# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rrr-sr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H80 As F30 N16 O11 S' _chemical_formula_weight 2238.68 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' As As 0.0499 2.0058 '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 21.4103(19) _cell_length_b 26.030(2) _cell_length_c 20.5147(18) _cell_angle_alpha 90.00 _cell_angle_beta 111.082(2) _cell_angle_gamma 90.00 _cell_volume 10667.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9974 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 24.27 _exptl_crystal_description BLOCK _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4556 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8225 _exptl_absorpt_correction_T_max 0.9231 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 126046 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0286 _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 -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 18770 _reflns_number_gt 14429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'MERCURY 2.3' _computing_publication_material 'ORTEP 3V.2' _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. ; 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 0.000 344 86 ' ' 2 0.488 0.726 0.015 74 13 ' ' 3 0.512 0.274 -0.016 74 13 ' ' 4 0.838 0.216 0.028 9 1 ' ' 5 0.663 0.492 0.161 14 1 ' ' 6 1.002 0.500 0.502 342 86 ' ' 7 0.343 -0.012 0.347 13 1 ' ' 8 0.488 0.774 0.515 74 13 ' ' 9 0.512 0.226 0.484 74 13 ' ' 10 0.162 0.716 0.472 9 1 ' ' 11 0.838 0.284 0.528 9 1 ' ' 12 0.657 0.012 0.653 12 1 ' ' 13 0.343 0.512 0.847 13 1 ' ' 14 0.162 0.784 0.972 9 1 ' ' _platon_squeeze_details ; The unit cell contains one water and two dimethyl sulfoxide molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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^)+(0.1892P)^2^+65.9409P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18770 _refine_ls_number_parameters 1283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.2890 _refine_ls_wR_factor_gt 0.2715 _refine_ls_goodness_of_fit_ref 0.850 _refine_ls_restrained_S_all 0.850 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F10 F 0.3598(3) 0.9468(2) 0.5453(3) 0.101(2) Uani 1 1 d . . . F12 F -0.0293(4) 0.8420(3) 0.8698(4) 0.138(3) Uani 1 1 d . . . F9 F 0.4062(4) 1.0182(3) 0.4813(4) 0.147(3) Uani 1 1 d . . . C88 C 0.3071(9) 0.7792(7) 0.9550(9) 0.154(6) Uiso 1 1 d . . . C57 C 0.0672(6) 0.7966(4) 0.3982(7) 0.116(4) Uani 1 1 d . . . H57A H 0.0672 0.7680 0.3678 0.139 Uiso 1 1 calc R . . H57B H 0.1060 0.7925 0.4407 0.139 Uiso 1 1 calc R . . F3 F 0.5972(2) 0.9487(2) 1.0796(2) 0.0895(17) Uani 1 1 d . . . As1 As 0.27331(2) 0.964320(18) 0.79836(3) 0.02684(17) Uani 1 1 d . . . F16 F 0.8801(2) 0.49088(14) 0.9034(2) 0.0577(9) Uani 1 1 d . . . N10 N 0.9150(2) 0.47525(18) 0.7878(2) 0.0420(11) Uani 1 1 d . . . H10 H 0.8748 0.4641 0.7677 0.050 Uiso 1 1 calc R . . O6 O 0.7076(2) 0.66467(14) 0.7894(2) 0.0513(11) Uani 1 1 d . . . C63 C 0.1590(3) 0.9392(2) 0.3521(3) 0.0512(15) Uani 1 1 d . . . H63A H 0.1126 0.9470 0.3446 0.061 Uiso 1 1 calc R . . H63B H 0.1822 0.9348 0.4020 0.061 Uiso 1 1 calc R . . C59 C 0.1094(3) 0.8934(3) 0.2402(3) 0.0524(15) Uani 1 1 d . . . H59A H 0.0681 0.9068 0.2429 0.063 Uiso 1 1 calc R . . H59B H 0.1259 0.9188 0.2158 0.063 Uiso 1 1 calc R . . C60 C 0.0934(3) 0.8472(3) 0.1978(3) 0.0593(18) Uani 1 1 d . . . H60A H 0.0660 0.8250 0.2144 0.071 Uiso 1 1 calc R . . H60B H 0.1345 0.8291 0.2032 0.071 Uiso 1 1 calc R . . C55 C 0.1424(3) 0.8459(2) 0.3545(3) 0.0502(15) Uani 1 1 d . . . H55A H 0.1453 0.8140 0.3312 0.060 Uiso 1 1 calc R . . H55B H 0.1760 0.8443 0.4012 0.060 Uiso 1 1 calc R . . C56 C 0.0763(4) 0.8475(3) 0.3613(4) 0.069(2) Uani 1 1 d . . . H56A H 0.0414 0.8502 0.3155 0.082 Uiso 1 1 calc R . . H56B H 0.0734 0.8770 0.3888 0.082 Uiso 1 1 calc R . . C61 C 0.0561(4) 0.8585(3) 0.1203(3) 0.065(2) Uani 1 1 d . . . H61A H 0.0145 0.8757 0.1158 0.078 Uiso 1 1 calc R . . H61B H 0.0828 0.8827 0.1054 0.078 Uiso 1 1 calc R . . C67 C 0.2282(3) 0.8780(3) 0.3116(3) 0.0589(18) Uani 1 1 d . . . H67A H 0.2377 0.9047 0.2835 0.071 Uiso 1 1 calc R . . H67B H 0.2252 0.8458 0.2869 0.071 Uiso 1 1 calc R . . C62 C 0.0403(5) 0.8155(4) 0.0723(4) 0.090(3) Uani 1 1 d . . . H62A H 0.0809 0.8013 0.0702 0.135 Uiso 1 1 calc R . . H62B H 0.0123 0.8270 0.0267 0.135 Uiso 1 1 calc R . . H62C H 0.0171 0.7897 0.0883 0.135 Uiso 1 1 calc R . . C68 C 0.2871(4) 0.8746(4) 0.3801(4) 0.077(2) Uani 1 1 d . . . H68A H 0.2859 0.9039 0.4089 0.093 Uiso 1 1 calc R . . H68B H 0.2826 0.8438 0.4046 0.093 Uiso 1 1 calc R . . C69 C 0.3508(4) 0.8736(4) 0.3712(4) 0.076(2) Uani 1 1 d . . . H69A H 0.3547 0.9051 0.3478 0.091 Uiso 1 1 calc R . . H69B H 0.3497 0.8455 0.3397 0.091 Uiso 1 1 calc R . . C64 C 0.1888(5) 0.9845(3) 0.3289(5) 0.086(3) Uani 1 1 d . . . H64A H 0.2360 0.9782 0.3391 0.103 Uiso 1 1 calc R . . H64B H 0.1672 0.9887 0.2788 0.103 Uiso 1 1 calc R . . C66 C 0.1971(8) 1.0822(4) 0.3390(7) 0.141(6) Uani 1 1 d . . . H66A H 0.2432 1.0822 0.3431 0.211 Uiso 1 1 calc R . . H66B H 0.1896 1.1098 0.3664 0.211 Uiso 1 1 calc R . . H66C H 0.1691 1.0869 0.2909 0.211 Uiso 1 1 calc R . . C58 C 0.0108(6) 0.7924(5) 0.4155(6) 0.076(3) Uani 0.69 1 d P . . H58A H 0.0082 0.8215 0.4432 0.114 Uiso 0.69 1 calc PR . . H58B H 0.0132 0.7615 0.4417 0.114 Uiso 0.69 1 calc PR . . H58C H -0.0283 0.7915 0.3737 0.114 Uiso 0.69 1 calc PR . . C65 C 0.1809(6) 1.0328(3) 0.3645(5) 0.096(3) Uani 1 1 d . . . H65A H 0.1348 1.0345 0.3618 0.115 Uiso 1 1 calc R . . H65B H 0.2087 1.0298 0.4135 0.115 Uiso 1 1 calc R . . N15 N 0.1614(2) 0.88889(17) 0.3164(2) 0.0369(10) Uani 1 1 d . . . C12 C 0.2338(3) 0.9253(3) 0.5755(3) 0.0525(17) Uani 1 1 d . . . C13 C 0.2892(3) 1.0063(3) 0.5711(3) 0.0576(18) Uani 1 1 d . . . C10 C 0.2401(4) 0.8064(3) 0.5913(4) 0.069(2) Uani 1 1 d . . . H10A H 0.2195 0.7735 0.5739 0.083 Uiso 1 1 calc R . . H10B H 0.2600 0.8194 0.5589 0.083 Uiso 1 1 calc R . . C18 C 0.2679(4) 1.0567(3) 0.5669(4) 0.0641(19) Uani 1 1 d . . . C14 C 0.3353(4) 0.9941(4) 0.5409(4) 0.085(3) Uani 1 1 d . . . C15 C 0.3610(5) 1.0310(5) 0.5096(6) 0.104(4) Uani 1 1 d . . . C11 C 0.1861(3) 0.8444(3) 0.5953(3) 0.0583(18) Uani 1 1 d . . . H11A H 0.1509 0.8471 0.5498 0.070 Uiso 1 1 calc R . . H11B H 0.1665 0.8314 0.6279 0.070 Uiso 1 1 calc R . . C16 C 0.3401(6) 1.0793(5) 0.5070(6) 0.107(4) Uani 1 1 d . . . C17 C 0.2925(5) 1.0930(4) 0.5358(5) 0.083(2) Uani 1 1 d . . . C21 C 0.1915(4) 0.8004(2) 0.7823(4) 0.0620(19) Uani 1 1 d . . . C19 C 0.2781(4) 0.7586(2) 0.7013(4) 0.073(2) Uani 1 1 d . . . H19A H 0.3025 0.7279 0.6980 0.088 Uiso 1 1 calc R . . H19B H 0.2306 0.7506 0.6830 0.088 Uiso 1 1 calc R . . C27 C 0.0566(5) 0.8411(3) 0.8216(5) 0.079(2) Uani 1 1 d . . . C22 C 0.0818(4) 0.8295(2) 0.7702(4) 0.067(2) Uani 1 1 d . . . C20 C 0.2985(4) 0.7747(3) 0.7762(4) 0.070(2) Uani 1 1 d . . . H20A H 0.2985 0.7450 0.8048 0.084 Uiso 1 1 calc R . . H20B H 0.3437 0.7884 0.7920 0.084 Uiso 1 1 calc R . . C25 C -0.0513(6) 0.8062(3) 0.7591(6) 0.090(3) Uani 1 1 d . . . C23 C 0.0368(5) 0.8059(3) 0.7128(4) 0.072(2) Uani 1 1 d . . . C24 C -0.0286(5) 0.7933(3) 0.7054(6) 0.087(3) Uani 1 1 d . . . C26 C -0.0064(6) 0.8293(3) 0.8165(6) 0.096(3) Uani 1 1 d . . . C3 C 0.4414(3) 0.8866(2) 0.7581(3) 0.0463(14) Uani 1 1 d . . . C4 C 0.4813(3) 0.9305(2) 0.8705(3) 0.0421(13) Uani 1 1 d . . . C9 C 0.5153(3) 0.9760(3) 0.8953(4) 0.0526(17) Uani 1 1 d . . . C8 C 0.5547(3) 0.9828(3) 0.9646(4) 0.0579(18) Uani 1 1 d . . . C5 C 0.4885(3) 0.8915(3) 0.9179(3) 0.0534(16) Uani 1 1 d . . . C7 C 0.5608(3) 0.9438(4) 1.0104(4) 0.066(2) Uani 1 1 d . . . C1 C 0.3587(4) 0.7957(3) 0.6581(4) 0.070(2) Uani 1 1 d . . . H1A H 0.3581 0.7712 0.6223 0.084 Uiso 1 1 calc R . . H1B H 0.3885 0.7824 0.7026 0.084 Uiso 1 1 calc R . . C6 C 0.5289(4) 0.8967(3) 0.9874(3) 0.063(2) Uani 1 1 d . . . C2 C 0.3857(4) 0.8465(3) 0.6437(3) 0.068(2) Uani 1 1 d . . . H2A H 0.4296 0.8409 0.6414 0.081 Uiso 1 1 calc R . . H2B H 0.3565 0.8591 0.5985 0.081 Uiso 1 1 calc R . . N3 N 0.4395(2) 0.92750(19) 0.8004(2) 0.0427(11) Uani 1 1 d . . . H3 H 0.4115 0.9520 0.7828 0.051 Uiso 1 1 calc R . . N4 N 0.2142(3) 0.89510(19) 0.6179(2) 0.0480(13) Uani 1 1 d . . . H4 H 0.2185 0.9059 0.6588 0.058 Uiso 1 1 calc R . . N2 N 0.3909(3) 0.8855(2) 0.6967(2) 0.0488(13) Uani 1 1 d . . . H2 H 0.3602 0.9086 0.6879 0.059 Uiso 1 1 calc R . . N5 N 0.2655(3) 0.9700(2) 0.6064(3) 0.0516(14) Uani 1 1 d . . . H5 H 0.2710 0.9756 0.6494 0.062 Uiso 1 1 calc R . . N1 N 0.2919(3) 0.7996(2) 0.6600(3) 0.0601(16) Uani 1 1 d . . . N6 N 0.2529(3) 0.8137(2) 0.7850(3) 0.0626(16) Uani 1 1 d . . . H6 H 0.2655 0.8452 0.7919 0.075 Uiso 1 1 calc R . . N7 N 0.1480(3) 0.8401(2) 0.7774(3) 0.0672(17) Uani 1 1 d . . . H7 H 0.1614 0.8714 0.7788 0.081 Uiso 1 1 calc R . . O1 O 0.4877(2) 0.8550(2) 0.7757(2) 0.0610(13) Uani 1 1 d . . . O2 O 0.2260(3) 0.9148(2) 0.5143(2) 0.0710(16) Uani 1 1 d . . . O3 O 0.1755(3) 0.75541(18) 0.7850(3) 0.0788(17) Uani 1 1 d . . . F1 F 0.51022(19) 1.01555(16) 0.8524(2) 0.0651(10) Uani 1 1 d . . . F5 F 0.4529(2) 0.84731(16) 0.8977(2) 0.0691(11) Uani 1 1 d . . . F2 F 0.58606(19) 1.0271(2) 0.9870(3) 0.0859(16) Uani 1 1 d . . . F4 F 0.5329(3) 0.8581(2) 1.0317(2) 0.0966(17) Uani 1 1 d . . . F6 F 0.2208(2) 1.07003(16) 0.5924(2) 0.0664(11) Uani 1 1 d . . . F7 F 0.2716(4) 1.1418(2) 0.5328(4) 0.130(3) Uani 1 1 d . . . F8 F 0.3632(4) 1.1161(3) 0.4749(5) 0.152(3) Uani 1 1 d . . . F15 F 0.0573(3) 0.7940(2) 0.6592(3) 0.0919(15) Uani 1 1 d . . . F11 F 0.0956(3) 0.8645(2) 0.8795(3) 0.1087(19) Uani 1 1 d . . . F14 F -0.0681(3) 0.7687(3) 0.6482(4) 0.116(2) Uani 1 1 d . . . F13 F -0.1118(3) 0.7950(2) 0.7538(4) 0.124(2) Uani 1 1 d . . . C36 C 0.9342(3) 0.4630(2) 0.9107(3) 0.0473(15) Uani 1 1 d . . . C30 C 0.9396(3) 0.5114(2) 0.7539(3) 0.0397(12) Uani 1 1 d . . . C31 C 0.9538(3) 0.4563(2) 0.8539(3) 0.0433(14) Uani 1 1 d . . . C40 C 0.7446(3) 0.4879(3) 0.4757(3) 0.0583(19) Uani 1 1 d . . . C28 C 0.9098(3) 0.6219(3) 0.6866(4) 0.0567(18) Uani 1 1 d . . . H28A H 0.9349 0.6212 0.7365 0.068 Uiso 1 1 calc R . . H28B H 0.9309 0.6466 0.6658 0.068 Uiso 1 1 calc R . . C45 C 0.7973(4) 0.4534(3) 0.4990(3) 0.0618(19) Uani 1 1 d . . . C32 C 1.0114(4) 0.4282(2) 0.8649(4) 0.0561(17) Uani 1 1 d . . . C39 C 0.7326(3) 0.5741(3) 0.5140(3) 0.0544(17) Uani 1 1 d . . . C29 C 0.9120(3) 0.5694(3) 0.6563(3) 0.0526(16) Uani 1 1 d . . . H29A H 0.8812 0.5687 0.6081 0.063 Uiso 1 1 calc R . . H29B H 0.9567 0.5632 0.6564 0.063 Uiso 1 1 calc R . . C35 C 0.9707(4) 0.4425(3) 0.9760(3) 0.062(2) Uani 1 1 d . . . C38 C 0.7363(3) 0.6541(3) 0.5761(4) 0.070(2) Uani 1 1 d . . . H38A H 0.7159 0.6680 0.6076 0.084 Uiso 1 1 calc R . . H38B H 0.7174 0.6720 0.5318 0.084 Uiso 1 1 calc R . . C34 C 1.0287(5) 0.4159(3) 0.9851(4) 0.072(2) Uani 1 1 d . . . C41 C 0.7031(3) 0.4846(4) 0.4071(4) 0.071(2) Uani 1 1 d . . . C33 C 1.0488(4) 0.4088(3) 0.9291(4) 0.071(2) Uani 1 1 d . . . C37 C 0.8106(3) 0.6634(3) 0.6061(4) 0.066(2) Uani 1 1 d . . . H37A H 0.8309 0.6503 0.5741 0.079 Uiso 1 1 calc R . . H37B H 0.8191 0.7001 0.6113 0.079 Uiso 1 1 calc R . . C42 C 0.7133(4) 0.4473(5) 0.3628(4) 0.085(3) Uani 1 1 d . . . C44 C 0.8073(5) 0.4159(4) 0.4563(4) 0.075(2) Uani 1 1 d . . . C43 C 0.7650(4) 0.4134(4) 0.3882(4) 0.079(3) Uani 1 1 d . . . C48 C 0.7102(3) 0.6212(2) 0.7660(3) 0.0451(14) Uani 1 1 d . . . C49 C 0.5932(3) 0.6075(2) 0.7407(3) 0.0501(16) Uani 1 1 d . . . C50 C 0.5656(3) 0.6530(3) 0.7048(4) 0.062(2) Uani 1 1 d . . . C46 C 0.8351(3) 0.6660(2) 0.7326(4) 0.0542(17) Uani 1 1 d . . . H46A H 0.7958 0.6878 0.7160 0.065 Uiso 1 1 calc R . . H46B H 0.8740 0.6877 0.7533 0.065 Uiso 1 1 calc R . . C54 C 0.5566(3) 0.5816(3) 0.7735(4) 0.0581(18) Uani 1 1 d . . . C47 C 0.8288(3) 0.6291(2) 0.7877(3) 0.0468(14) Uani 1 1 d . . . H47A H 0.8657 0.6049 0.8009 0.056 Uiso 1 1 calc R . . H47B H 0.8309 0.6482 0.8290 0.056 Uiso 1 1 calc R . . C51 C 0.5061(5) 0.6721(4) 0.7060(5) 0.085(3) Uani 1 1 d . . . C52 C 0.4708(4) 0.6455(5) 0.7377(5) 0.092(3) Uani 1 1 d . . . C53 C 0.4955(4) 0.5996(4) 0.7712(4) 0.082(3) Uani 1 1 d . . . N9 N 0.8944(2) 0.5286(2) 0.6946(2) 0.0452(12) Uani 1 1 d . . . H9 H 0.8548 0.5156 0.6791 0.054 Uiso 1 1 calc R . . N13 N 0.7660(2) 0.60132(17) 0.7608(3) 0.0420(11) Uani 1 1 d . . . H13 H 0.7645 0.5719 0.7413 0.050 Uiso 1 1 calc R . . N14 N 0.6546(2) 0.58950(18) 0.7419(3) 0.0479(12) Uani 1 1 d . . . H14 H 0.6581 0.5589 0.7277 0.058 Uiso 1 1 calc R . . N8 N 0.8415(2) 0.6383(2) 0.6744(3) 0.0522(14) Uani 1 1 d . . . N11 N 0.7205(3) 0.6003(2) 0.5654(3) 0.0564(14) Uani 1 1 d . . . H11 H 0.7033 0.5846 0.5918 0.068 Uiso 1 1 calc R . . N12 N 0.7330(3) 0.5227(2) 0.5232(3) 0.0544(14) Uani 1 1 d . . . H12 H 0.7260 0.5107 0.5590 0.065 Uiso 1 1 calc R . . F30 F 0.57986(18) 0.53711(16) 0.8071(2) 0.0651(11) Uani 1 1 d . . . F21 F 0.8401(2) 0.45696(19) 0.56557(19) 0.0726(12) Uani 1 1 d . . . F26 F 0.5973(2) 0.67868(15) 0.6695(2) 0.0689(12) Uani 1 1 d . . . F20 F 1.0318(2) 0.41813(16) 0.8109(2) 0.0720(12) Uani 1 1 d . . . F17 F 0.9503(3) 0.44967(18) 1.0294(2) 0.0814(15) Uani 1 1 d . . . F25 F 0.6507(2) 0.5163(3) 0.3811(2) 0.0933(18) Uani 1 1 d . . . F19 F 1.1048(3) 0.3821(2) 0.9384(3) 0.1058(19) Uani 1 1 d . . . F27 F 0.4826(3) 0.7167(2) 0.6727(3) 0.111(2) Uani 1 1 d . . . F18 F 1.0644(3) 0.3969(2) 1.0482(3) 0.105(2) Uani 1 1 d . . . F22 F 0.8588(3) 0.3834(3) 0.4810(3) 0.1075(19) Uani 1 1 d . . . F29 F 0.4620(2) 0.5719(3) 0.8055(3) 0.1055(19) Uani 1 1 d . . . F23 F 0.7757(3) 0.3761(3) 0.3461(3) 0.108(2) Uani 1 1 d . . . F24 F 0.6730(3) 0.4454(3) 0.2958(2) 0.125(3) Uani 1 1 d . . . F28 F 0.4122(3) 0.6634(3) 0.7383(4) 0.145(3) Uani 1 1 d . . . O4 O 0.99858(19) 0.52521(16) 0.7770(2) 0.0463(10) Uani 1 1 d . . . O5 O 0.7412(2) 0.5947(2) 0.4644(3) 0.0667(14) Uani 1 1 d . . . O7 O 0.31957(17) 0.98373(13) 0.75219(18) 0.0308(7) Uani 1 1 d . . . O10 O 0.21011(17) 0.92713(13) 0.74953(18) 0.0332(8) Uani 1 1 d . . . O9 O 0.24612(17) 1.01289(13) 0.83349(18) 0.0332(8) Uani 1 1 d . . . O8 O 0.3278(2) 0.92643(16) 0.8644(2) 0.0453(9) Uani 1 1 d . . . H8 H 0.3081 0.9151 0.8890 0.068 Uiso 1 1 calc R . . C70 C 0.4140(4) 0.8679(5) 0.4352(5) 0.110(4) Uani 1 1 d . . . H70A H 0.4250 0.9002 0.4591 0.165 Uiso 1 1 calc R . . H70B H 0.4502 0.8571 0.4212 0.165 Uiso 1 1 calc R . . H70C H 0.4069 0.8426 0.4660 0.165 Uiso 1 1 calc R . . S1 S 0.2896(2) 0.83289(17) 0.9923(2) 0.0548(10) Uiso 0.49 1 d P . . S1A S 0.3226(5) 0.8301(4) 0.9623(5) 0.062(2) Uiso 0.20 1 d P . . S1B S 0.3101(4) 0.8454(3) 1.0051(4) 0.0629(18) Uiso 0.31 1 d P . . O11 O 0.2717(3) 0.8787(2) 0.9438(3) 0.089(2) Uani 1 1 d . . . C87 C 0.3743(8) 0.8523(6) 1.0401(9) 0.144(5) Uiso 1 1 d . . . N16 N 0.6758(3) 0.8136(2) 0.7957(3) 0.0508(13) Uani 1 1 d . . . C80 C 0.5936(5) 0.8760(4) 0.7082(6) 0.091(3) Uani 1 1 d . . . C79 C 0.6513(5) 0.8691(4) 0.7787(6) 0.096(3) Uiso 1 1 d . . . C82 C 0.5177(6) 0.9439(5) 0.6308(6) 0.104(3) Uani 1 1 d . . . C81 C 0.5750(6) 0.9345(5) 0.7009(7) 0.112(4) Uiso 1 1 d . . . C76 C 0.7704(5) 0.7672(4) 0.8770(6) 0.103(4) Uani 1 1 d . . . H76A H 0.7740 0.7464 0.8393 0.123 Uiso 1 1 calc R . . H76B H 0.7418 0.7493 0.8970 0.123 Uiso 1 1 calc R . . C75 C 0.7419(4) 0.8159(4) 0.8505(5) 0.089(3) Uani 1 1 d . . . H75A H 0.7719 0.8337 0.8323 0.106 Uiso 1 1 calc R . . H75B H 0.7388 0.8361 0.8889 0.106 Uiso 1 1 calc R . . C71 C 0.6708(6) 0.7857(3) 0.7316(4) 0.085(3) Uani 1 1 d . . . C72 C 0.7254(6) 0.8078(5) 0.7023(6) 0.109(4) Uiso 1 1 d . . . C73 C 0.7029(12) 0.7824(9) 0.6277(12) 0.201(8) Uiso 1 1 d . . . C83 C 0.6236(4) 0.7832(4) 0.8172(6) 0.093(3) Uani 1 1 d . . . C85 C 0.5727(7) 0.7604(6) 0.8999(7) 0.119(4) Uiso 1 1 d . . . C84 C 0.6194(7) 0.7962(6) 0.8809(8) 0.129(4) Uiso 1 1 d . . . C77 C 0.8452(5) 0.7756(3) 0.9371(5) 0.088(3) Uani 1 1 d . . . H77A H 0.8764 0.7876 0.9159 0.106 Uiso 1 1 calc R . . H77B H 0.8432 0.8010 0.9710 0.106 Uiso 1 1 calc R . . C78 C 0.8668(6) 0.7264(4) 0.9710(5) 0.101(3) Uani 1 1 d . . . H78A H 0.8671 0.7278 1.0178 0.152 Uiso 1 1 calc R . . H78B H 0.9110 0.7188 0.9720 0.152 Uiso 1 1 calc R . . H78C H 0.8364 0.7001 0.9454 0.152 Uiso 1 1 calc R . . C86 C 0.5812(12) 0.7098(10) 0.9061(13) 0.219(9) Uiso 1 1 d . . . C74 C 0.7637(16) 0.7967(13) 0.6008(17) 0.278(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 F10 0.101(4) 0.147(5) 0.080(3) 0.058(3) 0.063(3) 0.080(4) F12 0.194(7) 0.102(5) 0.167(7) -0.020(4) 0.125(6) -0.057(5) F9 0.123(5) 0.224(8) 0.144(6) 0.089(6) 0.108(5) 0.068(5) C57 0.137(10) 0.100(8) 0.138(10) -0.062(7) 0.084(8) -0.051(7) F3 0.043(2) 0.168(5) 0.043(2) -0.035(3) -0.0018(18) 0.035(3) As1 0.0266(3) 0.0241(3) 0.0296(3) -0.00088(19) 0.0098(2) -0.00125(18) F16 0.061(2) 0.054(2) 0.065(2) -0.0056(18) 0.0303(19) -0.0168(18) N10 0.033(2) 0.043(3) 0.040(3) 0.004(2) 0.001(2) -0.0051(19) O6 0.052(2) 0.028(2) 0.060(3) -0.0073(18) 0.004(2) 0.0082(17) C63 0.050(4) 0.049(4) 0.043(3) 0.001(3) 0.004(3) 0.000(3) C59 0.053(4) 0.059(4) 0.040(3) 0.002(3) 0.010(3) 0.003(3) C60 0.045(4) 0.087(5) 0.040(3) -0.008(3) 0.008(3) 0.000(3) C55 0.060(4) 0.046(3) 0.045(3) -0.002(3) 0.019(3) 0.006(3) C56 0.070(5) 0.087(5) 0.056(4) -0.009(4) 0.031(4) -0.026(4) C61 0.051(4) 0.098(6) 0.042(4) -0.020(4) 0.011(3) -0.006(4) C67 0.049(4) 0.085(5) 0.039(3) -0.007(3) 0.012(3) 0.007(3) C62 0.093(6) 0.114(7) 0.049(4) -0.015(5) 0.009(4) -0.021(6) C68 0.066(5) 0.110(7) 0.040(4) -0.003(4) -0.001(3) 0.030(5) C69 0.060(5) 0.088(6) 0.074(5) -0.022(4) 0.016(4) 0.013(4) C64 0.107(7) 0.070(5) 0.068(5) -0.004(4) 0.016(5) -0.036(5) C66 0.177(13) 0.079(7) 0.122(10) 0.006(7) 0.001(9) -0.063(8) C58 0.077(8) 0.096(9) 0.065(7) 0.001(6) 0.040(6) -0.030(7) C65 0.123(8) 0.044(4) 0.088(6) 0.003(4) -0.002(6) -0.003(4) N15 0.044(3) 0.041(2) 0.028(2) -0.0012(18) 0.015(2) 0.002(2) C12 0.049(3) 0.068(4) 0.031(3) 0.008(3) 0.003(3) 0.034(3) C13 0.049(4) 0.089(5) 0.036(3) 0.021(3) 0.016(3) 0.022(3) C10 0.063(4) 0.061(4) 0.052(4) -0.029(3) -0.017(3) 0.028(3) C18 0.068(4) 0.083(5) 0.049(4) 0.013(4) 0.030(4) 0.003(4) C14 0.075(5) 0.136(8) 0.060(5) 0.046(5) 0.042(4) 0.047(5) C15 0.095(7) 0.145(10) 0.099(7) 0.046(7) 0.068(6) 0.043(7) C11 0.052(4) 0.060(4) 0.041(3) -0.008(3) -0.010(3) 0.017(3) C16 0.099(7) 0.131(9) 0.117(9) 0.050(7) 0.069(7) 0.004(7) C17 0.094(6) 0.075(6) 0.094(6) 0.015(5) 0.048(5) 0.002(5) C21 0.077(5) 0.037(3) 0.060(4) 0.012(3) 0.011(4) -0.016(3) C19 0.067(5) 0.028(3) 0.088(5) -0.003(3) -0.017(4) 0.010(3) C27 0.109(7) 0.054(4) 0.071(5) -0.001(4) 0.029(5) -0.033(5) C22 0.083(5) 0.033(3) 0.083(5) 0.019(3) 0.028(4) -0.010(3) C20 0.074(5) 0.040(4) 0.068(5) 0.015(3) -0.007(4) -0.003(3) C25 0.108(8) 0.050(5) 0.106(8) 0.019(5) 0.030(6) -0.014(5) C23 0.088(6) 0.064(5) 0.054(5) 0.002(4) 0.015(4) 0.000(4) C24 0.073(6) 0.060(5) 0.106(7) 0.006(5) 0.007(5) -0.017(4) C26 0.141(9) 0.048(5) 0.124(9) 0.018(5) 0.078(8) -0.022(5) C3 0.039(3) 0.057(4) 0.039(3) 0.002(3) 0.009(3) 0.019(3) C4 0.025(3) 0.062(4) 0.037(3) -0.001(3) 0.008(2) 0.015(2) C9 0.023(3) 0.078(5) 0.057(4) -0.014(3) 0.015(3) 0.011(3) C8 0.028(3) 0.078(5) 0.067(5) -0.020(4) 0.016(3) 0.006(3) C5 0.049(4) 0.065(4) 0.039(3) -0.002(3) 0.008(3) 0.012(3) C7 0.030(3) 0.113(7) 0.049(4) -0.035(4) 0.006(3) 0.019(4) C1 0.077(5) 0.054(4) 0.053(4) -0.017(3) -0.007(4) 0.033(4) C6 0.053(4) 0.089(5) 0.038(4) 0.006(4) 0.007(3) 0.034(4) C2 0.057(4) 0.102(6) 0.032(3) -0.011(3) 0.000(3) 0.039(4) N3 0.036(2) 0.053(3) 0.037(3) 0.002(2) 0.010(2) 0.017(2) N4 0.057(3) 0.048(3) 0.030(2) 0.000(2) 0.004(2) 0.024(2) N2 0.046(3) 0.060(3) 0.032(3) 0.003(2) 0.005(2) 0.023(2) N5 0.055(3) 0.072(4) 0.032(3) 0.014(2) 0.021(2) 0.023(3) N1 0.052(3) 0.046(3) 0.056(3) -0.016(3) -0.011(3) 0.019(2) N6 0.086(4) 0.031(3) 0.055(3) 0.011(2) 0.005(3) -0.007(3) N7 0.091(5) 0.030(3) 0.070(4) 0.013(3) 0.016(3) -0.009(3) O1 0.055(3) 0.076(3) 0.042(2) -0.005(2) 0.004(2) 0.035(2) O2 0.077(3) 0.112(4) 0.016(2) 0.006(2) 0.007(2) 0.047(3) O3 0.092(4) 0.034(2) 0.094(4) 0.024(2) 0.015(3) -0.012(2) F1 0.049(2) 0.063(2) 0.083(3) 0.002(2) 0.023(2) -0.0011(18) F5 0.082(3) 0.062(2) 0.050(2) 0.0089(19) 0.008(2) 0.013(2) F2 0.037(2) 0.107(4) 0.104(4) -0.051(3) 0.014(2) -0.008(2) F4 0.103(4) 0.125(4) 0.044(2) 0.021(3) 0.006(2) 0.040(3) F6 0.081(3) 0.061(2) 0.071(3) 0.002(2) 0.045(2) 0.011(2) F7 0.181(7) 0.083(4) 0.171(7) 0.026(4) 0.117(6) -0.004(4) F8 0.162(7) 0.153(6) 0.198(8) 0.058(6) 0.134(6) -0.007(5) F15 0.087(3) 0.092(4) 0.074(3) -0.002(3) 0.002(3) -0.004(3) F11 0.135(5) 0.109(4) 0.088(4) -0.013(3) 0.047(4) -0.047(4) F14 0.073(3) 0.115(5) 0.129(5) -0.021(4) 0.000(3) -0.017(3) F13 0.096(4) 0.078(4) 0.215(8) 0.024(4) 0.076(5) -0.011(3) C36 0.056(4) 0.032(3) 0.049(4) 0.003(2) 0.013(3) -0.015(3) C30 0.031(3) 0.049(3) 0.034(3) -0.002(2) 0.004(2) 0.000(2) C31 0.049(3) 0.027(3) 0.041(3) 0.003(2) 0.001(3) -0.005(2) C40 0.038(3) 0.108(6) 0.036(3) 0.013(3) 0.022(3) -0.013(3) C28 0.035(3) 0.074(5) 0.058(4) 0.023(3) 0.012(3) -0.013(3) C45 0.061(4) 0.095(5) 0.031(3) 0.008(3) 0.018(3) -0.005(4) C32 0.067(4) 0.041(3) 0.048(4) -0.002(3) 0.005(3) 0.006(3) C39 0.029(3) 0.087(5) 0.043(4) 0.026(3) 0.008(3) -0.005(3) C29 0.034(3) 0.079(5) 0.042(3) 0.017(3) 0.010(3) -0.005(3) C35 0.091(5) 0.044(4) 0.043(4) 0.007(3) 0.016(4) -0.029(4) C38 0.047(4) 0.079(5) 0.066(5) 0.034(4) 0.001(3) -0.001(3) C34 0.096(6) 0.043(4) 0.048(4) 0.014(3) -0.011(4) -0.010(4) C41 0.035(3) 0.140(8) 0.038(4) 0.012(4) 0.015(3) -0.007(4) C33 0.076(5) 0.041(4) 0.069(5) 0.007(3) -0.006(4) 0.017(3) C37 0.053(4) 0.073(5) 0.060(4) 0.037(4) 0.006(3) -0.012(3) C42 0.055(5) 0.170(10) 0.033(4) -0.010(5) 0.019(3) -0.025(5) C44 0.081(6) 0.100(6) 0.050(4) 0.001(4) 0.031(4) 0.007(5) C43 0.073(5) 0.133(8) 0.042(4) -0.018(5) 0.033(4) -0.021(5) C48 0.047(3) 0.031(3) 0.052(4) 0.002(2) 0.010(3) 0.005(2) C49 0.045(3) 0.044(3) 0.054(4) -0.020(3) 0.008(3) 0.009(3) C50 0.045(4) 0.057(4) 0.063(4) -0.023(4) -0.006(3) 0.012(3) C46 0.042(3) 0.043(3) 0.063(4) 0.014(3) 0.001(3) -0.015(3) C54 0.033(3) 0.073(5) 0.062(4) -0.015(4) 0.009(3) 0.015(3) C47 0.041(3) 0.040(3) 0.052(4) 0.002(3) 0.008(3) -0.003(2) C51 0.065(5) 0.091(6) 0.067(5) -0.019(5) -0.018(4) 0.041(5) C52 0.041(4) 0.135(9) 0.084(6) -0.014(6) 0.003(4) 0.047(5) C53 0.037(4) 0.138(8) 0.065(5) -0.019(5) 0.013(4) 0.025(5) N9 0.027(2) 0.063(3) 0.038(3) 0.010(2) 0.003(2) -0.008(2) N13 0.045(3) 0.031(2) 0.054(3) -0.003(2) 0.022(2) -0.004(2) N14 0.046(3) 0.027(2) 0.072(4) -0.010(2) 0.022(3) 0.004(2) N8 0.039(3) 0.060(3) 0.051(3) 0.022(3) 0.009(2) -0.010(2) N11 0.038(3) 0.077(4) 0.048(3) 0.020(3) 0.008(2) -0.005(3) N12 0.042(3) 0.090(4) 0.031(3) 0.017(3) 0.012(2) -0.007(3) F30 0.040(2) 0.070(3) 0.089(3) -0.001(2) 0.028(2) 0.0036(18) F21 0.075(3) 0.099(3) 0.0324(19) 0.006(2) 0.0053(19) 0.016(2) F26 0.077(3) 0.050(2) 0.057(2) -0.0077(19) -0.002(2) 0.008(2) F20 0.069(3) 0.062(2) 0.075(3) -0.006(2) 0.015(2) 0.021(2) F17 0.122(4) 0.075(3) 0.048(2) 0.001(2) 0.032(2) -0.047(3) F25 0.038(2) 0.189(6) 0.049(2) 0.019(3) 0.0111(18) 0.007(3) F19 0.099(4) 0.077(3) 0.108(4) 0.024(3) -0.005(3) 0.044(3) F27 0.089(4) 0.104(4) 0.099(4) -0.004(3) -0.018(3) 0.065(3) F18 0.134(5) 0.075(3) 0.063(3) 0.035(2) -0.015(3) -0.009(3) F22 0.132(5) 0.132(5) 0.055(3) -0.004(3) 0.029(3) 0.041(4) F29 0.046(2) 0.170(6) 0.105(4) -0.002(4) 0.033(3) 0.025(3) F23 0.120(4) 0.161(6) 0.060(3) -0.035(3) 0.052(3) -0.018(4) F24 0.067(3) 0.262(8) 0.039(2) -0.025(4) 0.011(2) -0.021(4) F28 0.072(3) 0.201(7) 0.147(6) 0.003(5) 0.021(4) 0.091(4) O4 0.032(2) 0.056(2) 0.041(2) 0.0037(18) 0.0011(17) -0.0052(17) O5 0.043(2) 0.101(4) 0.057(3) 0.039(3) 0.019(2) 0.005(2) O7 0.0332(18) 0.0270(17) 0.0366(19) 0.0027(14) 0.0180(15) -0.0008(14) O10 0.0351(18) 0.0257(17) 0.0372(19) -0.0015(14) 0.0110(15) -0.0058(14) O9 0.0296(17) 0.0344(19) 0.0345(19) -0.0115(15) 0.0105(15) -0.0037(14) O8 0.043(2) 0.044(2) 0.046(2) 0.0157(18) 0.0123(18) 0.0088(18) C70 0.051(5) 0.187(12) 0.076(6) -0.010(7) 0.004(4) 0.036(6) O11 0.121(5) 0.100(4) 0.068(4) 0.039(3) 0.060(4) 0.045(4) N16 0.050(3) 0.047(3) 0.055(3) -0.014(2) 0.018(2) 0.004(2) C80 0.081(6) 0.095(7) 0.100(7) 0.014(5) 0.036(5) 0.030(5) C82 0.100(7) 0.120(8) 0.102(8) 0.038(7) 0.049(6) 0.034(6) C76 0.073(6) 0.086(7) 0.157(10) -0.062(7) 0.052(6) -0.013(5) C75 0.062(5) 0.100(7) 0.090(6) -0.017(5) 0.010(5) 0.007(5) C71 0.151(9) 0.035(4) 0.053(4) -0.010(3) 0.020(5) -0.016(4) C83 0.064(5) 0.110(8) 0.108(8) 0.034(6) 0.033(5) 0.021(5) C77 0.079(6) 0.070(5) 0.093(6) -0.013(5) 0.002(5) 0.023(4) C78 0.117(8) 0.086(7) 0.086(7) -0.021(5) 0.019(6) 0.006(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 F10 C14 1.330(11) . ? F12 C26 1.389(12) . ? F9 C15 1.339(10) . ? C88 S1A 1.360(19) . ? C88 S1 1.698(18) . ? C88 S1B 1.993(19) . ? C57 C58 1.379(14) . ? C57 C56 1.574(14) . ? F3 C7 1.356(8) . ? As1 O9 1.661(3) . ? As1 O10 1.672(3) 1 ? As1 O10 1.672(3) . ? As1 O7 1.676(3) . ? As1 O7 1.676(3) 1 ? As1 O8 1.741(4) . ? F16 C36 1.329(8) . ? N10 C30 1.380(8) . ? N10 C31 1.402(7) . ? O6 C48 1.237(7) . ? C63 C64 1.497(10) . ? C63 N15 1.512(8) . ? C59 C60 1.451(10) . ? C59 N15 1.563(7) . ? C60 C61 1.527(9) . ? C55 C56 1.472(10) . ? C55 N15 1.502(8) . ? C61 C62 1.449(11) . ? C67 N15 1.496(8) . ? C67 C68 1.515(9) . ? C68 C69 1.440(11) . ? C69 C70 1.517(11) . ? C64 C65 1.492(13) . ? C66 C65 1.477(13) . ? C12 O2 1.237(7) . ? C12 N4 1.345(9) . ? C12 N5 1.381(9) . ? C13 C14 1.378(10) . ? C13 C18 1.381(11) . ? C13 N5 1.393(9) . ? C10 N1 1.457(8) . ? C10 C11 1.547(9) . ? C18 F6 1.336(8) . ? C18 C17 1.350(11) . ? C14 C15 1.375(14) . ? C15 C16 1.329(16) . ? C11 N4 1.454(9) . ? C16 F8 1.352(11) . ? C16 C17 1.396(14) . ? C17 F7 1.341(11) . ? C21 O3 1.226(8) . ? C21 N6 1.342(10) . ? C21 N7 1.371(10) . ? C19 N1 1.459(10) . ? C19 C20 1.500(11) . ? C27 F11 1.328(10) . ? C27 C26 1.351(14) . ? C27 C22 1.379(12) . ? C22 C23 1.370(11) . ? C22 N7 1.399(10) . ? C20 N6 1.465(10) . ? C25 F13 1.292(12) . ? C25 C26 1.363(15) . ? C25 C24 1.395(15) . ? C23 F15 1.359(10) . ? C23 C24 1.393(13) . ? C24 F14 1.337(11) . ? C3 O1 1.237(7) . ? C3 N2 1.333(7) . ? C3 N3 1.383(8) . ? C4 C5 1.375(9) . ? C4 C9 1.389(9) . ? C4 N3 1.397(7) . ? C9 F1 1.332(8) . ? C9 C8 1.379(10) . ? C8 F2 1.330(9) . ? C8 C7 1.357(12) . ? C5 F5 1.360(8) . ? C5 C6 1.382(9) . ? C7 C6 1.399(12) . ? C1 N1 1.446(10) . ? C1 C2 1.514(12) . ? C6 F4 1.337(9) . ? C2 N2 1.463(8) . ? C36 C31 1.382(9) . ? C36 C35 1.392(9) . ? C30 O4 1.233(7) . ? C30 N9 1.330(7) . ? C31 C32 1.382(9) . ? C40 C41 1.370(9) . ? C40 C45 1.387(11) . ? C40 N12 1.416(10) . ? C28 N8 1.454(8) . ? C28 C29 1.511(10) . ? C45 F21 1.346(8) . ? C45 C44 1.378(11) . ? C32 F20 1.353(8) . ? C32 C33 1.369(10) . ? C39 O5 1.221(7) . ? C39 N12 1.350(9) . ? C39 N11 1.356(9) . ? C29 N9 1.449(8) . ? C35 F17 1.330(9) . ? C35 C34 1.375(12) . ? C38 N11 1.439(10) . ? C38 C37 1.505(10) . ? C34 F18 1.339(8) . ? C34 C33 1.376(13) . ? C41 F25 1.341(10) . ? C41 C42 1.398(13) . ? C33 F19 1.339(9) . ? C37 N8 1.471(8) . ? C42 F24 1.336(9) . ? C42 C43 1.365(14) . ? C44 F22 1.336(10) . ? C44 C43 1.366(11) . ? C43 F23 1.372(10) . ? C48 N13 1.342(8) . ? C48 N14 1.386(8) . ? C49 C54 1.378(10) . ? C49 N14 1.387(8) . ? C49 C50 1.407(10) . ? C50 F26 1.336(10) . ? C50 C51 1.377(12) . ? C46 N8 1.442(9) . ? C46 C47 1.526(9) . ? C54 F30 1.349(8) . ? C54 C53 1.376(9) . ? C47 N13 1.448(7) . ? C51 F27 1.349(11) . ? C51 C52 1.351(15) . ? C52 F28 1.343(9) . ? C52 C53 1.385(15) . ? C53 F29 1.375(11) . ? O7 O7 0.000(7) 1 ? O10 O10 0.000(10) 1 ? S1 S1B 0.533(8) . ? S1 S1A 1.093(10) . ? S1 O11 1.511(7) 1 ? S1 O11 1.511(7) . ? S1 C87 1.797(17) . ? S1A S1B 1.080(11) . ? S1A O11 1.622(11) 1 ? S1A O11 1.622(11) . ? S1A C87 1.684(19) . ? S1B C87 1.316(17) . ? S1B O11 1.504(9) 1 ? S1B O11 1.504(9) . ? O11 O11 0.000(13) 1 ? N16 C75 1.456(10) . ? N16 C71 1.472(9) . ? N16 C79 1.533(12) . ? N16 C83 1.558(11) . ? C80 C79 1.537(15) . ? C80 C81 1.567(16) . ? C82 C81 1.539(16) . ? C76 C75 1.427(14) . ? C76 C77 1.647(13) . ? C71 C72 1.603(15) . ? C72 C73 1.58(2) . ? C73 C74 1.63(3) . ? C83 C84 1.383(17) . ? C85 C86 1.33(3) . ? C85 C84 1.518(19) . ? C77 C78 1.451(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 S1A C88 S1 40.0(6) . . ? S1A C88 S1B 30.8(6) . . ? S1 C88 S1B 13.8(3) . . ? C58 C57 C56 117.5(11) . . ? O9 As1 O10 111.48(17) . 1 ? O9 As1 O10 111.48(17) . . ? O10 As1 O10 0.0(3) 1 . ? O9 As1 O7 112.73(17) . . ? O10 As1 O7 110.57(17) 1 . ? O10 As1 O7 110.57(17) . . ? O9 As1 O7 112.73(17) . 1 ? O10 As1 O7 110.57(17) 1 1 ? O10 As1 O7 110.57(17) . 1 ? O7 As1 O7 0.00(16) . 1 ? O9 As1 O8 109.55(19) . . ? O10 As1 O8 108.02(19) 1 . ? O10 As1 O8 108.02(19) . . ? O7 As1 O8 104.12(18) . . ? O7 As1 O8 104.12(18) 1 . ? C30 N10 C31 121.8(5) . . ? C64 C63 N15 115.8(6) . . ? C60 C59 N15 117.8(5) . . ? C59 C60 C61 112.8(7) . . ? C56 C55 N15 118.6(6) . . ? C55 C56 C57 108.2(8) . . ? C62 C61 C60 117.7(8) . . ? N15 C67 C68 116.5(6) . . ? C69 C68 C67 113.2(7) . . ? C68 C69 C70 118.9(8) . . ? C65 C64 C63 111.8(8) . . ? C66 C65 C64 118.6(11) . . ? C67 N15 C55 109.7(5) . . ? C67 N15 C63 113.3(5) . . ? C55 N15 C63 109.3(4) . . ? C67 N15 C59 107.7(4) . . ? C55 N15 C59 110.3(5) . . ? C63 N15 C59 106.5(4) . . ? O2 C12 N4 124.5(7) . . ? O2 C12 N5 121.1(7) . . ? N4 C12 N5 114.4(5) . . ? C14 C13 C18 117.7(7) . . ? C14 C13 N5 122.0(7) . . ? C18 C13 N5 120.2(6) . . ? N1 C10 C11 110.4(5) . . ? F6 C18 C17 118.7(8) . . ? F6 C18 C13 120.1(6) . . ? C17 C18 C13 121.2(7) . . ? F10 C14 C15 117.7(7) . . ? F10 C14 C13 120.8(8) . . ? C15 C14 C13 121.4(9) . . ? C16 C15 F9 120.2(10) . . ? C16 C15 C14 119.7(9) . . ? F9 C15 C14 120.1(10) . . ? N4 C11 C10 111.4(6) . . ? C15 C16 F8 120.9(10) . . ? C15 C16 C17 120.7(9) . . ? F8 C16 C17 118.4(11) . . ? F7 C17 C18 120.3(8) . . ? F7 C17 C16 120.4(9) . . ? C18 C17 C16 119.4(9) . . ? O3 C21 N6 122.0(8) . . ? O3 C21 N7 122.1(8) . . ? N6 C21 N7 115.9(6) . . ? N1 C19 C20 110.2(5) . . ? F11 C27 C26 117.6(9) . . ? F11 C27 C22 119.4(8) . . ? C26 C27 C22 123.0(9) . . ? C23 C22 C27 114.1(8) . . ? C23 C22 N7 123.5(8) . . ? C27 C22 N7 122.4(8) . . ? N6 C20 C19 111.0(6) . . ? F13 C25 C26 123.1(12) . . ? F13 C25 C24 120.1(10) . . ? C26 C25 C24 116.8(10) . . ? F15 C23 C22 117.8(8) . . ? F15 C23 C24 117.6(8) . . ? C22 C23 C24 124.6(9) . . ? F14 C24 C23 120.1(10) . . ? F14 C24 C25 121.3(9) . . ? C23 C24 C25 118.6(9) . . ? C27 C26 C25 122.9(10) . . ? C27 C26 F12 120.7(10) . . ? C25 C26 F12 116.5(10) . . ? O1 C3 N2 123.6(6) . . ? O1 C3 N3 122.0(5) . . ? N2 C3 N3 114.3(5) . . ? C5 C4 C9 117.4(6) . . ? C5 C4 N3 123.7(6) . . ? C9 C4 N3 118.8(6) . . ? F1 C9 C8 117.2(7) . . ? F1 C9 C4 120.7(6) . . ? C8 C9 C4 122.1(7) . . ? F2 C8 C7 119.9(7) . . ? F2 C8 C9 120.8(8) . . ? C7 C8 C9 119.3(7) . . ? F5 C5 C4 120.0(5) . . ? F5 C5 C6 118.2(7) . . ? C4 C5 C6 121.8(7) . . ? F3 C7 C8 122.0(8) . . ? F3 C7 C6 117.6(8) . . ? C8 C7 C6 120.4(6) . . ? N1 C1 C2 113.2(5) . . ? F4 C6 C5 119.4(8) . . ? F4 C6 C7 121.6(7) . . ? C5 C6 C7 118.9(7) . . ? N2 C2 C1 113.2(6) . . ? C3 N3 C4 122.4(5) . . ? C12 N4 C11 121.0(6) . . ? C3 N2 C2 122.4(5) . . ? C12 N5 C13 123.0(6) . . ? C1 N1 C10 113.5(6) . . ? C1 N1 C19 111.8(6) . . ? C10 N1 C19 114.1(6) . . ? C21 N6 C20 120.2(6) . . ? C21 N7 C22 119.6(6) . . ? F16 C36 C31 119.4(5) . . ? F16 C36 C35 118.8(7) . . ? C31 C36 C35 121.8(7) . . ? O4 C30 N9 124.1(5) . . ? O4 C30 N10 121.9(5) . . ? N9 C30 N10 114.0(5) . . ? C32 C31 C36 117.0(6) . . ? C32 C31 N10 121.7(6) . . ? C36 C31 N10 121.2(6) . . ? C41 C40 C45 117.4(8) . . ? C41 C40 N12 122.6(7) . . ? C45 C40 N12 120.0(6) . . ? N8 C28 C29 111.8(5) . . ? F21 C45 C44 119.3(7) . . ? F21 C45 C40 118.6(7) . . ? C44 C45 C40 122.1(7) . . ? F20 C32 C33 117.8(7) . . ? F20 C32 C31 120.1(6) . . ? C33 C32 C31 122.0(7) . . ? O5 C39 N12 123.7(7) . . ? O5 C39 N11 123.7(7) . . ? N12 C39 N11 112.6(5) . . ? N9 C29 C28 112.7(5) . . ? F17 C35 C34 120.4(7) . . ? F17 C35 C36 120.1(8) . . ? C34 C35 C36 119.4(7) . . ? N11 C38 C37 112.0(6) . . ? F18 C34 C35 119.4(9) . . ? F18 C34 C33 121.1(9) . . ? C35 C34 C33 119.5(6) . . ? F25 C41 C40 120.6(8) . . ? F25 C41 C42 118.2(7) . . ? C40 C41 C42 121.1(8) . . ? F19 C33 C32 120.8(8) . . ? F19 C33 C34 118.9(7) . . ? C32 C33 C34 120.3(7) . . ? N8 C37 C38 111.4(5) . . ? F24 C42 C43 120.2(9) . . ? F24 C42 C41 120.1(9) . . ? C43 C42 C41 119.7(7) . . ? F22 C44 C43 120.7(8) . . ? F22 C44 C45 120.1(7) . . ? C43 C44 C45 119.2(9) . . ? C42 C43 C44 120.4(8) . . ? C42 C43 F23 120.9(7) . . ? C44 C43 F23 118.6(9) . . ? O6 C48 N13 123.3(6) . . ? O6 C48 N14 122.1(5) . . ? N13 C48 N14 114.6(5) . . ? C54 C49 N14 121.9(6) . . ? C54 C49 C50 117.5(6) . . ? N14 C49 C50 120.7(7) . . ? F26 C50 C51 118.8(8) . . ? F26 C50 C49 120.4(6) . . ? C51 C50 C49 120.8(9) . . ? N8 C46 C47 111.0(5) . . ? F30 C54 C53 118.7(8) . . ? F30 C54 C49 120.0(5) . . ? C53 C54 C49 121.2(8) . . ? N13 C47 C46 110.4(5) . . ? F27 C51 C52 120.9(9) . . ? F27 C51 C50 118.8(11) . . ? C52 C51 C50 120.3(9) . . ? F28 C52 C51 120.8(10) . . ? F28 C52 C53 119.0(11) . . ? C51 C52 C53 120.2(7) . . ? F29 C53 C54 118.0(9) . . ? F29 C53 C52 122.1(7) . . ? C54 C53 C52 119.9(9) . . ? C30 N9 C29 119.9(5) . . ? C48 N13 C47 120.5(5) . . ? C48 N14 C49 119.5(5) . . ? C46 N8 C28 113.1(5) . . ? C46 N8 C37 114.9(6) . . ? C28 N8 C37 111.9(5) . . ? C39 N11 C38 120.6(6) . . ? C39 N12 C40 122.1(5) . . ? O7 O7 As1 0(10) 1 . ? O10 O10 As1 0(4) 1 . ? S1B S1 S1A 74.5(11) . . ? S1B S1 O11 79.2(11) . 1 ? S1A S1 O11 75.1(6) . 1 ? S1B S1 O11 79.2(11) . . ? S1A S1 O11 75.1(6) . . ? O11 S1 O11 0.0(8) 1 . ? S1B S1 C88 116.5(12) . . ? S1A S1 C88 53.1(8) . . ? O11 S1 C88 113.4(7) 1 . ? O11 S1 C88 113.4(7) . . ? S1B S1 C87 21.4(11) . . ? S1A S1 C87 66.1(8) . . ? O11 S1 C87 96.0(6) 1 . ? O11 S1 C87 96.0(6) . . ? C88 S1 C87 97.7(8) . . ? S1B S1A S1 28.4(5) . . ? S1B S1A C88 109.0(12) . . ? S1 S1A C88 86.9(10) . . ? S1B S1A O11 64.1(6) . 1 ? S1 S1A O11 64.2(6) . 1 ? C88 S1A O11 128.1(10) . 1 ? S1B S1A O11 64.1(6) . . ? S1 S1A O11 64.2(6) . . ? C88 S1A O11 128.1(10) . . ? O11 S1A O11 0.0(4) 1 . ? S1B S1A C87 51.4(8) . . ? S1 S1A C87 77.4(8) . . ? C88 S1A C87 119.4(11) . . ? O11 S1A C87 96.4(8) 1 . ? O11 S1A C87 96.4(8) . . ? S1 S1B S1A 77.1(12) . . ? S1 S1B C87 150.1(15) . . ? S1A S1B C87 88.8(10) . . ? S1 S1B O11 80.5(11) . 1 ? S1A S1B O11 75.7(7) . 1 ? C87 S1B O11 121.8(10) . 1 ? S1 S1B O11 80.5(11) . . ? S1A S1B O11 75.7(7) . . ? C87 S1B O11 121.8(10) . . ? O11 S1B O11 0.0(5) 1 . ? S1 S1B C88 49.7(10) . . ? S1A S1B C88 40.1(8) . . ? C87 S1B C88 103.5(10) . . ? O11 S1B C88 99.2(7) 1 . ? O11 S1B C88 99.2(7) . . ? O11 O11 S1B 0(10) 1 . ? O11 O11 S1 0(10) 1 . ? S1B O11 S1 20.4(3) . . ? O11 O11 S1A 0(10) 1 . ? S1B O11 S1A 40.2(4) . . ? S1 O11 S1A 40.6(4) . . ? S1B C87 S1A 39.9(6) . . ? S1B C87 S1 8.5(4) . . ? S1A C87 S1 36.4(5) . . ? C75 N16 C71 116.6(7) . . ? C75 N16 C79 107.2(7) . . ? C71 N16 C79 110.6(6) . . ? C75 N16 C83 113.5(7) . . ? C71 N16 C83 99.9(7) . . ? C79 N16 C83 108.8(6) . . ? C79 C80 C81 107.1(9) . . ? N16 C79 C80 114.7(8) . . ? C82 C81 C80 109.5(10) . . ? C75 C76 C77 109.6(7) . . ? C76 C75 N16 115.0(8) . . ? N16 C71 C72 109.2(7) . . ? C73 C72 C71 101.8(12) . . ? C72 C73 C74 103.4(19) . . ? C84 C83 N16 116.0(11) . . ? C86 C85 C84 123.5(16) . . ? C83 C84 C85 111.4(12) . . ? C78 C77 C76 107.3(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N12 H12 O9 0.86 2.07 2.823(6) 146.1 2_646 N11 H11 O9 0.86 2.41 2.988(6) 124.9 2_646 N14 H14 O7 0.86 2.02 2.802(6) 150.6 2_646 N9 H9 O9 0.86 2.08 2.882(6) 154.1 2_646 N13 H13 O9 0.86 2.12 2.957(6) 163.0 2_646 O8 H8 O11 0.82 1.84 2.654(7) 169.6 1 N3 H3 O7 0.86 2.02 2.808(6) 152.8 1 N4 H4 O10 0.86 2.01 2.859(6) 169.2 1 N5 H5 O7 0.86 2.00 2.815(6) 158.0 1 N6 H6 O10 0.86 2.44 3.099(6) 133.8 1 N7 H7 O10 0.86 2.00 2.788(7) 151.7 1 N10 H10 O10 0.86 1.97 2.803(6) 161.7 2_646 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.623 _refine_diff_density_min -1.123 _refine_diff_density_rms 0.143 _database_code_depnum_ccdc_archive 'CCDC 910790'