.2414 1.1191 0.0166 0.064 Uiso 1 1 calc R . . B1 B 0.3435(2) 1.3197(5) 0.1740(4) 0.083(2) Uani 1 1 d DU . . F1 F 0.32056(18) 1.3308(4) 0.1020(3) 0.148(2) Uani 1 1 d DU . . F2 F 0.3610(2) 1.2190(5) 0.1855(4) 0.170(2) Uani 1 1 d DU . . F3 F 0.3739(3) 1.3877(7) 0.2072(4) 0.306(6) Uani 1 1 d DU . . F4 F 0.3219(3) 1.3020(6) 0.2078(4) 0.203(3) Uani 1 1 d DU . . 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 0.071(2) 0.0519(19) 0.064(2) 0.0021(16) 0.0434(19) 0.0173(17) O2 0.0460(18) 0.101(3) 0.066(2) -0.023(2) 0.0399(17) -0.0026(18) O3 0.0535(18) 0.0417(16) 0.0575(18) 0.0028(14) 0.0363(16) -0.0026(14) O4 0.127(4) 0.043(2) 0.056(2) -0.0006(16) 0.043(2) 0.002(2) O5 0.110(3) 0.0514(19) 0.079(2) -0.0145(17) 0.078(2) -0.012(2) O6 0.069(2) 0.0407(16) 0.0620(19) 0.0004(14) 0.0510(18) -0.0006(15) N1 0.0383(18) 0.0411(19) 0.046(2) -0.0007(16) 0.0267(16) -0.0027(15) C1 0.059(3) 0.082(4) 0.114(5) 0.002(4) 0.057(4) -0.010(3) C2 0.053(3) 0.121(6) 0.070(4) 0.022(4) 0.039(3) 0.014(4) C3 0.085(4) 0.064(4) 0.139(6) -0.004(4) 0.082(5) -0.018(3) C4 0.155(8) 0.101(6) 0.230(11) -0.065(7) 0.147(9) -0.062(6) C5 0.127(6) 0.083(5) 0.193(9) -0.054(5) 0.124(7) -0.060(5) C6 0.041(2) 0.061(3) 0.056(3) 0.012(2) 0.031(2) 0.005(2) C7 0.032(2) 0.061(3) 0.047(2) 0.006(2) 0.0202(19) -0.001(2) C8 0.058(3) 0.063(3) 0.075(3) -0.020(3) 0.041(3) -0.007(3) C9 0.046(3) 0.078(4) 0.066(3) -0.023(3) 0.035(2) -0.003(3) C10 0.054(3) 0.047(2) 0.048(2) -0.002(2) 0.035(2) -0.006(2) C11 0.039(2) 0.065(3) 0.048(3) -0.004(2) 0.026(2) 0.004(2) C12 0.043(2) 0.060(3) 0.054(3) 0.000(2) 0.033(2) -0.010(2) C13 0.051(3) 0.047(2) 0.037(2) -0.0054(18) 0.028(2) -0.006(2) C14 0.072(3) 0.050(3) 0.050(3) 0.003(2) 0.044(2) 0.009(2) C15 0.056(3) 0.053(3) 0.054(3) 0.007(2) 0.033(2) 0.013(2) C16 0.061(3) 0.049(3) 0.060(3) -0.011(2) 0.043(3) -0.001(2) C17 0.044(2) 0.063(3) 0.052(3) -0.005(2) 0.029(2) -0.011(2) C18 0.041(2) 0.040(2) 0.045(2) -0.0053(18) 0.027(2) -0.0034(18) C19 0.060(3) 0.063(3) 0.074(3) 0.013(3) 0.042(3) 0.019(3) C20 0.050(3) 0.056(3) 0.069(3) 0.015(2) 0.043(3) 0.009(2) C21 0.087(4) 0.057(3) 0.076(4) 0.006(3) 0.063(3) 0.010(3) C22 0.084(4) 0.055(3) 0.093(4) 0.002(3) 0.068(4) 0.007(3) C23 0.069(4) 0.049(3) 0.161(7) 0.001(4) 0.071(5) 0.009(3) C24 0.066(4) 0.071(4) 0.123(6) 0.006(4) 0.042(4) 0.014(3) C25 0.057(3) 0.066(3) 0.087(4) -0.012(3) 0.038(3) -0.002(3) C26 0.044(3) 0.069(3) 0.061(3) -0.002(3) 0.028(2) 0.009(2) C27 0.048(3) 0.081(4) 0.047(3) -0.003(3) 0.029(2) 0.001(3) C28 0.049(3) 0.073(3) 0.067(3) -0.002(3) 0.041(2) 0.003(2) C29 0.052(3) 0.098(4) 0.063(3) -0.003(3) 0.038(3) 0.001(3) C30 0.060(3) 0.108(5) 0.066(3) -0.002(3) 0.048(3) 0.016(3) C31 0.082(4) 0.080(4) 0.052(3) -0.009(3) 0.043(3) 0.002(3) C32 0.063(3) 0.080(4) 0.062(3) -0.014(3) 0.045(3) -0.013(3) C33 0.067(3) 0.046(3) 0.047(3) 0.002(2) 0.035(2) -0.001(2) C34 0.081(4) 0.041(3) 0.051(3) -0.004(2) 0.033(3) 0.009(2) C35 0.140(6) 0.045(3) 0.062(3) -0.004(2) 0.064(4) -0.019(3) C36 0.058(3) 0.046(2) 0.065(3) 0.001(2) 0.043(3) -0.001(2) C37 0.082(4) 0.059(3) 0.057(3) -0.008(2) 0.051(3) -0.010(3) C38 0.071(3) 0.045(2) 0.069(3) -0.001(2) 0.053(3) -0.005(2) B1 0.111(6) 0.063(4) 0.064(4) 0.003(3) 0.041(4) -0.028(4) F1 0.152(4) 0.157(5) 0.092(3) 0.033(3) 0.039(3) -0.033(4) F2 0.170(5) 0.149(4) 0.177(6) 0.052(4) 0.086(4) 0.033(4) F3 0.402(12) 0.259(8) 0.116(4) 0.001(5) 0.051(6) -0.245(9) F4 0.319(9) 0.183(6) 0.214(7) 0.016(5) 0.214(7) -0.014(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C20 1.373(6) . ? O1 C19 1.422(6) . ? O2 C27 1.370(6) . ? O2 C26 1.453(6) . ? O3 C18 1.376(5) . ? O3 C33 1.428(5) . ? O4 C35 1.323(7) . ? O4 C34 1.430(6) . ? O5 C36 1.385(6) . ? O5 C37 1.448(6) . ? O6 C13 1.362(5) . ? O6 C38 1.474(5) . ? N1 C10 1.333(5) . ? N1 C9 1.338(6) . ? N1 C12 1.488(5) . ? C1 C6 1.400(8) . ? C1 C2 1.435(8) . ? C1 H1A 0.9500 . ? C2 C3 1.293(9) . ? C2 H2A 0.9500 . ? C3 C4 1.283(10) . ? C4 C5 1.430(10) . ? C4 H4A 0.9500 . ? C5 C6 1.352(8) . ? C5 H5A 0.9500 . ? C6 C7 1.475(6) . ? C7 C11 1.371(7) . ? C7 C8 1.392(7) . ? C8 C9 1.378(7) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 C11 1.377(6) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C12 1.477(9) 7_556 ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.376(6) . ? C13 C18 1.398(6) . ? C14 C15 1.365(7) . ? C14 H14A 0.9500 . ? C15 C16 1.375(7) . ? C15 C19 1.515(7) . ? C16 C17 1.399(7) . ? C16 C26 1.513(7) . ? C17 C18 1.390(6) . ? C17 H17A 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C25 1.367(8) . ? C20 C21 1.398(7) . ? C21 C22 1.389(7) . ? C21 H21A 0.9500 . ? C22 C23 1.343(9) . ? C22 H22A 0.9500 . ? C23 C24 1.391(10) . ? C23 H23A 0.9500 . ? C24 C25 1.385(9) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.366(7) . ? C27 C28 1.381(7) . ? C28 C29 1.390(7) . ? C28 H28A 0.9500 . ? C29 C30 1.343(8) . ? C29 H29A 0.9500 . ? C30 C31 1.370(8) . ? C30 H30A 0.9500 . ? C31 C32 1.386(7) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.509(7) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.499(7) 7_565 ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C35 1.499(7) 7_565 ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.493(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? B1 F1 1.263(7) . ? B1 F3 1.292(8) . ? B1 F4 1.349(8) . ? B1 F2 1.397(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 C20 O1 C19 116.5(4) . . ? C27 O2 C26 118.9(4) . . ? C18 O3 C33 115.8(3) . . ? C35 O4 C34 114.1(4) . . ? C36 O5 C37 113.9(4) . . ? C13 O6 C38 115.8(3) . . ? C10 N1 C9 119.9(4) . . ? C10 N1 C12 121.2(4) . . ? C9 N1 C12 119.0(4) . . ? C6 C1 C2 116.4(6) . . ? C6 C1 H1A 121.8 . . ? C2 C1 H1A 121.8 . . ? C3 C2 C1 125.0(6) . . ? C3 C2 H2A 117.5 . . ? C1 C2 H2A 117.5 . . ? C4 C3 C2 117.4(6) . . ? C3 C4 C5 123.2(8) . . ? C3 C4 H4A 118.4 . . ? C5 C4 H4A 118.4 . . ? C6 C5 C4 119.4(7) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C1 117.7(5) . . ? C5 C6 C7 121.8(5) . . ? C1 C6 C7 120.2(5) . . ? C11 C7 C8 116.9(4) . . ? C11 C7 C6 124.0(4) . . ? C8 C7 C6 119.0(4) . . ? C9 C8 C7 119.6(5) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? N1 C9 C8 121.7(4) . . ? N1 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? N1 C10 C11 120.2(4) . . ? N1 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C7 C11 C10 121.7(4) . . ? C7 C11 H11A 119.2 . . ? C10 C11 H11A 119.2 . . ? C12 C12 N1 109.3(4) 7_556 . ? C12 C12 H12A 109.8 7_556 . ? N1 C12 H12A 109.8 . . ? C12 C12 H12B 109.8 7_556 . ? N1 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? O6 C13 C14 125.6(4) . . ? O6 C13 C18 115.8(4) . . ? C14 C13 C18 118.6(4) . . ? C15 C14 C13 122.6(4) . . ? C15 C14 H14A 118.7 . . ? C13 C14 H14A 118.7 . . ? C14 C15 C16 119.6(4) . . ? C14 C15 C19 118.4(4) . . ? C16 C15 C19 122.1(4) . . ? C15 C16 C17 119.3(4) . . ? C15 C16 C26 124.2(4) . . ? C17 C16 C26 116.4(4) . . ? C18 C17 C16 120.7(4) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? O3 C18 C17 124.4(4) . . ? O3 C18 C13 116.5(3) . . ? C17 C18 C13 119.1(4) . . ? O1 C19 C15 108.9(4) . . ? O1 C19 H19A 109.9 . . ? C15 C19 H19A 109.9 . . ? O1 C19 H19B 109.9 . . ? C15 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C25 C20 O1 125.0(5) . . ? C25 C20 C21 120.6(5) . . ? O1 C20 C21 114.2(4) . . ? C22 C21 C20 118.8(5) . . ? C22 C21 H21A 120.6 . . ? C20 C21 H21A 120.6 . . ? C23 C22 C21 121.1(6) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 119.8(6) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C20 C25 C24 119.0(6) . . ? C20 C25 H25A 120.5 . . ? C24 C25 H25A 120.5 . . ? O2 C26 C16 105.9(4) . . ? O2 C26 H26A 110.6 . . ? C16 C26 H26A 110.6 . . ? O2 C26 H26B 110.6 . . ? C16 C26 H26B 110.6 . . ? H26A C26 H26B 108.7 . . ? C32 C27 O2 115.5(5) . . ? C32 C27 C28 121.4(5) . . ? O2 C27 C28 123.1(5) . . ? C27 C28 C29 117.6(5) . . ? C27 C28 H28A 121.2 . . ? C29 C28 H28A 121.2 . . ? C30 C29 C28 122.1(5) . . ? C30 C29 H29A 119.0 . . ? C28 C29 H29A 119.0 . . ? C29 C30 C31 119.2(5) . . ? C29 C30 H30A 120.4 . . ? C31 C30 H30A 120.4 . . ? C30 C31 C32 120.9(5) . . ? C30 C31 H31A 119.5 . . ? C32 C31 H31A 119.5 . . ? C27 C32 C31 118.7(5) . . ? C27 C32 H32A 120.7 . . ? C31 C32 H32A 120.7 . . ? O3 C33 C34 108.3(4) . . ? O3 C33 H33A 110.0 . . ? C34 C33 H33A 110.0 . . ? O3 C33 H33B 110.0 . . ? C34 C33 H33B 110.0 . . ? H33A C33 H33B 108.4 . . ? O4 C34 C33 107.0(4) . . ? O4 C34 H34A 110.3 . . ? C33 C34 H34A 110.3 . . ? O4 C34 H34B 110.3 . . ? C33 C34 H34B 110.3 . . ? H34A C34 H34B 108.6 . . ? O4 C35 C36 113.2(5) . 7_565 ? O4 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 7_565 . ? O4 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 7_565 . ? H35A C35 H35B 107.8 . . ? O5 C36 C35 112.2(4) . 7_565 ? O5 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 7_565 . ? O5 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 7_565 . ? H36A C36 H36B 107.9 . . ? O5 C37 C38 110.0(4) . . ? O5 C37 H37A 109.7 . . ? C38 C37 H37A 109.7 . . ? O5 C37 H37B 109.7 . . ? C38 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? O6 C38 C37 105.5(4) . . ? O6 C38 H38A 110.6 . . ? C37 C38 H38A 110.6 . . ? O6 C38 H38B 110.6 . . ? C37 C38 H38B 110.6 . . ? H38A C38 H38B 108.8 . . ? F1 B1 F3 113.1(6) . . ? F1 B1 F4 114.8(7) . . ? F3 B1 F4 116.2(7) . . ? F1 B1 F2 105.0(6) . . ? F3 B1 F2 108.6(8) . . ? F4 B1 F2 97.0(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.879 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.115 # Attachment '- DM81.cif' data_dm81 _database_code_depnum_ccdc_archive 'CCDC 864512' #TrackingRef '- DM81.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H57 Cl3 O12' _chemical_formula_weight 992.34 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 12.554(4) _cell_length_b 13.774(5) _cell_length_c 15.329(5) _cell_angle_alpha 80.404(5) _cell_angle_beta 68.495(4) _cell_angle_gamma 89.969(5) _cell_volume 2426.4(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 286 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6547 _exptl_absorpt_correction_T_max 0.8621 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22005 _diffrn_reflns_av_R_equivalents 0.0850 _diffrn_reflns_av_sigmaI/netI 0.1182 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8433 _reflns_number_gt 4246 _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. The unit cell contains 2 molecules of chloroform. Attempts to model these solvent molecules did not give satisfactory residuals or chemcially reasonable bond parameters. The 2 molecules of chloroform were then treated as a diffuse contributions to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.070 0.000 0.500 321 125 ' ' _platon_squeeze_details ; ; _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 8433 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2106 _refine_ls_R_factor_gt 0.1434 _refine_ls_wR_factor_ref 0.3936 _refine_ls_wR_factor_gt 0.3560 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.165 _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 O101 O 1.2539(4) 0.4526(4) -0.3609(3) 0.0571(15) Uani 1 1 d . . . O102 O 1.3177(4) 0.6560(3) -0.1775(3) 0.0430(12) Uani 1 1 d . . . O103 O 0.8430(3) 0.6123(3) -0.0630(3) 0.0376(11) Uani 1 1 d . . . O104 O 0.6456(3) 0.6620(3) 0.0967(3) 0.0410(12) Uani 1 1 d . . . O105 O 0.3436(3) 0.6214(3) 0.1864(3) 0.0405(11) Uani 1 1 d . . . O106 O 0.1532(3) 0.4959(3) 0.1882(3) 0.0388(11) Uani 1 1 d . . . C101 C 0.9464(5) 0.5189(4) -0.1763(4) 0.0284(14) Uani 1 1 d . . . C102 C 1.0500(6) 0.4821(5) -0.2274(5) 0.0375(16) Uani 1 1 d . . . H10A H 1.0519 0.4432 -0.2735 0.045 Uiso 1 1 calc R . . C103 C 1.1516(5) 0.5008(4) -0.2128(4) 0.0327(15) Uani 1 1 d . . . C104 C 1.1457(5) 0.5540(4) -0.1437(5) 0.0320(15) Uani 1 1 d . . . C105 C 1.0442(5) 0.5924(5) -0.0914(5) 0.0385(16) Uani 1 1 d . . . H10B H 1.0423 0.6294 -0.0439 0.046 Uiso 1 1 calc R . . C106 C 0.9469(5) 0.5762(4) -0.1093(4) 0.0302(14) Uani 1 1 d . . . C107 C 1.2602(6) 0.4635(6) -0.2719(5) 0.0440(17) Uani 1 1 d . . . H10C H 1.3255 0.5103 -0.2829 0.053 Uiso 1 1 calc R . . H10D H 1.2725 0.3990 -0.2386 0.053 Uiso 1 1 calc R . . C108 C 1.3432(6) 0.4165(5) -0.4254(5) 0.0478(18) Uani 1 1 d . . . C109 C 1.4381(7) 0.3847(6) -0.4078(6) 0.060(2) Uani 1 1 d . . . H10E H 1.4453 0.3879 -0.3487 0.072 Uiso 1 1 calc R . . C110 C 1.5229(8) 0.3478(8) -0.4787(8) 0.086(3) Uani 1 1 d . . . H11A H 1.5907 0.3270 -0.4693 0.103 Uiso 1 1 calc R . . C111 C 1.5100(10) 0.3407(8) -0.5648(7) 0.084(3) Uani 1 1 d . . . H11B H 1.5680 0.3136 -0.6124 0.100 Uiso 1 1 calc R . . C112 C 1.4148(9) 0.3725(8) -0.5801(7) 0.081(3) Uani 1 1 d . . . H11C H 1.4057 0.3680 -0.6382 0.097 Uiso 1 1 calc R . . C113 C 1.3321(7) 0.4110(7) -0.5105(6) 0.064(2) Uani 1 1 d . . . H11D H 1.2659 0.4345 -0.5212 0.077 Uiso 1 1 calc R . . C114 C 1.2492(5) 0.5691(4) -0.1171(5) 0.0380(16) Uani 1 1 d . . . H11E H 1.2233 0.5769 -0.0495 0.046 Uiso 1 1 calc R . . H11F H 1.2956 0.5108 -0.1250 0.046 Uiso 1 1 calc R . . C115 C 1.4251(5) 0.6700(5) -0.1770(5) 0.0357(15) Uani 1 1 d . . . C116 C 1.4855(7) 0.7571(6) -0.2326(5) 0.056(2) Uani 1 1 d . . . H11G H 1.4508 0.8030 -0.2658 0.067 Uiso 1 1 calc R . . C117 C 1.5936(8) 0.7759(8) -0.2390(7) 0.074(3) Uani 1 1 d . . . H11H H 1.6343 0.8359 -0.2766 0.089 Uiso 1 1 calc R . . C118 C 1.6458(7) 0.7119(8) -0.1937(6) 0.062(2) Uani 1 1 d . . . H11I H 1.7237 0.7253 -0.2025 0.075 Uiso 1 1 calc R . . C119 C 1.5871(7) 0.6280(7) -0.1354(6) 0.066(3) Uani 1 1 d . . . H11J H 1.6231 0.5847 -0.1013 0.079 Uiso 1 1 calc R . . C120 C 1.4703(6) 0.6040(5) -0.1247(5) 0.0430(18) Uani 1 1 d . . . H12A H 1.4275 0.5461 -0.0840 0.052 Uiso 1 1 calc R . . C121 C 0.8450(5) 0.6820(4) -0.0028(5) 0.0347(15) Uani 1 1 d . . . H12B H 0.9084 0.7332 -0.0375 0.042 Uiso 1 1 calc R . . H12C H 0.8565 0.6478 0.0548 0.042 Uiso 1 1 calc R . . C122 C 0.7306(5) 0.7286(4) 0.0247(4) 0.0331(15) Uani 1 1 d . . . H12D H 0.7367 0.7903 0.0481 0.040 Uiso 1 1 calc R . . H12E H 0.7090 0.7452 -0.0318 0.040 Uiso 1 1 calc R . . C123 C 0.5345(5) 0.6863(5) 0.1057(4) 0.0336(15) Uani 1 1 d . . . H12F H 0.5183 0.6715 0.0506 0.040 Uiso 1 1 calc R . . H12G H 0.5272 0.7577 0.1067 0.040 Uiso 1 1 calc R . . C124 C 0.4504(6) 0.6274(5) 0.1965(5) 0.0403(17) Uani 1 1 d . . . H12H H 0.4766 0.5605 0.2084 0.048 Uiso 1 1 calc R . . H12I H 0.4436 0.6601 0.2510 0.048 Uiso 1 1 calc R . . C125 C 0.2624(5) 0.5611(6) 0.2671(5) 0.0482(19) Uani 1 1 d . . . H12J H 0.2553 0.5874 0.3251 0.058 Uiso 1 1 calc R . . H12K H 0.2889 0.4935 0.2737 0.058 Uiso 1 1 calc R . . C126 C 0.1480(5) 0.5576(5) 0.2578(5) 0.0401(16) Uani 1 1 d . . . H12L H 0.0877 0.5298 0.3202 0.048 Uiso 1 1 calc R . . H12M H 0.1290 0.6250 0.2367 0.048 Uiso 1 1 calc R . . O201 O 1.7566(4) 1.1887(4) -0.3551(4) 0.0672(17) Uani 1 1 d . . . O202 O 1.8182(4) 0.9127(3) -0.1790(3) 0.0428(12) Uani 1 1 d . . . O203 O 1.3404(3) 0.9106(3) -0.0622(3) 0.0373(11) Uani 1 1 d . . . O204 O 1.1430(3) 0.8036(3) 0.0962(3) 0.0383(11) Uani 1 1 d . . . O205 O 0.8407(4) 0.8120(3) 0.1885(3) 0.0424(12) Uani 1 1 d . . . O206 O 0.6515(4) 0.9377(3) 0.1925(3) 0.0446(12) Uani 1 1 d . . . C201 C 1.4484(5) 1.0428(5) -0.1795(4) 0.0316(14) Uani 1 1 d . . . C202 C 1.5513(6) 1.0988(5) -0.2324(5) 0.0406(16) Uani 1 1 d . . . H20A H 1.5547 1.1532 -0.2807 0.049 Uiso 1 1 calc R . . C203 C 1.6496(5) 1.0736(5) -0.2130(5) 0.0344(15) Uani 1 1 d . . . C204 C 1.6461(5) 0.9985(4) -0.1431(5) 0.0338(15) Uani 1 1 d . . . C205 C 1.5436(5) 0.9430(5) -0.0910(4) 0.0342(15) Uani 1 1 d . . . H20B H 1.5410 0.8896 -0.0421 0.041 Uiso 1 1 calc R . . C206 C 1.4465(5) 0.9636(4) -0.1088(4) 0.0260(13) Uani 1 1 d . . . C207 C 1.7612(6) 1.1323(6) -0.2740(5) 0.0501(19) Uani 1 1 d . . . H20C H 1.7808 1.1760 -0.2362 0.060 Uiso 1 1 calc R . . H20D H 1.8230 1.0864 -0.2922 0.060 Uiso 1 1 calc R . . C208 C 1.8530(5) 1.2396(5) -0.4198(4) 0.066(2) Uani 1 1 d G . . C209 C 1.9575(6) 1.2393(6) -0.4078(5) 0.099(4) Uani 1 1 d G . . H20E H 1.9623 1.2062 -0.3499 0.119 Uiso 1 1 calc R . . C210 C 2.0550(5) 1.2874(8) -0.4805(6) 0.213(11) Uani 1 1 d G . . H21A H 2.1264 1.2871 -0.4723 0.255 Uiso 1 1 calc R . . C211 C 2.0479(6) 1.3358(7) -0.5651(5) 0.213(11) Uani 1 1 d G . . H21B H 2.1145 1.3686 -0.6148 0.255 Uiso 1 1 calc R . . C212 C 1.9434(8) 1.3361(6) -0.5772(4) 0.132(6) Uani 1 1 d G . . H21C H 1.9386 1.3692 -0.6350 0.158 Uiso 1 1 calc R . . C213 C 1.8459(6) 1.2880(6) -0.5045(5) 0.100(4) Uani 1 1 d G . . H21D H 1.7745 1.2882 -0.5127 0.120 Uiso 1 1 calc R . . C214 C 1.7475(5) 0.9750(5) -0.1155(5) 0.0378(16) Uani 1 1 d . . . H21E H 1.7922 1.0366 -0.1214 0.045 Uiso 1 1 calc R . . H21F H 1.7215 0.9402 -0.0485 0.045 Uiso 1 1 calc R . . C215 C 1.9243(6) 0.8986(5) -0.1776(5) 0.0430(17) Uani 1 1 d . . . C216 C 1.9882(7) 0.8374(6) -0.2395(6) 0.060(2) Uani 1 1 d . . . H21G H 1.9566 0.8085 -0.2774 0.072 Uiso 1 1 calc R . . C217 C 2.0967(8) 0.8205(7) -0.2439(7) 0.077(3) Uani 1 1 d . . . H21H H 2.1392 0.7789 -0.2861 0.093 Uiso 1 1 calc R . . C218 C 2.1484(6) 0.8582(7) -0.1931(6) 0.062(2) Uani 1 1 d . . . H21I H 2.2239 0.8430 -0.1979 0.074 Uiso 1 1 calc R . . C219 C 2.0843(7) 0.9224(6) -0.1315(6) 0.065(3) Uani 1 1 d . . . H21J H 2.1188 0.9531 -0.0964 0.078 Uiso 1 1 calc R . . C220 C 1.9705(6) 0.9407(5) -0.1221(5) 0.0440(18) Uani 1 1 d . . . H22A H 1.9265 0.9808 -0.0788 0.053 Uiso 1 1 calc R . . C221 C 1.3413(5) 0.8186(4) -0.0029(5) 0.0364(15) Uani 1 1 d . . . H22B H 1.3541 0.8308 0.0545 0.044 Uiso 1 1 calc R . . H22C H 1.4040 0.7799 -0.0382 0.044 Uiso 1 1 calc R . . C222 C 1.2278(5) 0.7626(5) 0.0256(5) 0.0387(16) Uani 1 1 d . . . H22D H 1.2063 0.7654 -0.0307 0.046 Uiso 1 1 calc R . . H22E H 1.2338 0.6925 0.0505 0.046 Uiso 1 1 calc R . . C223 C 1.0312(5) 0.7759(5) 0.1070(5) 0.0382(16) Uani 1 1 d . . . H22F H 1.0234 0.7039 0.1091 0.046 Uiso 1 1 calc R . . H22G H 1.0141 0.8103 0.0520 0.046 Uiso 1 1 calc R . . C224 C 0.9494(5) 0.8019(5) 0.1962(5) 0.0404(17) Uani 1 1 d . . . H22H H 0.9434 0.7497 0.2510 0.049 Uiso 1 1 calc R . . H22I H 0.9767 0.8647 0.2070 0.049 Uiso 1 1 calc R . . C225 C 0.7612(5) 0.8467(6) 0.2713(5) 0.0464(18) Uani 1 1 d . . . H22J H 0.7892 0.9127 0.2746 0.056 Uiso 1 1 calc R . . H22K H 0.7554 0.8008 0.3301 0.056 Uiso 1 1 calc R . . C226 C 0.6470(6) 0.8523(5) 0.2633(5) 0.0461(18) Uani 1 1 d . . . H22L H 0.6275 0.7917 0.2440 0.055 Uiso 1 1 calc R . . H22M H 0.5875 0.8584 0.3255 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O101 0.040(3) 0.096(4) 0.039(3) -0.026(3) -0.013(2) 0.018(3) O102 0.034(3) 0.053(3) 0.045(3) -0.011(2) -0.017(2) 0.008(2) O103 0.029(2) 0.040(3) 0.046(3) -0.013(2) -0.015(2) 0.004(2) O104 0.026(2) 0.044(3) 0.053(3) -0.007(2) -0.015(2) 0.007(2) O105 0.023(2) 0.056(3) 0.041(3) -0.003(2) -0.013(2) -0.003(2) O106 0.025(2) 0.051(3) 0.043(3) -0.018(2) -0.012(2) -0.006(2) C101 0.027(3) 0.028(3) 0.026(3) -0.003(3) -0.006(3) 0.001(3) C102 0.044(4) 0.039(4) 0.032(4) -0.006(3) -0.016(3) -0.005(3) C103 0.024(3) 0.032(3) 0.037(4) -0.005(3) -0.006(3) 0.006(3) C104 0.029(3) 0.024(3) 0.046(4) -0.007(3) -0.016(3) 0.000(3) C105 0.032(4) 0.040(4) 0.046(4) -0.014(3) -0.014(3) 0.004(3) C106 0.028(3) 0.024(3) 0.034(4) 0.002(3) -0.009(3) 0.003(3) C107 0.041(4) 0.060(5) 0.031(4) -0.005(3) -0.015(3) 0.008(3) C108 0.042(4) 0.052(4) 0.051(5) -0.017(4) -0.016(4) 0.010(3) C109 0.053(5) 0.078(6) 0.048(5) -0.015(4) -0.014(4) 0.021(4) C110 0.057(6) 0.096(8) 0.105(8) -0.018(7) -0.031(6) 0.031(5) C111 0.101(8) 0.093(7) 0.057(6) -0.038(6) -0.019(6) 0.023(6) C112 0.079(7) 0.100(8) 0.072(7) -0.045(6) -0.027(6) 0.020(6) C113 0.058(5) 0.084(6) 0.054(5) -0.027(5) -0.019(4) 0.012(5) C114 0.030(4) 0.025(3) 0.059(5) -0.005(3) -0.017(3) -0.001(3) C115 0.030(4) 0.041(4) 0.036(4) -0.019(3) -0.007(3) 0.002(3) C116 0.047(5) 0.069(5) 0.044(5) -0.018(4) -0.003(4) -0.016(4) C117 0.054(6) 0.102(8) 0.058(6) -0.043(5) 0.000(5) -0.012(5) C118 0.025(4) 0.103(7) 0.064(6) -0.037(5) -0.014(4) 0.000(5) C119 0.050(5) 0.097(7) 0.072(6) -0.056(6) -0.030(5) 0.029(5) C120 0.038(4) 0.050(4) 0.061(5) -0.034(4) -0.031(4) 0.019(3) C121 0.030(3) 0.027(3) 0.050(4) -0.011(3) -0.016(3) 0.001(3) C122 0.044(4) 0.024(3) 0.033(4) -0.005(3) -0.015(3) 0.005(3) C123 0.021(3) 0.042(4) 0.036(4) -0.009(3) -0.008(3) 0.005(3) C124 0.047(4) 0.036(4) 0.055(5) -0.021(3) -0.033(4) 0.014(3) C125 0.026(4) 0.069(5) 0.053(5) -0.020(4) -0.015(3) 0.002(3) C126 0.036(4) 0.052(4) 0.034(4) -0.011(3) -0.013(3) -0.004(3) O201 0.048(3) 0.081(4) 0.061(4) 0.022(3) -0.021(3) -0.009(3) O202 0.028(3) 0.054(3) 0.051(3) -0.020(2) -0.015(2) 0.005(2) O203 0.028(2) 0.038(3) 0.044(3) -0.007(2) -0.013(2) 0.0009(19) O204 0.025(2) 0.045(3) 0.043(3) -0.007(2) -0.011(2) -0.003(2) O205 0.025(2) 0.053(3) 0.048(3) -0.001(2) -0.016(2) 0.003(2) O206 0.030(3) 0.049(3) 0.052(3) 0.001(2) -0.017(2) 0.010(2) C201 0.028(3) 0.038(4) 0.031(3) -0.011(3) -0.011(3) 0.005(3) C202 0.041(4) 0.039(4) 0.048(4) -0.006(3) -0.024(3) 0.003(3) C203 0.026(3) 0.044(4) 0.033(4) -0.013(3) -0.007(3) 0.004(3) C204 0.025(3) 0.032(3) 0.050(4) -0.018(3) -0.015(3) 0.004(3) C205 0.038(4) 0.030(3) 0.031(4) -0.008(3) -0.009(3) 0.000(3) C206 0.029(3) 0.027(3) 0.024(3) -0.011(3) -0.009(3) 0.005(3) C207 0.032(4) 0.073(5) 0.040(4) -0.001(4) -0.010(3) 0.005(4) C208 0.060(6) 0.056(5) 0.075(6) 0.005(5) -0.026(5) -0.008(4) C209 0.069(7) 0.149(11) 0.066(7) 0.031(7) -0.030(5) -0.030(7) C210 0.136(12) 0.223(18) 0.27(2) 0.155(17) -0.148(14) -0.138(13) C211 0.26(2) 0.173(15) 0.24(2) 0.109(14) -0.197(18) -0.160(15) C212 0.209(15) 0.110(9) 0.063(7) 0.051(7) -0.064(9) -0.082(10) C213 0.086(8) 0.132(10) 0.065(7) 0.008(7) -0.021(6) 0.015(7) C214 0.032(4) 0.031(3) 0.048(4) -0.010(3) -0.010(3) 0.002(3) C215 0.036(4) 0.040(4) 0.038(4) 0.016(3) -0.006(3) -0.001(3) C216 0.049(5) 0.064(5) 0.068(6) -0.020(4) -0.019(4) 0.023(4) C217 0.052(6) 0.089(7) 0.078(7) 0.003(6) -0.016(5) 0.021(5) C218 0.023(4) 0.103(7) 0.054(5) 0.000(5) -0.013(4) 0.010(4) C219 0.050(5) 0.070(6) 0.070(6) 0.026(5) -0.032(5) -0.012(4) C220 0.037(4) 0.035(4) 0.057(5) 0.008(3) -0.021(4) -0.007(3) C221 0.042(4) 0.027(3) 0.043(4) -0.008(3) -0.018(3) 0.010(3) C222 0.042(4) 0.032(3) 0.048(4) -0.011(3) -0.022(3) 0.009(3) C223 0.044(4) 0.033(3) 0.035(4) 0.003(3) -0.015(3) 0.005(3) C224 0.029(4) 0.043(4) 0.049(4) 0.004(3) -0.018(3) -0.002(3) C225 0.029(4) 0.067(5) 0.041(4) 0.001(4) -0.016(3) 0.000(3) C226 0.039(4) 0.048(4) 0.048(4) 0.007(3) -0.020(3) 0.001(3) _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 O101 C108 1.354(8) . ? O101 C107 1.427(8) . ? O102 C115 1.366(7) . ? O102 C114 1.442(7) . ? O103 C106 1.375(7) . ? O103 C121 1.443(7) . ? O104 C123 1.396(7) . ? O104 C122 1.413(7) . ? O105 C124 1.409(7) . ? O105 C125 1.412(8) . ? O106 C101 1.348(7) 2_665 ? O106 C126 1.455(7) . ? C101 O106 1.348(7) 2_665 ? C101 C102 1.395(9) . ? C101 C106 1.398(9) . ? C102 C103 1.404(8) . ? C102 H10A 0.9500 . ? C103 C104 1.366(9) . ? C103 C107 1.481(9) . ? C104 C105 1.392(8) . ? C104 C114 1.522(8) . ? C105 C106 1.372(9) . ? C105 H10B 0.9500 . ? C107 H10C 0.9900 . ? C107 H10D 0.9900 . ? C108 C109 1.371(10) . ? C108 C113 1.376(11) . ? C109 C110 1.382(12) . ? C109 H10E 0.9500 . ? C110 C111 1.406(14) . ? C110 H11A 0.9500 . ? C111 C112 1.358(13) . ? C111 H11B 0.9500 . ? C112 C113 1.369(11) . ? C112 H11C 0.9500 . ? C113 H11D 0.9500 . ? C114 H11E 0.9900 . ? C114 H11F 0.9900 . ? C115 C120 1.371(9) . ? C115 C116 1.388(10) . ? C116 C117 1.347(11) . ? C116 H11G 0.9500 . ? C117 C118 1.349(13) . ? C117 H11H 0.9500 . ? C118 C119 1.360(13) . ? C118 H11I 0.9500 . ? C119 C120 1.446(10) . ? C119 H11J 0.9500 . ? C120 H12A 0.9500 . ? C121 C122 1.516(8) . ? C121 H12B 0.9900 . ? C121 H12C 0.9900 . ? C122 H12D 0.9900 . ? C122 H12E 0.9900 . ? C123 C124 1.503(9) . ? C123 H12F 0.9900 . ? C123 H12G 0.9900 . ? C124 H12H 0.9900 . ? C124 H12I 0.9900 . ? C125 C126 1.496(9) . ? C125 H12J 0.9900 . ? C125 H12K 0.9900 . ? C126 H12L 0.9900 . ? C126 H12M 0.9900 . ? O201 C208 1.353(7) . ? O201 C207 1.371(8) . ? O202 C215 1.354(8) . ? O202 C214 1.454(7) . ? O203 C206 1.395(7) . ? O203 C221 1.433(7) . ? O204 C223 1.397(7) . ? O204 C222 1.408(8) . ? O205 C224 1.417(7) . ? O205 C225 1.452(8) . ? O206 C201 1.360(7) 2_775 ? O206 C226 1.446(8) . ? C201 O206 1.360(7) 2_775 ? C201 C202 1.395(9) . ? C201 C206 1.397(8) . ? C202 C203 1.403(9) . ? C202 H20A 0.9500 . ? C203 C204 1.348(9) . ? C203 C207 1.510(9) . ? C204 C205 1.386(8) . ? C204 C214 1.502(9) . ? C205 C206 1.364(8) . ? C205 H20B 0.9500 . ? C207 H20C 0.9900 . ? C207 H20D 0.9900 . ? C208 C209 1.3900 . ? C208 C213 1.3900 . ? C209 C210 1.3900 . ? C209 H20E 0.9500 . ? C210 C211 1.3900 . ? C210 H21A 0.9500 . ? C211 C212 1.3900 . ? C211 H21B 0.9500 . ? C212 C213 1.3900 . ? C212 H21C 0.9500 . ? C213 H21D 0.9500 . ? C214 H21E 0.9900 . ? C214 H21F 0.9900 . ? C215 C220 1.388(10) . ? C215 C216 1.400(10) . ? C216 C217 1.361(11) . ? C216 H21G 0.9500 . ? C217 C218 1.343(13) . ? C217 H21H 0.9500 . ? C218 C219 1.428(12) . ? C218 H21I 0.9500 . ? C219 C220 1.410(10) . ? C219 H21J 0.9500 . ? C220 H22A 0.9500 . ? C221 C222 1.499(9) . ? C221 H22B 0.9900 . ? C221 H22C 0.9900 . ? C222 H22D 0.9900 . ? C222 H22E 0.9900 . ? C223 C224 1.479(9) . ? C223 H22F 0.9900 . ? C223 H22G 0.9900 . ? C224 H22H 0.9900 . ? C224 H22I 0.9900 . ? C225 C226 1.484(9) . ? C225 H22J 0.9900 . ? C225 H22K 0.9900 . ? C226 H22L 0.9900 . ? C226 H22M 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C108 O101 C107 119.1(5) . . ? C115 O102 C114 117.2(5) . . ? C106 O103 C121 115.5(5) . . ? C123 O104 C122 112.5(5) . . ? C124 O105 C125 110.6(5) . . ? C101 O106 C126 115.1(5) 2_665 . ? O106 C101 C102 124.6(6) 2_665 . ? O106 C101 C106 118.0(5) 2_665 . ? C102 C101 C106 117.4(6) . . ? C103 C102 C101 122.2(6) . . ? C103 C102 H10A 118.9 . . ? C101 C102 H10A 118.9 . . ? C104 C103 C102 117.7(6) . . ? C104 C103 C107 122.4(6) . . ? C102 C103 C107 119.8(6) . . ? C103 C104 C105 121.9(6) . . ? C103 C104 C114 120.9(6) . . ? C105 C104 C114 117.1(6) . . ? C106 C105 C104 119.3(6) . . ? C106 C105 H10B 120.4 . . ? C104 C105 H10B 120.4 . . ? O103 C106 C105 123.9(6) . . ? O103 C106 C101 114.7(5) . . ? C105 C106 C101 121.4(6) . . ? O101 C107 C103 109.0(5) . . ? O101 C107 H10C 109.9 . . ? C103 C107 H10C 109.9 . . ? O101 C107 H10D 109.9 . . ? C103 C107 H10D 109.9 . . ? H10C C107 H10D 108.3 . . ? O101 C108 C109 123.2(7) . . ? O101 C108 C113 115.6(7) . . ? C109 C108 C113 121.2(7) . . ? C108 C109 C110 117.9(8) . . ? C108 C109 H10E 121.1 . . ? C110 C109 H10E 121.1 . . ? C109 C110 C111 120.6(9) . . ? C109 C110 H11A 119.7 . . ? C111 C110 H11A 119.7 . . ? C112 C111 C110 120.2(9) . . ? C112 C111 H11B 119.9 . . ? C110 C111 H11B 119.9 . . ? C113 C112 C111 119.0(9) . . ? C113 C112 H11C 120.5 . . ? C111 C112 H11C 120.5 . . ? C112 C113 C108 121.1(8) . . ? C112 C113 H11D 119.4 . . ? C108 C113 H11D 119.4 . . ? O102 C114 C104 109.3(5) . . ? O102 C114 H11E 109.8 . . ? C104 C114 H11E 109.8 . . ? O102 C114 H11F 109.8 . . ? C104 C114 H11F 109.8 . . ? H11E C114 H11F 108.3 . . ? O102 C115 C120 123.0(6) . . ? O102 C115 C116 115.0(6) . . ? C120 C115 C116 122.0(7) . . ? C117 C116 C115 119.3(9) . . ? C117 C116 H11G 120.3 . . ? C115 C116 H11G 120.3 . . ? C116 C117 C118 121.9(10) . . ? C116 C117 H11H 119.1 . . ? C118 C117 H11H 119.0 . . ? C117 C118 C119 120.0(8) . . ? C117 C118 H11I 120.0 . . ? C119 C118 H11I 120.0 . . ? C118 C119 C120 120.7(8) . . ? C118 C119 H11J 119.6 . . ? C120 C119 H11J 119.6 . . ? C115 C120 C119 115.8(7) . . ? C115 C120 H12A 122.1 . . ? C119 C120 H12A 122.1 . . ? O103 C121 C122 107.4(5) . . ? O103 C121 H12B 110.2 . . ? C122 C121 H12B 110.2 . . ? O103 C121 H12C 110.2 . . ? C122 C121 H12C 110.2 . . ? H12B C121 H12C 108.5 . . ? O104 C122 C121 109.5(5) . . ? O104 C122 H12D 109.8 . . ? C121 C122 H12D 109.8 . . ? O104 C122 H12E 109.8 . . ? C121 C122 H12E 109.8 . . ? H12D C122 H12E 108.2 . . ? O104 C123 C124 109.2(5) . . ? O104 C123 H12F 109.8 . . ? C124 C123 H12F 109.8 . . ? O104 C123 H12G 109.8 . . ? C124 C123 H12G 109.8 . . ? H12F C123 H12G 108.3 . . ? O105 C124 C123 107.8(5) . . ? O105 C124 H12H 110.2 . . ? C123 C124 H12H 110.2 . . ? O105 C124 H12I 110.2 . . ? C123 C124 H12I 110.2 . . ? H12H C124 H12I 108.5 . . ? O105 C125 C126 110.5(6) . . ? O105 C125 H12J 109.5 . . ? C126 C125 H12J 109.5 . . ? O105 C125 H12K 109.5 . . ? C126 C125 H12K 109.5 . . ? H12J C125 H12K 108.1 . . ? O106 C126 C125 108.4(5) . . ? O106 C126 H12L 110.0 . . ? C125 C126 H12L 110.0 . . ? O106 C126 H12M 110.0 . . ? C125 C126 H12M 110.0 . . ? H12L C126 H12M 108.4 . . ? C208 O201 C207 119.2(5) . . ? C215 O202 C214 116.8(5) . . ? C206 O203 C221 115.5(5) . . ? C223 O204 C222 113.5(5) . . ? C224 O205 C225 110.1(5) . . ? C201 O206 C226 116.2(5) 2_775 . ? O206 C201 C202 123.0(6) 2_775 . ? O206 C201 C206 117.9(5) 2_775 . ? C202 C201 C206 119.0(6) . . ? C201 C202 C203 118.9(6) . . ? C201 C202 H20A 120.6 . . ? C203 C202 H20A 120.6 . . ? C204 C203 C202 121.6(6) . . ? C204 C203 C207 120.5(6) . . ? C202 C203 C207 118.0(6) . . ? C203 C204 C205 119.2(6) . . ? C203 C204 C214 122.7(6) . . ? C205 C204 C214 118.0(6) . . ? C206 C205 C204 121.2(6) . . ? C206 C205 H20B 119.4 . . ? C204 C205 H20B 119.4 . . ? C205 C206 O203 125.4(5) . . ? C205 C206 C201 120.1(6) . . ? O203 C206 C201 114.5(5) . . ? O201 C207 C203 112.9(6) . . ? O201 C207 H20C 109.0 . . ? C203 C207 H20C 109.0 . . ? O201 C207 H20D 109.0 . . ? C203 C207 H20D 109.0 . . ? H20C C207 H20D 107.8 . . ? O201 C208 C209 123.2(5) . . ? O201 C208 C213 116.7(5) . . ? C209 C208 C213 120.0 . . ? C210 C209 C208 120.0 . . ? C210 C209 H20E 120.0 . . ? C208 C209 H20E 120.0 . . ? C211 C210 C209 120.0 . . ? C211 C210 H21A 120.0 . . ? C209 C210 H21A 120.0 . . ? C212 C211 C210 120.0 . . ? C212 C211 H21B 120.0 . . ? C210 C211 H21B 120.0 . . ? C211 C212 C213 120.0 . . ? C211 C212 H21C 120.0 . . ? C213 C212 H21C 120.0 . . ? C212 C213 C208 120.0 . . ? C212 C213 H21D 120.0 . . ? C208 C213 H21D 120.0 . . ? O202 C214 C204 107.8(5) . . ? O202 C214 H21E 110.1 . . ? C204 C214 H21E 110.1 . . ? O202 C214 H21F 110.1 . . ? C204 C214 H21F 110.1 . . ? H21E C214 H21F 108.5 . . ? O202 C215 C220 124.8(7) . . ? O202 C215 C216 114.4(7) . . ? C220 C215 C216 120.8(7) . . ? C217 C216 C215 118.4(9) . . ? C217 C216 H21G 120.8 . . ? C215 C216 H21G 120.8 . . ? C218 C217 C216 124.9(10) . . ? C218 C217 H21H 117.5 . . ? C216 C217 H21H 117.5 . . ? C217 C218 C219 116.8(8) . . ? C217 C218 H21I 121.6 . . ? C219 C218 H21I 121.6 . . ? C220 C219 C218 120.8(8) . . ? C220 C219 H21J 119.6 . . ? C218 C219 H21J 119.6 . . ? C215 C220 C219 118.2(8) . . ? C215 C220 H22A 120.9 . . ? C219 C220 H22A 120.9 . . ? O203 C221 C222 108.4(5) . . ? O203 C221 H22B 110.0 . . ? C222 C221 H22B 110.0 . . ? O203 C221 H22C 110.0 . . ? C222 C221 H22C 110.0 . . ? H22B C221 H22C 108.4 . . ? O204 C222 C221 110.0(5) . . ? O204 C222 H22D 109.7 . . ? C221 C222 H22D 109.7 . . ? O204 C222 H22E 109.7 . . ? C221 C222 H22E 109.7 . . ? H22D C222 H22E 108.2 . . ? O204 C223 C224 109.4(5) . . ? O204 C223 H22F 109.8 . . ? C224 C223 H22F 109.8 . . ? O204 C223 H22G 109.8 . . ? C224 C223 H22G 109.8 . . ? H22F C223 H22G 108.2 . . ? O205 C224 C223 108.7(5) . . ? O205 C224 H22H 109.9 . . ? C223 C224 H22H 109.9 . . ? O205 C224 H22I 109.9 . . ? C223 C224 H22I 109.9 . . ? H22H C224 H22I 108.3 . . ? O205 C225 C226 108.9(6) . . ? O205 C225 H22J 109.9 . . ? C226 C225 H22J 109.9 . . ? O205 C225 H22K 109.9 . . ? C226 C225 H22K 109.9 . . ? H22J C225 H22K 108.3 . . ? O206 C226 C225 108.2(6) . . ? O206 C226 H22L 110.1 . . ? C225 C226 H22L 110.1 . . ? O206 C226 H22M 110.1 . . ? C225 C226 H22M 110.1 . . ? H22L C226 H22M 108.4 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.898 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.126 # Attachment '- JY1.cif' data_jy1 _database_code_depnum_ccdc_archive 'CCDC 864513' #TrackingRef '- JY1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H116 F12 N4 O26 S4' _chemical_formula_weight 2194.25 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.729(3) _cell_length_b 16.8628(19) _cell_length_c 23.505(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.7570(10) _cell_angle_gamma 90.00 _cell_volume 10524(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 623 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 24.71 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4592 _exptl_absorpt_coefficient_mu 0.188 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6208 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48517 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.71 _reflns_number_total 8956 _reflns_number_gt 5844 _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. One triflate anion was treated as a rigid groups with equivalent S-O and C-F bond lengths and equivalent O-S-O and F-C-F angles using SADI, SIMU and DELU restraints. A second triflate anion and a water molecule were disordered and treated with a 50:50 model and restrained using SAME to be equivalent to the first trtiflate ion. ; _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^)+(0.1201P)^2^+78.1659P] 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 8956 _refine_ls_number_parameters 757 _refine_ls_number_restraints 275 _refine_ls_R_factor_all 0.1499 _refine_ls_R_factor_gt 0.1090 _refine_ls_wR_factor_ref 0.3206 _refine_ls_wR_factor_gt 0.2910 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.22847(17) 0.5323(3) 0.83175(18) 0.0528(11) Uani 1 1 d . . . O2 O 0.31081(16) 0.5020(3) 0.7479(2) 0.0568(12) Uani 1 1 d . . . O3 O 0.13503(15) 0.4545(3) 0.56229(17) 0.0472(11) Uani 1 1 d . . . O4 O 0.09079(17) 0.4378(4) 0.43319(19) 0.0701(15) Uani 1 1 d . . . O5 O -0.02427(17) 0.4423(3) 0.62424(18) 0.0645(14) Uani 1 1 d . . . O6 O 0.08444(15) 0.4617(3) 0.64135(17) 0.0475(11) Uani 1 1 d . . . C23 C 0.1323(2) 0.4922(4) 0.6574(3) 0.0421(14) Uani 1 1 d . . . C24 C 0.1541(2) 0.5281(4) 0.7118(3) 0.0459(15) Uani 1 1 d . . . H24A H 0.1346 0.5351 0.7387 0.055 Uiso 1 1 calc R . . C25 C 0.2042(2) 0.5543(4) 0.7280(3) 0.0476(16) Uani 1 1 d . . . C26 C 0.2324(2) 0.5449(4) 0.6878(3) 0.0449(15) Uani 1 1 d . . . C27 C 0.2095(2) 0.5129(4) 0.6322(3) 0.0447(15) Uani 1 1 d . . . H27A H 0.2282 0.5089 0.6043 0.054 Uiso 1 1 calc R . . C28 C 0.1591(2) 0.4862(4) 0.6161(2) 0.0401(14) Uani 1 1 d . . . C29 C 0.2253(3) 0.5913(4) 0.7878(3) 0.0497(16) Uani 1 1 d . . . H29A H 0.2591 0.6134 0.7915 0.060 Uiso 1 1 calc R . . H29B H 0.2032 0.6351 0.7931 0.060 Uiso 1 1 calc R . . C30 C 0.2456(3) 0.5651(4) 0.8897(3) 0.0531(17) Uani 1 1 d . . . H30A H 0.2204 0.6032 0.8957 0.064 Uiso 1 1 calc R . . H30B H 0.2775 0.5941 0.8941 0.064 Uiso 1 1 calc R . . C31 C 0.2539(2) 0.5011(4) 0.9354(3) 0.0496(16) Uani 1 1 d . . . C32 C 0.2865(3) 0.5147(5) 0.9919(3) 0.0596(19) Uani 1 1 d . . . H32A H 0.3023 0.5649 1.0012 0.072 Uiso 1 1 calc R . . C33 C 0.2958(3) 0.4561(6) 1.0342(3) 0.071(2) Uani 1 1 d . . . H33A H 0.3185 0.4657 1.0724 0.085 Uiso 1 1 calc R . . C34 C 0.2725(3) 0.3832(5) 1.0216(4) 0.071(2) Uani 1 1 d . . . H34A H 0.2790 0.3426 1.0509 0.085 Uiso 1 1 calc R . . C35 C 0.2404(3) 0.3701(5) 0.9673(3) 0.069(2) Uani 1 1 d . . . H35A H 0.2246 0.3198 0.9583 0.082 Uiso 1 1 calc R . . C36 C 0.2301(3) 0.4288(4) 0.9243(3) 0.0551(17) Uani 1 1 d . . . H36A H 0.2063 0.4191 0.8868 0.066 Uiso 1 1 calc R . . C37 C 0.2881(2) 0.5609(4) 0.7050(3) 0.0529(17) Uani 1 1 d . . . H37A H 0.3009 0.5570 0.6699 0.064 Uiso 1 1 calc R . . H37B H 0.2955 0.6147 0.7223 0.064 Uiso 1 1 calc R . . C38 C 0.3634(2) 0.5092(5) 0.7707(3) 0.0607(19) Uani 1 1 d . . . H38A H 0.3726 0.5656 0.7794 0.073 Uiso 1 1 calc R . . H38B H 0.3797 0.4905 0.7408 0.073 Uiso 1 1 calc R . . C39 C 0.3815(2) 0.4614(4) 0.8259(3) 0.0523(17) Uani 1 1 d . . . C40 C 0.4294(3) 0.4271(5) 0.8415(4) 0.070(2) Uani 1 1 d . . . H40A H 0.4497 0.4321 0.8153 0.084 Uiso 1 1 calc R . . C41 C 0.4478(3) 0.3859(5) 0.8946(4) 0.070(2) Uani 1 1 d . . . H41A H 0.4804 0.3628 0.9047 0.085 Uiso 1 1 calc R . . C42 C 0.4180(3) 0.3793(5) 0.9322(3) 0.065(2) Uani 1 1 d . . . H42A H 0.4307 0.3530 0.9693 0.078 Uiso 1 1 calc R . . C43 C 0.3696(3) 0.4104(5) 0.9167(3) 0.0622(19) Uani 1 1 d . . . H43A H 0.3487 0.4035 0.9420 0.075 Uiso 1 1 calc R . . C44 C 0.3522(3) 0.4516(4) 0.8637(3) 0.0567(18) Uani 1 1 d . . . H44A H 0.3192 0.4737 0.8533 0.068 Uiso 1 1 calc R . . C45 C 0.1640(2) 0.4423(5) 0.5213(3) 0.0547(17) Uani 1 1 d . . . H45A H 0.1952 0.4128 0.5410 0.066 Uiso 1 1 calc R . . H45B H 0.1735 0.4941 0.5079 0.066 Uiso 1 1 calc R . . C46 C 0.1331(3) 0.3963(5) 0.4692(3) 0.0623(19) Uani 1 1 d . . . H46A H 0.1548 0.3805 0.4443 0.075 Uiso 1 1 calc R . . H46B H 0.1212 0.3471 0.4838 0.075 Uiso 1 1 calc R . . C47 C 0.1015(3) 0.4888(6) 0.3905(3) 0.070(2) Uani 1 1 d . . . H47A H 0.1234 0.4611 0.3702 0.084 Uiso 1 1 calc R . . H47B H 0.1197 0.5364 0.4105 0.084 Uiso 1 1 calc R . . C48 C -0.0538(3) 0.4868(5) 0.6540(3) 0.067(2) Uani 1 1 d . . . H48A H -0.0349 0.5343 0.6730 0.081 Uiso 1 1 calc R . . H48B H -0.0613 0.4539 0.6853 0.081 Uiso 1 1 calc R . . C49 C 0.0156(3) 0.3996(5) 0.6639(3) 0.0607(19) Uani 1 1 d . . . H49A H 0.0237 0.3529 0.6427 0.073 Uiso 1 1 calc R . . H49B H 0.0040 0.3798 0.6973 0.073 Uiso 1 1 calc R . . C50 C 0.0627(2) 0.4472(4) 0.6885(3) 0.0508(16) Uani 1 1 d . . . H50A H 0.0547 0.4980 0.7048 0.061 Uiso 1 1 calc R . . H50B H 0.0867 0.4175 0.7209 0.061 Uiso 1 1 calc R . . N1 N 0.76752(19) 0.1949(3) 1.2820(2) 0.0446(12) Uani 1 1 d . . . N2 N 0.96880(17) 0.4059(3) 1.46823(19) 0.0364(11) Uani 1 1 d . . . C1 C 0.5952(4) 0.3693(9) 1.0173(6) 0.147(6) Uani 1 1 d . . . H1A H 0.6163 0.3340 1.0014 0.220 Uiso 1 1 calc R . . H1B H 0.6157 0.4130 1.0389 0.220 Uiso 1 1 calc R . . H1C H 0.5679 0.3906 0.9845 0.220 Uiso 1 1 calc R . . C2 C 0.5415(4) 0.3798(6) 1.0827(4) 0.100(3) Uani 1 1 d . . . H2A H 0.5626 0.4233 1.1037 0.150 Uiso 1 1 calc R . . H2B H 0.5267 0.3516 1.1101 0.150 Uiso 1 1 calc R . . H2C H 0.5145 0.4012 1.0496 0.150 Uiso 1 1 calc R . . C3 C 0.5393(3) 0.2567(5) 1.0272(4) 0.091(3) Uani 1 1 d . . . H3A H 0.5593 0.2181 1.0124 0.136 Uiso 1 1 calc R . . H3B H 0.5128 0.2784 0.9937 0.136 Uiso 1 1 calc R . . H3C H 0.5239 0.2303 1.0548 0.136 Uiso 1 1 calc R . . C4 C 0.5731(3) 0.3232(5) 1.0590(3) 0.063(2) Uani 1 1 d . . . C5 C 0.6151(3) 0.2839(4) 1.1090(3) 0.0529(17) Uani 1 1 d . . . C6 C 0.6098(3) 0.2704(5) 1.1648(3) 0.0604(19) Uani 1 1 d . . . H6A H 0.5808 0.2906 1.1737 0.073 Uiso 1 1 calc R . . C7 C 0.6446(3) 0.2291(4) 1.2078(3) 0.0567(18) Uani 1 1 d . . . H7A H 0.6389 0.2198 1.2453 0.068 Uiso 1 1 calc R . . C8 C 0.6879(2) 0.2008(4) 1.1971(3) 0.0519(17) Uani 1 1 d . . . C9 C 0.6953(3) 0.2170(4) 1.1429(3) 0.0556(17) Uani 1 1 d . . . H9A H 0.7253 0.1999 1.1348 0.067 Uiso 1 1 calc R . . C10 C 0.6592(3) 0.2581(4) 1.1000(3) 0.0581(18) Uani 1 1 d . . . H10A H 0.6652 0.2688 1.0630 0.070 Uiso 1 1 calc R . . C11 C 0.7241(2) 0.1494(4) 1.2423(3) 0.0528(17) Uani 1 1 d . . . H11A H 0.7055 0.1228 1.2671 0.063 Uiso 1 1 calc R . . H11B H 0.7374 0.1078 1.2212 0.063 Uiso 1 1 calc R . . C12 C 0.7615(2) 0.2320(4) 1.3299(3) 0.0498(16) Uani 1 1 d . . . H12A H 0.7298 0.2307 1.3378 0.060 Uiso 1 1 calc R . . C13 C 0.8013(2) 0.2718(4) 1.3677(3) 0.0459(15) Uani 1 1 d . . . H13A H 0.7970 0.2974 1.4019 0.055 Uiso 1 1 calc R . . C14 C 0.8481(2) 0.2750(3) 1.3559(2) 0.0386(13) Uani 1 1 d . . . C15 C 0.8519(2) 0.2384(4) 1.3048(3) 0.0446(15) Uani 1 1 d . . . H15A H 0.8826 0.2408 1.2946 0.054 Uiso 1 1 calc R . . C16 C 0.8110(3) 0.1985(4) 1.2687(3) 0.0482(16) Uani 1 1 d . . . H16A H 0.8139 0.1732 1.2338 0.058 Uiso 1 1 calc R . . C17 C 0.8912(2) 0.3184(3) 1.3958(2) 0.0379(13) Uani 1 1 d . . . C18 C 0.8924(2) 0.3357(4) 1.4545(2) 0.0406(14) Uani 1 1 d . . . H18A H 0.8665 0.3170 1.4701 0.049 Uiso 1 1 calc R . . C19 C 0.9315(2) 0.3802(4) 1.4891(2) 0.0426(14) Uani 1 1 d . . . H19A H 0.9320 0.3929 1.5286 0.051 Uiso 1 1 calc R . . C20 C 0.9696(2) 0.3858(4) 1.4128(2) 0.0418(14) Uani 1 1 d . . . H20A H 0.9971 0.4016 1.3990 0.050 Uiso 1 1 calc R . . C21 C 0.9312(2) 0.3428(3) 1.3766(3) 0.0402(14) Uani 1 1 d . . . H21A H 0.9320 0.3296 1.3376 0.048 Uiso 1 1 calc R . . C22 C 1.0089(2) 0.4570(4) 1.5048(3) 0.0412(14) Uani 1 1 d . . . H22A H 1.0401 0.4501 1.4930 0.049 Uiso 1 1 calc R . . H22B H 1.0160 0.4426 1.5472 0.049 Uiso 1 1 calc R . . S1 S -0.11680(9) 0.26810(14) 0.63627(9) 0.0737(6) Uani 1 1 d DU . . O7 O -0.0991(3) 0.3258(4) 0.6818(3) 0.111(2) Uani 1 1 d DU . . O8 O -0.1109(3) 0.2888(5) 0.5807(2) 0.112(2) Uani 1 1 d DU . . O9 O -0.1645(2) 0.2337(4) 0.6344(3) 0.0933(19) Uani 1 1 d DU . . C51 C -0.0751(3) 0.1888(6) 0.6613(4) 0.092(3) Uani 1 1 d DU . . F1 F -0.0836(3) 0.1278(4) 0.6234(4) 0.142(3) Uani 1 1 d DU . . F2 F -0.0270(2) 0.2118(5) 0.6683(3) 0.146(3) Uani 1 1 d DU . . F3 F -0.0770(3) 0.1604(4) 0.7136(3) 0.143(3) Uani 1 1 d DU . . S2A S 0.16393(16) 0.1947(2) 0.38540(16) 0.0631(10) Uani 0.50 1 d PDU A -1 O10A O 0.1738(5) 0.2030(6) 0.4467(4) 0.079(3) Uani 0.50 1 d PDU A -1 O11A O 0.1604(5) 0.2650(5) 0.3527(5) 0.082(3) Uani 0.50 1 d PDU A -1 O12A O 0.1867(3) 0.1266(4) 0.3685(3) 0.0284(15) Uani 0.50 1 d PDU A -1 C52A C 0.1010(5) 0.1589(9) 0.3611(6) 0.087(4) Uani 0.50 1 d PDU A -1 F4A F 0.0680(5) 0.2081(10) 0.3751(6) 0.124(4) Uani 0.50 1 d PDU A -1 F5A F 0.0860(5) 0.1500(9) 0.3017(4) 0.120(4) Uani 0.50 1 d PDU A -1 F6A F 0.0962(5) 0.0858(7) 0.3846(5) 0.118(4) Uani 0.50 1 d PDU A -1 O1WA O 0.0782(7) 0.3525(9) 0.2680(7) 0.102(5) Uani 0.50 1 d P B -1 S2B S 0.0562(3) 0.3014(4) 0.2934(4) 0.127(2) Uani 0.50 1 d PDU C -2 O10B O 0.1075(6) 0.3122(16) 0.3014(12) 0.192(10) Uani 0.50 1 d PDU C -2 O11B O 0.0410(10) 0.3161(16) 0.3454(10) 0.247(12) Uani 0.50 1 d PDU C -2 O12B O 0.0209(8) 0.334(2) 0.2428(11) 0.283(15) Uani 0.50 1 d PDU C -2 C52B C 0.0375(9) 0.2035(11) 0.2914(13) 0.276(14) Uani 0.50 1 d PDU C -2 F4B F -0.0126(9) 0.2090(17) 0.2885(10) 0.279(12) Uani 0.50 1 d PDU C -2 F5B F 0.0484(17) 0.1728(18) 0.2448(18) 0.44(2) Uani 0.50 1 d PDU C -2 F6B F 0.0582(12) 0.1567(13) 0.3385(16) 0.353(17) Uani 0.50 1 d PDU C -2 O1WB O 0.2273(4) 0.2369(6) 0.4654(4) 0.063(3) Uani 0.50 1 d P D -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.060(3) 0.049(3) 0.040(2) -0.004(2) -0.001(2) -0.002(2) O2 0.041(3) 0.053(3) 0.065(3) 0.002(2) -0.003(2) 0.000(2) O3 0.038(2) 0.066(3) 0.035(2) 0.000(2) 0.0063(18) 0.003(2) O4 0.048(3) 0.124(5) 0.038(2) 0.008(3) 0.011(2) -0.006(3) O5 0.046(3) 0.112(4) 0.033(2) -0.007(3) 0.008(2) -0.010(3) O6 0.041(2) 0.068(3) 0.032(2) 0.003(2) 0.0089(18) 0.001(2) C23 0.035(3) 0.047(4) 0.040(3) 0.009(3) 0.004(3) 0.003(3) C24 0.049(4) 0.051(4) 0.034(3) 0.006(3) 0.005(3) 0.008(3) C25 0.051(4) 0.045(4) 0.036(3) 0.006(3) -0.005(3) 0.002(3) C26 0.039(3) 0.045(4) 0.045(3) 0.010(3) 0.004(3) 0.000(3) C27 0.043(3) 0.056(4) 0.035(3) 0.007(3) 0.011(3) 0.001(3) C28 0.037(3) 0.046(4) 0.034(3) 0.006(3) 0.004(3) 0.009(3) C29 0.057(4) 0.040(3) 0.044(4) 0.001(3) 0.002(3) 0.000(3) C30 0.061(4) 0.054(4) 0.044(4) -0.012(3) 0.014(3) -0.005(3) C31 0.042(3) 0.064(4) 0.042(3) -0.004(3) 0.011(3) 0.007(3) C32 0.054(4) 0.073(5) 0.050(4) -0.011(4) 0.013(3) -0.011(4) C33 0.052(4) 0.117(7) 0.039(4) 0.009(4) 0.006(3) 0.001(5) C34 0.073(5) 0.080(6) 0.060(5) 0.023(4) 0.020(4) 0.014(5) C35 0.086(6) 0.059(5) 0.063(5) 0.000(4) 0.024(4) 0.005(4) C36 0.057(4) 0.064(5) 0.043(4) 0.001(3) 0.012(3) 0.003(4) C37 0.047(4) 0.058(4) 0.049(4) 0.007(3) 0.007(3) -0.003(3) C38 0.043(4) 0.070(5) 0.065(4) -0.003(4) 0.009(3) -0.004(3) C39 0.040(4) 0.054(4) 0.057(4) -0.010(3) 0.004(3) 0.004(3) C40 0.048(4) 0.079(6) 0.080(5) -0.002(4) 0.011(4) -0.002(4) C41 0.044(4) 0.076(6) 0.076(5) -0.002(4) -0.005(4) 0.010(4) C42 0.063(5) 0.060(5) 0.058(4) -0.008(4) -0.006(4) 0.005(4) C43 0.062(5) 0.066(5) 0.052(4) -0.006(4) 0.006(3) 0.010(4) C44 0.049(4) 0.057(4) 0.055(4) -0.011(3) 0.001(3) 0.009(3) C45 0.049(4) 0.074(5) 0.041(4) -0.001(3) 0.013(3) 0.001(3) C46 0.054(4) 0.086(6) 0.045(4) -0.007(4) 0.012(3) -0.006(4) C47 0.050(4) 0.117(7) 0.048(4) 0.002(4) 0.022(3) -0.007(4) C48 0.057(4) 0.107(6) 0.037(4) -0.005(4) 0.012(3) -0.012(4) C49 0.057(4) 0.086(5) 0.039(4) 0.006(4) 0.013(3) -0.011(4) C50 0.049(4) 0.067(4) 0.034(3) 0.005(3) 0.007(3) 0.003(3) N1 0.042(3) 0.040(3) 0.041(3) 0.000(2) -0.004(2) -0.002(2) N2 0.036(3) 0.038(3) 0.032(2) -0.001(2) 0.003(2) -0.004(2) C1 0.071(6) 0.204(14) 0.149(10) 0.126(11) 0.006(7) 0.008(8) C2 0.098(7) 0.083(6) 0.089(7) -0.010(5) -0.023(5) 0.027(6) C3 0.080(6) 0.069(5) 0.086(6) -0.023(5) -0.035(5) 0.009(4) C4 0.047(4) 0.067(5) 0.065(5) 0.009(4) 0.001(3) -0.008(4) C5 0.048(4) 0.054(4) 0.051(4) 0.002(3) 0.005(3) -0.013(3) C6 0.046(4) 0.074(5) 0.059(4) 0.003(4) 0.012(3) -0.002(4) C7 0.046(4) 0.072(5) 0.046(4) 0.003(3) 0.002(3) -0.003(3) C8 0.050(4) 0.046(4) 0.047(4) -0.003(3) -0.007(3) -0.015(3) C9 0.048(4) 0.060(4) 0.054(4) -0.009(3) 0.007(3) -0.004(3) C10 0.060(4) 0.062(5) 0.046(4) 0.001(3) 0.005(3) -0.009(4) C11 0.050(4) 0.046(4) 0.050(4) 0.000(3) -0.003(3) -0.009(3) C12 0.043(4) 0.051(4) 0.051(4) 0.006(3) 0.007(3) -0.011(3) C13 0.046(4) 0.048(4) 0.038(3) -0.004(3) 0.004(3) -0.008(3) C14 0.043(3) 0.037(3) 0.031(3) 0.000(2) 0.002(2) -0.002(3) C15 0.042(3) 0.052(4) 0.037(3) -0.001(3) 0.008(3) -0.002(3) C16 0.056(4) 0.047(4) 0.034(3) -0.005(3) 0.001(3) -0.002(3) C17 0.032(3) 0.041(3) 0.035(3) 0.002(3) 0.000(2) 0.002(3) C18 0.046(3) 0.045(3) 0.030(3) -0.002(3) 0.010(3) -0.010(3) C19 0.043(3) 0.052(4) 0.029(3) -0.004(3) 0.005(3) -0.006(3) C20 0.045(3) 0.048(4) 0.032(3) -0.001(3) 0.012(3) -0.005(3) C21 0.042(3) 0.042(3) 0.034(3) -0.004(3) 0.007(3) -0.004(3) C22 0.036(3) 0.047(3) 0.036(3) -0.005(3) 0.002(2) -0.009(3) S1 0.0882(15) 0.0821(15) 0.0546(11) 0.0024(10) 0.0267(11) -0.0019(12) O7 0.177(7) 0.093(5) 0.073(4) -0.017(3) 0.050(4) -0.045(5) O8 0.130(6) 0.157(7) 0.060(3) 0.019(4) 0.042(4) 0.003(5) O9 0.069(4) 0.130(5) 0.079(4) -0.008(4) 0.019(3) 0.002(3) C51 0.074(5) 0.097(7) 0.108(7) 0.004(5) 0.029(6) -0.006(5) F1 0.129(5) 0.088(4) 0.222(7) -0.036(5) 0.071(5) 0.003(4) F2 0.078(4) 0.165(7) 0.188(7) 0.013(5) 0.026(4) -0.012(4) F3 0.139(6) 0.149(6) 0.146(5) 0.066(5) 0.048(5) 0.037(5) S2A 0.078(2) 0.062(2) 0.055(2) 0.0034(17) 0.0289(19) -0.0040(19) O10A 0.111(9) 0.068(7) 0.059(5) -0.017(5) 0.025(6) 0.004(6) O11A 0.125(10) 0.051(5) 0.085(7) 0.006(5) 0.054(7) 0.004(6) O12A 0.046(4) 0.024(3) 0.013(3) 0.000(3) 0.006(3) 0.008(3) C52A 0.066(7) 0.128(12) 0.073(8) 0.003(9) 0.028(7) -0.002(7) F4A 0.092(7) 0.179(12) 0.111(8) 0.017(8) 0.045(7) 0.031(9) F5A 0.141(10) 0.136(10) 0.059(5) -0.021(6) -0.011(6) -0.014(8) F6A 0.143(10) 0.115(8) 0.108(8) -0.020(6) 0.054(8) -0.057(7) O1WA 0.145(13) 0.097(10) 0.087(10) 0.011(8) 0.072(10) 0.017(10) S2B 0.123(5) 0.135(5) 0.150(6) -0.027(5) 0.081(4) -0.043(4) O10B 0.125(10) 0.21(2) 0.27(3) 0.00(2) 0.106(14) -0.041(15) O11B 0.29(3) 0.27(3) 0.271(19) -0.09(2) 0.22(2) -0.05(2) O12B 0.16(2) 0.38(3) 0.28(2) 0.07(3) 0.029(19) -0.04(2) C52B 0.39(3) 0.186(15) 0.37(4) -0.080(14) 0.30(3) -0.150(18) F4B 0.33(2) 0.34(3) 0.24(2) -0.084(19) 0.19(2) -0.222(18) F5B 0.62(5) 0.28(3) 0.57(4) -0.24(3) 0.43(5) -0.13(4) F6B 0.46(3) 0.139(16) 0.65(5) 0.07(2) 0.45(3) 0.06(2) O1WB 0.070(7) 0.062(6) 0.067(6) -0.005(5) 0.034(5) 0.003(5) _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 C30 1.419(7) . ? O1 C29 1.418(7) . ? O2 C38 1.406(8) . ? O2 C37 1.425(8) . ? O3 C28 1.358(7) . ? O3 C45 1.436(7) . ? O4 C46 1.417(9) . ? O4 C47 1.417(9) . ? O5 C49 1.420(8) . ? O5 C48 1.433(9) . ? O6 C23 1.371(7) . ? O6 C50 1.428(7) . ? C23 C24 1.384(8) . ? C23 C28 1.386(8) . ? C24 C25 1.403(9) . ? C24 H24A 0.9500 . ? C25 C26 1.399(9) . ? C25 C29 1.494(8) . ? C26 C27 1.385(9) . ? C26 C37 1.505(9) . ? C27 C28 1.414(8) . ? C27 H27A 0.9500 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.493(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.375(10) . ? C31 C32 1.392(9) . ? C32 C33 1.373(11) . ? C32 H32A 0.9500 . ? C33 C34 1.381(12) . ? C33 H33A 0.9500 . ? C34 C35 1.347(11) . ? C34 H34A 0.9500 . ? C35 C36 1.383(10) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.488(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C44 1.376(10) . ? C39 C40 1.397(10) . ? C40 C41 1.391(11) . ? C40 H40A 0.9500 . ? C41 C42 1.379(11) . ? C41 H41A 0.9500 . ? C42 C43 1.388(10) . ? C42 H42A 0.9500 . ? C43 C44 1.385(10) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.494(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.489(10) 5_566 ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C47 1.489(10) 5_566 ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.499(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? N1 C16 1.331(8) . ? N1 C12 1.340(8) . ? N1 C11 1.505(8) . ? N2 C19 1.339(7) . ? N2 C20 1.352(7) . ? N2 C22 1.471(7) . ? C1 C4 1.513(12) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.507(12) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.514(11) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.545(10) . ? C5 C10 1.370(10) . ? C5 C6 1.380(10) . ? C6 C7 1.371(10) . ? C6 H6A 0.9500 . ? C7 C8 1.381(10) . ? C7 H7A 0.9500 . ? C8 C9 1.373(10) . ? C8 C11 1.507(9) . ? C9 C10 1.384(10) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.375(9) . ? C12 H12A 0.9500 . ? C13 C14 1.404(9) . ? C13 H13A 0.9500 . ? C14 C15 1.381(8) . ? C14 C17 1.482(8) . ? C15 C16 1.381(9) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C21 1.375(8) . ? C17 C18 1.401(8) . ? C18 C19 1.375(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.365(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C22 1.526(12) 5_768 ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? S1 O8 1.407(5) . ? S1 O7 1.425(6) . ? S1 O9 1.433(6) . ? S1 C51 1.755(10) . ? C51 F1 1.336(9) . ? C51 F3 1.336(9) . ? C51 F2 1.351(9) . ? S2A O10A 1.395(9) . ? S2A O11A 1.402(9) . ? S2A O12A 1.421(7) . ? S2A C52A 1.779(14) . ? C52A F5A 1.345(12) . ? C52A F4A 1.345(13) . ? C52A F6A 1.374(13) . ? S2B O10B 1.392(12) . ? S2B O12B 1.414(13) . ? S2B O11B 1.424(12) . ? S2B C52B 1.727(17) . ? C52B F5B 1.325(15) . ? C52B F6B 1.346(15) . ? C52B F4B 1.373(15) . ? 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 C30 O1 C29 111.1(5) . . ? C38 O2 C37 114.0(5) . . ? C28 O3 C45 117.6(5) . . ? C46 O4 C47 114.6(5) . . ? C49 O5 C48 113.1(5) . . ? C23 O6 C50 116.2(4) . . ? O6 C23 C24 123.3(6) . . ? O6 C23 C28 116.8(5) . . ? C24 C23 C28 119.9(6) . . ? C23 C24 C25 121.6(6) . . ? C23 C24 H24A 119.2 . . ? C25 C24 H24A 119.2 . . ? C26 C25 C24 118.8(6) . . ? C26 C25 C29 122.8(6) . . ? C24 C25 C29 118.4(6) . . ? C27 C26 C25 119.3(6) . . ? C27 C26 C37 118.6(6) . . ? C25 C26 C37 121.8(6) . . ? C26 C27 C28 121.7(6) . . ? C26 C27 H27A 119.2 . . ? C28 C27 H27A 119.2 . . ? O3 C28 C23 117.6(5) . . ? O3 C28 C27 123.8(5) . . ? C23 C28 C27 118.5(5) . . ? O1 C29 C25 108.5(5) . . ? O1 C29 H29A 110.0 . . ? C25 C29 H29A 110.0 . . ? O1 C29 H29B 110.0 . . ? C25 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? O1 C30 C31 110.4(5) . . ? O1 C30 H30A 109.6 . . ? C31 C30 H30A 109.6 . . ? O1 C30 H30B 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C36 C31 C32 118.1(7) . . ? C36 C31 C30 122.6(6) . . ? C32 C31 C30 119.3(7) . . ? C33 C32 C31 120.5(7) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C32 C33 C34 120.4(7) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C35 C34 C33 119.4(8) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C34 C35 C36 121.0(8) . . ? C34 C35 H35A 119.5 . . ? C36 C35 H35A 119.5 . . ? C31 C36 C35 120.6(7) . . ? C31 C36 H36A 119.7 . . ? C35 C36 H36A 119.7 . . ? O2 C37 C26 106.0(5) . . ? O2 C37 H37A 110.5 . . ? C26 C37 H37A 110.5 . . ? O2 C37 H37B 110.5 . . ? C26 C37 H37B 110.5 . . ? H37A C37 H37B 108.7 . . ? O2 C38 C39 109.6(6) . . ? O2 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? O2 C38 H38B 109.7 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C44 C39 C40 118.5(7) . . ? C44 C39 C38 121.0(6) . . ? C40 C39 C38 120.5(7) . . ? C41 C40 C39 121.1(8) . . ? C41 C40 H40A 119.5 . . ? C39 C40 H40A 119.5 . . ? C42 C41 C40 118.9(7) . . ? C42 C41 H41A 120.5 . . ? C40 C41 H41A 120.5 . . ? C41 C42 C43 120.9(7) . . ? C41 C42 H42A 119.6 . . ? C43 C42 H42A 119.6 . . ? C44 C43 C42 119.2(8) . . ? C44 C43 H43A 120.4 . . ? C42 C43 H43A 120.4 . . ? C39 C44 C43 121.4(7) . . ? C39 C44 H44A 119.3 . . ? C43 C44 H44A 119.3 . . ? O3 C45 C46 109.0(5) . . ? O3 C45 H45A 109.9 . . ? C46 C45 H45A 109.9 . . ? O3 C45 H45B 109.9 . . ? C46 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? O4 C46 C45 114.4(7) . . ? O4 C46 H46A 108.7 . . ? C45 C46 H46A 108.7 . . ? O4 C46 H46B 108.7 . . ? C45 C46 H46B 108.7 . . ? H46A C46 H46B 107.6 . . ? O4 C47 C48 109.8(6) . 5_566 ? O4 C47 H47A 109.7 . . ? C48 C47 H47A 109.7 5_566 . ? O4 C47 H47B 109.7 . . ? C48 C47 H47B 109.7 5_566 . ? H47A C47 H47B 108.2 . . ? O5 C48 C47 108.6(5) . 5_566 ? O5 C48 H48A 110.0 . . ? C47 C48 H48A 110.0 5_566 . ? O5 C48 H48B 110.0 . . ? C47 C48 H48B 110.0 5_566 . ? H48A C48 H48B 108.3 . . ? O5 C49 C50 114.2(6) . . ? O5 C49 H49A 108.7 . . ? C50 C49 H49A 108.7 . . ? O5 C49 H49B 108.7 . . ? C50 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? O6 C50 C49 107.8(5) . . ? O6 C50 H50A 110.1 . . ? C49 C50 H50A 110.1 . . ? O6 C50 H50B 110.1 . . ? C49 C50 H50B 110.1 . . ? H50A C50 H50B 108.5 . . ? C16 N1 C12 121.1(5) . . ? C16 N1 C11 119.7(5) . . ? C12 N1 C11 119.2(6) . . ? C19 N2 C20 120.0(5) . . ? C19 N2 C22 120.6(5) . . ? C20 N2 C22 119.4(5) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C1 107.5(9) . . ? C2 C4 C3 108.0(7) . . ? C1 C4 C3 111.6(9) . . ? C2 C4 C5 112.5(7) . . ? C1 C4 C5 110.9(6) . . ? C3 C4 C5 106.4(6) . . ? C10 C5 C6 116.1(6) . . ? C10 C5 C4 122.0(6) . . ? C6 C5 C4 121.9(7) . . ? C7 C6 C5 122.6(7) . . ? C7 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 . . ? C6 C7 C8 120.3(7) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C9 C8 C7 118.1(6) . . ? C9 C8 C11 121.4(7) . . ? C7 C8 C11 120.4(6) . . ? C8 C9 C10 120.3(7) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C5 C10 C9 122.4(7) . . ? C5 C10 H10A 118.8 . . ? C9 C10 H10A 118.8 . . ? N1 C11 C8 113.3(5) . . ? N1 C11 H11A 108.9 . . ? C8 C11 H11A 108.9 . . ? N1 C11 H11B 108.9 . . ? C8 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N1 C12 C13 120.0(6) . . ? N1 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C14 120.4(6) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 117.6(5) . . ? C15 C14 C17 121.2(5) . . ? C13 C14 C17 121.2(5) . . ? C16 C15 C14 119.7(6) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? N1 C16 C15 121.2(6) . . ? N1 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? C21 C17 C18 117.9(5) . . ? C21 C17 C14 121.4(5) . . ? C18 C17 C14 120.7(5) . . ? C19 C18 C17 119.2(5) . . ? C19 C18 H18A 120.4 . . ? C17 C18 H18A 120.4 . . ? N2 C19 C18 121.4(5) . . ? N2 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? N2 C20 C21 120.5(5) . . ? N2 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C20 C21 C17 120.8(5) . . ? C20 C21 H21A 119.6 . . ? C17 C21 H21A 119.6 . . ? N2 C22 C22 108.3(6) . 5_768 ? N2 C22 H22A 110.0 . . ? C22 C22 H22A 110.0 5_768 . ? N2 C22 H22B 110.0 . . ? C22 C22 H22B 110.0 5_768 . ? H22A C22 H22B 108.4 . . ? O8 S1 O7 114.9(4) . . ? O8 S1 O9 115.1(4) . . ? O7 S1 O9 114.5(4) . . ? O8 S1 C51 105.0(5) . . ? O7 S1 C51 102.6(5) . . ? O9 S1 C51 102.5(4) . . ? F1 C51 F3 107.0(8) . . ? F1 C51 F2 106.3(8) . . ? F3 C51 F2 106.9(8) . . ? F1 C51 S1 113.0(7) . . ? F3 C51 S1 112.5(7) . . ? F2 C51 S1 110.8(7) . . ? O10A S2A O11A 116.3(7) . . ? O10A S2A O12A 113.6(6) . . ? O11A S2A O12A 119.8(6) . . ? O10A S2A C52A 104.4(7) . . ? O11A S2A C52A 101.7(7) . . ? O12A S2A C52A 96.4(6) . . ? F5A C52A F4A 107.2(12) . . ? F5A C52A F6A 106.3(12) . . ? F4A C52A F6A 107.6(12) . . ? F5A C52A S2A 110.6(10) . . ? F4A C52A S2A 112.7(11) . . ? F6A C52A S2A 112.0(10) . . ? O10B S2B O12B 119.7(15) . . ? O10B S2B O11B 113.9(15) . . ? O12B S2B O11B 110.5(16) . . ? O10B S2B C52B 114.6(13) . . ? O12B S2B C52B 102.5(15) . . ? O11B S2B C52B 91.7(12) . . ? F5B C52B F6B 108(2) . . ? F5B C52B F4B 117(2) . . ? F6B C52B F4B 105.5(17) . . ? F5B C52B S2B 104.9(16) . . ? F6B C52B S2B 119.0(17) . . ? F4B C52B S2B 103.2(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.830 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.081