#------------------------------------------------------------------------------ #$Date: 2020-08-22 05:15:44 +0300 (Sat, 22 Aug 2020) $ #$Revision: 255575 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705233.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7705233 loop_ _publ_author_name 'Sha, Fanrui' 'Shimizu, Emily A.' 'Slocumb, Hannah S.' 'Towell, Sydney E.' 'Zhen, Yi' 'Porter, Hanna Z.' 'Takase, Michael' 'Johnson, Adam' _publ_section_title ; Catalytic intramolecular hydroamination of aminoallenes using titanium and tantalum complexes of sterically encumbered chiral sulfonamides ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02557G _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_sum 'C35 H39 F6 N4 O3 S Ta' _chemical_formula_weight 890.71 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-12-06 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.8756(13) _cell_length_b 11.4888(11) _cell_length_c 34.989(5) _cell_measurement_reflns_used 9749 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 74.44 _cell_measurement_theta_min 4.60 _cell_volume 3567.8(8) _computing_cell_refinement 'SAINT v8.38A (Bruker-AXS, 2013)' _computing_data_collection 'APEX3 v2017.3-0 (Bruker-AXS, 2017)' _computing_data_reduction 'SAINT v8.38A (Bruker-AXS, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.69 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_unetI/netI 0.0317 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 41686 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.559 _diffrn_reflns_theta_min 2.526 _diffrn_source 'I\mS HB micro-focus sealed tube' _exptl_absorpt_coefficient_mu 6.865 _exptl_absorpt_correction_T_max 0.7538 _exptl_absorpt_correction_T_min 0.4480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Sheldrick, 2014)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1776 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.494 _refine_diff_density_min -1.376 _refine_diff_density_rms 0.078 _refine_ls_abs_structure_details ; Flack x determined using 2982 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.084(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 457 _refine_ls_number_reflns 7123 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.082 _refine_ls_R_factor_all 0.0205 _refine_ls_R_factor_gt 0.0205 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+3.9293P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.0506 _reflns_Friedel_coverage 0.735 _reflns_Friedel_fraction_full 0.967 _reflns_Friedel_fraction_max 0.954 _reflns_number_gt 7105 _reflns_number_total 7123 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02557g2.cif _cod_data_source_block V19229 _cod_database_code 7705233 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.197 _shelx_estimated_absorpt_t_max 0.426 _shelx_res_file ; TITL V19229 in P2(1)2(1)2(1) V19229.res created by SHELXL-2018/3 at 10:28:24 on 06-Jun-2019 CELL 1.54178 8.87560 11.48880 34.98890 90.0000 90.0000 90.0000 ZERR 4.00 0.00130 0.00110 0.00510 0.0000 0.0000 0.0000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F TA S UNIT 140 156 16 12 24 4 4 TEMP -173 SIZE 0.15 0.25 0.35 ACTA WPDB -2 CONF L.S. 10 BOND $H FMAP 2 PLAN 20 WGHT 0.011200 3.929300 FVAR 0.10491 TA1 6 0.512807 0.198907 0.404955 11.00000 0.01064 0.01197 = 0.01082 0.00303 0.00062 0.00166 O1 4 0.395569 0.282608 0.366737 11.00000 0.01402 0.00960 = 0.01452 0.00242 0.00041 -0.00156 C1 1 0.440495 0.388829 0.349218 11.00000 0.01430 0.00979 = 0.00862 0.00196 -0.00079 0.00065 C11 1 0.419131 0.488791 0.378036 11.00000 0.01312 0.01633 = 0.00975 -0.00002 -0.00328 0.00674 C12 1 0.509934 0.587317 0.378517 11.00000 0.02026 0.01486 = 0.01979 -0.00259 -0.00247 0.00072 AFIX 43 H12 2 0.589391 0.594970 0.360499 11.00000 -1.20000 AFIX 0 C13 1 0.484831 0.675283 0.405421 11.00000 0.03324 0.01567 = 0.02929 -0.00938 -0.01123 0.00647 AFIX 43 H13 2 0.547629 0.742242 0.405636 11.00000 -1.20000 AFIX 0 C14 1 0.368866 0.665357 0.431779 11.00000 0.03461 0.03107 = 0.01885 -0.01369 -0.00929 0.01565 AFIX 43 H14 2 0.352716 0.724793 0.450205 11.00000 -1.20000 AFIX 0 C15 1 0.277192 0.568491 0.431018 11.00000 0.02387 0.03251 = 0.01419 -0.00587 -0.00032 0.01628 AFIX 43 H15 2 0.197638 0.561616 0.449042 11.00000 -1.20000 AFIX 0 C16 1 0.299546 0.480636 0.404219 11.00000 0.01700 0.02014 = 0.01368 0.00036 0.00123 0.00591 AFIX 43 H16 2 0.234053 0.415258 0.403630 11.00000 -1.20000 AFIX 0 C21 1 0.340602 0.412612 0.314487 11.00000 0.01188 0.01599 = 0.00816 -0.00146 0.00093 0.00461 C22 1 0.356028 0.515556 0.293503 11.00000 0.01953 0.01819 = 0.01211 -0.00096 -0.00287 0.00225 AFIX 43 H22 2 0.430094 0.571059 0.300718 11.00000 -1.20000 AFIX 0 C23 1 0.264124 0.537270 0.262260 11.00000 0.02420 0.02176 = 0.01389 0.00451 -0.00073 0.00459 AFIX 43 H23 2 0.277015 0.606703 0.247882 11.00000 -1.20000 AFIX 0 C24 1 0.153521 0.458129 0.251910 11.00000 0.02069 0.02757 = 0.01614 -0.00038 -0.00551 0.00554 AFIX 43 H24 2 0.090521 0.473160 0.230522 11.00000 -1.20000 AFIX 0 C25 1 0.135379 0.356424 0.273080 11.00000 0.01915 0.02398 = 0.01738 -0.00443 -0.00243 -0.00313 AFIX 43 H25 2 0.059334 0.302154 0.266186 11.00000 -1.20000 AFIX 0 C26 1 0.228309 0.333894 0.304345 11.00000 0.01548 0.01714 = 0.01322 -0.00013 -0.00007 -0.00055 AFIX 43 H26 2 0.214942 0.264602 0.318769 11.00000 -1.20000 AFIX 0 C2 1 0.609084 0.369961 0.339264 11.00000 0.01139 0.01520 = 0.00664 0.00021 -0.00032 0.00054 AFIX 13 H2 2 0.658534 0.446862 0.334585 11.00000 -1.20000 AFIX 0 N1 3 0.667853 0.318374 0.375387 11.00000 0.01053 0.01311 = 0.00910 0.00118 -0.00129 -0.00004 S1 7 0.844821 0.326346 0.383131 11.00000 0.01050 0.01575 = 0.01055 0.00140 -0.00025 0.00064 O2 4 0.934410 0.288858 0.351054 11.00000 0.01548 0.02021 = 0.01830 0.00012 0.00339 0.00265 O3 4 0.873985 0.274444 0.419870 11.00000 0.01674 0.02131 = 0.01473 0.00609 -0.00447 0.00033 C41 1 0.887217 0.477626 0.388618 11.00000 0.00972 0.01826 = 0.01464 0.00138 -0.00040 -0.00194 C42 1 0.940205 0.542923 0.357976 11.00000 0.01455 0.02107 = 0.00898 -0.00110 -0.00060 0.00061 AFIX 43 H42 2 0.956471 0.507615 0.333774 11.00000 -1.20000 AFIX 0 C43 1 0.968972 0.660685 0.363346 11.00000 0.01774 0.01844 = 0.01845 0.00361 0.00128 0.00204 C47 1 1.030339 0.733074 0.331247 11.00000 0.03574 0.02087 = 0.02437 0.00377 0.00737 0.00479 F1 5 0.992032 0.691668 0.297147 11.00000 0.06432 0.03804 = 0.01707 0.00861 0.00529 0.00078 F2 5 1.181808 0.736464 0.331856 11.00000 0.03665 0.04098 = 0.04860 0.00731 0.01718 -0.00940 F3 5 0.984432 0.843586 0.333442 11.00000 0.07910 0.02268 = 0.04081 0.01146 0.02516 0.01813 C44 1 0.950175 0.712752 0.398971 11.00000 0.01817 0.01896 = 0.01991 -0.00064 -0.00161 0.00330 AFIX 43 H44 2 0.969920 0.793367 0.402353 11.00000 -1.20000 AFIX 0 C45 1 0.902331 0.645239 0.429322 11.00000 0.01539 0.02518 = 0.01428 -0.00356 -0.00098 -0.00026 C48 1 0.888790 0.696613 0.468476 11.00000 0.02712 0.02338 = 0.01737 -0.00344 -0.00159 0.00336 F4 5 0.951473 0.801798 0.471205 11.00000 0.07088 0.02884 = 0.02402 -0.00710 -0.00606 -0.00661 F5 5 0.956000 0.631114 0.494904 11.00000 0.06569 0.03255 = 0.01307 -0.00131 -0.00569 0.01190 F6 5 0.746173 0.709792 0.479346 11.00000 0.02612 0.09706 = 0.03743 -0.03740 0.00627 0.00141 C46 1 0.869545 0.527628 0.424497 11.00000 0.01463 0.02548 = 0.01100 0.00157 -0.00095 -0.00210 AFIX 43 H46 2 0.835527 0.482157 0.445468 11.00000 -1.20000 AFIX 0 C3 1 0.633024 0.289970 0.304404 11.00000 0.01445 0.01589 = 0.01264 -0.00078 -0.00024 0.00101 AFIX 23 H3A 2 0.731823 0.250776 0.307020 11.00000 -1.20000 H3B 2 0.554299 0.228927 0.304580 11.00000 -1.20000 AFIX 0 C31 1 0.628349 0.352254 0.266140 11.00000 0.01682 0.02246 = 0.01140 -0.00145 0.00100 0.00937 C32 1 0.726424 0.444638 0.258866 11.00000 0.02282 0.02971 = 0.01608 0.00390 0.00107 0.00211 AFIX 43 H32 2 0.797029 0.467781 0.277805 11.00000 -1.20000 AFIX 0 C33 1 0.721400 0.502976 0.224078 11.00000 0.03077 0.03442 = 0.02287 0.00984 0.00918 0.00690 AFIX 43 H33 2 0.787489 0.566509 0.219501 11.00000 -1.20000 AFIX 0 C34 1 0.620020 0.468677 0.195967 11.00000 0.03788 0.04440 = 0.01197 0.00727 0.00461 0.01680 AFIX 43 H34 2 0.615942 0.508896 0.172266 11.00000 -1.20000 AFIX 0 C35 1 0.525142 0.375480 0.202808 11.00000 0.03192 0.04141 = 0.01224 -0.00493 -0.00438 0.01588 AFIX 43 H35 2 0.456725 0.350853 0.183557 11.00000 -1.20000 AFIX 0 C36 1 0.529282 0.317904 0.237522 11.00000 0.02522 0.02584 = 0.01309 -0.00668 -0.00089 0.00995 AFIX 43 H36 2 0.463509 0.254018 0.241855 11.00000 -1.20000 AFIX 0 N2 3 0.339805 0.089090 0.409393 11.00000 0.01531 0.01534 = 0.02862 0.00619 -0.00044 -0.00018 C51 1 0.184872 0.129141 0.406066 11.00000 0.01310 0.03555 = 0.11548 0.04030 0.00203 0.00291 AFIX 137 H51A 2 0.139708 0.096846 0.382812 11.00000 -1.50000 H51B 2 0.183276 0.214339 0.404754 11.00000 -1.50000 H51C 2 0.127258 0.103219 0.428393 11.00000 -1.50000 AFIX 0 C52 1 0.340862 -0.036269 0.413978 11.00000 0.02481 0.01801 = 0.03466 0.00729 0.00001 -0.00562 AFIX 137 H52A 2 0.283953 -0.057370 0.436958 11.00000 -1.50000 H52B 2 0.445026 -0.063499 0.416502 11.00000 -1.50000 H52C 2 0.294321 -0.072712 0.391575 11.00000 -1.50000 AFIX 0 N3 3 0.508225 0.263255 0.456759 11.00000 0.02094 0.02191 = 0.01110 0.00595 0.00288 0.00124 C53 1 0.555154 0.380888 0.466984 11.00000 0.02058 0.02313 = 0.01232 -0.00366 -0.00192 0.00075 AFIX 137 H53A 2 0.471606 0.421297 0.479604 11.00000 -1.50000 H53B 2 0.583883 0.423410 0.443823 11.00000 -1.50000 H53C 2 0.641501 0.376984 0.484393 11.00000 -1.50000 AFIX 0 C54 1 0.450236 0.202821 0.490596 11.00000 0.04597 0.03498 = 0.01364 0.00442 0.01135 -0.00606 AFIX 137 H54A 2 0.524230 0.208012 0.511315 11.00000 -1.50000 H54B 2 0.432059 0.120851 0.484367 11.00000 -1.50000 H54C 2 0.355649 0.239195 0.498729 11.00000 -1.50000 AFIX 0 N4 3 0.663304 0.073863 0.403653 11.00000 0.01585 0.01625 = 0.02158 0.00387 -0.00158 0.00090 C55 1 0.733717 0.024395 0.437406 11.00000 0.03131 0.02320 = 0.03048 0.01049 -0.00472 0.01012 AFIX 137 H55A 2 0.715596 -0.059728 0.438025 11.00000 -1.50000 H55B 2 0.690666 0.060326 0.460342 11.00000 -1.50000 H55C 2 0.842414 0.039199 0.436633 11.00000 -1.50000 AFIX 0 C56 1 0.726674 0.027497 0.368583 11.00000 0.02277 0.01834 = 0.03299 -0.00516 0.00096 0.00695 AFIX 137 H56A 2 0.834250 0.046353 0.367362 11.00000 -1.50000 H56B 2 0.674881 0.062025 0.346598 11.00000 -1.50000 H56C 2 0.713688 -0.057198 0.368105 11.00000 -1.50000 AFIX 0 HKLF 4 REM V19229 in P2(1)2(1)2(1) REM wR2 = 0.050643, GooF = S = 1.08217, Restrained GooF = 1.08217 for all data REM R1 = 0.020463 for 7105 Fo > 4sig(Fo) and 0.020526 for all 7123 data REM 457 parameters refined using 0 restraints END WGHT 0.0112 3.9293 REM Highest difference peak 0.494, deepest hole -1.376, 1-sigma level 0.078 Q1 1 0.3783 0.1388 0.4043 11.00000 0.05 0.49 Q2 1 0.5254 0.2322 0.4420 11.00000 0.05 0.46 Q3 1 0.5193 0.1768 0.4432 11.00000 0.05 0.44 Q4 1 0.4785 0.2145 0.3655 11.00000 0.05 0.42 Q5 1 0.5943 0.1072 0.4067 11.00000 0.05 0.37 Q6 1 0.6426 0.1375 0.4001 11.00000 0.05 0.37 Q7 1 1.0093 0.6951 0.3506 11.00000 0.05 0.36 Q8 1 0.6428 0.2370 0.3851 11.00000 0.05 0.34 Q9 1 0.7582 0.6381 0.4866 11.00000 0.05 0.33 Q10 1 0.3721 0.2619 0.4046 11.00000 0.05 0.32 Q11 1 0.9782 0.6053 0.3643 11.00000 0.05 0.32 Q12 1 0.6772 0.2412 0.4051 11.00000 0.05 0.32 Q13 1 0.9851 0.6837 0.3795 11.00000 0.05 0.31 Q14 1 0.5179 0.3168 0.4550 11.00000 0.05 0.30 Q15 1 0.7329 0.2577 0.3769 11.00000 0.05 0.30 Q16 1 1.0632 0.5971 0.2857 11.00000 0.05 0.29 Q17 1 0.0087 0.1154 0.4076 11.00000 0.05 0.28 Q18 1 0.4358 0.4386 0.3651 11.00000 0.05 0.28 Q19 1 0.4386 0.2447 0.3174 11.00000 0.05 0.28 Q20 1 0.8341 0.7995 0.4745 11.00000 0.05 0.28 ; _shelx_res_checksum 28521 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.51281(2) 0.19891(2) 0.40495(2) 0.01114(6) Uani 1 1 d . . . . . O1 O 0.3956(3) 0.2826(2) 0.36674(7) 0.0127(5) Uani 1 1 d . . . . . C1 C 0.4405(4) 0.3888(3) 0.34922(10) 0.0109(7) Uani 1 1 d . . . . . C11 C 0.4191(4) 0.4888(3) 0.37804(10) 0.0131(7) Uani 1 1 d . . . . . C12 C 0.5099(5) 0.5873(3) 0.37852(10) 0.0183(7) Uani 1 1 d . . . . . H12 H 0.589391 0.594970 0.360499 0.022 Uiso 1 1 calc R U . . . C13 C 0.4848(5) 0.6753(3) 0.40542(12) 0.0261(9) Uani 1 1 d . . . . . H13 H 0.547629 0.742242 0.405636 0.031 Uiso 1 1 calc R U . . . C14 C 0.3689(6) 0.6654(4) 0.43178(13) 0.0282(11) Uani 1 1 d . . . . . H14 H 0.352716 0.724793 0.450205 0.034 Uiso 1 1 calc R U . . . C15 C 0.2772(5) 0.5685(4) 0.43102(12) 0.0235(10) Uani 1 1 d . . . . . H15 H 0.197638 0.561616 0.449042 0.028 Uiso 1 1 calc R U . . . C16 C 0.2995(4) 0.4806(3) 0.40422(12) 0.0169(7) Uani 1 1 d . . . . . H16 H 0.234053 0.415258 0.403630 0.020 Uiso 1 1 calc R U . . . C21 C 0.3406(4) 0.4126(3) 0.31449(10) 0.0120(7) Uani 1 1 d . . . . . C22 C 0.3560(5) 0.5156(4) 0.29350(11) 0.0166(8) Uani 1 1 d . . . . . H22 H 0.430094 0.571059 0.300718 0.020 Uiso 1 1 calc R U . . . C23 C 0.2641(5) 0.5373(4) 0.26226(12) 0.0200(9) Uani 1 1 d . . . . . H23 H 0.277015 0.606703 0.247882 0.024 Uiso 1 1 calc R U . . . C24 C 0.1535(5) 0.4581(4) 0.25191(12) 0.0215(9) Uani 1 1 d . . . . . H24 H 0.090521 0.473160 0.230522 0.026 Uiso 1 1 calc R U . . . C25 C 0.1354(5) 0.3564(4) 0.27308(12) 0.0202(9) Uani 1 1 d . . . . . H25 H 0.059334 0.302154 0.266186 0.024 Uiso 1 1 calc R U . . . C26 C 0.2283(4) 0.3339(3) 0.30434(11) 0.0153(8) Uani 1 1 d . . . . . H26 H 0.214942 0.264602 0.318769 0.018 Uiso 1 1 calc R U . . . C2 C 0.6091(4) 0.3700(3) 0.33926(10) 0.0111(7) Uani 1 1 d . . . . . H2 H 0.658534 0.446862 0.334585 0.013 Uiso 1 1 calc R U . . . N1 N 0.6679(3) 0.3184(3) 0.37539(8) 0.0109(6) Uani 1 1 d . . . . . S1 S 0.84482(10) 0.32635(8) 0.38313(2) 0.01226(18) Uani 1 1 d . . . . . O2 O 0.9344(3) 0.2889(3) 0.35105(8) 0.0180(5) Uani 1 1 d . . . . . O3 O 0.8740(3) 0.2744(2) 0.41987(8) 0.0176(6) Uani 1 1 d . . . . . C41 C 0.8872(4) 0.4776(4) 0.38862(11) 0.0142(8) Uani 1 1 d . . . . . C42 C 0.9402(4) 0.5429(3) 0.35798(11) 0.0149(8) Uani 1 1 d . . . . . H42 H 0.956471 0.507615 0.333774 0.018 Uiso 1 1 calc R U . . . C43 C 0.9690(5) 0.6607(3) 0.36335(11) 0.0182(8) Uani 1 1 d . . . . . C47 C 1.0303(6) 0.7331(4) 0.33125(13) 0.0270(10) Uani 1 1 d . . . . . F1 F 0.9920(4) 0.6917(2) 0.29715(7) 0.0398(6) Uani 1 1 d . . . . . F2 F 1.1818(4) 0.7365(3) 0.33186(10) 0.0421(8) Uani 1 1 d . . . . . F3 F 0.9844(5) 0.8436(2) 0.33344(8) 0.0475(9) Uani 1 1 d . . . . . C44 C 0.9502(4) 0.7128(4) 0.39897(11) 0.0190(8) Uani 1 1 d . . . . . H44 H 0.969920 0.793367 0.402353 0.023 Uiso 1 1 calc R U . . . C45 C 0.9023(5) 0.6452(4) 0.42932(12) 0.0183(8) Uani 1 1 d . . . . . C48 C 0.8888(5) 0.6966(4) 0.46848(11) 0.0226(8) Uani 1 1 d . . . . . F4 F 0.9515(4) 0.8018(3) 0.47121(8) 0.0412(7) Uani 1 1 d . . . . . F5 F 0.9560(4) 0.6311(2) 0.49490(7) 0.0371(8) Uani 1 1 d . . . . . F6 F 0.7462(3) 0.7098(4) 0.47935(9) 0.0535(10) Uani 1 1 d . . . . . C46 C 0.8695(5) 0.5276(4) 0.42450(11) 0.0170(8) Uani 1 1 d . . . . . H46 H 0.835527 0.482157 0.445468 0.020 Uiso 1 1 calc R U . . . C3 C 0.6330(4) 0.2900(4) 0.30440(10) 0.0143(7) Uani 1 1 d . . . . . H3A H 0.731823 0.250776 0.307020 0.017 Uiso 1 1 calc R U . . . H3B H 0.554299 0.228927 0.304580 0.017 Uiso 1 1 calc R U . . . C31 C 0.6283(5) 0.3523(4) 0.26614(11) 0.0169(8) Uani 1 1 d . . . . . C32 C 0.7264(5) 0.4446(4) 0.25887(13) 0.0229(9) Uani 1 1 d . . . . . H32 H 0.797029 0.467781 0.277805 0.027 Uiso 1 1 calc R U . . . C33 C 0.7214(6) 0.5030(5) 0.22408(13) 0.0294(10) Uani 1 1 d . . . . . H33 H 0.787489 0.566509 0.219501 0.035 Uiso 1 1 calc R U . . . C34 C 0.6200(6) 0.4687(5) 0.19597(13) 0.0314(11) Uani 1 1 d . . . . . H34 H 0.615942 0.508896 0.172266 0.038 Uiso 1 1 calc R U . . . C35 C 0.5251(6) 0.3755(4) 0.20281(11) 0.0285(10) Uani 1 1 d . . . . . H35 H 0.456725 0.350853 0.183557 0.034 Uiso 1 1 calc R U . . . C36 C 0.5293(5) 0.3179(4) 0.23752(10) 0.0214(8) Uani 1 1 d . . . . . H36 H 0.463509 0.254018 0.241855 0.026 Uiso 1 1 calc R U . . . N2 N 0.3398(4) 0.0891(3) 0.40939(12) 0.0198(7) Uani 1 1 d . . . . . C51 C 0.1849(5) 0.1291(5) 0.4061(3) 0.0547(19) Uani 1 1 d . . . . . H51A H 0.139708 0.096846 0.382812 0.082 Uiso 1 1 calc R U . . . H51B H 0.183276 0.214339 0.404754 0.082 Uiso 1 1 calc R U . . . H51C H 0.127258 0.103219 0.428393 0.082 Uiso 1 1 calc R U . . . C52 C 0.3409(5) -0.0363(4) 0.41398(14) 0.0258(10) Uani 1 1 d . . . . . H52A H 0.283953 -0.057370 0.436958 0.039 Uiso 1 1 calc R U . . . H52B H 0.445026 -0.063499 0.416502 0.039 Uiso 1 1 calc R U . . . H52C H 0.294321 -0.072712 0.391575 0.039 Uiso 1 1 calc R U . . . N3 N 0.5082(4) 0.2633(3) 0.45676(8) 0.0180(7) Uani 1 1 d . . . . . C53 C 0.5552(5) 0.3809(4) 0.46698(11) 0.0187(9) Uani 1 1 d . . . . . H53A H 0.471606 0.421297 0.479604 0.028 Uiso 1 1 calc R U . . . H53B H 0.583883 0.423410 0.443823 0.028 Uiso 1 1 calc R U . . . H53C H 0.641501 0.376984 0.484393 0.028 Uiso 1 1 calc R U . . . C54 C 0.4502(6) 0.2028(5) 0.49060(11) 0.0315(10) Uani 1 1 d . . . . . H54A H 0.524230 0.208012 0.511315 0.047 Uiso 1 1 calc R U . . . H54B H 0.432059 0.120851 0.484367 0.047 Uiso 1 1 calc R U . . . H54C H 0.355649 0.239195 0.498729 0.047 Uiso 1 1 calc R U . . . N4 N 0.6633(4) 0.0739(3) 0.40365(12) 0.0179(7) Uani 1 1 d . . . . . C55 C 0.7337(6) 0.0244(4) 0.43741(14) 0.0283(11) Uani 1 1 d . . . . . H55A H 0.715596 -0.059728 0.438025 0.042 Uiso 1 1 calc R U . . . H55B H 0.690666 0.060326 0.460342 0.042 Uiso 1 1 calc R U . . . H55C H 0.842414 0.039199 0.436633 0.042 Uiso 1 1 calc R U . . . C56 C 0.7267(6) 0.0275(4) 0.36858(14) 0.0247(10) Uani 1 1 d . . . . . H56A H 0.834250 0.046353 0.367362 0.037 Uiso 1 1 calc R U . . . H56B H 0.674881 0.062025 0.346598 0.037 Uiso 1 1 calc R U . . . H56C H 0.713688 -0.057198 0.368105 0.037 Uiso 1 1 calc R U . . . 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 Ta1 0.01064(8) 0.01197(8) 0.01082(8) 0.00303(6) 0.00062(6) 0.00166(6) O1 0.0140(13) 0.0096(13) 0.0145(12) 0.0024(10) 0.0004(9) -0.0016(10) C1 0.0143(18) 0.0098(17) 0.0086(16) 0.0020(14) -0.0008(13) 0.0006(14) C11 0.0131(18) 0.0163(19) 0.0098(16) 0.0000(14) -0.0033(13) 0.0067(14) C12 0.020(2) 0.0149(16) 0.0198(17) -0.0026(14) -0.0025(17) 0.0007(17) C13 0.033(2) 0.0157(17) 0.029(2) -0.0094(16) -0.011(2) 0.0065(16) C14 0.035(3) 0.031(3) 0.019(2) -0.0137(18) -0.0093(19) 0.016(2) C15 0.024(2) 0.033(3) 0.0142(19) -0.0059(18) -0.0003(16) 0.0163(19) C16 0.0170(18) 0.0201(19) 0.0137(17) 0.0004(17) 0.0012(17) 0.0059(14) C21 0.0119(18) 0.0160(18) 0.0082(16) -0.0015(14) 0.0009(13) 0.0046(14) C22 0.020(2) 0.018(2) 0.0121(18) -0.0010(15) -0.0029(15) 0.0023(16) C23 0.024(2) 0.022(2) 0.0139(19) 0.0045(16) -0.0007(16) 0.0046(17) C24 0.021(2) 0.028(2) 0.016(2) -0.0004(17) -0.0055(16) 0.0055(17) C25 0.019(2) 0.024(2) 0.0174(19) -0.0044(16) -0.0024(16) -0.0031(17) C26 0.0155(19) 0.0171(19) 0.0132(18) -0.0001(14) -0.0001(14) -0.0005(14) C2 0.0114(18) 0.0152(19) 0.0066(16) 0.0002(14) -0.0003(13) 0.0005(14) N1 0.0105(14) 0.0131(16) 0.0091(14) 0.0012(12) -0.0013(11) 0.0000(12) S1 0.0105(4) 0.0157(5) 0.0105(4) 0.0014(3) -0.0003(3) 0.0006(3) O2 0.0155(13) 0.0202(14) 0.0183(13) 0.0001(12) 0.0034(10) 0.0026(11) O3 0.0167(14) 0.0213(15) 0.0147(12) 0.0061(11) -0.0045(10) 0.0003(11) C41 0.0097(18) 0.018(2) 0.0146(18) 0.0014(15) -0.0004(14) -0.0019(15) C42 0.0146(18) 0.021(2) 0.0090(16) -0.0011(15) -0.0006(13) 0.0006(14) C43 0.018(2) 0.0184(18) 0.0184(18) 0.0036(14) 0.0013(16) 0.0020(15) C47 0.036(3) 0.021(2) 0.024(2) 0.0038(16) 0.007(2) 0.0048(18) F1 0.0643(19) 0.0380(14) 0.0171(11) 0.0086(10) 0.0053(12) 0.001(2) F2 0.0366(18) 0.0410(18) 0.0486(19) 0.0073(15) 0.0172(15) -0.0094(13) F3 0.079(3) 0.0227(13) 0.0408(16) 0.0115(12) 0.0252(19) 0.0181(17) C44 0.0182(17) 0.0190(18) 0.0199(18) -0.0006(16) -0.0016(14) 0.0033(15) C45 0.015(2) 0.025(2) 0.0143(19) -0.0036(16) -0.0010(15) -0.0003(16) C48 0.027(2) 0.023(2) 0.0174(19) -0.0034(18) -0.0016(15) 0.003(2) F4 0.071(2) 0.0288(14) 0.0240(13) -0.0071(12) -0.0061(13) -0.0066(16) F5 0.066(2) 0.0325(14) 0.0131(11) -0.0013(10) -0.0057(12) 0.0119(14) F6 0.0261(15) 0.097(3) 0.0374(16) -0.0374(19) 0.0063(12) 0.0014(19) C46 0.015(2) 0.025(2) 0.0110(17) 0.0016(16) -0.0009(15) -0.0021(16) C3 0.0145(17) 0.0159(18) 0.0126(17) -0.0008(15) -0.0002(13) 0.0010(16) C31 0.017(2) 0.022(2) 0.0114(18) -0.0014(15) 0.0010(15) 0.0094(16) C32 0.023(2) 0.030(2) 0.0161(19) 0.0039(17) 0.0011(17) 0.0021(18) C33 0.031(3) 0.034(3) 0.023(2) 0.010(2) 0.0092(18) 0.007(2) C34 0.038(3) 0.044(3) 0.012(2) 0.0073(19) 0.0046(18) 0.017(2) C35 0.032(3) 0.041(3) 0.0122(17) -0.0049(17) -0.0044(18) 0.016(2) C36 0.025(2) 0.026(2) 0.0131(16) -0.0067(15) -0.0009(15) 0.0100(18) N2 0.0153(16) 0.0153(16) 0.029(2) 0.0062(17) -0.0004(15) -0.0002(12) C51 0.013(2) 0.036(3) 0.115(6) 0.040(4) 0.002(3) 0.0029(19) C52 0.025(2) 0.018(2) 0.035(3) 0.0073(18) 0.0000(18) -0.0056(17) N3 0.0209(18) 0.0219(15) 0.0111(13) 0.0059(12) 0.0029(14) 0.0012(15) C53 0.021(2) 0.023(2) 0.0123(18) -0.0037(15) -0.0019(14) 0.0007(16) C54 0.046(3) 0.035(2) 0.0136(19) 0.0044(19) 0.0114(17) -0.006(2) N4 0.0159(15) 0.0162(16) 0.0216(17) 0.0039(17) -0.0016(15) 0.0009(12) C55 0.031(3) 0.023(2) 0.030(2) 0.010(2) -0.005(2) 0.010(2) C56 0.023(2) 0.018(2) 0.033(2) -0.0052(18) 0.0010(19) 0.0070(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -5.7959 5.2718 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ta1 N3 115.97(12) . . ? O1 Ta1 N4 135.16(15) . . ? N3 Ta1 N4 108.18(16) . . ? O1 Ta1 N2 87.39(13) . . ? N3 Ta1 N2 98.68(16) . . ? N4 Ta1 N2 93.60(13) . . ? O1 Ta1 N1 72.76(11) . . ? N3 Ta1 N1 102.27(13) . . ? N4 Ta1 N1 91.15(13) . . ? N2 Ta1 N1 155.86(14) . . ? C1 O1 Ta1 124.7(2) . . ? O1 C1 C21 109.5(3) . . ? O1 C1 C11 108.8(3) . . ? C21 C1 C11 108.4(3) . . ? O1 C1 C2 104.3(3) . . ? C21 C1 C2 113.9(3) . . ? C11 C1 C2 111.7(3) . . ? C12 C11 C16 119.0(4) . . ? C12 C11 C1 123.0(3) . . ? C16 C11 C1 118.0(4) . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 120.4(4) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.4(4) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.9(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 119.9(4) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C26 C21 C22 119.1(3) . . ? C26 C21 C1 120.1(3) . . ? C22 C21 C1 120.8(3) . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 120.3(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.6(4) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C26 120.3(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 120.2(4) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? N1 C2 C3 112.7(3) . . ? N1 C2 C1 101.7(3) . . ? C3 C2 C1 113.2(3) . . ? N1 C2 H2 109.7 . . ? C3 C2 H2 109.7 . . ? C1 C2 H2 109.7 . . ? C2 N1 S1 117.7(2) . . ? C2 N1 Ta1 115.3(2) . . ? S1 N1 Ta1 124.81(17) . . ? O3 S1 O2 118.17(17) . . ? O3 S1 N1 107.73(17) . . ? O2 S1 N1 113.17(16) . . ? O3 S1 C41 105.58(18) . . ? O2 S1 C41 104.94(18) . . ? N1 S1 C41 106.32(18) . . ? C46 C41 C42 120.8(4) . . ? C46 C41 S1 118.4(3) . . ? C42 C41 S1 120.8(3) . . ? C43 C42 C41 118.9(4) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C42 C43 C44 121.1(4) . . ? C42 C43 C47 120.4(4) . . ? C44 C43 C47 118.4(4) . . ? F1 C47 F3 108.3(4) . . ? F1 C47 F2 106.3(4) . . ? F3 C47 F2 106.0(4) . . ? F1 C47 C43 112.4(4) . . ? F3 C47 C43 111.9(4) . . ? F2 C47 C43 111.5(4) . . ? C45 C44 C43 118.9(4) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C44 C45 C46 121.0(4) . . ? C44 C45 C48 120.4(4) . . ? C46 C45 C48 118.5(4) . . ? F6 C48 F5 107.0(4) . . ? F6 C48 F4 105.9(4) . . ? F5 C48 F4 106.0(3) . . ? F6 C48 C45 112.5(4) . . ? F5 C48 C45 112.1(4) . . ? F4 C48 C45 112.9(4) . . ? C41 C46 C45 119.2(4) . . ? C41 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C31 C3 C2 114.4(3) . . ? C31 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? C31 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C36 C31 C32 118.6(4) . . ? C36 C31 C3 121.2(4) . . ? C32 C31 C3 120.1(4) . . ? C33 C32 C31 120.4(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.2(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C35 C34 C33 119.4(4) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 120.4(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C31 120.9(4) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? C52 N2 C51 109.2(4) . . ? C52 N2 Ta1 129.2(3) . . ? C51 N2 Ta1 121.4(3) . . ? N2 C51 H51A 109.5 . . ? N2 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N2 C52 H52A 109.5 . . ? N2 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N2 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C53 N3 C54 109.9(3) . . ? C53 N3 Ta1 124.8(2) . . ? C54 N3 Ta1 125.2(3) . . ? N3 C53 H53A 109.5 . . ? N3 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N3 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N3 C54 H54A 109.5 . . ? N3 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N3 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 N4 C55 112.2(3) . . ? C56 N4 Ta1 123.5(3) . . ? C55 N4 Ta1 124.1(3) . . ? N4 C55 H55A 109.5 . . ? N4 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N4 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N4 C56 H56A 109.5 . . ? N4 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N4 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? 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 Ta1 O1 1.948(3) . ? Ta1 N3 1.958(3) . ? Ta1 N4 1.962(3) . ? Ta1 N2 1.993(3) . ? Ta1 N1 2.202(3) . ? O1 C1 1.423(5) . ? C1 C21 1.529(5) . ? C1 C11 1.540(5) . ? C1 C2 1.552(5) . ? C11 C12 1.390(6) . ? C11 C16 1.405(6) . ? C12 C13 1.399(5) . ? C12 H12 0.9500 . ? C13 C14 1.387(7) . ? C13 H13 0.9500 . ? C14 C15 1.379(7) . ? C14 H14 0.9500 . ? C15 C16 1.392(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.392(6) . ? C21 C22 1.399(6) . ? C22 C23 1.387(6) . ? C22 H22 0.9500 . ? C23 C24 1.386(7) . ? C23 H23 0.9500 . ? C24 C25 1.393(6) . ? C24 H24 0.9500 . ? C25 C26 1.394(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C2 N1 1.490(5) . ? C2 C3 1.542(5) . ? C2 H2 1.0000 . ? N1 S1 1.597(3) . ? S1 O3 1.440(3) . ? S1 O2 1.441(3) . ? S1 C41 1.789(4) . ? C41 C46 1.389(6) . ? C41 C42 1.390(5) . ? C42 C43 1.390(6) . ? C42 H42 0.9500 . ? C43 C44 1.393(6) . ? C43 C47 1.500(6) . ? C47 F1 1.329(5) . ? C47 F3 1.336(5) . ? C47 F2 1.345(6) . ? C44 C45 1.382(6) . ? C44 H44 0.9500 . ? C45 C46 1.392(6) . ? C45 C48 1.496(6) . ? C48 F6 1.330(5) . ? C48 F5 1.333(5) . ? C48 F4 1.334(6) . ? C46 H46 0.9500 . ? C3 C31 1.519(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C31 C36 1.390(6) . ? C31 C32 1.396(6) . ? C32 C33 1.390(6) . ? C32 H32 0.9500 . ? C33 C34 1.390(7) . ? C33 H33 0.9500 . ? C34 C35 1.383(8) . ? C34 H34 0.9500 . ? C35 C36 1.384(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? N2 C52 1.449(5) . ? N2 C51 1.455(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N3 C53 1.459(5) . ? N3 C54 1.466(5) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? N4 C56 1.451(6) . ? N4 C55 1.452(6) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ta1 O1 C1 C21 166.5(2) . . . . ? Ta1 O1 C1 C11 -75.1(3) . . . . ? Ta1 O1 C1 C2 44.2(3) . . . . ? O1 C1 C11 C12 148.9(3) . . . . ? C21 C1 C11 C12 -92.1(4) . . . . ? C2 C1 C11 C12 34.3(5) . . . . ? O1 C1 C11 C16 -32.9(4) . . . . ? C21 C1 C11 C16 86.1(4) . . . . ? C2 C1 C11 C16 -147.5(3) . . . . ? C16 C11 C12 C13 1.8(6) . . . . ? C1 C11 C12 C13 180.0(4) . . . . ? C11 C12 C13 C14 -0.2(6) . . . . ? C12 C13 C14 C15 -0.7(6) . . . . ? C13 C14 C15 C16 0.1(7) . . . . ? C14 C15 C16 C11 1.5(6) . . . . ? C12 C11 C16 C15 -2.4(6) . . . . ? C1 C11 C16 C15 179.3(4) . . . . ? O1 C1 C21 C26 -1.0(5) . . . . ? C11 C1 C21 C26 -119.6(4) . . . . ? C2 C1 C21 C26 115.4(4) . . . . ? O1 C1 C21 C22 176.2(3) . . . . ? C11 C1 C21 C22 57.6(4) . . . . ? C2 C1 C21 C22 -67.4(5) . . . . ? C26 C21 C22 C23 -2.1(6) . . . . ? C1 C21 C22 C23 -179.3(4) . . . . ? C21 C22 C23 C24 1.3(6) . . . . ? C22 C23 C24 C25 -0.1(7) . . . . ? C23 C24 C25 C26 -0.4(7) . . . . ? C22 C21 C26 C25 1.6(6) . . . . ? C1 C21 C26 C25 178.9(4) . . . . ? C24 C25 C26 C21 -0.4(6) . . . . ? O1 C1 C2 N1 -46.0(3) . . . . ? C21 C1 C2 N1 -165.4(3) . . . . ? C11 C1 C2 N1 71.4(4) . . . . ? O1 C1 C2 C3 75.1(4) . . . . ? C21 C1 C2 C3 -44.2(5) . . . . ? C11 C1 C2 C3 -167.5(3) . . . . ? C3 C2 N1 S1 79.7(4) . . . . ? C1 C2 N1 S1 -158.9(3) . . . . ? C3 C2 N1 Ta1 -84.6(3) . . . . ? C1 C2 N1 Ta1 36.9(3) . . . . ? C2 N1 S1 O3 178.3(3) . . . . ? Ta1 N1 S1 O3 -19.1(3) . . . . ? C2 N1 S1 O2 -49.2(3) . . . . ? Ta1 N1 S1 O2 113.4(2) . . . . ? C2 N1 S1 C41 65.5(3) . . . . ? Ta1 N1 S1 C41 -131.9(2) . . . . ? O3 S1 C41 C46 -28.8(4) . . . . ? O2 S1 C41 C46 -154.4(3) . . . . ? N1 S1 C41 C46 85.4(3) . . . . ? O3 S1 C41 C42 149.5(3) . . . . ? O2 S1 C41 C42 24.0(4) . . . . ? N1 S1 C41 C42 -96.2(3) . . . . ? C46 C41 C42 C43 -2.9(6) . . . . ? S1 C41 C42 C43 178.8(3) . . . . ? C41 C42 C43 C44 2.1(6) . . . . ? C41 C42 C43 C47 178.3(4) . . . . ? C42 C43 C47 F1 27.2(6) . . . . ? C44 C43 C47 F1 -156.5(4) . . . . ? C42 C43 C47 F3 149.3(4) . . . . ? C44 C43 C47 F3 -34.3(6) . . . . ? C42 C43 C47 F2 -92.0(5) . . . . ? C44 C43 C47 F2 84.3(5) . . . . ? C42 C43 C44 C45 0.1(6) . . . . ? C47 C43 C44 C45 -176.2(4) . . . . ? C43 C44 C45 C46 -1.6(6) . . . . ? C43 C44 C45 C48 176.7(4) . . . . ? C44 C45 C48 F6 108.6(5) . . . . ? C46 C45 C48 F6 -73.1(6) . . . . ? C44 C45 C48 F5 -130.8(4) . . . . ? C46 C45 C48 F5 47.5(5) . . . . ? C44 C45 C48 F4 -11.2(6) . . . . ? C46 C45 C48 F4 167.2(4) . . . . ? C42 C41 C46 C45 1.5(6) . . . . ? S1 C41 C46 C45 179.9(3) . . . . ? C44 C45 C46 C41 0.8(6) . . . . ? C48 C45 C46 C41 -177.5(4) . . . . ? N1 C2 C3 C31 -159.2(3) . . . . ? C1 C2 C3 C31 86.1(4) . . . . ? C2 C3 C31 C36 -124.2(4) . . . . ? C2 C3 C31 C32 56.9(5) . . . . ? C36 C31 C32 C33 1.9(6) . . . . ? C3 C31 C32 C33 -179.2(4) . . . . ? C31 C32 C33 C34 -1.0(7) . . . . ? C32 C33 C34 C35 -0.5(7) . . . . ? C33 C34 C35 C36 1.0(7) . . . . ? C34 C35 C36 C31 0.0(7) . . . . ? C32 C31 C36 C35 -1.4(6) . . . . ? C3 C31 C36 C35 179.7(4) . . . . ?