# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Stephen Loeb' _publ_contact_author_adress ; 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_contact_letter ; This structure is part of a study on the preparation and characterization of [2]rotaxane ligand with terminal terpyridine groups that can bind Zn(II) and Ru(II). ; _publ_section_title ; Complexes of a [2]rotaxane ligand with terminal terpyridine groups ; loop_ _publ_author_name S.Loeb D.Mercer data_dm18 _database_code_depnum_ccdc_archive 'CCDC 819991' #TrackingRef '- DM18.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H118 Cl2 F18 N20 O34 Ru2 S6' _chemical_formula_weight 3311.84 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' Ru Ru -1.2594 0.8363 '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 14.056(3) _cell_length_b 14.073(3) _cell_length_c 22.616(5) _cell_angle_alpha 78.454(4) _cell_angle_beta 83.369(4) _cell_angle_gamma 62.894(3) _cell_volume 3900.2(16) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 428 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1690 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6570 _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 37004 _diffrn_reflns_av_R_equivalents 0.1452 _diffrn_reflns_av_sigmaI/netI 0.2872 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13674 _reflns_number_gt 4085 _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 weakly diffracting. The unit cell contains an estimated 4 molecules of nitromethane which were treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. Three of the four anions in the asymmetric unit were input as triflate (CF3SO3-), the other as chloride (Cl-). Two of the anion sites were disordered (50:50) between triflate and chloride ion. SADI, SIMU and DELU commands were used to restrain one of the triflate ions as a rigid group. SAME, SIMU and DELU commands were also used to restrain like anions to be approximately equal. Four ISOR commands were necessary to restrain F10 and F11 (triflate ion), N8 (terpyridine) and C46 (axle) to have approximate isotropic behaviour. AFIX 66 commands were used to restrain the three pyridine rings of the unsubstituted terpy ligand to be idealized hexagons with C-C and C-N bonds equal to 1.39 A. ; 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 0.000 0.000 0.000 500 196 ' ' 2 0.500 0.500 0.500 256 80 ' ' _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^)+(0.1590P)^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 13674 _refine_ls_number_parameters 928 _refine_ls_number_restraints 502 _refine_ls_R_factor_all 0.2567 _refine_ls_R_factor_gt 0.1212 _refine_ls_wR_factor_ref 0.3350 _refine_ls_wR_factor_gt 0.2830 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.890 _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 Ru1 Ru -2.76177(8) -1.74548(10) 2.41382(5) 0.0580(5) Uani 1 1 d . . . N4 N -2.6268(7) -1.8156(8) 2.4617(4) 0.051(3) Uani 1 1 d . . . N5 N -2.6657(6) -1.7091(8) 2.3546(4) 0.046(3) Uani 1 1 d . . . N6 N -2.8626(6) -1.6550(8) 2.3427(4) 0.048(3) Uani 1 1 d . . . N7 N -2.1588(7) -1.5688(9) 2.0988(4) 0.045(3) Uani 1 1 d . . . N8 N -1.6432(6) -1.8973(8) 1.9968(4) 0.048(3) Uani 1 1 d U . . C1 C -2.8177(7) -1.9229(9) 2.4328(4) 0.080(5) Uani 1 1 d G . . N1 N -2.7555(7) -1.8836(6) 2.3933(5) 0.068(3) Uani 1 1 d G . . C2 C -2.7022(7) -1.9346(10) 2.3444(4) 0.075(5) Uani 1 1 d G . . H2A H -2.6597 -1.9077 2.3174 0.091 Uiso 1 1 calc R . . C3 C -2.7112(10) -2.0249(10) 2.3351(5) 0.106(7) Uani 1 1 d G . . H3A H -2.6748 -2.0597 2.3018 0.127 Uiso 1 1 calc R . . C4 C -2.7734(11) -2.0641(7) 2.3747(8) 0.124(8) Uani 1 1 d G . . H4A H -2.7795 -2.1258 2.3683 0.148 Uiso 1 1 calc R . . C5 C -2.8267(8) -2.0132(10) 2.4235(6) 0.116(7) Uani 1 1 d G . . H5A H -2.8692 -2.0400 2.4505 0.140 Uiso 1 1 calc R . . N2 N -2.8541(6) -1.7768(9) 2.4780(4) 0.091(5) Uani 1 1 d G . . C6 C -2.8695(7) -1.8685(9) 2.4810(5) 0.095(7) Uani 1 1 d G . . C7 C -2.9261(9) -1.8979(9) 2.5297(6) 0.120(8) Uani 1 1 d G . . H7A H -2.9367 -1.9606 2.5317 0.144 Uiso 1 1 calc R . . C8 C -2.9673(8) -1.8358(12) 2.5754(5) 0.151(10) Uani 1 1 d G . . H8A H -3.0059 -1.8559 2.6086 0.181 Uiso 1 1 calc R . . C9 C -2.9518(8) -1.7441(11) 2.5724(4) 0.119(7) Uani 1 1 d G . . H9A H -2.9800 -1.7016 2.6037 0.143 Uiso 1 1 calc R . . C10 C -2.8952(7) -1.7146(8) 2.5238(5) 0.077(5) Uani 1 1 d G . . N3 N -2.8059(7) -1.6168(9) 2.4576(5) 0.092(5) Uani 1 1 d G . . C11 C -2.8630(8) -1.6252(9) 2.5113(5) 0.100(6) Uani 1 1 d G . . C12 C -2.8862(8) -1.5527(12) 2.5507(4) 0.115(7) Uani 1 1 d G . . H12A H -2.9252 -1.5584 2.5873 0.139 Uiso 1 1 calc R . . C13 C -2.8524(10) -1.4719(11) 2.5364(7) 0.145(8) Uani 1 1 d G . . H13A H -2.8683 -1.4224 2.5633 0.174 Uiso 1 1 calc R . . C14 C -2.7954(10) -1.4636(10) 2.4828(7) 0.115(7) Uani 1 1 d G . . H14A H -2.7723 -1.4084 2.4731 0.138 Uiso 1 1 calc R . . C15 C -2.7721(7) -1.5360(12) 2.4434(5) 0.089(5) Uani 1 1 d G . . H15A H -2.7332 -1.5303 2.4067 0.107 Uiso 1 1 calc R . . C16 C -2.6129(9) -1.8648(11) 2.5192(6) 0.067(4) Uani 1 1 d . . . H16A H -2.6705 -1.8760 2.5402 0.080 Uiso 1 1 calc R . . C17 C -2.5193(10) -1.9011(12) 2.5506(6) 0.080(5) Uani 1 1 d . . . H17A H -2.5124 -1.9352 2.5917 0.096 Uiso 1 1 calc R . . C18 C -2.4372(9) -1.8840(12) 2.5180(7) 0.085(5) Uani 1 1 d . . . H18A H -2.3721 -1.9069 2.5375 0.102 Uiso 1 1 calc R . . C19 C -2.4460(10) -1.8350(12) 2.4582(5) 0.082(5) Uani 1 1 d . . . H19A H -2.3882 -1.8261 2.4360 0.098 Uiso 1 1 calc R . . C20 C -2.5426(9) -1.8001(10) 2.4326(5) 0.056(4) Uani 1 1 d . . . C21 C -2.5658(9) -1.7422(11) 2.3701(5) 0.054(4) Uani 1 1 d . . . C22 C -2.4942(9) -1.7150(10) 2.3311(6) 0.063(4) Uani 1 1 d . . . H22A H -2.4231 -1.7384 2.3428 0.075 Uiso 1 1 calc R . . C23 C -2.5301(8) -1.6506(10) 2.2727(5) 0.051(3) Uani 1 1 d . . . C24 C -2.6382(8) -1.6164(9) 2.2610(5) 0.047(3) Uani 1 1 d . . . H24A H -2.6670 -1.5709 2.2240 0.056 Uiso 1 1 calc R . . C25 C -2.7009(8) -1.6468(9) 2.3011(5) 0.039(3) Uani 1 1 d . . . C26 C -2.8150(9) -1.6172(11) 2.2929(5) 0.058(4) Uani 1 1 d . . . C27 C -2.8742(9) -1.5521(10) 2.2452(6) 0.061(4) Uani 1 1 d . . . H27A H -2.8411 -1.5239 2.2121 0.074 Uiso 1 1 calc R . . C28 C -2.9802(9) -1.5252(12) 2.2430(6) 0.074(5) Uani 1 1 d . . . H28A H -3.0198 -1.4825 2.2080 0.088 Uiso 1 1 calc R . . C29 C -3.0274(9) -1.5613(12) 2.2922(6) 0.066(4) Uani 1 1 d . . . H29A H -3.1025 -1.5380 2.2936 0.079 Uiso 1 1 calc R . . C30 C -2.9661(8) -1.6322(11) 2.3406(6) 0.060(4) Uani 1 1 d . . . H30A H -2.9976 -1.6647 2.3724 0.072 Uiso 1 1 calc R . . C31 C -2.4602(8) -1.6150(10) 2.2309(5) 0.044(3) Uani 1 1 d . . . C32 C -2.3785(10) -1.6034(10) 2.2518(6) 0.064(4) Uani 1 1 d . . . H32A H -2.3640 -1.6230 2.2937 0.077 Uiso 1 1 calc R . . C33 C -2.3180(11) -1.5636(12) 2.2126(7) 0.078(5) Uani 1 1 d . . . H33A H -2.2655 -1.5515 2.2285 0.093 Uiso 1 1 calc R . . C34 C -2.3305(8) -1.5407(8) 2.1517(6) 0.045(3) Uani 1 1 d . . . C35 C -2.4130(8) -1.5532(9) 2.1303(5) 0.049(3) Uani 1 1 d . . . H35A H -2.4264 -1.5362 2.0883 0.059 Uiso 1 1 calc R . . C36 C -2.4750(8) -1.5906(9) 2.1709(6) 0.051(3) Uani 1 1 d . . . H36A H -2.5304 -1.5993 2.1558 0.061 Uiso 1 1 calc R . . C37 C -2.2700(8) -1.4882(9) 2.1079(6) 0.058(4) Uani 1 1 d . . . H37A H -2.3060 -1.4582 2.0687 0.070 Uiso 1 1 calc R . . H37B H -2.2703 -1.4279 2.1243 0.070 Uiso 1 1 calc R . . C38 C -2.1327(8) -1.6628(12) 2.0890(6) 0.059(4) Uani 1 1 d . . . H38A H -2.1874 -1.6860 2.0945 0.071 Uiso 1 1 calc R . . C39 C -2.0372(9) -1.7325(9) 2.0717(6) 0.064(4) Uani 1 1 d . . . H39A H -2.0242 -1.8028 2.0665 0.077 Uiso 1 1 calc R . . C40 C -1.9560(8) -1.6998(10) 2.0615(5) 0.043(3) Uani 1 1 d . . . C41 C -1.9815(8) -1.5972(12) 2.0714(5) 0.054(4) Uani 1 1 d . . . H41A H -1.9288 -1.5712 2.0653 0.064 Uiso 1 1 calc R . . C42 C -2.0833(9) -1.5328(10) 2.0903(5) 0.050(3) Uani 1 1 d . . . H42A H -2.1009 -1.4623 2.0973 0.061 Uiso 1 1 calc R . . C43 C -1.8456(8) -1.7739(10) 2.0388(5) 0.037(3) Uani 1 1 d . . . C44 C -1.8200(9) -1.8667(11) 2.0212(6) 0.059(4) Uani 1 1 d . . . H44A H -1.8736 -1.8908 2.0235 0.070 Uiso 1 1 calc R . . C45 C -1.7201(8) -1.9300(10) 2.0000(6) 0.063(4) Uani 1 1 d . . . H45A H -1.7053 -1.9961 1.9876 0.075 Uiso 1 1 calc R . . C46 C -1.6654(8) -1.8076(10) 2.0148(6) 0.053(3) Uani 1 1 d U . . H46A H -1.6090 -1.7877 2.0135 0.063 Uiso 1 1 calc R . . C47 C -1.7616(9) -1.7406(9) 2.0350(6) 0.052(3) Uani 1 1 d . . . H47A H -1.7740 -1.6743 2.0463 0.063 Uiso 1 1 calc R . . C48 C -1.5353(8) -1.9650(10) 1.9739(6) 0.058(4) Uani 1 1 d . . . H48A H -1.5046 -1.9183 1.9496 0.070 Uiso 1 1 calc R . . H48B H -1.5397 -2.0112 1.9475 0.070 Uiso 1 1 calc R . . O1 O -1.6257(7) -2.0746(8) 2.1323(4) 0.069(3) Uani 1 1 d . . . O2 O -1.5374(8) -2.2278(9) 2.0443(6) 0.091(4) Uani 1 1 d . . . O3 O -1.4139(8) -1.8641(10) 2.0725(6) 0.090(3) Uani 1 1 d . . . O4 O -1.5736(6) -1.9197(7) 2.1427(4) 0.064(2) Uani 1 1 d . . . C49 C -1.6742(11) -1.9077(11) 2.1619(6) 0.061(4) Uani 1 1 d . . . C50 C -1.7493(11) -1.8166(13) 2.1853(6) 0.075(4) Uani 1 1 d . . . H50A H -1.7336 -1.7583 2.1871 0.089 Uiso 1 1 calc R . . C51 C -1.8501(13) -1.8131(15) 2.2066(7) 0.088(5) Uani 1 1 d . . . H51A H -1.9009 -1.7528 2.2241 0.106 Uiso 1 1 calc R . . C52 C -1.8740(12) -1.8902(15) 2.2027(7) 0.079(5) Uani 1 1 d . . . H52A H -1.9419 -1.8855 2.2174 0.095 Uiso 1 1 calc R . . C53 C -1.8024(13) -1.9798(12) 2.1773(7) 0.079(4) Uani 1 1 d . . . H53A H -1.8229 -2.0340 2.1737 0.095 Uiso 1 1 calc R . . C54 C -1.7018(10) -1.9911(13) 2.1573(6) 0.062(4) Uani 1 1 d . . . C55 C -1.6478(11) -2.1626(11) 2.1356(7) 0.076(4) Uani 1 1 d . . . H55A H -1.7128 -2.1410 2.1130 0.091 Uiso 1 1 calc R . . H55B H -1.6595 -2.1908 2.1781 0.091 Uiso 1 1 calc R . . C56 C -1.5504(12) -2.2488(12) 2.1076(11) 0.110(7) Uani 1 1 d . . . H56A H -1.4855 -2.2582 2.1261 0.132 Uiso 1 1 calc R . . H56B H -1.5549 -2.3184 2.1186 0.132 Uiso 1 1 calc R . . C57 C -1.6008(12) -2.2539(12) 2.0129(9) 0.082(5) Uani 1 1 d . . . H57A H -1.5901 -2.3288 2.0290 0.099 Uiso 1 1 calc R . . H57B H -1.6773 -2.2042 2.0186 0.099 Uiso 1 1 calc R . . C58 C -1.4277(12) -1.7552(15) 2.0482(10) 0.096(6) Uani 1 1 d . . . H58A H -1.5033 -1.7029 2.0538 0.115 Uiso 1 1 calc R . . H58B H -1.3828 -1.7374 2.0704 0.115 Uiso 1 1 calc R . . C59 C -1.4278(12) -1.8801(15) 2.1362(11) 0.113(7) Uani 1 1 d . . . H59A H -1.3965 -1.8410 2.1528 0.135 Uiso 1 1 calc R . . H59B H -1.3870 -1.9582 2.1520 0.135 Uiso 1 1 calc R . . C60 C -1.5372(14) -1.8449(14) 2.1580(7) 0.094(5) Uani 1 1 d . . . H60A H -1.5821 -1.7698 2.1385 0.113 Uiso 1 1 calc R . . H60B H -1.5416 -1.8472 2.2022 0.113 Uiso 1 1 calc R . . S1 S -2.7387(3) -2.4895(3) 2.06501(17) 0.0755(11) Uani 1 1 d DU . . O5 O -2.8137(7) -2.4935(7) 2.0286(4) 0.092(3) Uani 1 1 d DU . . O6 O -2.7126(6) -2.5662(7) 2.1188(4) 0.082(3) Uani 1 1 d DU . . O7 O -2.6497(7) -2.4785(8) 2.0312(4) 0.092(3) Uani 1 1 d DU . . C61 C -2.8080(11) -2.3648(12) 2.0902(6) 0.100(4) Uani 1 1 d DU . . F1 F -2.8324(8) -2.2818(8) 2.0445(4) 0.138(4) Uani 1 1 d DU . . F2 F -2.8967(7) -2.3568(7) 2.1215(4) 0.135(4) Uani 1 1 d DU . . F3 F -2.7460(9) -2.3521(9) 2.1257(5) 0.149(4) Uani 1 1 d DU . . S2 S -2.8305(3) -2.2237(5) 2.6070(2) 0.1131(17) Uani 1 1 d DU . . O8 O -2.8953(10) -2.1724(13) 2.5587(6) 0.196(7) Uani 1 1 d DU . . O9 O -2.7421(9) -2.2071(14) 2.6139(6) 0.197(7) Uani 1 1 d DU . . O10 O -2.7988(13) -2.3360(10) 2.6247(8) 0.210(7) Uani 1 1 d DU . . C62 C -2.9183(12) -2.1677(14) 2.6670(7) 0.133(5) Uani 1 1 d DU . . F4 F -2.9522(9) -2.0606(10) 2.6610(6) 0.159(4) Uani 1 1 d DU . . F5 F -3.0095(8) -2.1792(11) 2.6736(6) 0.171(5) Uani 1 1 d DU . . F6 F -2.8725(8) -2.2107(11) 2.7186(5) 0.181(5) Uani 1 1 d DU . . S3 S -3.2541(10) -2.2467(11) 2.1707(7) 0.121(4) Uani 0.50 1 d PDU A 1 O11 O -3.216(2) -2.175(2) 2.1818(17) 0.251(13) Uani 0.50 1 d PDU A 1 O12 O -3.1789(18) -2.3539(16) 2.1713(14) 0.243(15) Uani 0.50 1 d PDU A 1 O13 O -3.3291(13) -2.2153(18) 2.1258(7) 0.111(8) Uani 0.50 1 d PDU A 1 C63 C -3.331(2) -2.250(2) 2.2380(10) 0.178(10) Uani 0.50 1 d PDU A 1 F7 F -3.368(3) -2.321(2) 2.2411(11) 0.284(14) Uani 0.50 1 d PDU A 1 F8 F -3.269(3) -2.273(3) 2.2832(11) 0.305(16) Uani 0.50 1 d PDU A 1 F9 F -3.4191(19) -2.1609(19) 2.2431(11) 0.194(9) Uani 0.50 1 d PDU A 1 S4 S -2.7042(16) -2.3305(15) 2.3322(9) 0.259(8) Uani 0.50 1 d PDU B 1 O14 O -2.778(3) -2.295(2) 2.3808(13) 0.246(13) Uani 0.50 1 d PDU B 1 O15 O -2.632(2) -2.4418(17) 2.3390(15) 0.245(12) Uani 0.50 1 d PDU B 1 O16 O -2.653(2) -2.270(2) 2.2987(11) 0.185(10) Uani 0.50 1 d PDU B 1 C64 C -2.797(2) -2.315(2) 2.2803(14) 0.323(14) Uani 0.50 1 d PDU B 1 F10 F -2.735(3) -2.349(4) 2.2328(15) 0.362(15) Uani 0.50 1 d PDU B 1 F11 F -2.853(3) -2.369(3) 2.3027(18) 0.264(13) Uani 0.50 1 d PDU B 1 F12 F -2.861(3) -2.211(2) 2.264(2) 0.327(15) Uani 0.50 1 d PDU B 1 Cl3 Cl -3.244(2) -2.260(2) 2.1535(13) 0.260(11) Uani 0.50 1 d PU C 2 Cl4 Cl -2.840(3) -2.295(2) 2.2959(12) 0.320(13) Uani 0.50 1 d PU 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 Ru1 0.0356(6) 0.0922(10) 0.0510(7) 0.0085(6) -0.0114(5) -0.0385(6) N4 0.049(6) 0.091(8) 0.027(6) 0.000(6) -0.002(5) -0.048(6) N5 0.011(4) 0.085(8) 0.038(6) -0.015(6) 0.015(4) -0.020(5) N6 0.028(5) 0.074(8) 0.052(6) -0.017(6) -0.003(5) -0.027(5) N7 0.024(5) 0.053(7) 0.058(7) -0.028(6) 0.018(4) -0.014(5) N8 0.012(4) 0.032(6) 0.081(7) -0.018(5) 0.013(4) 0.007(4) C1 0.049(9) 0.118(15) 0.076(11) 0.026(10) -0.012(8) -0.055(10) N1 0.044(6) 0.035(7) 0.112(10) 0.002(7) -0.038(7) -0.005(6) C2 0.048(8) 0.080(13) 0.063(10) -0.002(9) -0.025(8) 0.003(9) C3 0.083(13) 0.059(13) 0.164(19) 0.002(12) -0.056(12) -0.018(10) C4 0.085(14) 0.135(19) 0.16(2) -0.068(17) -0.050(13) -0.033(14) C5 0.054(10) 0.106(16) 0.19(2) 0.018(15) -0.049(12) -0.047(11) N2 0.028(6) 0.177(14) 0.054(8) 0.021(9) -0.007(5) -0.050(8) C6 0.044(9) 0.113(14) 0.131(15) 0.062(12) -0.034(9) -0.062(10) C7 0.047(10) 0.20(2) 0.109(15) -0.006(15) -0.024(10) -0.055(12) C8 0.096(15) 0.18(3) 0.19(3) 0.01(2) -0.021(16) -0.088(17) C9 0.078(12) 0.18(2) 0.072(12) -0.010(13) 0.019(10) -0.047(13) C10 0.033(7) 0.103(13) 0.066(10) 0.019(9) 0.010(7) -0.020(8) N3 0.021(6) 0.138(13) 0.067(9) -0.019(9) 0.018(5) 0.004(7) C11 0.052(10) 0.132(18) 0.099(15) -0.050(13) -0.014(10) -0.011(11) C12 0.068(11) 0.15(2) 0.144(18) -0.068(16) 0.031(11) -0.051(12) C13 0.127(18) 0.15(2) 0.19(3) -0.066(18) 0.010(17) -0.075(16) C14 0.086(13) 0.17(2) 0.108(15) -0.047(15) 0.032(11) -0.076(14) C15 0.083(11) 0.123(16) 0.079(12) -0.020(12) -0.002(9) -0.059(12) C16 0.044(7) 0.111(12) 0.057(9) -0.012(9) 0.002(7) -0.046(8) C17 0.060(9) 0.122(14) 0.057(9) 0.016(9) -0.029(7) -0.045(9) C18 0.026(7) 0.127(14) 0.101(12) -0.003(11) -0.026(7) -0.034(8) C19 0.057(8) 0.136(14) 0.033(8) 0.027(8) -0.034(7) -0.036(9) C20 0.048(7) 0.071(10) 0.046(8) 0.010(7) -0.024(6) -0.025(7) C21 0.052(8) 0.091(11) 0.044(8) -0.019(7) 0.025(6) -0.056(8) C22 0.029(6) 0.081(10) 0.067(9) 0.004(8) -0.016(6) -0.017(7) C23 0.035(6) 0.072(10) 0.053(8) -0.006(7) -0.006(6) -0.030(7) C24 0.035(6) 0.061(9) 0.045(7) 0.003(6) -0.013(5) -0.024(6) C25 0.025(6) 0.067(9) 0.029(7) 0.003(6) 0.001(5) -0.029(6) C26 0.045(7) 0.094(11) 0.043(8) -0.010(8) 0.002(6) -0.037(8) C27 0.037(7) 0.075(10) 0.057(9) 0.007(8) -0.010(6) -0.016(7) C28 0.026(7) 0.126(13) 0.056(9) -0.011(9) -0.010(6) -0.022(8) C29 0.028(7) 0.098(12) 0.069(10) -0.026(9) -0.002(7) -0.023(7) C30 0.031(6) 0.091(11) 0.060(9) -0.005(8) -0.003(6) -0.032(7) C31 0.025(6) 0.079(10) 0.028(7) -0.028(6) 0.010(5) -0.018(6) C32 0.062(8) 0.080(11) 0.063(9) 0.012(8) -0.023(7) -0.048(8) C33 0.068(9) 0.110(13) 0.070(11) -0.004(10) -0.002(8) -0.058(10) C34 0.021(6) 0.020(7) 0.073(10) -0.012(6) 0.006(6) 0.009(5) C35 0.021(6) 0.065(9) 0.038(7) -0.006(6) 0.004(5) -0.001(6) C36 0.019(6) 0.056(9) 0.077(10) -0.041(8) 0.004(6) -0.005(6) C37 0.038(7) 0.029(8) 0.085(10) 0.001(7) 0.003(7) -0.001(6) C38 0.021(6) 0.058(10) 0.086(10) -0.046(8) 0.027(6) 0.000(7) C39 0.045(8) 0.024(8) 0.127(13) -0.024(8) 0.006(8) -0.016(6) C40 0.034(6) 0.049(9) 0.045(7) -0.014(7) -0.002(5) -0.016(6) C41 0.024(6) 0.080(11) 0.065(9) -0.009(8) -0.001(6) -0.030(7) C42 0.050(8) 0.051(9) 0.060(8) -0.014(7) 0.001(6) -0.029(7) C43 0.029(6) 0.037(8) 0.045(7) 0.005(6) -0.009(5) -0.018(6) C44 0.029(7) 0.051(9) 0.098(11) -0.024(8) -0.009(7) -0.013(7) C45 0.019(6) 0.056(9) 0.099(11) -0.046(8) 0.017(6) 0.004(6) C46 0.015(6) 0.042(8) 0.088(9) -0.023(7) 0.011(6) 0.001(6) C47 0.040(7) 0.031(8) 0.090(10) -0.033(7) 0.003(7) -0.011(6) C48 0.034(7) 0.053(9) 0.086(10) -0.010(7) -0.005(6) -0.019(6) O1 0.053(6) 0.071(7) 0.085(7) -0.027(6) 0.009(5) -0.026(5) O2 0.071(7) 0.088(9) 0.127(10) -0.054(8) 0.026(7) -0.038(6) O3 0.074(7) 0.086(9) 0.128(10) -0.042(8) 0.027(7) -0.049(6) O4 0.039(5) 0.066(6) 0.089(7) -0.024(5) 0.007(5) -0.021(5) C49 0.057(9) 0.041(9) 0.059(9) -0.002(7) -0.014(7) 0.001(8) C50 0.064(10) 0.079(12) 0.094(12) -0.017(9) -0.005(9) -0.042(9) C51 0.070(11) 0.099(15) 0.070(11) -0.023(10) 0.009(9) -0.015(10) C52 0.048(9) 0.082(14) 0.089(12) 0.000(11) -0.013(8) -0.017(10) C53 0.082(11) 0.055(11) 0.087(12) -0.016(9) -0.012(9) -0.015(9) C54 0.027(7) 0.082(12) 0.064(9) 0.004(8) -0.006(6) -0.018(8) C55 0.080(10) 0.037(9) 0.112(13) -0.008(8) 0.012(9) -0.033(9) C56 0.052(10) 0.041(10) 0.23(2) -0.041(14) -0.018(13) -0.005(8) C57 0.067(10) 0.059(11) 0.141(17) -0.054(11) 0.013(11) -0.034(9) C58 0.059(10) 0.109(17) 0.145(18) -0.062(14) 0.001(11) -0.044(10) C59 0.055(10) 0.104(15) 0.21(2) -0.070(16) 0.014(13) -0.048(10) C60 0.122(15) 0.108(14) 0.085(12) -0.043(11) 0.000(10) -0.068(12) S1 0.071(2) 0.090(3) 0.072(3) 0.004(2) -0.018(2) -0.045(2) O5 0.084(7) 0.085(7) 0.115(8) 0.028(6) -0.050(6) -0.052(6) O6 0.066(6) 0.092(7) 0.076(6) 0.007(5) -0.019(5) -0.032(5) O7 0.080(6) 0.092(8) 0.110(8) -0.003(6) 0.009(5) -0.053(6) C61 0.110(11) 0.094(8) 0.106(13) -0.003(6) 0.010(8) -0.061(9) F1 0.168(9) 0.092(6) 0.160(9) 0.029(6) -0.021(7) -0.079(7) F2 0.114(7) 0.089(7) 0.169(10) -0.007(6) 0.047(6) -0.034(6) F3 0.196(10) 0.154(10) 0.145(9) -0.052(7) -0.009(7) -0.108(9) S2 0.064(3) 0.156(5) 0.131(4) 0.012(4) -0.035(2) -0.067(3) O8 0.129(11) 0.259(15) 0.144(10) -0.078(10) -0.080(8) -0.002(11) O9 0.109(9) 0.355(18) 0.169(12) 0.054(13) -0.035(8) -0.170(12) O10 0.197(16) 0.160(9) 0.262(19) -0.013(10) -0.013(13) -0.076(10) C62 0.110(12) 0.188(12) 0.113(9) 0.015(12) -0.013(8) -0.089(13) F4 0.119(8) 0.176(9) 0.172(11) -0.008(7) -0.004(7) -0.065(7) F5 0.099(7) 0.237(13) 0.192(11) -0.034(10) 0.014(6) -0.093(9) F6 0.106(8) 0.245(13) 0.119(7) 0.026(8) -0.027(6) -0.032(8) S3 0.096(7) 0.104(8) 0.168(9) -0.076(8) -0.073(6) -0.011(6) O11 0.20(3) 0.21(2) 0.44(4) -0.22(3) 0.04(2) -0.112(19) O12 0.167(18) 0.132(15) 0.37(3) -0.19(2) -0.223(16) 0.094(14) O13 0.050(11) 0.148(19) 0.065(11) 0.037(12) -0.029(8) -0.001(11) C63 0.36(3) 0.11(3) 0.082(12) -0.02(2) -0.061(13) -0.101(17) F7 0.62(5) 0.22(2) 0.115(19) -0.01(2) 0.01(2) -0.28(3) F8 0.43(4) 0.27(3) 0.148(12) -0.07(2) -0.13(2) -0.05(3) F9 0.25(2) 0.18(2) 0.15(2) -0.036(17) 0.032(14) -0.102(19) S4 0.31(2) 0.199(16) 0.34(2) -0.080(17) 0.090(14) -0.179(16) O14 0.29(4) 0.20(3) 0.28(2) -0.01(2) 0.11(2) -0.18(3) O15 0.37(3) 0.167(17) 0.29(4) -0.09(2) 0.06(2) -0.196(18) O16 0.26(3) 0.14(2) 0.13(2) -0.033(18) 0.096(18) -0.09(2) C64 0.36(3) 0.28(3) 0.37(3) -0.09(3) 0.037(14) -0.181(17) F10 0.39(2) 0.36(2) 0.339(18) -0.068(17) 0.028(15) -0.178(16) F11 0.320(19) 0.22(2) 0.30(2) -0.091(16) -0.013(14) -0.141(17) F12 0.30(3) 0.26(2) 0.57(5) -0.12(2) -0.04(2) -0.227(18) Cl3 0.25(2) 0.21(2) 0.28(2) -0.081(17) -0.022(18) -0.050(16) Cl4 0.41(3) 0.23(2) 0.27(2) -0.152(19) 0.029(19) -0.06(2) _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 N5 1.953(8) . ? Ru1 N2 1.954(7) . ? Ru1 N4 2.022(9) . ? Ru1 N1 2.049(9) . ? Ru1 N3 2.049(10) . ? Ru1 N6 2.069(9) . ? N4 C16 1.336(14) . ? N4 C20 1.371(13) . ? N5 C21 1.328(13) . ? N5 C25 1.340(12) . ? N6 C30 1.343(12) . ? N6 C26 1.383(14) . ? N7 C38 1.262(14) . ? N7 C42 1.350(13) . ? N7 C37 1.474(13) . ? N8 C46 1.294(14) . ? N8 C45 1.344(14) . ? N8 C48 1.475(13) . ? C1 N1 1.3900 . ? C1 C5 1.3900 . ? C1 C6 1.395(14) . ? N1 C2 1.3900 . ? 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 H5A 0.9500 . ? N2 C6 1.3900 . ? N2 C10 1.3900 . ? C6 C7 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 1.490(14) . ? N3 C11 1.3900 . ? N3 C15 1.3900 . ? C11 C12 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 H15A 0.9500 . ? C16 C17 1.399(15) . ? C16 H16A 0.9500 . ? C17 C18 1.386(17) . ? C17 H17A 0.9500 . ? C18 C19 1.380(17) . ? C18 H18A 0.9500 . ? C19 C20 1.371(14) . ? C19 H19A 0.9500 . ? C20 C21 1.474(15) . ? C21 C22 1.396(14) . ? C22 C23 1.442(15) . ? C22 H22A 0.9500 . ? C23 C24 1.409(13) . ? C23 C31 1.467(14) . ? C24 C25 1.338(13) . ? C24 H24A 0.9500 . ? C25 C26 1.486(14) . ? C26 C27 1.345(15) . ? C27 C28 1.364(15) . ? C27 H27A 0.9500 . ? C28 C29 1.361(16) . ? C28 H28A 0.9500 . ? C29 C30 1.390(16) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.348(15) . ? C31 C32 1.378(14) . ? C32 C33 1.373(16) . ? C32 H32A 0.9500 . ? C33 C34 1.364(16) . ? C33 H33A 0.9500 . ? C34 C35 1.400(15) . ? C34 C37 1.528(15) . ? C35 C36 1.385(15) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.323(14) . ? C38 H38A 0.9500 . ? C39 C40 1.394(14) . ? C39 H39A 0.9500 . ? C40 C41 1.380(15) . ? C40 C43 1.521(15) . ? C41 C42 1.373(15) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C44 1.318(15) . ? C43 C47 1.444(14) . ? C44 C45 1.369(15) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C47 1.340(14) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 C48 1.51(2) 2_219 ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? O1 C54 1.352(15) . ? O1 C55 1.395(14) . ? O2 C57 1.408(16) . ? O2 C56 1.41(2) . ? O3 C59 1.42(2) . ? O3 C58 1.451(19) . ? O4 C49 1.374(15) . ? O4 C60 1.472(15) . ? C49 C50 1.397(18) . ? C49 C54 1.418(18) . ? C50 C51 1.425(19) . ? C50 H50A 0.9500 . ? C51 C52 1.30(2) . ? C51 H51A 0.9500 . ? C52 C53 1.389(19) . ? C52 H52A 0.9500 . ? C53 C54 1.380(18) . ? C53 H53A 0.9500 . ? C55 C56 1.529(19) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.391(19) 2_219 ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C57 1.391(19) 2_219 ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.44(2) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? S1 O6 1.413(8) . ? S1 O5 1.438(7) . ? S1 O7 1.442(8) . ? S1 C61 1.752(16) . ? C61 F2 1.330(11) . ? C61 F1 1.336(11) . ? C61 F3 1.339(12) . ? S2 O8 1.364(9) . ? S2 O9 1.396(9) . ? S2 O10 1.414(11) . ? S2 C62 1.772(17) . ? C62 F6 1.295(12) . ? C62 F4 1.340(13) . ? C62 F5 1.352(12) . ? S3 O12 1.391(13) . ? S3 O11 1.407(14) . ? S3 O13 1.408(13) . ? S3 C63 1.77(2) . ? C63 F9 1.309(15) . ? C63 F7 1.311(15) . ? C63 F8 1.317(15) . ? S4 O15 1.413(14) . ? S4 O16 1.415(13) . ? S4 O14 1.419(14) . ? S4 C64 1.77(2) . ? C64 F10 1.324(15) . ? C64 F11 1.323(15) . ? C64 F12 1.321(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 N5 Ru1 N2 175.0(5) . . ? N5 Ru1 N4 79.9(4) . . ? N2 Ru1 N4 96.9(3) . . ? N5 Ru1 N1 105.1(4) . . ? N2 Ru1 N1 79.1(5) . . ? N4 Ru1 N1 97.7(4) . . ? N5 Ru1 N3 95.8(5) . . ? N2 Ru1 N3 80.1(5) . . ? N4 Ru1 N3 86.0(4) . . ? N1 Ru1 N3 159.1(5) . . ? N5 Ru1 N6 78.5(4) . . ? N2 Ru1 N6 104.5(3) . . ? N4 Ru1 N6 158.3(3) . . ? N1 Ru1 N6 89.7(3) . . ? N3 Ru1 N6 94.3(4) . . ? C16 N4 C20 116.6(9) . . ? C16 N4 Ru1 128.4(7) . . ? C20 N4 Ru1 114.6(7) . . ? C21 N5 C25 120.5(9) . . ? C21 N5 Ru1 118.3(7) . . ? C25 N5 Ru1 121.1(6) . . ? C30 N6 C26 118.8(10) . . ? C30 N6 Ru1 126.6(8) . . ? C26 N6 Ru1 114.5(7) . . ? C38 N7 C42 118.0(10) . . ? C38 N7 C37 124.1(10) . . ? C42 N7 C37 116.8(11) . . ? C46 N8 C45 119.0(9) . . ? C46 N8 C48 121.6(10) . . ? C45 N8 C48 119.4(10) . . ? N1 C1 C5 120.0 . . ? N1 C1 C6 117.5(11) . . ? C5 C1 C6 122.5(11) . . ? C1 N1 C2 120.0 . . ? C1 N1 Ru1 112.6(8) . . ? C2 N1 Ru1 127.3(8) . . ? C3 C2 N1 120.0 . . ? C3 C2 H2A 120.0 . . ? N1 C2 H2A 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C1 120.0 . . ? C4 C5 H5A 120.0 . . ? C1 C5 H5A 120.0 . . ? C6 N2 C10 120.0 . . ? C6 N2 Ru1 119.2(7) . . ? C10 N2 Ru1 120.5(7) . . ? N2 C6 C7 120.0 . . ? N2 C6 C1 111.5(10) . . ? C7 C6 C1 128.4(10) . . ? C8 C7 C6 120.0 . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 N2 120.0 . . ? C9 C10 C11 130.8(9) . . ? N2 C10 C11 109.2(9) . . ? C11 N3 C15 120.0 . . ? C11 N3 Ru1 112.6(8) . . ? C15 N3 Ru1 126.7(8) . . ? C12 C11 N3 120.0 . . ? C12 C11 C10 123.1(11) . . ? N3 C11 C10 116.9(11) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C14 C15 N3 120.0 . . ? C14 C15 H15A 120.0 . . ? N3 C15 H15A 120.0 . . ? N4 C16 C17 124.4(11) . . ? N4 C16 H16A 117.8 . . ? C17 C16 H16A 117.8 . . ? C18 C17 C16 115.7(12) . . ? C18 C17 H17A 122.2 . . ? C16 C17 H17A 122.2 . . ? C19 C18 C17 122.7(11) . . ? C19 C18 H18A 118.7 . . ? C17 C18 H18A 118.7 . . ? C20 C19 C18 116.5(12) . . ? C20 C19 H19A 121.8 . . ? C18 C19 H19A 121.8 . . ? N4 C20 C19 124.1(11) . . ? N4 C20 C21 113.1(9) . . ? C19 C20 C21 122.8(11) . . ? N5 C21 C22 121.4(11) . . ? N5 C21 C20 113.9(9) . . ? C22 C21 C20 124.5(11) . . ? C21 C22 C23 118.8(10) . . ? C21 C22 H22A 120.6 . . ? C23 C22 H22A 120.6 . . ? C24 C23 C22 115.8(10) . . ? C24 C23 C31 122.6(10) . . ? C22 C23 C31 121.3(9) . . ? C25 C24 C23 121.2(10) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C24 C25 N5 122.3(9) . . ? C24 C25 C26 125.5(10) . . ? N5 C25 C26 112.2(9) . . ? C27 C26 N6 119.9(10) . . ? C27 C26 C25 126.3(11) . . ? N6 C26 C25 113.6(10) . . ? C26 C27 C28 122.1(12) . . ? C26 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 . . ? C27 C28 C29 118.1(12) . . ? C27 C28 H28A 121.0 . . ? C29 C28 H28A 121.0 . . ? C28 C29 C30 120.1(11) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? N6 C30 C29 120.5(11) . . ? N6 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C36 C31 C32 117.7(11) . . ? C36 C31 C23 121.2(10) . . ? C32 C31 C23 121.0(10) . . ? C33 C32 C31 120.4(12) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C34 C33 C32 122.5(13) . . ? C34 C33 H33A 118.8 . . ? C32 C33 H33A 118.8 . . ? C33 C34 C35 117.1(11) . . ? C33 C34 C37 123.0(12) . . ? C35 C34 C37 119.3(11) . . ? C36 C35 C34 119.4(11) . . ? C36 C35 H35A 120.3 . . ? C34 C35 H35A 120.3 . . ? C31 C36 C35 122.8(11) . . ? C31 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? N7 C37 C34 110.1(9) . . ? N7 C37 H37A 109.6 . . ? C34 C37 H37A 109.6 . . ? N7 C37 H37B 109.6 . . ? C34 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? N7 C38 C39 126.8(12) . . ? N7 C38 H38A 116.6 . . ? C39 C38 H38A 116.6 . . ? C38 C39 C40 118.0(12) . . ? C38 C39 H39A 121.0 . . ? C40 C39 H39A 121.0 . . ? C41 C40 C39 117.0(10) . . ? C41 C40 C43 122.3(10) . . ? C39 C40 C43 120.7(11) . . ? C42 C41 C40 119.6(11) . . ? C42 C41 H41A 120.2 . . ? C40 C41 H41A 120.2 . . ? N7 C42 C41 120.6(12) . . ? N7 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C44 C43 C47 116.6(10) . . ? C44 C43 C40 125.1(10) . . ? C47 C43 C40 118.3(11) . . ? C43 C44 C45 123.3(12) . . ? C43 C44 H44A 118.4 . . ? C45 C44 H44A 118.4 . . ? N8 C45 C44 119.1(12) . . ? N8 C45 H45A 120.4 . . ? C44 C45 H45A 120.4 . . ? N8 C46 C47 125.2(11) . . ? N8 C46 H46A 117.4 . . ? C47 C46 H46A 117.4 . . ? C46 C47 C43 116.8(11) . . ? C46 C47 H47A 121.6 . . ? C43 C47 H47A 121.6 . . ? N8 C48 C48 109.5(13) . 2_219 ? N8 C48 H48A 109.8 . . ? C48 C48 H48A 109.8 2_219 . ? N8 C48 H48B 109.8 . . ? C48 C48 H48B 109.8 2_219 . ? H48A C48 H48B 108.2 . . ? C54 O1 C55 115.0(11) . . ? C57 O2 C56 113.4(14) . . ? C59 O3 C58 111.9(14) . . ? C49 O4 C60 118.4(11) . . ? O4 C49 C50 122.2(13) . . ? O4 C49 C54 118.4(12) . . ? C50 C49 C54 119.5(14) . . ? C49 C50 C51 118.4(14) . . ? C49 C50 H50A 120.8 . . ? C51 C50 H50A 120.8 . . ? C52 C51 C50 121.5(16) . . ? C52 C51 H51A 119.2 . . ? C50 C51 H51A 119.2 . . ? C51 C52 C53 121.3(16) . . ? C51 C52 H52A 119.4 . . ? C53 C52 H52A 119.4 . . ? C54 C53 C52 120.9(15) . . ? C54 C53 H53A 119.5 . . ? C52 C53 H53A 119.5 . . ? O1 C54 C53 126.0(15) . . ? O1 C54 C49 115.6(11) . . ? C53 C54 C49 118.4(15) . . ? O1 C55 C56 106.4(11) . . ? O1 C55 H55A 110.5 . . ? C56 C55 H55A 110.5 . . ? O1 C55 H55B 110.5 . . ? C56 C55 H55B 110.5 . . ? H55A C55 H55B 108.6 . . ? O2 C56 C55 116.2(14) . . ? O2 C56 H56A 108.2 . . ? C55 C56 H56A 108.2 . . ? O2 C56 H56B 108.2 . . ? C55 C56 H56B 108.2 . . ? H56A C56 H56B 107.4 . . ? C58 C57 O2 109.4(14) 2_219 . ? C58 C57 H57A 109.8 2_219 . ? O2 C57 H57A 109.8 . . ? C58 C57 H57B 109.8 2_219 . ? O2 C57 H57B 109.8 . . ? H57A C57 H57B 108.2 . . ? C57 C58 O3 110.7(15) 2_219 . ? C57 C58 H58A 109.5 2_219 . ? O3 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 2_219 . ? O3 C58 H58B 109.5 . . ? H58A C58 H58B 108.1 . . ? O3 C59 C60 115.1(16) . . ? O3 C59 H59A 108.5 . . ? C60 C59 H59A 108.5 . . ? O3 C59 H59B 108.5 . . ? C60 C59 H59B 108.5 . . ? H59A C59 H59B 107.5 . . ? C59 C60 O4 106.7(13) . . ? C59 C60 H60A 110.4 . . ? O4 C60 H60A 110.4 . . ? C59 C60 H60B 110.4 . . ? O4 C60 H60B 110.4 . . ? H60A C60 H60B 108.6 . . ? O6 S1 O5 114.3(5) . . ? O6 S1 O7 115.6(5) . . ? O5 S1 O7 114.1(6) . . ? O6 S1 C61 103.9(6) . . ? O5 S1 C61 104.5(6) . . ? O7 S1 C61 102.3(6) . . ? F2 C61 F1 109.5(11) . . ? F2 C61 F3 108.2(12) . . ? F1 C61 F3 105.1(11) . . ? F2 C61 S1 111.9(10) . . ? F1 C61 S1 111.7(10) . . ? F3 C61 S1 110.1(10) . . ? O8 S2 O9 122.5(10) . . ? O8 S2 O10 117.0(11) . . ? O9 S2 O10 106.7(10) . . ? O8 S2 C62 101.6(8) . . ? O9 S2 C62 103.2(8) . . ? O10 S2 C62 102.8(9) . . ? F6 C62 F4 107.0(15) . . ? F6 C62 F5 105.4(13) . . ? F4 C62 F5 104.0(13) . . ? F6 C62 S2 111.4(12) . . ? F4 C62 S2 112.4(11) . . ? F5 C62 S2 115.9(12) . . ? O12 S3 O11 116.7(16) . . ? O12 S3 O13 110.1(13) . . ? O11 S3 O13 121.0(18) . . ? O12 S3 C63 104.5(17) . . ? O11 S3 C63 98.7(15) . . ? O13 S3 C63 102.3(12) . . ? F9 C63 F7 102(2) . . ? F9 C63 F8 110(2) . . ? F7 C63 F8 112(2) . . ? F9 C63 S3 116.0(18) . . ? F7 C63 S3 110.4(17) . . ? F8 C63 S3 106.8(18) . . ? O15 S4 O16 109.3(18) . . ? O15 S4 O14 117(2) . . ? O16 S4 O14 123.2(18) . . ? O15 S4 C64 103.9(16) . . ? O16 S4 C64 102.0(16) . . ? O14 S4 C64 97.3(16) . . ? F10 C64 F11 115(3) . . ? F10 C64 F12 107(2) . . ? F11 C64 F12 111(2) . . ? F10 C64 S4 102(2) . . ? F11 C64 S4 112(2) . . ? F12 C64 S4 110(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.049 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.137 # Attachment '- dm30a.cif' data_dm30a _database_code_depnum_ccdc_archive 'CCDC 819992' #TrackingRef '- dm30a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C200 H210 B2 F50 N26 O82 S14 Zn4' _chemical_formula_weight 5971.88 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' Zn Zn 0.2839 1.4301 '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' _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 24.665(14) _cell_length_b 26.270(15) _cell_length_c 21.104(12) _cell_angle_alpha 90.00 _cell_angle_beta 108.612(7) _cell_angle_gamma 90.00 _cell_volume 12959(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6104 _exptl_absorpt_coefficient_mu 0.603 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.9421 _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 121682 _diffrn_reflns_av_R_equivalents 0.8375 _diffrn_reflns_av_sigmaI/netI 0.7726 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 22775 _reflns_number_gt 4281 _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. SADI, SIMU and DELU commands were used to restrain all seven triflate (CF3SO3-) ions and the single tetrafluoroborate (BF4-) ion as rigid groups. 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. ; _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^)+(0.1565P)^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 22775 _refine_ls_number_parameters 1534 _refine_ls_number_restraints 476 _refine_ls_R_factor_all 0.4726 _refine_ls_R_factor_gt 0.1241 _refine_ls_wR_factor_ref 0.4350 _refine_ls_wR_factor_gt 0.2584 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.934 _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 Zn1 Zn 1.12290(9) -0.87431(8) -0.00119(10) 0.0505(7) Uani 1 1 d . . . O1W O 1.1156(5) -0.8126(4) -0.0600(5) 0.063(4) Uani 1 1 d . . . H1WA H 1.1464 -0.8086 -0.0692 0.095 Uiso 1 1 d R . . H1WB H 1.1097 -0.7866 -0.0390 0.095 Uiso 1 1 d R . . B1 B 1.2004(12) -0.8110(10) 0.1156(13) 0.065(8) Uani 1 1 d . . . F32 F 1.2402(5) -0.8034(4) 0.0859(6) 0.082(4) Uani 1 1 d . . . F31 F 1.1573(5) -0.7734(4) 0.0954(5) 0.074(3) Uani 1 1 d . . . F30 F 1.2223(5) -0.8140(4) 0.1832(5) 0.089(4) Uani 1 1 d . . . F33 F 1.1687(5) -0.8617(4) 0.0920(5) 0.087(4) Uani 1 1 d . . . N1 N 1.0389(4) -0.8686(5) 0.0082(5) 0.038(4) Uani 1 1 d G . . C1 C 1.0223(6) -0.8320(4) 0.0458(5) 0.053(6) Uani 1 1 d G . . H1A H 1.0470 -0.8055 0.0653 0.063 Uiso 1 1 calc R . . C2 C 0.9688(6) -0.8350(5) 0.0543(5) 0.056(6) Uani 1 1 d G . . H2A H 0.9576 -0.8104 0.0795 0.067 Uiso 1 1 calc R . . C3 C 0.9318(4) -0.8746(6) 0.0252(6) 0.061(6) Uani 1 1 d G . . H3A H 0.8960 -0.8766 0.0309 0.074 Uiso 1 1 calc R . . C4 C 0.9485(5) -0.9112(4) -0.0124(6) 0.057(6) Uani 1 1 d G . . H4A H 0.9238 -0.9377 -0.0318 0.068 Uiso 1 1 calc R . . C5 C 1.0020(6) -0.9083(4) -0.0209(5) 0.042(5) Uani 1 1 d G . . N2 N 1.0809(6) -0.9369(3) -0.0491(4) 0.040(4) Uani 1 1 d G . . C6 C 1.0228(6) -0.9443(4) -0.0600(5) 0.046(5) Uani 1 1 d G . . C7 C 0.9945(4) -0.9844(5) -0.1000(6) 0.049(5) Uani 1 1 d G . . H7A H 0.9556 -0.9894 -0.1073 0.059 Uiso 1 1 calc R . . C8 C 1.0241(6) -1.0169(4) -0.1291(5) 0.042(5) Uani 1 1 d G . . C9 C 1.0822(6) -1.0095(4) -0.1183(5) 0.051(5) Uani 1 1 d G . . H9A H 1.1021 -1.0312 -0.1377 0.062 Uiso 1 1 calc R . . C10 C 1.1106(4) -0.9694(5) -0.0783(5) 0.044(5) Uani 1 1 d G . . C11 C 1.1700(5) -0.9580(5) -0.0637(5) 0.045(5) Uani 1 1 d G . . C12 C 1.2090(7) -0.9888(4) -0.0808(6) 0.060(6) Uani 1 1 d G . . H12A H 1.1970 -1.0192 -0.1035 0.072 Uiso 1 1 calc R . . C13 C 1.2660(6) -0.9742(6) -0.0639(7) 0.072(7) Uani 1 1 d G . . H13A H 1.2921 -0.9949 -0.0753 0.086 Uiso 1 1 calc R . . C14 C 1.2840(4) -0.9288(6) -0.0300(7) 0.070(7) Uani 1 1 d G . . H14A H 1.3222 -0.9190 -0.0187 0.084 Uiso 1 1 calc R . . C15 C 1.2450(6) -0.8980(4) -0.0129(5) 0.075(7) Uani 1 1 d G . . H15A H 1.2571 -0.8676 0.0098 0.091 Uiso 1 1 calc R . . N3 N 1.1880(5) -0.9126(4) -0.0298(5) 0.042(4) Uani 1 1 d G . . C16 C 0.9925(6) -1.0564(4) -0.1737(5) 0.042(5) Uani 1 1 d G . . C17 C 0.9421(6) -1.0757(5) -0.1674(5) 0.050(5) Uani 1 1 d G . . H17A H 0.9270 -1.0619 -0.1360 0.060 Uiso 1 1 calc R . . C18 C 0.9141(4) -1.1157(5) -0.2079(7) 0.060(6) Uani 1 1 d G . . H18A H 0.8803 -1.1286 -0.2036 0.072 Uiso 1 1 calc R . . C19 C 0.9366(6) -1.1363(4) -0.2548(6) 0.051(5) Uani 1 1 d G . . C20 C 0.9870(6) -1.1170(5) -0.2611(5) 0.051(5) Uani 1 1 d G . . H20A H 1.0021 -1.1309 -0.2925 0.061 Uiso 1 1 calc R . . C21 C 1.0150(4) -1.0771(5) -0.2206(6) 0.051(5) Uani 1 1 d G . . H21A H 1.0488 -1.0642 -0.2249 0.061 Uiso 1 1 calc R . . C22 C 0.9081(8) -1.1820(6) -0.2957(8) 0.053(5) Uani 1 1 d . . . H22A H 0.8669 -1.1773 -0.3123 0.063 Uiso 1 1 calc R . . H22B H 0.9217 -1.1863 -0.3337 0.063 Uiso 1 1 calc R . . N4 N 0.9227(6) -1.2278(3) -0.2514(5) 0.044(4) Uani 1 1 d G . . C23 C 0.8866(4) -1.2448(5) -0.2170(6) 0.056(6) Uani 1 1 d G . . H23A H 0.8511 -1.2295 -0.2243 0.067 Uiso 1 1 calc R . . C24 C 0.9034(6) -1.2848(5) -0.1718(6) 0.058(6) Uani 1 1 d G . . H24A H 0.8792 -1.2961 -0.1488 0.070 Uiso 1 1 calc R . . C25 C 0.9564(6) -1.3077(4) -0.1609(5) 0.044(5) Uani 1 1 d G . . C26 C 0.9925(4) -1.2907(5) -0.1952(7) 0.051(5) Uani 1 1 d G . . H26A H 1.0280 -1.3061 -0.1879 0.061 Uiso 1 1 calc R . . C27 C 0.9757(6) -1.2508(5) -0.2405(6) 0.068(6) Uani 1 1 d G . . H27A H 0.9999 -1.2394 -0.2634 0.082 Uiso 1 1 calc R . . C28 C 0.9678(6) -1.3503(4) -0.1152(5) 0.045(5) Uani 1 1 d G . . C29 C 0.9256(4) -1.3765(5) -0.0979(6) 0.046(5) Uani 1 1 d G . . H29A H 0.8875 -1.3669 -0.1159 0.055 Uiso 1 1 calc R . . C30 C 0.9404(5) -1.4173(4) -0.0536(6) 0.058(6) Uani 1 1 d G . . H30A H 0.9122 -1.4348 -0.0420 0.069 Uiso 1 1 calc R . . N5 N 0.9974(6) -1.4317(3) -0.0267(4) 0.050(4) Uani 1 1 d G . . C31 C 1.0395(4) -1.4055(4) -0.0439(5) 0.045(5) Uani 1 1 d G . . H31A H 1.0776 -1.4152 -0.0259 0.054 Uiso 1 1 calc R . . C32 C 1.0247(5) -1.3648(4) -0.0882(6) 0.049(6) Uani 1 1 d G . . H32A H 1.0529 -1.3472 -0.0998 0.059 Uiso 1 1 calc R . . C33 C 1.0109(7) -1.4752(6) 0.0202(8) 0.049(5) Uani 1 1 d . . . H33A H 0.9924 -1.4708 0.0541 0.059 Uiso 1 1 calc R . . H33B H 1.0519 -1.4773 0.0423 0.059 Uiso 1 1 calc R . . O1 O 1.0853(6) -0.5007(5) 0.1722(6) 0.067(4) Uani 1 1 d . . . O2 O 0.8545(6) -0.5373(6) -0.0804(7) 0.079(4) Uani 1 1 d . . . O3 O 0.8793(6) -0.4776(5) 0.0329(6) 0.067(4) Uani 1 1 d . . . O4 O 0.9766(6) -0.5042(5) 0.1548(6) 0.057(4) Uani 1 1 d . . . C34 C 1.0084(7) -0.5367(5) 0.2005(6) 0.056(6) Uani 1 1 d G . . C35 C 0.9868(6) -0.5707(7) 0.2368(8) 0.085(8) Uani 1 1 d G . . H35A H 0.9477 -0.5714 0.2308 0.102 Uiso 1 1 calc R . . C36 C 1.0234(9) -0.6037(5) 0.2822(7) 0.088(8) Uani 1 1 d G . . H36A H 1.0090 -0.6264 0.3065 0.105 Uiso 1 1 calc R . . C37 C 1.0818(9) -0.6026(5) 0.2912(6) 0.073(8) Uani 1 1 d G . . H37A H 1.1063 -0.6247 0.3216 0.087 Uiso 1 1 calc R . . C38 C 1.1034(6) -0.5686(7) 0.2549(8) 0.073(7) Uani 1 1 d G . . H38A H 1.1425 -0.5679 0.2609 0.087 Uiso 1 1 calc R . . C39 C 1.0667(8) -0.5357(5) 0.2095(6) 0.068(7) Uani 1 1 d G . . C40 C 1.1451(11) -0.4941(9) 0.1911(10) 0.087(8) Uani 1 1 d . . . H40A H 1.1630 -0.5250 0.1823 0.104 Uiso 1 1 calc R . . H40B H 1.1603 -0.4866 0.2385 0.104 Uiso 1 1 calc R . . C41 C 1.1574(9) -0.4510(9) 0.1515(11) 0.092(8) Uani 1 1 d . . . H41A H 1.1346 -0.4218 0.1555 0.111 Uiso 1 1 calc R . . H41B H 1.1974 -0.4416 0.1705 0.111 Uiso 1 1 calc R . . C42 C 0.8105(10) -0.5081(10) -0.0693(10) 0.100(9) Uani 1 1 d . . . H42A H 0.7737 -0.5245 -0.0890 0.120 Uiso 1 1 calc R . . H42B H 0.8091 -0.4745 -0.0888 0.120 Uiso 1 1 calc R . . C43 C 0.8248(8) -0.5044(8) 0.0063(10) 0.067(6) Uani 1 1 d . . . H43A H 0.7950 -0.4860 0.0173 0.081 Uiso 1 1 calc R . . H43B H 0.8278 -0.5382 0.0256 0.081 Uiso 1 1 calc R . . C44 C 0.8917(8) -0.4597(8) 0.0991(10) 0.064(6) Uani 1 1 d . . . H44A H 0.8564 -0.4480 0.1053 0.076 Uiso 1 1 calc R . . H44B H 0.9170 -0.4305 0.1051 0.076 Uiso 1 1 calc R . . C45 C 0.9192(9) -0.4985(8) 0.1531(9) 0.065(6) Uani 1 1 d . . . H45A H 0.9178 -0.4867 0.1961 0.078 Uiso 1 1 calc R . . H45B H 0.8992 -0.5308 0.1429 0.078 Uiso 1 1 calc R . . Zn2 Zn 1.40214(11) -0.20043(10) 0.01924(15) 0.0911(10) Uani 1 1 d . . . O2W O 1.3712(7) -0.1883(6) -0.0828(8) 0.131(6) Uani 1 1 d . . . H2WA H 1.3988 -0.1893 -0.0986 0.197 Uiso 1 1 d R . . H2WB H 1.3553 -0.1592 -0.0904 0.197 Uiso 1 1 d R . . O4W O 1.4297(7) -0.2273(6) 0.1191(8) 0.129(6) Uani 1 1 d . . . H4WA H 1.4653 -0.2335 0.1306 0.194 Uiso 1 1 d R . . H4WB H 1.4234 -0.2045 0.1444 0.194 Uiso 1 1 d R . . O3W O 1.4136(6) -0.2743(5) -0.0064(8) 0.129(6) Uani 1 1 d . . . H3WA H 1.4472 -0.2777 -0.0084 0.193 Uiso 1 1 d R . . H3WB H 1.4090 -0.2941 0.0233 0.193 Uiso 1 1 d R . . N101 N 1.3176(5) -0.1925(6) 0.0238(7) 0.081(6) Uani 1 1 d G . . C101 C 1.2793(8) -0.2328(5) 0.0138(7) 0.088(8) Uani 1 1 d G . . H10A H 1.2890 -0.2644 0.0007 0.105 Uiso 1 1 calc R . . C102 C 1.2266(7) -0.2259(6) 0.0233(8) 0.108(9) Uani 1 1 d G . . H10B H 1.2010 -0.2529 0.0166 0.130 Uiso 1 1 calc R . . C103 C 1.2121(5) -0.1787(8) 0.0429(7) 0.105(9) Uani 1 1 d G . . H10C H 1.1769 -0.1741 0.0493 0.126 Uiso 1 1 calc R . . C104 C 1.2504(8) -0.1383(5) 0.0529(7) 0.089(8) Uani 1 1 d G . . H10D H 1.2407 -0.1067 0.0660 0.107 Uiso 1 1 calc R . . C105 C 1.3031(6) -0.1452(5) 0.0433(7) 0.085(8) Uani 1 1 d G . . N102 N 1.3973(7) -0.1261(4) 0.0515(6) 0.071(5) Uani 1 1 d G . . C106 C 1.3462(6) -0.1067(5) 0.0560(6) 0.067(6) Uani 1 1 d G . . C107 C 1.3427(5) -0.0559(6) 0.0725(7) 0.078(7) Uani 1 1 d G . . H10E H 1.3085 -0.0429 0.0755 0.093 Uiso 1 1 calc R . . C108 C 1.3902(7) -0.0245(4) 0.0846(6) 0.062(6) Uani 1 1 d G . . C109 C 1.4413(6) -0.0438(6) 0.0801(7) 0.076(7) Uani 1 1 d G . . H10F H 1.4731 -0.0228 0.0882 0.091 Uiso 1 1 calc R . . C110 C 1.4449(5) -0.0946(6) 0.0636(7) 0.069(6) Uani 1 1 d G . . C111 C 1.4935(7) -0.1199(6) 0.0569(7) 0.083(7) Uani 1 1 d G . . C112 C 1.5477(9) -0.0982(5) 0.0761(7) 0.087(8) Uani 1 1 d G . . H11A H 1.5528 -0.0647 0.0914 0.104 Uiso 1 1 calc R . . C113 C 1.5943(6) -0.1264(8) 0.0725(7) 0.088(7) Uani 1 1 d G . . H11B H 1.6306 -0.1118 0.0854 0.105 Uiso 1 1 calc R . . C114 C 1.5868(7) -0.1763(8) 0.0497(8) 0.109(9) Uani 1 1 d G . . H11C H 1.6179 -0.1952 0.0473 0.131 Uiso 1 1 calc R . . C115 C 1.5326(9) -0.1981(5) 0.0304(7) 0.093(8) Uani 1 1 d G . . H11D H 1.5275 -0.2315 0.0151 0.112 Uiso 1 1 calc R . . N103 N 1.4859(6) -0.1699(7) 0.0340(6) 0.081(6) Uani 1 1 d G . . C116 C 1.3853(6) 0.0284(4) 0.1059(6) 0.056(6) Uani 1 1 d G . . C117 C 1.3444(5) 0.0411(5) 0.1358(6) 0.066(6) Uani 1 1 d G . . H11E H 1.3200 0.0162 0.1425 0.080 Uiso 1 1 calc R . . C118 C 1.3399(5) 0.0909(6) 0.1555(6) 0.051(5) Uani 1 1 d G . . H11F H 1.3125 0.0994 0.1755 0.061 Uiso 1 1 calc R . . C119 C 1.3763(6) 0.1282(4) 0.1455(6) 0.059(6) Uani 1 1 d G . . C120 C 1.4172(5) 0.1156(5) 0.1156(6) 0.071(7) Uani 1 1 d G . . H12B H 1.4416 0.1405 0.1088 0.085 Uiso 1 1 calc R . . C121 C 1.4217(5) 0.0657(6) 0.0958(6) 0.059(6) Uani 1 1 d G . . H12C H 1.4491 0.0572 0.0759 0.071 Uiso 1 1 calc R . . C122 C 1.3718(8) 0.1777(8) 0.1761(10) 0.071(7) Uani 1 1 d . . . H12D H 1.3948 0.1771 0.2229 0.085 Uiso 1 1 calc R . . H12E H 1.3323 0.1835 0.1736 0.085 Uiso 1 1 calc R . . N104 N 1.3913(6) 0.2201(4) 0.1422(7) 0.065(5) Uani 1 1 d G . . C123 C 1.3575(4) 0.2381(5) 0.0802(7) 0.069(6) Uani 1 1 d G . . H12F H 1.3221 0.2232 0.0590 0.082 Uiso 1 1 calc R . . C124 C 1.3765(5) 0.2783(5) 0.0500(5) 0.057(6) Uani 1 1 d G . . H12G H 1.3539 0.2903 0.0086 0.069 Uiso 1 1 calc R . . C125 C 1.4294(6) 0.3005(4) 0.0818(6) 0.048(5) Uani 1 1 d G . . C126 C 1.4632(4) 0.2825(5) 0.1437(6) 0.068(6) Uani 1 1 d G . . H12H H 1.4986 0.2974 0.1650 0.082 Uiso 1 1 calc R . . C127 C 1.4442(6) 0.2423(5) 0.1739(5) 0.070(6) Uani 1 1 d G . . H12I H 1.4668 0.2303 0.2154 0.084 Uiso 1 1 calc R . . C128 C 1.4492(7) 0.3457(4) 0.0530(7) 0.052(5) Uani 1 1 d G . . C129 C 1.4091(4) 0.3767(6) 0.0085(7) 0.067(6) Uani 1 1 d G . . H12J H 1.3705 0.3684 -0.0042 0.080 Uiso 1 1 calc R . . C130 C 1.4267(6) 0.4203(5) -0.0168(5) 0.061(6) Uani 1 1 d G . . H13B H 1.3999 0.4411 -0.0465 0.074 Uiso 1 1 calc R . . N105 N 1.4845(7) 0.4328(4) 0.0023(6) 0.061(5) Uani 1 1 d G . . C131 C 1.5246(5) 0.4017(6) 0.0467(7) 0.062(6) Uani 1 1 d G . . H13C H 1.5632 0.4100 0.0594 0.074 Uiso 1 1 calc R . . C132 C 1.5070(6) 0.3581(5) 0.0720(6) 0.063(6) Uani 1 1 d G . . H13D H 1.5338 0.3374 0.1018 0.076 Uiso 1 1 calc R . . C133 C 1.5028(9) 0.4790(6) -0.0212(9) 0.068(6) Uani 1 1 d . . . H13E H 1.4794 0.4855 -0.0671 0.081 Uiso 1 1 calc R . . H13F H 1.5423 0.4758 -0.0199 0.081 Uiso 1 1 calc R . . O101 O 1.5260(8) -0.5397(6) 0.1739(7) 0.082(5) Uani 1 1 d . . . O102 O 1.6205(7) -0.5104(6) 0.1250(7) 0.093(5) Uani 1 1 d . . . O103 O 1.3487(10) -0.4843(11) -0.0141(12) 0.187(11) Uani 1 1 d . . . O104 O 1.4169(8) -0.5289(7) 0.1137(8) 0.099(6) Uani 1 1 d . . . C134 C 1.4286(12) -0.5648(7) 0.1632(8) 0.110(11) Uani 1 1 d G . . C135 C 1.3939(7) -0.5968(9) 0.1861(12) 0.130(14) Uani 1 1 d G . . H13G H 1.3544 -0.5956 0.1666 0.156 Uiso 1 1 calc R . . C136 C 1.4183(11) -0.6304(7) 0.2383(12) 0.132(14) Uani 1 1 d G . . H13H H 1.3951 -0.6517 0.2536 0.159 Uiso 1 1 calc R . . C137 C 1.4774(12) -0.6321(7) 0.2675(8) 0.149(16) Uani 1 1 d G . . H13I H 1.4937 -0.6546 0.3024 0.179 Uiso 1 1 calc R . . C138 C 1.5121(7) -0.6002(9) 0.2446(11) 0.18(2) Uani 1 1 d G . . H13J H 1.5516 -0.6013 0.2641 0.219 Uiso 1 1 calc R . . C139 C 1.4876(11) -0.5666(8) 0.1924(11) 0.103(10) Uani 1 1 d G . . C140 C 1.5839(12) -0.5402(10) 0.2132(11) 0.099(8) Uani 1 1 d . . . H14B H 1.6006 -0.5731 0.2095 0.119 Uiso 1 1 calc R . . H14C H 1.5873 -0.5347 0.2598 0.119 Uiso 1 1 calc R . . C141 C 1.6149(11) -0.4998(9) 0.1903(12) 0.100(8) Uani 1 1 d . . . H14D H 1.5948 -0.4678 0.1883 0.120 Uiso 1 1 calc R . . H14E H 1.6528 -0.4960 0.2226 0.120 Uiso 1 1 calc R . . C142 C 1.6719(11) -0.5326(9) 0.1253(14) 0.114(10) Uani 1 1 d . . . H14F H 1.6780 -0.5636 0.1517 0.137 Uiso 1 1 calc R . . H14G H 1.7031 -0.5094 0.1466 0.137 Uiso 1 1 calc R . . C143 C 1.6730(17) -0.5452(12) 0.0546(18) 0.160(17) Uani 1 1 d . . . H14H H 1.7126 -0.5489 0.0562 0.192 Uiso 1 1 calc R . . H14I H 1.6544 -0.5778 0.0414 0.192 Uiso 1 1 calc R . . C144 C 1.3494(12) -0.4676(16) 0.0527(16) 0.153(15) Uani 1 1 d . . . H14J H 1.3128 -0.4530 0.0508 0.183 Uiso 1 1 calc R . . H14K H 1.3791 -0.4424 0.0705 0.183 Uiso 1 1 calc R . . C145 C 1.3610(17) -0.5141(13) 0.0944(19) 0.150(14) Uani 1 1 d . . . H14L H 1.3501 -0.5081 0.1340 0.180 Uiso 1 1 calc R . . H14M H 1.3374 -0.5416 0.0695 0.180 Uiso 1 1 calc R . . S1 S 1.1877(2) -0.9944(2) 0.1202(3) 0.0646(16) Uani 1 1 d DU . . O5 O 1.1280(4) -0.9864(4) 0.0815(5) 0.061(3) Uani 1 1 d DU . . O6 O 1.2168(5) -0.9504(4) 0.1566(6) 0.071(4) Uani 1 1 d DU . . O7 O 1.2203(5) -1.0219(5) 0.0844(7) 0.094(4) Uani 1 1 d DU . . C46 C 1.1837(7) -1.0373(6) 0.1848(8) 0.103(6) Uani 1 1 d DU . . F1 F 1.1569(6) -1.0796(5) 0.1564(7) 0.145(6) Uani 1 1 d DU . . F2 F 1.1576(6) -1.0180(6) 0.2244(7) 0.153(5) Uani 1 1 d DU . . F3 F 1.2366(6) -1.0504(5) 0.2205(7) 0.153(6) Uani 1 1 d DU . . S2 S 1.5165(4) -0.3446(3) 0.1454(4) 0.134(3) Uani 1 1 d DU . . O8 O 1.4812(9) -0.3459(7) 0.0746(7) 0.206(10) Uani 1 1 d DU . . O9 O 1.5702(6) -0.3732(6) 0.1635(7) 0.125(6) Uani 1 1 d DU . . O10 O 1.5196(7) -0.2940(5) 0.1758(6) 0.118(5) Uani 1 1 d DU . . C47 C 1.4714(8) -0.3780(7) 0.1862(10) 0.152(7) Uani 1 1 d DU . . F4 F 1.4693(7) -0.4289(7) 0.1734(11) 0.235(8) Uani 1 1 d DU . . F5 F 1.4164(7) -0.3634(7) 0.1694(9) 0.203(7) Uani 1 1 d DU . . F6 F 1.4919(7) -0.3744(7) 0.2537(8) 0.202(7) Uani 1 1 d DU . . S3 S 0.9904(3) -1.2071(2) -0.4346(3) 0.0762(17) Uani 1 1 d DU . . O11 O 0.9660(6) -1.2428(4) -0.3986(6) 0.088(4) Uani 1 1 d DU . . O12 O 0.9799(6) -1.2196(4) -0.5040(5) 0.089(4) Uani 1 1 d DU . . O13 O 0.9809(7) -1.1544(4) -0.4228(6) 0.116(5) Uani 1 1 d DU . . C48 C 1.0647(8) -1.2130(7) -0.3977(8) 0.122(6) Uani 1 1 d DU . . F7 F 1.0828(7) -1.2607(6) -0.4026(7) 0.176(6) Uani 1 1 d DU . . F8 F 1.0785(7) -1.2026(6) -0.3317(7) 0.169(6) Uani 1 1 d DU . . F9 F 1.0938(8) -1.1811(7) -0.4240(9) 0.227(8) Uani 1 1 d DU . . S4 S 1.1754(4) -0.3406(3) -0.1124(5) 0.140(3) Uani 1 1 d DU . . O14 O 1.1589(8) -0.3917(6) -0.1071(12) 0.212(10) Uani 1 1 d DU . . O15 O 1.1350(7) -0.3018(6) -0.1096(10) 0.161(7) Uani 1 1 d DU . . C49 C 1.1646(9) -0.3340(7) -0.2010(10) 0.179(8) Uani 1 1 d DU . . F10 F 1.2023(9) -0.3670(8) -0.2115(11) 0.286(11) Uani 1 1 d DU . . F11 F 1.1783(10) -0.2882(7) -0.2180(11) 0.283(11) Uani 1 1 d DU . . F12 F 1.1126(9) -0.3458(8) -0.2426(10) 0.235(8) Uani 1 1 d DU . . S5 S 1.2366(3) -0.7732(2) -0.1278(3) 0.0836(19) Uani 1 1 d DU . . O16 O 1.2342(6) -0.3284(7) -0.0798(10) 0.184(8) Uani 1 1 d DU . . O17 O 1.1797(5) -0.7928(6) -0.1355(6) 0.099(5) Uani 1 1 d DU . . O18 O 1.2787(5) -0.7818(5) -0.0648(6) 0.092(4) Uani 1 1 d DU . . O19 O 1.2348(6) -0.7225(5) -0.1541(7) 0.115(5) Uani 1 1 d DU . . C50 C 1.2586(7) -0.8100(7) -0.1867(8) 0.112(6) Uani 1 1 d DU . . F13 F 1.3089(6) -0.7959(7) -0.1892(7) 0.188(7) Uani 1 1 d DU . . F14 F 1.2615(7) -0.8586(6) -0.1731(7) 0.171(6) Uani 1 1 d DU . . F15 F 1.2232(6) -0.8045(6) -0.2468(7) 0.153(6) Uani 1 1 d DU . . S6 S 1.3858(4) -0.0549(3) -0.1213(4) 0.122(3) Uani 1 1 d DU . . O20 O 1.3412(7) -0.0850(6) -0.1099(10) 0.156(7) Uani 1 1 d DU . . O21 O 1.4336(8) -0.0835(7) -0.1225(13) 0.216(9) Uani 1 1 d DU . . O22 O 1.3961(9) -0.0084(6) -0.0870(11) 0.206(9) Uani 1 1 d DU . . C51 C 1.3527(10) -0.0406(9) -0.2068(10) 0.265(13) Uani 1 1 d DU . . F16 F 1.3057(11) -0.0128(12) -0.2144(11) 0.356(15) Uani 1 1 d DU . . F17 F 1.3395(14) -0.0805(12) -0.2480(14) 0.406(17) Uani 1 1 d DU . . F18 F 1.3921(13) -0.0125(11) -0.2224(14) 0.368(15) Uani 1 1 d DU . . S7 S 1.3686(5) -0.2954(5) -0.2553(5) 0.182(4) Uani 1 1 d DU . . O23 O 1.3663(13) -0.3252(9) -0.2017(11) 0.286(13) Uani 1 1 d DU . . O24 O 1.4082(10) -0.2556(8) -0.2395(13) 0.271(12) Uani 1 1 d DU . . O25 O 1.3671(8) -0.3224(8) -0.3132(9) 0.194(9) Uani 1 1 d DU . . C52 C 1.3056(10) -0.2582(8) -0.2796(11) 0.236(12) Uani 1 1 d DU . . F19 F 1.2988(11) -0.2253(11) -0.3296(12) 0.341(13) Uani 1 1 d DU . . F20 F 1.2627(9) -0.2920(11) -0.2965(12) 0.347(14) Uani 1 1 d DU . . F21 F 1.3026(10) -0.2332(10) -0.2263(11) 0.320(13) Uani 1 1 d DU . . O5W O 1.4539(10) -0.1873(9) -0.1359(12) 0.229(11) Uani 1 1 d . . . H5WA H 1.4286 -0.2049 -0.1642 0.343 Uiso 1 1 d R . . H5WB H 1.4446 -0.1564 -0.1332 0.343 Uiso 1 1 d R . . O6W O 1.3409(6) -0.3304(5) -0.0907(8) 0.116(6) Uani 1 1 d . . . H6WA H 1.3222 -0.3267 -0.0636 0.174 Uiso 1 1 d R . . H6WB H 1.3183 -0.3339 -0.1304 0.174 Uiso 1 1 d R . . O1S O 1.2800(8) -0.8940(9) 0.4186(10) 0.148(9) Uani 1 1 d . . . O2S O 1.2057(8) -0.8949(6) 0.3412(9) 0.121(7) Uani 1 1 d . . . N1S N 1.2568(9) -0.8915(8) 0.3599(13) 0.090(7) Uani 1 1 d . . . C1S C 1.2873(10) -0.8811(9) 0.3150(11) 0.106(9) Uani 1 1 d . . . H1SA H 1.2614 -0.8815 0.2701 0.159 Uiso 1 1 calc R . . H1SB H 1.3162 -0.9065 0.3198 0.159 Uiso 1 1 calc R . . H1SC H 1.3049 -0.8482 0.3247 0.159 Uiso 1 1 calc R . . O3S O 1.2024(9) -0.8730(9) 0.5818(14) 0.198(12) Uani 1 1 d . . . O4S O 1.2750(10) -0.8456(12) 0.5628(16) 0.194(13) Uani 1 1 d . . . N2S N 1.2284(14) -0.8494(11) 0.5484(14) 0.137(11) Uani 1 1 d . . . C2S C 1.1885(10) -0.8169(8) 0.4976(11) 0.109(9) Uani 1 1 d . . . H2SA H 1.2081 -0.8020 0.4695 0.163 Uiso 1 1 calc R . . H2SB H 1.1742 -0.7905 0.5193 0.163 Uiso 1 1 calc R . . H2SC H 1.1571 -0.8372 0.4708 0.163 Uiso 1 1 calc R . . O5S O 1.1645(12) -1.1018(10) -0.2025(14) 0.199(13) Uani 1 1 d . . . O6S O 1.1594(14) -1.1261(11) -0.1191(14) 0.247(16) Uani 1 1 d . . . N3S N 1.1751(12) -1.1321(12) -0.1626(15) 0.139(11) Uani 1 1 d . . . C3S C 1.2150(15) -1.1710(14) -0.1649(18) 0.24(2) Uani 1 1 d . . . H3SA H 1.2244 -1.1678 -0.2055 0.359 Uiso 1 1 calc R . . H3SB H 1.1983 -1.2038 -0.1636 0.359 Uiso 1 1 calc R . . H3SC H 1.2491 -1.1674 -0.1273 0.359 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 Zn1 0.0562(16) 0.0477(15) 0.0480(14) -0.0015(12) 0.0170(12) -0.0051(12) O1W 0.093(10) 0.046(8) 0.069(9) 0.013(7) 0.049(8) 0.005(7) B1 0.07(2) 0.06(2) 0.045(18) -0.014(14) -0.020(16) 0.021(17) F32 0.056(8) 0.083(9) 0.121(11) 0.000(7) 0.050(8) -0.013(7) F31 0.091(9) 0.063(8) 0.076(8) -0.016(7) 0.038(7) -0.008(7) F30 0.115(10) 0.072(9) 0.053(8) -0.004(6) -0.011(7) -0.022(7) F33 0.096(9) 0.086(9) 0.074(8) -0.012(7) 0.019(7) -0.009(8) N1 0.027(9) 0.043(10) 0.045(9) 0.017(8) 0.011(8) -0.008(8) C1 0.083(18) 0.045(13) 0.039(12) -0.020(10) 0.032(12) -0.006(12) C2 0.065(16) 0.048(14) 0.049(13) 0.002(11) 0.010(12) 0.006(12) C3 0.068(16) 0.072(16) 0.060(14) -0.020(12) 0.042(12) 0.010(14) C4 0.036(14) 0.075(16) 0.058(14) 0.015(12) 0.013(11) -0.001(12) C5 0.059(15) 0.048(13) 0.005(9) 0.004(9) -0.007(10) 0.007(11) N2 0.075(12) 0.021(9) 0.028(8) -0.005(6) 0.021(9) 0.014(8) C6 0.046(14) 0.064(16) 0.043(13) 0.035(11) 0.035(11) 0.028(12) C7 0.065(15) 0.043(13) 0.039(12) 0.003(10) 0.015(11) -0.021(12) C8 0.045(14) 0.036(12) 0.045(12) 0.003(10) 0.015(11) 0.000(11) C9 0.040(14) 0.070(15) 0.027(11) 0.018(10) -0.014(9) -0.004(11) C10 0.016(11) 0.075(15) 0.034(11) 0.007(11) -0.002(9) -0.017(11) C11 0.068(16) 0.047(14) 0.015(10) 0.003(9) 0.005(10) -0.001(12) C12 0.054(15) 0.048(14) 0.081(15) -0.015(11) 0.027(13) -0.007(12) C13 0.069(19) 0.074(18) 0.084(17) -0.009(14) 0.041(14) 0.017(14) C14 0.044(14) 0.10(2) 0.063(15) 0.006(14) 0.017(12) 0.021(14) C15 0.068(18) 0.095(19) 0.069(15) 0.008(13) 0.030(14) -0.013(16) N3 0.040(10) 0.052(11) 0.037(9) 0.002(8) 0.015(8) -0.001(8) C16 0.053(14) 0.056(14) 0.016(10) 0.007(9) 0.012(10) 0.009(12) C17 0.062(15) 0.050(14) 0.032(12) 0.001(10) 0.008(11) 0.007(11) C18 0.062(15) 0.075(17) 0.046(13) 0.005(12) 0.023(12) -0.012(13) C19 0.071(16) 0.042(13) 0.036(12) -0.004(10) 0.011(11) -0.017(12) C20 0.078(16) 0.048(14) 0.040(12) 0.007(11) 0.038(12) 0.014(12) C21 0.050(13) 0.040(13) 0.073(15) -0.015(11) 0.036(12) -0.004(10) C22 0.078(15) 0.050(13) 0.035(11) 0.027(10) 0.026(11) 0.016(11) N4 0.053(11) 0.040(10) 0.035(9) -0.013(8) 0.008(9) -0.001(9) C23 0.039(13) 0.057(15) 0.078(16) -0.007(12) 0.027(13) 0.000(11) C24 0.064(16) 0.051(14) 0.059(14) 0.018(11) 0.018(12) -0.005(12) C25 0.046(13) 0.035(12) 0.031(11) -0.002(9) -0.018(10) -0.003(11) C26 0.071(15) 0.046(13) 0.047(13) 0.010(10) 0.036(12) 0.001(11) C27 0.11(2) 0.044(14) 0.074(16) -0.007(12) 0.055(15) -0.004(13) C28 0.039(13) 0.059(14) 0.032(11) 0.007(10) 0.004(10) 0.035(12) C29 0.044(13) 0.052(13) 0.052(12) 0.002(11) 0.030(11) -0.003(11) C30 0.080(18) 0.050(14) 0.041(13) 0.012(11) 0.016(12) 0.012(12) N5 0.089(14) 0.037(10) 0.022(9) -0.002(7) 0.016(10) 0.009(10) C31 0.041(13) 0.054(14) 0.055(13) -0.004(11) 0.035(11) -0.015(11) C32 0.110(19) 0.011(11) 0.036(11) 0.001(9) 0.035(12) -0.022(11) C33 0.055(13) 0.054(14) 0.039(12) 0.014(10) 0.017(10) 0.010(11) O1 0.060(10) 0.098(12) 0.043(9) 0.015(8) 0.016(8) 0.006(9) O2 0.062(11) 0.117(13) 0.057(11) -0.010(9) 0.016(9) -0.018(9) O3 0.069(11) 0.095(11) 0.046(9) -0.002(8) 0.030(8) -0.007(9) O4 0.073(11) 0.056(9) 0.043(8) -0.012(7) 0.021(8) 0.001(8) C34 0.072(18) 0.049(15) 0.039(14) -0.018(12) 0.009(13) 0.011(13) C35 0.17(3) 0.046(15) 0.043(14) -0.002(11) 0.047(17) -0.027(17) C36 0.14(3) 0.068(19) 0.053(17) -0.035(14) 0.034(17) -0.033(18) C37 0.15(3) 0.046(15) 0.021(12) 0.006(10) 0.032(15) 0.030(16) C38 0.085(18) 0.095(19) 0.037(13) -0.009(13) 0.017(14) -0.007(16) C39 0.08(2) 0.085(19) 0.023(13) -0.009(12) -0.001(13) 0.012(16) C40 0.11(2) 0.11(2) 0.051(15) 0.007(14) 0.041(16) -0.003(18) C41 0.071(17) 0.13(2) 0.072(18) -0.039(17) 0.011(14) -0.025(15) C42 0.08(2) 0.17(3) 0.046(16) -0.002(16) 0.026(15) 0.003(19) C43 0.050(15) 0.085(17) 0.085(18) -0.004(13) 0.048(13) 0.009(13) C44 0.052(14) 0.090(17) 0.055(15) -0.015(13) 0.026(12) 0.014(12) C45 0.056(16) 0.087(17) 0.047(14) -0.019(12) 0.008(12) 0.000(13) Zn2 0.076(2) 0.076(2) 0.116(3) -0.0189(18) 0.0230(18) 0.0103(16) O2W 0.131(15) 0.114(14) 0.144(16) 0.003(12) 0.037(12) 0.030(11) O4W 0.117(14) 0.119(14) 0.158(16) 0.024(12) 0.052(12) 0.043(11) O3W 0.111(13) 0.081(12) 0.195(17) -0.055(12) 0.052(12) 0.012(10) N101 0.039(11) 0.064(13) 0.125(16) -0.010(12) 0.004(11) 0.000(11) C101 0.046(16) 0.084(19) 0.13(2) -0.046(15) 0.016(15) -0.010(15) C102 0.10(2) 0.064(19) 0.15(2) -0.016(17) 0.032(19) 0.014(16) C103 0.036(15) 0.11(2) 0.15(2) 0.04(2) 0.011(15) 0.015(17) C104 0.062(17) 0.045(16) 0.16(2) -0.005(14) 0.030(17) -0.017(14) C105 0.061(18) 0.059(18) 0.110(19) -0.018(14) -0.008(15) 0.032(14) N102 0.073(13) 0.044(11) 0.092(13) 0.001(10) 0.023(11) 0.017(11) C106 0.024(14) 0.080(19) 0.087(16) 0.002(14) 0.003(12) -0.002(13) C107 0.082(19) 0.045(15) 0.109(19) 0.007(13) 0.034(15) -0.015(14) C108 0.038(14) 0.076(17) 0.072(15) 0.020(13) 0.016(12) -0.009(14) C109 0.051(17) 0.055(17) 0.115(19) -0.004(14) 0.018(14) 0.001(12) C110 0.044(16) 0.068(18) 0.094(17) 0.004(14) 0.021(13) 0.008(14) C111 0.08(2) 0.10(2) 0.054(15) 0.011(15) 0.004(14) 0.025(18) C112 0.066(18) 0.10(2) 0.104(19) -0.003(15) 0.042(17) 0.010(18) C113 0.09(2) 0.08(2) 0.110(19) 0.017(17) 0.059(16) -0.009(18) C114 0.13(3) 0.09(2) 0.12(2) 0.004(18) 0.06(2) 0.011(19) C115 0.080(18) 0.082(19) 0.12(2) -0.023(15) 0.037(18) 0.019(18) N103 0.092(16) 0.076(14) 0.074(13) -0.030(11) 0.025(11) 0.026(12) C116 0.057(15) 0.048(15) 0.070(15) 0.013(12) 0.029(12) -0.004(12) C117 0.092(18) 0.061(17) 0.060(14) -0.003(12) 0.044(13) -0.021(13) C118 0.041(13) 0.060(15) 0.057(13) 0.000(12) 0.022(10) -0.011(11) C119 0.080(17) 0.030(13) 0.068(14) 0.016(12) 0.024(13) -0.018(13) C120 0.056(16) 0.040(16) 0.103(18) 0.006(13) 0.005(13) 0.004(12) C121 0.037(13) 0.062(16) 0.069(14) 0.005(13) 0.003(11) -0.004(12) C122 0.068(16) 0.074(17) 0.074(15) 0.021(13) 0.028(13) -0.033(13) N104 0.067(13) 0.055(12) 0.064(12) -0.010(10) 0.009(10) -0.012(10) C123 0.080(17) 0.071(17) 0.057(15) -0.011(12) 0.025(14) -0.012(14) C124 0.049(15) 0.055(15) 0.056(13) 0.007(12) 0.000(12) 0.009(11) C125 0.046(13) 0.060(14) 0.032(12) -0.025(11) 0.005(10) -0.011(11) C126 0.056(14) 0.075(17) 0.058(15) -0.012(12) -0.004(12) -0.041(12) C127 0.076(17) 0.065(16) 0.047(13) 0.002(12) -0.012(13) -0.016(13) C128 0.069(16) 0.021(12) 0.073(15) 0.002(11) 0.033(13) -0.006(12) C129 0.055(15) 0.044(14) 0.094(17) -0.016(13) 0.012(13) -0.019(13) C130 0.067(18) 0.054(16) 0.052(14) -0.017(12) 0.004(12) 0.007(12) N105 0.079(14) 0.055(13) 0.048(11) -0.015(9) 0.017(10) -0.016(12) C131 0.071(17) 0.039(14) 0.083(17) -0.009(12) 0.035(14) -0.021(13) C132 0.051(16) 0.062(16) 0.077(15) -0.024(13) 0.020(12) -0.013(12) C133 0.099(17) 0.043(15) 0.082(17) 0.004(11) 0.060(14) -0.029(14) O101 0.093(14) 0.087(12) 0.063(11) -0.003(9) 0.021(10) -0.022(10) O102 0.099(14) 0.113(14) 0.062(11) 0.023(9) 0.020(10) 0.021(11) O103 0.21(2) 0.24(3) 0.107(19) 0.032(18) 0.037(17) 0.12(2) O104 0.080(13) 0.154(17) 0.072(12) -0.025(11) 0.037(11) 0.023(12) C134 0.13(3) 0.16(3) 0.033(17) -0.018(18) 0.01(2) 0.01(3) C135 0.12(3) 0.13(3) 0.19(4) -0.07(3) 0.13(3) -0.05(2) C136 0.23(5) 0.09(2) 0.10(2) 0.015(19) 0.08(3) 0.02(2) C137 0.17(3) 0.18(4) 0.049(17) -0.03(2) -0.03(2) 0.07(3) C138 0.30(5) 0.12(3) 0.23(5) -0.09(3) 0.21(4) -0.11(3) C139 0.15(3) 0.12(3) 0.026(16) -0.023(15) 0.011(19) -0.02(2) C140 0.12(2) 0.10(2) 0.070(18) -0.018(16) 0.018(18) -0.016(19) C141 0.12(2) 0.09(2) 0.069(19) 0.002(16) 0.007(16) -0.020(17) C142 0.08(2) 0.09(2) 0.13(3) 0.034(18) -0.033(19) 0.022(16) C143 0.26(4) 0.14(3) 0.15(3) 0.11(3) 0.17(3) 0.10(3) C144 0.08(2) 0.27(5) 0.12(3) -0.08(3) 0.05(2) 0.05(3) C145 0.15(4) 0.14(3) 0.18(4) -0.04(3) 0.08(3) 0.00(3) S1 0.059(4) 0.055(4) 0.078(4) 0.000(3) 0.019(3) -0.010(3) O5 0.055(6) 0.064(9) 0.062(8) 0.012(6) 0.016(6) -0.011(6) O6 0.071(9) 0.070(8) 0.064(9) -0.009(6) 0.013(7) -0.020(7) O7 0.078(10) 0.073(10) 0.132(12) -0.021(8) 0.035(9) 0.004(8) C46 0.107(15) 0.084(15) 0.096(15) 0.037(9) -0.001(10) -0.020(12) F1 0.154(12) 0.084(9) 0.147(12) 0.047(7) -0.023(9) -0.047(8) F2 0.203(14) 0.168(13) 0.098(11) 0.051(9) 0.061(10) -0.011(11) F3 0.129(10) 0.107(11) 0.159(13) 0.057(9) -0.043(8) -0.018(8) S2 0.170(8) 0.130(7) 0.099(5) -0.009(5) 0.038(5) 0.065(6) O8 0.31(2) 0.203(19) 0.073(9) -0.031(10) 0.010(10) 0.158(17) O9 0.151(12) 0.115(13) 0.129(13) 0.021(11) 0.072(10) 0.070(10) O10 0.170(15) 0.101(10) 0.080(10) 0.002(8) 0.034(10) 0.060(9) C47 0.128(15) 0.163(15) 0.158(13) -0.06(2) 0.037(17) -0.008(17) F4 0.166(16) 0.147(12) 0.38(3) -0.072(14) 0.065(17) -0.025(11) F5 0.132(11) 0.218(17) 0.243(17) -0.090(16) 0.037(11) 0.007(11) F6 0.214(16) 0.251(19) 0.138(11) 0.012(12) 0.050(11) -0.053(16) S3 0.110(5) 0.068(4) 0.061(4) -0.002(3) 0.041(4) -0.009(4) O11 0.120(11) 0.094(10) 0.062(9) 0.004(8) 0.049(9) -0.015(9) O12 0.164(13) 0.059(9) 0.051(7) 0.002(6) 0.045(8) -0.003(9) O13 0.216(16) 0.066(7) 0.068(10) -0.013(7) 0.050(11) 0.003(10) C48 0.114(9) 0.156(18) 0.103(12) -0.018(17) 0.044(11) -0.031(12) F7 0.139(13) 0.226(15) 0.149(13) -0.032(12) 0.026(11) 0.063(11) F8 0.162(13) 0.215(17) 0.103(9) -0.048(11) 0.002(8) -0.029(12) F9 0.165(13) 0.310(19) 0.223(16) -0.001(17) 0.086(15) -0.119(16) S4 0.126(7) 0.126(7) 0.177(7) -0.033(7) 0.061(7) -0.036(6) O14 0.20(2) 0.133(12) 0.26(2) 0.025(16) 0.004(18) -0.068(12) O15 0.134(14) 0.173(15) 0.200(18) -0.049(16) 0.085(14) -0.026(11) C49 0.25(2) 0.12(2) 0.183(11) -0.076(17) 0.100(15) -0.055(19) F10 0.281(19) 0.30(2) 0.30(2) -0.21(2) 0.126(18) -0.031(19) F11 0.44(3) 0.212(17) 0.27(2) -0.021(16) 0.20(2) -0.137(19) F12 0.249(18) 0.28(2) 0.176(12) -0.043(17) 0.070(13) -0.076(16) S5 0.087(5) 0.084(5) 0.087(5) 0.002(4) 0.038(4) -0.003(4) O16 0.103(10) 0.24(2) 0.234(17) -0.122(17) 0.092(11) -0.072(12) O17 0.071(8) 0.156(14) 0.067(10) 0.026(10) 0.017(7) -0.022(9) O18 0.076(9) 0.117(12) 0.081(8) 0.002(8) 0.023(7) -0.019(9) O19 0.144(14) 0.087(9) 0.132(13) 0.024(9) 0.068(11) 0.007(9) C50 0.125(16) 0.130(12) 0.091(11) -0.002(15) 0.048(12) 0.022(17) F13 0.122(11) 0.33(2) 0.135(13) -0.014(15) 0.076(9) 0.010(13) F14 0.251(18) 0.122(11) 0.132(12) -0.014(9) 0.048(12) 0.067(11) F15 0.143(11) 0.214(16) 0.092(8) -0.004(9) 0.023(9) 0.066(12) S6 0.131(7) 0.097(7) 0.140(6) -0.005(5) 0.046(6) 0.002(5) O20 0.143(15) 0.127(15) 0.210(18) 0.002(14) 0.072(15) -0.008(11) O21 0.172(17) 0.21(2) 0.31(3) 0.016(19) 0.141(17) 0.035(13) O22 0.33(3) 0.088(13) 0.196(17) -0.014(12) 0.077(19) -0.041(13) C51 0.34(3) 0.32(4) 0.133(13) 0.026(15) 0.07(2) 0.03(2) F16 0.34(3) 0.48(4) 0.18(2) 0.09(2) -0.016(19) 0.12(3) F17 0.48(4) 0.54(4) 0.185(17) -0.14(3) 0.08(2) -0.05(3) F18 0.50(4) 0.40(4) 0.26(3) 0.13(2) 0.20(3) 0.01(3) S7 0.131(8) 0.254(14) 0.146(9) -0.040(9) 0.021(8) -0.013(7) O23 0.33(3) 0.38(3) 0.20(2) 0.045(18) 0.15(2) 0.12(2) O24 0.151(17) 0.22(2) 0.40(3) -0.118(19) 0.04(2) 0.015(13) O25 0.126(16) 0.31(3) 0.134(15) -0.049(14) 0.027(14) -0.025(14) C52 0.149(16) 0.37(4) 0.15(3) -0.038(17) 0.01(3) 0.041(14) F19 0.26(3) 0.52(4) 0.26(2) 0.10(2) 0.10(2) 0.16(2) F20 0.138(11) 0.67(4) 0.24(2) -0.11(2) 0.076(17) -0.10(2) F21 0.27(2) 0.47(4) 0.20(2) -0.064(19) 0.036(19) 0.14(2) O5W 0.21(2) 0.21(3) 0.28(3) -0.06(2) 0.10(2) 0.032(19) O6W 0.098(12) 0.083(12) 0.157(15) 0.001(11) 0.029(11) -0.014(10) O1S 0.112(17) 0.23(2) 0.084(14) 0.044(15) 0.001(12) -0.002(14) O2S 0.090(14) 0.131(16) 0.133(16) 0.035(12) 0.026(13) -0.024(12) N1S 0.044(15) 0.098(17) 0.12(2) -0.020(16) 0.013(17) -0.008(13) C1S 0.14(2) 0.11(2) 0.11(2) 0.025(16) 0.10(2) 0.031(17) O3S 0.107(17) 0.19(2) 0.30(3) 0.11(2) 0.074(19) 0.004(15) O4S 0.109(19) 0.22(3) 0.25(3) 0.08(2) 0.06(2) 0.00(2) N2S 0.13(3) 0.15(3) 0.12(2) 0.047(18) 0.02(2) -0.04(3) C2S 0.14(2) 0.09(2) 0.079(18) 0.031(15) 0.016(17) 0.039(17) O5S 0.22(3) 0.18(3) 0.19(3) 0.087(19) 0.04(2) 0.017(19) O6S 0.36(4) 0.25(3) 0.23(3) 0.07(2) 0.22(3) 0.14(3) N3S 0.16(2) 0.17(3) 0.13(3) 0.03(2) 0.11(2) 0.08(2) C3S 0.23(4) 0.25(4) 0.25(4) -0.08(4) 0.09(3) 0.12(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 F33 1.959(11) . ? Zn1 O1W 2.015(10) . ? Zn1 N2 2.032(9) . ? Zn1 N3 2.139(10) . ? Zn1 N1 2.149(9) . ? O1W H1WA 0.8497 . ? O1W H1WB 0.8502 . ? B1 F32 1.34(3) . ? B1 F30 1.36(2) . ? B1 F31 1.41(2) . ? B1 F33 1.54(3) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C1 H1A 0.9300 . ? C2 C3 1.3900 . ? C2 H2A 0.9300 . ? C3 C4 1.3900 . ? C3 H3A 0.9300 . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 C6 1.455(12) . ? N2 C6 1.3900 . ? N2 C10 1.3900 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C7 H7A 0.9300 . ? C8 C9 1.3900 . ? C8 C16 1.449(12) . ? C9 C10 1.3900 . ? C9 H9A 0.9300 . ? C10 C11 1.430(13) . ? C11 C12 1.3900 . ? C11 N3 1.3900 . ? C12 C13 1.3900 . ? C12 H12A 0.9300 . ? C13 C14 1.3900 . ? C13 H13A 0.9300 . ? C14 C15 1.3900 . ? C14 H14A 0.9300 . ? C15 N3 1.3900 . ? C15 H15A 0.9300 . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C17 H17A 0.9300 . ? C18 C19 1.3900 . ? C18 H18A 0.9300 . ? C19 C20 1.3900 . ? C19 C22 1.515(19) . ? C20 C21 1.3900 . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 N4 1.497(16) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? N4 C23 1.3900 . ? N4 C27 1.3900 . ? C23 C24 1.3900 . ? C23 H23A 0.9300 . ? C24 C25 1.3900 . ? C24 H24A 0.9300 . ? C25 C26 1.3900 . ? C25 C28 1.445(11) . ? 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 N5 1.3900 . ? C30 H30A 0.9300 . ? N5 C31 1.3900 . ? N5 C33 1.478(17) . ? C31 C32 1.3900 . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C33 1.55(3) 3_725 ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? O1 C39 1.380(16) . ? O1 C40 1.41(2) . ? O2 C42 1.41(2) . ? O2 C41 1.47(2) 3_745 ? O3 C44 1.413(18) . ? O3 C43 1.460(19) . ? O4 C34 1.340(15) . ? O4 C45 1.412(19) . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C35 H35A 0.9300 . ? C36 C37 1.3900 . ? C36 H36A 0.9300 . ? C37 C38 1.3900 . ? C37 H37A 0.9300 . ? C38 C39 1.3900 . ? C38 H38A 0.9300 . ? C40 C41 1.50(3) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 O2 1.47(2) 3_745 ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.52(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.52(2) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? Zn2 O3W 2.058(13) . ? Zn2 O2W 2.066(16) . ? Zn2 N102 2.084(11) . ? Zn2 O4W 2.118(16) . ? Zn2 N101 2.128(11) . ? Zn2 N103 2.145(12) . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8500 . ? O4W H4WA 0.8501 . ? O4W H4WB 0.8499 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8503 . ? N101 C101 1.3900 . ? N101 C105 1.3900 . ? C101 C102 1.3900 . ? C101 H10A 0.9300 . ? C102 C103 1.3900 . ? C102 H10B 0.9300 . ? C103 C104 1.3900 . ? C103 H10C 0.9300 . ? C104 C105 1.3900 . ? C104 H10D 0.9300 . ? C105 C106 1.429(15) . ? N102 C106 1.3900 . ? N102 C110 1.3900 . ? C106 C107 1.3900 . ? C107 C108 1.3900 . ? C107 H10E 0.9300 . ? C108 C109 1.3900 . ? C108 C116 1.477(14) . ? C109 C110 1.3900 . ? C109 H10F 0.9300 . ? C110 C111 1.418(15) . ? C111 C112 1.3900 . ? C111 N103 1.3900 . ? C112 C113 1.3900 . ? C112 H11A 0.9300 . ? C113 C114 1.3900 . ? C113 H11B 0.9300 . ? C114 C115 1.3900 . ? C114 H11C 0.9300 . ? C115 N103 1.3900 . ? C115 H11D 0.9300 . ? C116 C117 1.3900 . ? C116 C121 1.3900 . ? C117 C118 1.3900 . ? C117 H11E 0.9300 . ? C118 C119 1.3900 . ? C118 H11F 0.9300 . ? C119 C120 1.3900 . ? C119 C122 1.47(2) . ? C120 C121 1.3900 . ? C120 H12B 0.9300 . ? C121 H12C 0.9300 . ? C122 N104 1.485(18) . ? C122 H12D 0.9700 . ? C122 H12E 0.9700 . ? N104 C123 1.3900 . ? N104 C127 1.3900 . ? C123 C124 1.3900 . ? C123 H12F 0.9300 . ? C124 C125 1.3900 . ? C124 H12G 0.9300 . ? C125 C126 1.3900 . ? C125 C128 1.486(13) . ? C126 C127 1.3900 . ? C126 H12H 0.9300 . ? C127 H12I 0.9300 . ? C128 C129 1.3900 . ? C128 C132 1.3900 . ? C129 C130 1.3900 . ? C129 H12J 0.9300 . ? C130 N105 1.3900 . ? C130 H13B 0.9300 . ? N105 C131 1.3900 . ? N105 C133 1.438(18) . ? C131 C132 1.3900 . ? C131 H13C 0.9300 . ? C132 H13D 0.9300 . ? C133 C133 1.45(3) 3_865 ? C133 H13E 0.9700 . ? C133 H13F 0.9700 . ? O101 C139 1.334(18) . ? O101 C140 1.41(2) . ? O102 C142 1.39(3) . ? O102 C141 1.45(2) . ? O103 C143 1.15(2) 3_845 ? O103 C144 1.47(3) . ? O104 C145 1.36(3) . ? O104 C134 1.37(2) . ? C134 C135 1.3900 . ? C134 C139 1.3900 . ? C135 C136 1.3900 . ? C135 H13G 0.9300 . ? C136 C137 1.3900 . ? C136 H13H 0.9300 . ? C137 C138 1.3900 . ? C137 H13I 0.9300 . ? C138 C139 1.3900 . ? C138 H13J 0.9300 . ? C140 C141 1.48(3) . ? C140 H14B 0.9700 . ? C140 H14C 0.9700 . ? C141 H14D 0.9700 . ? C141 H14E 0.9700 . ? C142 C143 1.54(3) . ? C142 H14F 0.9700 . ? C142 H14G 0.9700 . ? C143 O103 1.15(2) 3_845 ? C143 H14H 0.9700 . ? C143 H14I 0.9700 . ? C144 C145 1.48(4) . ? C144 H14J 0.9700 . ? C144 H14K 0.9700 . ? C145 H14L 0.9700 . ? C145 H14M 0.9700 . ? S1 O6 1.446(10) . ? S1 O5 1.453(10) . ? S1 O7 1.459(11) . ? S1 C46 1.796(16) . ? C46 F2 1.310(14) . ? C46 F3 1.326(14) . ? C46 F1 1.332(14) . ? S2 O9 1.464(12) . ? S2 O10 1.465(12) . ? S2 O8 1.470(12) . ? S2 C47 1.834(18) . ? C47 F5 1.343(16) . ? C47 F6 1.354(16) . ? C47 F4 1.362(16) . ? S3 O13 1.439(11) . ? S3 O12 1.441(10) . ? S3 O11 1.453(10) . ? S3 C48 1.755(17) . ? C48 F9 1.333(14) . ? C48 F7 1.343(15) . ? C48 F8 1.351(15) . ? S4 O14 1.417(14) . ? S4 O16 1.431(14) . ? S4 O15 1.441(14) . ? S4 C49 1.811(18) . ? C49 F11 1.330(17) . ? C49 F12 1.339(16) . ? C49 F10 1.340(17) . ? S5 O18 1.421(11) . ? S5 O19 1.436(11) . ? S5 O17 1.455(11) . ? S5 C50 1.789(17) . ? C50 F15 1.299(14) . ? C50 F14 1.306(14) . ? C50 F13 1.314(14) . ? S6 O22 1.401(14) . ? S6 O21 1.405(14) . ? S6 O20 1.436(14) . ? S6 C51 1.766(19) . ? C51 F16 1.334(18) . ? C51 F17 1.335(18) . ? C51 F18 1.343(19) . ? S7 O23 1.391(17) . ? S7 O24 1.395(16) . ? S7 O25 1.403(16) . ? S7 C52 1.766(19) . ? C52 F21 1.325(18) . ? C52 F19 1.334(18) . ? C52 F20 1.341(18) . ? O5W H5WA 0.8500 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8499 . ? O6W H6WB 0.8500 . ? O1S N1S 1.19(2) . ? O2S N1S 1.197(19) . ? N1S C1S 1.41(3) . ? C1S H1SA 0.9600 . ? C1S H1SB 0.9600 . ? C1S H1SC 0.9600 . ? O3S N2S 1.26(3) . ? O4S N2S 1.09(3) . ? N2S C2S 1.48(3) . ? C2S H2SA 0.9600 . ? C2S H2SB 0.9600 . ? C2S H2SC 0.9600 . ? O5S N3S 1.13(3) . ? O6S N3S 1.12(2) . ? N3S C3S 1.43(3) . ? C3S H3SA 0.9600 . ? C3S H3SB 0.9600 . ? C3S H3SC 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F33 Zn1 O1W 113.0(5) . . ? F33 Zn1 N2 132.5(4) . . ? O1W Zn1 N2 114.4(4) . . ? F33 Zn1 N3 96.8(5) . . ? O1W Zn1 N3 97.6(4) . . ? N2 Zn1 N3 77.8(6) . . ? F33 Zn1 N1 99.2(5) . . ? O1W Zn1 N1 95.8(4) . . ? N2 Zn1 N1 75.4(5) . . ? N3 Zn1 N1 153.1(5) . . ? Zn1 O1W H1WA 109.2 . . ? Zn1 O1W H1WB 108.9 . . ? H1WA O1W H1WB 109.5 . . ? F32 B1 F30 113(2) . . ? F32 B1 F31 110(2) . . ? F30 B1 F31 112(2) . . ? F32 B1 F33 110.5(19) . . ? F30 B1 F33 106(2) . . ? F31 B1 F33 104.5(18) . . ? B1 F33 Zn1 122.7(12) . . ? C1 N1 C5 120.0 . . ? C1 N1 Zn1 124.7(8) . . ? C5 N1 Zn1 115.0(8) . . ? C2 C1 N1 120.0 . . ? C2 C1 H1A 120.0 . . ? N1 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 124.0(11) . . ? N1 C5 C6 116.0(11) . . ? C6 N2 C10 120.0 . . ? C6 N2 Zn1 122.1(8) . . ? C10 N2 Zn1 117.5(8) . . ? C7 C6 N2 120.0 . . ? C7 C6 C5 129.6(12) . . ? N2 C6 C5 110.3(11) . . ? C6 C7 C8 120.0 . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 C16 121.4(12) . . ? C7 C8 C16 118.5(12) . . ? C8 C9 C10 120.0 . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C9 C10 N2 120.0 . . ? C9 C10 C11 124.8(11) . . ? N2 C10 C11 115.2(11) . . ? C12 C11 N3 120.0 . . ? C12 C11 C10 124.7(12) . . ? N3 C11 C10 115.3(12) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14A 120.0 . . ? C15 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 Zn1 125.9(9) . . ? C11 N3 Zn1 113.8(9) . . ? C17 C16 C21 120.0 . . ? C17 C16 C8 120.7(12) . . ? C21 C16 C8 119.2(12) . . ? C18 C17 C16 120.0 . . ? C18 C17 H17A 120.0 . . ? C16 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 C22 120.0(12) . . ? C18 C19 C22 119.9(12) . . ? C19 C20 C21 120.0 . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? N4 C22 C19 107.7(12) . . ? N4 C22 H22A 110.2 . . ? C19 C22 H22A 110.2 . . ? N4 C22 H22B 110.2 . . ? C19 C22 H22B 110.2 . . ? H22A C22 H22B 108.5 . . ? C23 N4 C27 120.0 . . ? C23 N4 C22 121.2(12) . . ? C27 N4 C22 118.6(12) . . ? N4 C23 C24 120.0 . . ? N4 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 114.7(12) . . ? C26 C25 C28 125.2(12) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 N4 120.0 . . ? C26 C27 H27A 120.0 . . ? N4 C27 H27A 120.0 . . ? C29 C28 C32 120.0 . . ? C29 C28 C25 123.9(12) . . ? C32 C28 C25 116.1(12) . . ? C30 C29 C28 120.0 . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 N5 120.0 . . ? C29 C30 H30A 120.0 . . ? N5 C30 H30A 120.0 . . ? C31 N5 C30 120.0 . . ? C31 N5 C33 122.1(12) . . ? C30 N5 C33 117.9(12) . . ? N5 C31 C32 120.0 . . ? N5 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C28 120.0 . . ? C31 C32 H32A 120.0 . . ? C28 C32 H32A 120.0 . . ? N5 C33 C33 108.4(15) . 3_725 ? N5 C33 H33A 110.0 . . ? C33 C33 H33A 110.0 3_725 . ? N5 C33 H33B 110.0 . . ? C33 C33 H33B 110.0 3_725 . ? H33A C33 H33B 108.4 . . ? C39 O1 C40 115.4(15) . . ? C42 O2 C41 111.8(16) . 3_745 ? C44 O3 C43 115.0(14) . . ? C34 O4 C45 115.9(15) . . ? O4 C34 C35 124.6(16) . . ? O4 C34 C39 115.4(16) . . ? C35 C34 C39 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38A 120.0 . . ? C37 C38 H38A 120.0 . . ? O1 C39 C38 123.1(15) . . ? O1 C39 C34 116.9(15) . . ? C38 C39 C34 120.0 . . ? O1 C40 C41 108.4(19) . . ? O1 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? O1 C40 H40B 110.0 . . ? C41 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? O2 C41 C40 113.8(17) 3_745 . ? O2 C41 H41A 108.8 3_745 . ? C40 C41 H41A 108.8 . . ? O2 C41 H41B 108.8 3_745 . ? C40 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? O2 C42 C43 105.9(18) . . ? O2 C42 H42A 110.6 . . ? C43 C42 H42A 110.6 . . ? O2 C42 H42B 110.6 . . ? C43 C42 H42B 110.6 . . ? H42A C42 H42B 108.7 . . ? O3 C43 C42 108.2(16) . . ? O3 C43 H43A 110.1 . . ? C42 C43 H43A 110.1 . . ? O3 C43 H43B 110.1 . . ? C42 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? O3 C44 C45 115.0(16) . . ? O3 C44 H44A 108.5 . . ? C45 C44 H44A 108.5 . . ? O3 C44 H44B 108.5 . . ? C45 C44 H44B 108.5 . . ? H44A C44 H44B 107.5 . . ? O4 C45 C44 107.1(16) . . ? O4 C45 H45A 110.3 . . ? C44 C45 H45A 110.3 . . ? O4 C45 H45B 110.3 . . ? C44 C45 H45B 110.3 . . ? H45A C45 H45B 108.6 . . ? O3W Zn2 O2W 84.7(6) . . ? O3W Zn2 N102 175.1(6) . . ? O2W Zn2 N102 98.9(5) . . ? O3W Zn2 O4W 85.4(6) . . ? O2W Zn2 O4W 169.2(6) . . ? N102 Zn2 O4W 91.2(5) . . ? O3W Zn2 N101 108.8(6) . . ? O2W Zn2 N101 89.4(6) . . ? N102 Zn2 N101 74.6(7) . . ? O4W Zn2 N101 89.7(5) . . ? O3W Zn2 N103 100.7(7) . . ? O2W Zn2 N103 96.4(6) . . ? N102 Zn2 N103 75.8(7) . . ? O4W Zn2 N103 89.6(6) . . ? N101 Zn2 N103 150.3(7) . . ? Zn2 O2W H2WA 109.2 . . ? Zn2 O2W H2WB 109.3 . . ? H2WA O2W H2WB 109.5 . . ? Zn2 O4W H4WA 108.8 . . ? Zn2 O4W H4WB 109.0 . . ? H4WA O4W H4WB 109.5 . . ? Zn2 O3W H3WA 109.3 . . ? Zn2 O3W H3WB 108.8 . . ? H3WA O3W H3WB 109.5 . . ? C101 N101 C105 120.0 . . ? C101 N101 Zn2 123.1(10) . . ? C105 N101 Zn2 116.7(10) . . ? C102 C101 N101 120.0 . . ? C102 C101 H10A 120.0 . . ? N101 C101 H10A 120.0 . . ? C101 C102 C103 120.0 . . ? C101 C102 H10B 120.0 . . ? C103 C102 H10B 120.0 . . ? C102 C103 C104 120.0 . . ? C102 C103 H10C 120.0 . . ? C104 C103 H10C 120.0 . . ? C105 C104 C103 120.0 . . ? C105 C104 H10D 120.0 . . ? C103 C104 H10D 120.0 . . ? C104 C105 N101 120.0 . . ? C104 C105 C106 123.7(14) . . ? N101 C105 C106 116.2(14) . . ? C106 N102 C110 120.0 . . ? C106 N102 Zn2 120.8(10) . . ? C110 N102 Zn2 119.0(10) . . ? C107 C106 N102 120.0 . . ? C107 C106 C105 128.6(14) . . ? N102 C106 C105 111.4(14) . . ? C106 C107 C108 120.0 . . ? C106 C107 H10E 120.0 . . ? C108 C107 H10E 120.0 . . ? C109 C108 C107 120.0 . . ? C109 C108 C116 122.0(13) . . ? C107 C108 C116 117.9(13) . . ? C108 C109 C110 120.0 . . ? C108 C109 H10F 120.0 . . ? C110 C109 H10F 120.0 . . ? C109 C110 N102 120.0 . . ? C109 C110 C111 126.7(15) . . ? N102 C110 C111 113.3(15) . . ? C112 C111 N103 120.0 . . ? C112 C111 C110 123.0(16) . . ? N103 C111 C110 116.9(16) . . ? C113 C112 C111 120.0 . . ? C113 C112 H11A 120.0 . . ? C111 C112 H11A 120.0 . . ? C112 C113 C114 120.0 . . ? C112 C113 H11B 120.0 . . ? C114 C113 H11B 120.0 . . ? C115 C114 C113 120.0 . . ? C115 C114 H11C 120.0 . . ? C113 C114 H11C 120.0 . . ? N103 C115 C114 120.0 . . ? N103 C115 H11D 120.0 . . ? C114 C115 H11D 120.0 . . ? C115 N103 C111 120.0 . . ? C115 N103 Zn2 124.6(12) . . ? C111 N103 Zn2 114.9(12) . . ? C117 C116 C121 120.0 . . ? C117 C116 C108 120.3(13) . . ? C121 C116 C108 119.7(13) . . ? C116 C117 C118 120.0 . . ? C116 C117 H11E 120.0 . . ? C118 C117 H11E 120.0 . . ? C119 C118 C117 120.0 . . ? C119 C118 H11F 120.0 . . ? C117 C118 H11F 120.0 . . ? C118 C119 C120 120.0 . . ? C118 C119 C122 114.3(13) . . ? C120 C119 C122 125.3(13) . . ? C121 C120 C119 120.0 . . ? C121 C120 H12B 120.0 . . ? C119 C120 H12B 120.0 . . ? C120 C121 C116 120.0 . . ? C120 C121 H12C 120.0 . . ? C116 C121 H12C 120.0 . . ? C119 C122 N104 111.7(14) . . ? C119 C122 H12D 109.3 . . ? N104 C122 H12D 109.3 . . ? C119 C122 H12E 109.3 . . ? N104 C122 H12E 109.3 . . ? H12D C122 H12E 107.9 . . ? C123 N104 C127 120.0 . . ? C123 N104 C122 121.2(13) . . ? C127 N104 C122 118.8(13) . . ? C124 C123 N104 120.0 . . ? C124 C123 H12F 120.0 . . ? N104 C123 H12F 120.0 . . ? C123 C124 C125 120.0 . . ? C123 C124 H12G 120.0 . . ? C125 C124 H12G 120.0 . . ? C126 C125 C124 120.0 . . ? C126 C125 C128 118.6(12) . . ? C124 C125 C128 121.3(12) . . ? C125 C126 C127 120.0 . . ? C125 C126 H12H 120.0 . . ? C127 C126 H12H 120.0 . . ? C126 C127 N104 120.0 . . ? C126 C127 H12I 120.0 . . ? N104 C127 H12I 120.0 . . ? C129 C128 C132 120.0 . . ? C129 C128 C125 119.3(13) . . ? C132 C128 C125 120.7(13) . . ? C128 C129 C130 120.0 . . ? C128 C129 H12J 120.0 . . ? C130 C129 H12J 120.0 . . ? N105 C130 C129 120.0 . . ? N105 C130 H13B 120.0 . . ? C129 C130 H13B 120.0 . . ? C130 N105 C131 120.0 . . ? C130 N105 C133 120.3(15) . . ? C131 N105 C133 119.6(15) . . ? C132 C131 N105 120.0 . . ? C132 C131 H13C 120.0 . . ? N105 C131 H13C 120.0 . . ? C131 C132 C128 120.0 . . ? C131 C132 H13D 120.0 . . ? C128 C132 H13D 120.0 . . ? N105 C133 C133 109.1(18) . 3_865 ? N105 C133 H13E 109.9 . . ? C133 C133 H13E 109.9 3_865 . ? N105 C133 H13F 109.9 . . ? C133 C133 H13F 109.9 3_865 . ? H13E C133 H13F 108.3 . . ? C139 O101 C140 120(2) . . ? C142 O102 C141 116(2) . . ? C143 O103 C144 112(3) 3_845 . ? C145 O104 C134 112(2) . . ? O104 C134 C135 133(2) . . ? O104 C134 C139 107(2) . . ? C135 C134 C139 120.0 . . ? C136 C135 C134 120.0 . . ? C136 C135 H13G 120.0 . . ? C134 C135 H13G 120.0 . . ? C137 C136 C135 120.0 . . ? C137 C136 H13H 120.0 . . ? C135 C136 H13H 120.0 . . ? C136 C137 C138 120.0 . . ? C136 C137 H13I 120.0 . . ? C138 C137 H13I 120.0 . . ? C137 C138 C139 120.0 . . ? C137 C138 H13J 120.0 . . ? C139 C138 H13J 120.0 . . ? O101 C139 C138 114(2) . . ? O101 C139 C134 126(2) . . ? C138 C139 C134 120.0 . . ? O101 C140 C141 110(2) . . ? O101 C140 H14B 109.8 . . ? C141 C140 H14B 109.8 . . ? O101 C140 H14C 109.8 . . ? C141 C140 H14C 109.8 . . ? H14B C140 H14C 108.2 . . ? O102 C141 C140 112.7(19) . . ? O102 C141 H14D 109.0 . . ? C140 C141 H14D 109.0 . . ? O102 C141 H14E 109.0 . . ? C140 C141 H14E 109.0 . . ? H14D C141 H14E 107.8 . . ? O102 C142 C143 113(2) . . ? O102 C142 H14F 109.1 . . ? C143 C142 H14F 109.1 . . ? O102 C142 H14G 109.1 . . ? C143 C142 H14G 109.1 . . ? H14F C142 H14G 107.8 . . ? O103 C143 C142 115(3) 3_845 . ? O103 C143 H14H 108.5 3_845 . ? C142 C143 H14H 108.5 . . ? O103 C143 H14I 108.5 3_845 . ? C142 C143 H14I 108.5 . . ? H14H C143 H14I 107.5 . . ? O103 C144 C145 105(3) . . ? O103 C144 H14J 110.7 . . ? C145 C144 H14J 110.7 . . ? O103 C144 H14K 110.7 . . ? C145 C144 H14K 110.7 . . ? H14J C144 H14K 108.8 . . ? O104 C145 C144 114(3) . . ? O104 C145 H14L 108.9 . . ? C144 C145 H14L 108.9 . . ? O104 C145 H14M 108.9 . . ? C144 C145 H14M 108.9 . . ? H14L C145 H14M 107.7 . . ? O6 S1 O5 115.2(7) . . ? O6 S1 O7 114.1(7) . . ? O5 S1 O7 114.0(7) . . ? O6 S1 C46 103.7(8) . . ? O5 S1 C46 103.1(7) . . ? O7 S1 C46 104.8(9) . . ? F2 C46 F3 109.4(13) . . ? F2 C46 F1 109.7(13) . . ? F3 C46 F1 107.3(12) . . ? F2 C46 S1 113.4(13) . . ? F3 C46 S1 108.1(12) . . ? F1 C46 S1 108.7(12) . . ? O9 S2 O10 115.8(9) . . ? O9 S2 O8 116.5(8) . . ? O10 S2 O8 113.4(8) . . ? O9 S2 C47 105.3(10) . . ? O10 S2 C47 100.6(10) . . ? O8 S2 C47 102.4(13) . . ? F5 C47 F6 105.4(15) . . ? F5 C47 F4 104.8(15) . . ? F6 C47 F4 104.8(16) . . ? F5 C47 S2 116.9(17) . . ? F6 C47 S2 112.4(15) . . ? F4 C47 S2 111.5(17) . . ? O13 S3 O12 114.2(7) . . ? O13 S3 O11 114.3(8) . . ? O12 S3 O11 114.5(7) . . ? O13 S3 C48 102.4(10) . . ? O12 S3 C48 104.8(9) . . ? O11 S3 C48 105.0(9) . . ? F9 C48 F7 108.6(14) . . ? F9 C48 F8 108.0(14) . . ? F7 C48 F8 106.7(14) . . ? F9 C48 S3 112.5(15) . . ? F7 C48 S3 111.9(14) . . ? F8 C48 S3 108.8(13) . . ? O14 S4 O16 116.6(10) . . ? O14 S4 O15 116.6(10) . . ? O16 S4 O15 115.4(9) . . ? O14 S4 C49 102.8(13) . . ? O16 S4 C49 105.5(12) . . ? O15 S4 C49 95.8(12) . . ? F11 C49 F12 107.8(15) . . ? F11 C49 F10 106.9(16) . . ? F12 C49 F10 108.3(15) . . ? F11 C49 S4 113.4(17) . . ? F12 C49 S4 116.7(18) . . ? F10 C49 S4 103.2(16) . . ? O18 S5 O19 115.5(8) . . ? O18 S5 O17 116.1(7) . . ? O19 S5 O17 112.1(8) . . ? O18 S5 C50 105.7(9) . . ? O19 S5 C50 102.3(9) . . ? O17 S5 C50 103.1(9) . . ? F15 C50 F14 107.3(14) . . ? F15 C50 F13 106.2(13) . . ? F14 C50 F13 107.4(14) . . ? F15 C50 S5 111.0(13) . . ? F14 C50 S5 112.6(13) . . ? F13 C50 S5 112.0(14) . . ? O22 S6 O21 117.3(11) . . ? O22 S6 O20 114.7(10) . . ? O21 S6 O20 113.6(10) . . ? O22 S6 C51 106.9(13) . . ? O21 S6 C51 102.3(15) . . ? O20 S6 C51 99.2(13) . . ? F16 C51 F17 109.2(16) . . ? F16 C51 F18 109.9(17) . . ? F17 C51 F18 108.4(16) . . ? F16 C51 S6 109.9(18) . . ? F17 C51 S6 116(2) . . ? F18 C51 S6 103.5(18) . . ? O23 S7 O24 115.8(12) . . ? O23 S7 O25 115.2(12) . . ? O24 S7 O25 114.1(11) . . ? O23 S7 C52 106.7(17) . . ? O24 S7 C52 98.0(16) . . ? O25 S7 C52 104.5(14) . . ? F21 C52 F19 108.9(16) . . ? F21 C52 F20 107.6(17) . . ? F19 C52 F20 109.2(16) . . ? F21 C52 S7 108.0(18) . . ? F19 C52 S7 118(2) . . ? F20 C52 S7 104.9(18) . . ? H5WA O5W H5WB 114.4 . . ? H6WA O6W H6WB 110.4 . . ? O1S N1S O2S 117(3) . . ? O1S N1S C1S 122(2) . . ? O2S N1S C1S 121(3) . . ? N1S C1S H1SA 109.5 . . ? N1S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? N1S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O4S N2S O3S 125(4) . . ? O4S N2S C2S 123(3) . . ? O3S N2S C2S 111(3) . . ? N2S C2S H2SA 109.5 . . ? N2S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? N2S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O6S N3S O5S 117(3) . . ? O6S N3S C3S 124(4) . . ? O5S N3S C3S 118(3) . . ? N3S C3S H3SA 109.5 . . ? N3S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? N3S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.756 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.095