#------------------------------------------------------------------------------ #$Date: 2016-01-09 04:27:53 +0200 (Sat, 09 Jan 2016) $ #$Revision: 173696 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/19/1541920.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_1541920 loop_ _publ_author_name 'Chang, Meng-Yang' 'Cheng, Yu-Chieh' _publ_section_title ; Synthesis of Substituted Tetralins and Benzosuberans via BF3·OEt2-Mediated Formal (4 + 2) and (5 + 2) Stereocontrolled Cycloaddition of 4-Alkenols with Veratrol ; _journal_name_full 'Organic Letters' _journal_paper_doi 10.1021/acs.orglett.5b03696 _journal_year 2016 _chemical_formula_sum 'C25 H31 F O3 S' _chemical_formula_weight 430.56 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 90.7750(10) _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 15.2927(5) _cell_length_b 18.9203(5) _cell_length_c 22.9664(7) _cell_measurement_reflns_used 9905 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.3871 _cell_measurement_theta_min 2.4526 _cell_volume 6644.5(3) _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_collection 'APEX2 (Bruker AXS, 2010)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL-2014/6 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_laue_measured_fraction_full 0.999 _diffrn_reflns_laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 55647 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.414 _diffrn_reflns_theta_min 1.394 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Lump _exptl_crystal_F_000 2760 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.444 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.120 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 823 _refine_ls_number_reflns 13610 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.107 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0380 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+2.0463P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1018 _refine_ls_wR_factor_ref 0.1217 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11179 _reflns_number_total 13610 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol5b03696_si_012.cif _cod_data_source_block 150802LT_0m_a _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas ; _cod_database_code 1541920 _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. ; _shelxl_version_number 2014/6 _shelx_res_file ; TITL 150802LT_0m_a.res in P2(1)/n CELL 0.71073 15.2927 18.9203 22.9664 90.000 90.775 90.000 ZERR 12.000 0.0005 0.0005 0.0007 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H O F S UNIT 300 372 36 12 12 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 TEMP -173.000 WGHT 0.061200 2.046300 FVAR 0.24621 C1 1 0.163655 0.622816 0.194203 11.00000 0.01711 0.01269 = 0.01473 0.00095 0.00052 0.00051 AFIX 13 H1 2 0.208146 0.659547 0.204739 11.00000 -1.20000 AFIX 0 C2 1 0.082183 0.637530 0.230999 11.00000 0.02089 0.01787 = 0.01575 0.00053 0.00296 0.00244 AFIX 23 H2A 2 0.094002 0.623299 0.271834 11.00000 -1.20000 H2B 2 0.069488 0.688838 0.230583 11.00000 -1.20000 AFIX 0 C3 1 0.002398 0.597012 0.207487 11.00000 0.01920 0.01386 = 0.02422 0.00031 0.00751 0.00041 AFIX 13 H3 2 0.020931 0.546326 0.207531 11.00000 -1.20000 AFIX 0 C4 1 -0.079811 0.599058 0.246389 11.00000 0.02558 0.01914 = 0.03207 0.00147 0.01393 -0.00104 C5 1 -0.150489 0.553008 0.216343 11.00000 0.02668 0.02448 = 0.05806 -0.00707 0.02179 -0.00784 AFIX 23 H5A 2 -0.132342 0.502878 0.219082 11.00000 -1.20000 H5B 2 -0.205728 0.558082 0.237937 11.00000 -1.20000 AFIX 0 C6 1 -0.168195 0.570735 0.152632 11.00000 0.01693 0.03734 = 0.05569 -0.02047 0.00875 -0.00882 AFIX 23 H6A 2 -0.193686 0.618725 0.149744 11.00000 -1.20000 H6B 2 -0.211305 0.536859 0.136263 11.00000 -1.20000 AFIX 0 C7 1 -0.084703 0.567661 0.117259 11.00000 0.01819 0.03430 = 0.03858 -0.01519 0.00245 -0.00276 AFIX 23 H7A 2 -0.063207 0.518326 0.116268 11.00000 -1.20000 H7B 2 -0.097888 0.582403 0.076722 11.00000 -1.20000 AFIX 0 C8 1 -0.013406 0.615176 0.142631 11.00000 0.01269 0.02030 = 0.02216 -0.00459 0.00416 0.00036 C9 1 0.141749 0.632084 0.128866 11.00000 0.01445 0.01365 = 0.01554 0.00173 0.00091 -0.00044 AFIX 13 H9 2 0.128990 0.683380 0.122596 11.00000 -1.20000 AFIX 0 C10 1 0.320193 0.538738 0.192948 11.00000 0.01867 0.01751 = 0.01289 0.00260 -0.00116 0.00221 C11 1 0.377747 0.590109 0.213787 11.00000 0.02278 0.01780 = 0.01619 -0.00187 -0.00134 0.00333 AFIX 43 H11 2 0.358047 0.625865 0.239519 11.00000 -1.20000 AFIX 0 C12 1 0.464090 0.588389 0.196506 11.00000 0.02039 0.02179 = 0.01936 -0.00102 -0.00278 -0.00103 AFIX 43 H12 2 0.503256 0.623926 0.210046 11.00000 -1.20000 AFIX 0 C13 1 0.494922 0.535465 0.159543 11.00000 0.02179 0.02526 = 0.01438 0.00330 0.00017 0.00435 C14 1 0.436298 0.483703 0.140393 11.00000 0.02691 0.02067 = 0.01801 -0.00248 0.00016 0.00659 AFIX 43 H14 2 0.456331 0.446697 0.116003 11.00000 -1.20000 AFIX 0 C15 1 0.349562 0.485428 0.156351 11.00000 0.02401 0.01802 = 0.01749 -0.00127 -0.00358 0.00094 AFIX 43 H15 2 0.310102 0.450339 0.142387 11.00000 -1.20000 AFIX 0 C16 1 0.589049 0.534144 0.141133 11.00000 0.02409 0.03355 = 0.02419 0.00235 0.00577 0.00353 AFIX 137 H16A 2 0.614573 0.487913 0.150389 11.00000 -1.50000 H16B 2 0.621658 0.571144 0.161927 11.00000 -1.50000 H16C 2 0.592170 0.542513 0.099102 11.00000 -1.50000 AFIX 0 C17 1 0.214377 0.612698 0.087903 11.00000 0.01671 0.01437 = 0.01416 0.00458 0.00084 0.00337 C18 1 0.291437 0.652343 0.089983 11.00000 0.02186 0.01684 = 0.01899 0.00179 0.00220 0.00152 AFIX 43 H18 2 0.296532 0.690246 0.116945 11.00000 -1.20000 AFIX 0 C19 1 0.360492 0.637585 0.053614 11.00000 0.01943 0.02325 = 0.02398 0.00331 0.00381 -0.00145 AFIX 43 H19 2 0.413276 0.663985 0.055801 11.00000 -1.20000 AFIX 0 C20 1 0.350115 0.583307 0.014121 11.00000 0.02239 0.02738 = 0.01974 0.00267 0.00813 0.00784 C21 1 0.275310 0.543529 0.009815 11.00000 0.02606 0.02001 = 0.01816 -0.00041 0.00069 0.00548 AFIX 43 H21 2 0.270161 0.506797 -0.018224 11.00000 -1.20000 AFIX 0 C22 1 0.206984 0.558267 0.047559 11.00000 0.01875 0.01762 = 0.01793 0.00284 -0.00155 0.00220 AFIX 43 H22 2 0.154976 0.530857 0.045657 11.00000 -1.20000 AFIX 0 C23 1 -0.056715 0.566293 0.305724 11.00000 0.04496 0.03197 = 0.03793 0.01148 0.02560 0.00562 AFIX 137 H23A 2 -0.019414 0.598968 0.327957 11.00000 -1.50000 H23B 2 -0.025482 0.521678 0.299885 11.00000 -1.50000 H23C 2 -0.110492 0.557301 0.327238 11.00000 -1.50000 AFIX 0 C24 1 -0.116128 0.673452 0.257947 11.00000 0.02456 0.02305 = 0.02931 -0.00308 0.01169 -0.00025 AFIX 137 H24A 2 -0.140329 0.693081 0.221677 11.00000 -1.50000 H24B 2 -0.068941 0.704040 0.272468 11.00000 -1.50000 H24C 2 -0.162263 0.670651 0.287060 11.00000 -1.50000 AFIX 0 C25 1 -0.034037 0.692830 0.128738 11.00000 0.01790 0.02507 = 0.02113 0.00184 0.00111 0.00603 AFIX 137 H25A 2 0.004810 0.723506 0.151742 11.00000 -1.50000 H25B 2 -0.094982 0.702957 0.138420 11.00000 -1.50000 H25C 2 -0.025108 0.701594 0.087185 11.00000 -1.50000 AFIX 0 C26 1 0.353018 0.437030 0.345383 11.00000 0.01269 0.01420 = 0.01613 0.00241 -0.00173 -0.00089 AFIX 13 H26 2 0.307111 0.464410 0.323689 11.00000 -1.20000 AFIX 0 C27 1 0.438401 0.444515 0.311668 11.00000 0.01505 0.02160 = 0.01429 0.00251 0.00006 -0.00211 AFIX 23 H27A 2 0.434158 0.416992 0.275078 11.00000 -1.20000 H27B 2 0.447562 0.494756 0.301366 11.00000 -1.20000 AFIX 0 C28 1 0.516353 0.417996 0.348153 11.00000 0.01297 0.01566 = 0.01621 0.00135 0.00023 -0.00177 AFIX 13 H28 2 0.501475 0.367984 0.358029 11.00000 -1.20000 AFIX 0 C29 1 0.604380 0.413216 0.315311 11.00000 0.01265 0.02000 = 0.01825 -0.00004 0.00146 -0.00209 C30 1 0.670883 0.377945 0.357318 11.00000 0.01334 0.02265 = 0.02774 0.00097 0.00109 -0.00051 AFIX 23 H30A 2 0.653823 0.327974 0.363033 11.00000 -1.20000 H30B 2 0.729224 0.378361 0.339157 11.00000 -1.20000 AFIX 0 C31 1 0.677582 0.414268 0.417083 11.00000 0.01506 0.02423 = 0.02423 0.00030 -0.00274 -0.00029 AFIX 23 H31A 2 0.718155 0.387145 0.442530 11.00000 -1.20000 H31B 2 0.702134 0.462280 0.412160 11.00000 -1.20000 AFIX 0 C32 1 0.588434 0.419757 0.446487 11.00000 0.01600 0.02050 = 0.01627 -0.00072 -0.00207 -0.00052 AFIX 23 H32A 2 0.567307 0.371739 0.456066 11.00000 -1.20000 H32B 2 0.595016 0.446476 0.483349 11.00000 -1.20000 AFIX 0 C33 1 0.521127 0.456599 0.407338 11.00000 0.01095 0.01757 = 0.01687 0.00030 0.00111 -0.00209 C34 1 0.363800 0.471278 0.405870 11.00000 0.01310 0.01330 = 0.01700 0.00122 -0.00128 0.00000 AFIX 13 H34 2 0.373870 0.522904 0.399476 11.00000 -1.20000 AFIX 0 C35 1 0.155852 0.372790 0.300307 11.00000 0.01788 0.01873 = 0.01761 0.00035 -0.00101 -0.00277 AFIX 43 H35 2 0.185393 0.384082 0.265393 11.00000 -1.20000 AFIX 0 C36 1 0.202351 0.349517 0.349190 11.00000 0.01364 0.01215 = 0.01799 -0.00258 0.00023 -0.00269 C37 1 0.159355 0.330493 0.399811 11.00000 0.02058 0.01546 = 0.01802 -0.00092 0.00037 -0.00336 AFIX 43 H37 2 0.191390 0.313931 0.432810 11.00000 -1.20000 AFIX 0 C38 1 0.069398 0.336048 0.401368 11.00000 0.02160 0.01960 = 0.02294 0.00015 0.00646 -0.00504 AFIX 43 H38 2 0.039672 0.322295 0.435610 11.00000 -1.20000 AFIX 0 C39 1 0.021090 0.361442 0.353716 11.00000 0.01678 0.01806 = 0.03348 -0.00138 0.00160 -0.00270 C40 1 0.065812 0.379210 0.303416 11.00000 0.01816 0.02136 = 0.02542 0.00219 -0.00576 -0.00164 AFIX 43 H40 2 0.033887 0.396113 0.270489 11.00000 -1.20000 AFIX 0 C41 1 -0.076541 0.369572 0.356309 11.00000 0.01682 0.03731 = 0.05445 0.01231 0.00544 -0.00132 AFIX 137 H41A 2 -0.104704 0.330272 0.335537 11.00000 -1.50000 H41B 2 -0.093794 0.414344 0.338030 11.00000 -1.50000 H41C 2 -0.094788 0.369402 0.397049 11.00000 -1.50000 AFIX 0 C42 1 0.285486 0.464617 0.444987 11.00000 0.01319 0.01244 = 0.01831 -0.00431 0.00023 -0.00169 C43 1 0.287880 0.422331 0.494563 11.00000 0.01377 0.01666 = 0.01890 -0.00359 -0.00255 -0.00166 AFIX 43 H43 2 0.339192 0.396181 0.503954 11.00000 -1.20000 AFIX 0 C44 1 0.215400 0.418170 0.530473 11.00000 0.01809 0.02179 = 0.01827 -0.00074 0.00054 -0.00364 AFIX 43 H44 2 0.216555 0.389717 0.564557 11.00000 -1.20000 AFIX 0 C45 1 0.142213 0.456344 0.515241 11.00000 0.01639 0.02625 = 0.02399 -0.00419 0.00780 -0.00284 C46 1 0.137093 0.498532 0.466540 11.00000 0.01626 0.02115 = 0.03135 -0.00070 0.00183 0.00483 AFIX 43 H46 2 0.085250 0.524055 0.457272 11.00000 -1.20000 AFIX 0 C47 1 0.209970 0.502667 0.431367 11.00000 0.01877 0.01591 = 0.02247 0.00082 0.00044 0.00075 AFIX 43 H47 2 0.208345 0.531748 0.397649 11.00000 -1.20000 AFIX 0 C48 1 0.591476 0.365434 0.262001 11.00000 0.01867 0.02770 = 0.02409 -0.00515 0.00500 -0.00138 AFIX 137 H48A 2 0.558402 0.390998 0.231831 11.00000 -1.50000 H48B 2 0.559131 0.322963 0.273236 11.00000 -1.50000 H48C 2 0.648645 0.351785 0.246845 11.00000 -1.50000 AFIX 0 C49 1 0.640339 0.484158 0.293563 11.00000 0.01796 0.02681 = 0.02255 0.00303 0.00301 -0.00584 AFIX 137 H49A 2 0.687689 0.475478 0.266137 11.00000 -1.50000 H49B 2 0.662847 0.511577 0.326720 11.00000 -1.50000 H49C 2 0.593415 0.510666 0.273962 11.00000 -1.50000 AFIX 0 C50 1 0.538166 0.536616 0.405097 11.00000 0.01639 0.01937 = 0.02465 -0.00098 -0.00026 -0.00441 AFIX 137 H50A 2 0.503732 0.557544 0.373197 11.00000 -1.50000 H50B 2 0.600481 0.545168 0.398605 11.00000 -1.50000 H50C 2 0.521148 0.558150 0.442062 11.00000 -1.50000 AFIX 0 C51 1 0.350505 0.806042 0.379090 11.00000 0.01713 0.01379 = 0.01632 0.00100 -0.00058 0.00002 AFIX 13 H51 2 0.308826 0.840505 0.360832 11.00000 -1.20000 AFIX 0 C52 1 0.437432 0.813430 0.346669 11.00000 0.01868 0.02113 = 0.01577 0.00270 0.00122 -0.00131 AFIX 23 H52A 2 0.431700 0.791456 0.307683 11.00000 -1.20000 H52B 2 0.451024 0.864146 0.341259 11.00000 -1.20000 AFIX 0 C53 1 0.512438 0.777781 0.380761 11.00000 0.01473 0.01812 = 0.01857 0.00127 0.00078 -0.00225 AFIX 13 H53 2 0.492908 0.727825 0.386338 11.00000 -1.20000 AFIX 0 C54 1 0.600120 0.772067 0.347570 11.00000 0.01706 0.02692 = 0.02101 -0.00022 0.00218 -0.00260 C55 1 0.665887 0.733207 0.387767 11.00000 0.01571 0.02831 = 0.02851 0.00044 0.00213 0.00037 AFIX 23 H55A 2 0.647887 0.683099 0.390843 11.00000 -1.20000 H55B 2 0.724123 0.734257 0.369477 11.00000 -1.20000 AFIX 0 C56 1 0.674172 0.764012 0.449041 11.00000 0.01661 0.02777 = 0.02734 0.00407 -0.00199 -0.00119 AFIX 23 H56A 2 0.698895 0.812282 0.446846 11.00000 -1.20000 H56B 2 0.714839 0.734576 0.472579 11.00000 -1.20000 AFIX 0 C57 1 0.585438 0.766878 0.478656 11.00000 0.01905 0.02782 = 0.01857 0.00222 -0.00204 -0.00152 AFIX 23 H57A 2 0.563425 0.718180 0.484276 11.00000 -1.20000 H57B 2 0.592420 0.788988 0.517510 11.00000 -1.20000 AFIX 0 C58 1 0.519104 0.808846 0.442751 11.00000 0.01325 0.02065 = 0.01911 0.00213 0.00040 -0.00439 C59 1 0.192840 0.726455 0.381016 11.00000 0.01624 0.01653 = 0.01638 -0.00499 -0.00114 -0.00115 C60 1 0.157576 0.689116 0.427230 11.00000 0.02203 0.01549 = 0.02183 -0.00152 -0.00226 -0.00180 AFIX 43 H60 2 0.193628 0.659667 0.450927 11.00000 -1.20000 AFIX 0 C61 1 0.069027 0.695483 0.438229 11.00000 0.02380 0.02157 = 0.02071 -0.00246 0.00178 -0.00626 AFIX 43 H61 2 0.044390 0.669324 0.469273 11.00000 -1.20000 AFIX 0 C62 1 0.015361 0.739518 0.404645 11.00000 0.01816 0.02514 = 0.02653 -0.01010 -0.00017 -0.00209 C63 1 0.052786 0.775869 0.358217 11.00000 0.02093 0.02475 = 0.02376 -0.00210 -0.00831 0.00220 AFIX 43 H63 2 0.017087 0.805885 0.334775 11.00000 -1.20000 AFIX 0 C64 1 0.140521 0.769159 0.345621 11.00000 0.02280 0.02324 = 0.01559 -0.00037 -0.00300 -0.00491 AFIX 43 H64 2 0.164699 0.793300 0.313337 11.00000 -1.20000 AFIX 0 C65 1 -0.080146 0.747410 0.417689 11.00000 0.01986 0.04359 = 0.04314 -0.00958 0.00399 -0.00009 AFIX 137 H65A 2 -0.114629 0.718481 0.390439 11.00000 -1.50000 H65B 2 -0.097161 0.797107 0.413500 11.00000 -1.50000 H65C 2 -0.090948 0.731790 0.457635 11.00000 -1.50000 AFIX 0 C66 1 0.284566 0.819131 0.482132 11.00000 0.01892 0.01419 = 0.01463 -0.00266 -0.00239 -0.00196 C67 1 0.286026 0.771450 0.528342 11.00000 0.01536 0.01868 = 0.02070 0.00224 -0.00209 -0.00112 AFIX 43 H67 2 0.336232 0.742856 0.535016 11.00000 -1.20000 AFIX 0 C68 1 0.214680 0.765414 0.564700 11.00000 0.02076 0.02232 = 0.02086 0.00578 -0.00113 -0.00250 AFIX 43 H68 2 0.215873 0.733569 0.596683 11.00000 -1.20000 AFIX 0 C69 1 0.142331 0.806422 0.553489 11.00000 0.01870 0.02161 = 0.02118 -0.00254 0.00317 -0.00396 C70 1 0.137758 0.853937 0.508251 11.00000 0.02177 0.01934 = 0.02157 -0.00223 -0.00049 0.00545 AFIX 43 H70 2 0.086730 0.881507 0.501396 11.00000 -1.20000 AFIX 0 C71 1 0.210065 0.860192 0.473064 11.00000 0.02701 0.01582 = 0.01647 0.00004 -0.00116 0.00261 AFIX 43 H71 2 0.208855 0.893301 0.441966 11.00000 -1.20000 AFIX 0 C72 1 0.362859 0.828750 0.443239 11.00000 0.01816 0.01359 = 0.01704 0.00171 -0.00137 -0.00038 AFIX 13 H72 2 0.376184 0.880491 0.442836 11.00000 -1.20000 AFIX 0 C73 1 0.637788 0.843398 0.327652 11.00000 0.02309 0.03674 = 0.02810 0.00784 0.00516 -0.00592 AFIX 137 H73A 2 0.688347 0.835063 0.302800 11.00000 -1.50000 H73B 2 0.656057 0.871011 0.361807 11.00000 -1.50000 H73C 2 0.592939 0.869531 0.305670 11.00000 -1.50000 AFIX 0 C74 1 0.585528 0.726148 0.293233 11.00000 0.02231 0.04094 = 0.02403 -0.00654 0.00303 0.00220 AFIX 137 H74A 2 0.549761 0.752134 0.264708 11.00000 -1.50000 H74B 2 0.555388 0.682492 0.304127 11.00000 -1.50000 H74C 2 0.642114 0.714490 0.276161 11.00000 -1.50000 AFIX 0 C75 1 0.538307 0.888358 0.447731 11.00000 0.02132 0.02273 = 0.02483 -0.00184 -0.00013 -0.00671 AFIX 137 H75A 2 0.503833 0.914025 0.418319 11.00000 -1.50000 H75B 2 0.600697 0.896765 0.441417 11.00000 -1.50000 H75C 2 0.522636 0.904990 0.486631 11.00000 -1.50000 AFIX 0 F1 4 0.418219 0.568329 -0.021989 11.00000 0.02802 0.04360 = 0.03487 -0.00775 0.01764 0.00360 F2 4 0.070838 0.451773 0.550381 11.00000 0.01862 0.04776 = 0.03506 0.00499 0.01268 0.00284 F3 4 0.071847 0.800013 0.589069 11.00000 0.01976 0.03299 = 0.03525 0.00548 0.00954 0.00170 O1 3 0.166296 0.480941 0.183503 11.00000 0.02227 0.01548 = 0.02699 0.00267 -0.00185 -0.00209 O2 3 0.209511 0.536174 0.277554 11.00000 0.02476 0.02742 = 0.01648 0.00766 0.00157 0.00487 O3 3 0.065116 0.594307 0.111878 11.00000 0.01280 0.02004 = 0.01933 -0.00414 0.00145 0.00040 O4 3 0.340554 0.314989 0.291032 11.00000 0.01941 0.02554 = 0.02131 -0.00953 0.00246 -0.00053 O5 3 0.348501 0.309537 0.398540 11.00000 0.01963 0.01457 = 0.02216 0.00269 -0.00404 0.00026 O6 3 0.438468 0.444684 0.436235 11.00000 0.00974 0.01857 = 0.01512 0.00070 -0.00038 -0.00058 O7 3 0.312728 0.707213 0.304454 11.00000 0.02632 0.03948 = 0.03028 -0.01996 0.00925 -0.00715 O8 3 0.342958 0.667625 0.405713 11.00000 0.01888 0.01651 = 0.05312 0.00338 -0.00320 0.00199 O9 3 0.435504 0.795072 0.470138 11.00000 0.01403 0.02239 = 0.01580 0.00410 -0.00041 -0.00117 S1 5 0.209428 0.537899 0.214634 11.00000 0.01765 0.01531 = 0.01661 0.00337 -0.00011 0.00140 S2 5 0.317854 0.345181 0.346697 11.00000 0.01321 0.01408 = 0.01591 -0.00132 -0.00040 -0.00028 S3 5 0.305404 0.718563 0.366257 11.00000 0.01602 0.01668 = 0.02607 -0.00577 0.00217 -0.00020 HKLF 4 REM 150802LT_0m_a.res in P2(1)/n REM R1 = 0.0380 for 11179 Fo > 4sig(Fo) and 0.0514 for all 13610 data REM 823 parameters refined using 0 restraints END WGHT 0.0617 2.0204 REM Highest difference peak 0.444, deepest hole -0.545, 1-sigma level 0.120 Q1 1 -0.1075 0.3931 0.3109 11.00000 0.05 0.44 Q2 1 -0.1105 0.7754 0.3796 11.00000 0.05 0.41 Q3 1 -0.1008 0.6354 0.2471 11.00000 0.05 0.40 Q4 1 0.6824 0.5190 0.3097 11.00000 0.05 0.37 Q5 1 -0.1167 0.5794 0.2315 11.00000 0.05 0.37 ; 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5.77 0 -6 -6 145.79 5.82 0 -6 6 138.89 6.07 0 -6 6 118.72 6.01 0 -6 -6 132.32 5.32 0 -6 6 126.52 5.55 0 6 6 125.61 5.71 0 6 -6 132.70 6.09 0 6 -6 126.75 5.83 0 6 6 121.10 4.95 0 6 -6 142.22 6.13 0 6 -6 126.66 5.46 1 -6 6 5.92 1.38 1 -6 6 5.83 1.39 1 -6 6 6.86 1.19 -1 -6 -6 4.54 1.09 -1 -6 -6 7.17 1.27 -1 6 -6 9.32 1.35 1 6 6 6.69 1.06 1 6 6 6.99 1.38 -1 6 -6 10.50 1.66 1 6 6 8.15 1.36 -1 6 -6 11.88 1.83 2 -6 6 3.83 0.92 2 -6 6 4.87 1.21 -2 -6 -6 3.26 0.94 2 -6 6 3.33 1.40 -2 -6 -6 5.85 1.33 2 -6 6 4.97 1.28 -2 6 -6 3.75 1.04 2 6 6 5.91 1.41 -2 6 -6 4.74 1.22 -2 6 -6 4.27 0.92 2 6 6 6.09 1.33 3 -6 6 194.61 8.11 -3 -6 -6 179.17 7.76 -3 -6 -6 179.37 7.98 3 -6 6 201.69 7.62 3 6 6 191.76 8.19 3 6 6 201.62 7.68 -3 6 -6 209.57 7.75 -3 6 -6 194.68 7.34 -4 -6 -6 54.87 3.55 4 -6 6 56.97 3.66 4 -6 6 54.81 3.28 -4 -6 -6 55.99 3.74 4 6 6 48.66 3.65 -4 6 -6 48.48 3.08 -4 6 -6 55.16 3.06 5 -6 6 0.55 0.69 -5 -6 -6 -0.19 0.77 -5 -6 -6 0.51 0.92 5 -6 6 1.22 0.89 5 6 6 -0.01 0.86 -5 6 -6 -0.09 0.54 6 -6 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104.96 9.84 17 -7 -6 113.58 10.10 17 7 -6 125.40 11.55 -16 -7 6 3.46 2.33 16 -7 -6 0.36 2.29 16 7 -6 4.41 2.81 -15 -7 6 10.44 3.33 15 -7 -6 13.09 3.40 15 7 -6 3.85 2.60 14 -7 -6 12.77 3.25 -14 -7 6 12.90 3.28 14 7 -6 10.13 3.27 13 -7 -6 30.15 4.32 -13 -7 6 38.36 5.22 13 7 -6 42.18 5.73 -12 -7 6 167.01 9.75 12 -7 -6 191.07 9.76 12 7 -6 199.42 10.93 -11 -7 6 97.58 6.68 11 -7 -6 78.40 9.27 11 -7 -6 89.28 5.97 -11 7 6 88.21 5.08 11 7 -6 94.38 7.01 -10 -7 6 32.38 4.20 10 -7 -6 32.01 3.69 10 -7 -6 29.76 3.66 10 7 -6 27.14 4.07 -10 7 6 27.57 2.81 9 -7 -6 156.80 7.47 -9 -7 6 155.24 8.24 9 -7 -6 145.86 7.48 9 7 -6 136.64 8.21 8 -7 -6 160.40 7.84 8 -7 -6 192.37 8.02 -8 -7 6 175.21 8.86 8 7 -6 174.67 8.99 7 -7 -6 136.90 6.20 7 -7 -6 137.49 6.43 -7 -7 6 131.03 7.19 7 7 -6 125.15 7.12 -7 7 6 132.83 5.34 6 -7 -6 0.11 0.57 6 -7 -6 0.54 0.73 -6 -7 6 1.04 1.12 -6 -7 6 0.14 0.85 -6 7 6 0.12 0.41 6 7 -6 -0.83 0.81 -6 7 6 0.09 0.45 5 -7 -6 8.62 1.35 -5 -7 6 11.31 2.11 -5 -7 6 11.76 2.17 5 -7 -6 11.48 1.70 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8.59 -8 4 -14 102.95 6.61 8 4 14 106.58 9.21 9 -4 14 87.90 8.45 -9 -4 -14 73.12 7.10 9 4 14 99.63 9.45 -9 4 -14 84.46 6.20 10 -4 14 27.46 4.79 -10 -4 -14 39.60 5.48 -10 4 -14 27.26 4.16 10 4 14 23.66 4.97 11 -4 14 253.52 14.21 -11 -4 -14 252.94 13.31 11 4 14 260.19 14.45 -11 4 -14 262.68 12.69 -12 -4 -14 44.80 6.24 12 -4 14 45.09 6.64 -12 4 -14 51.58 6.14 12 4 14 51.46 7.22 13 -4 14 114.97 11.05 -13 -4 -14 126.57 9.29 13 4 14 136.47 12.50 -14 -4 -14 58.83 7.64 14 -4 14 47.23 7.40 14 4 14 47.81 7.41 -15 -4 -14 3.64 3.11 15 -4 14 3.03 3.08 15 4 14 2.95 2.94 -16 -4 -14 21.07 5.02 16 -4 14 17.80 5.09 16 4 14 15.71 4.90 -16 -5 14 11.14 4.09 16 -5 -14 2.08 2.90 16 5 -14 4.18 3.46 15 -5 -14 15.15 4.37 -15 -5 14 17.58 4.20 15 5 -14 10.70 3.95 14 -5 -14 9.62 3.49 -14 -5 14 5.84 2.97 14 5 -14 7.53 3.20 -13 -5 14 -0.78 1.79 13 -5 -14 2.43 2.45 13 5 -14 -0.03 2.34 12 -5 -14 5.53 2.60 -12 -5 14 7.72 2.85 12 5 -14 12.28 3.71 11 -5 -14 8.11 2.74 -11 -5 14 6.21 2.77 11 5 -14 16.15 3.89 -10 -5 14 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14 20.67 3.82 -6 -9 -14 13.88 3.13 6 -9 14 12.90 3.43 6 -9 14 12.34 3.42 6 9 14 8.31 2.88 -6 9 -14 10.68 2.53 6 9 14 15.67 2.99 7 -9 14 20.00 4.05 7 -9 14 25.67 4.60 -7 -9 -14 28.84 4.36 -7 9 -14 27.35 3.58 7 9 14 24.87 4.52 8 -9 14 30.42 5.38 -8 -9 -14 29.03 4.45 8 9 14 30.90 5.14 9 -9 14 28.88 5.03 -9 -9 -14 39.61 5.53 9 9 14 43.46 6.23 10 -9 14 21.71 4.69 -10 -9 -14 31.80 5.13 10 9 14 24.59 5.04 11 -9 14 25.88 5.23 -11 -9 -14 27.50 5.10 11 9 14 25.64 5.51 -12 -9 -14 2.07 2.48 12 -9 14 1.99 2.96 12 9 14 1.81 2.52 -13 -9 -14 6.40 3.33 13 -9 14 16.09 4.95 13 9 14 9.97 4.21 -14 -9 -14 118.02 11.47 14 -9 14 92.25 10.67 14 9 14 110.29 11.51 -14 -10 14 18.16 4.39 14 -10 -14 16.83 3.99 14 10 -14 20.79 5.30 -13 -10 14 3.24 2.50 13 -10 -14 2.14 2.47 13 10 -14 4.20 3.15 12 -10 -14 17.76 3.80 -12 -10 14 18.61 4.43 12 10 -14 19.89 4.61 11 -10 -14 61.59 6.23 -11 -10 14 92.56 8.95 11 10 -14 67.20 7.63 -10 -10 14 107.88 9.67 10 -10 -14 105.23 7.08 10 10 -14 86.16 8.62 -9 -10 14 191.40 11.51 9 -10 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-9 15 12.90 4.17 14 -9 -15 8.77 3.53 14 9 -15 9.15 3.76 -13 -9 15 6.58 3.23 13 -9 -15 3.45 2.56 13 9 -15 1.38 2.85 12 -9 -15 13.28 3.64 -12 -9 15 15.87 4.14 12 9 -15 18.09 4.46 -11 -9 15 15.24 4.23 11 -9 -15 15.42 3.54 11 9 -15 12.96 3.75 10 -9 -15 34.52 4.78 -10 -9 15 34.85 5.61 10 9 -15 23.82 4.62 9 -9 -15 12.47 3.13 -9 -9 15 10.70 3.44 9 9 -15 9.81 3.23 8 -9 -15 350.75 15.02 -8 -9 15 356.34 16.71 8 9 -15 346.09 16.18 7 -9 -15 103.80 6.90 -7 -9 15 115.97 8.34 7 9 -15 113.10 7.84 7 9 -15 120.80 8.00 -6 -9 15 24.75 4.48 6 -9 -15 36.53 4.34 6 9 -15 50.25 5.56 6 9 -15 47.74 5.64 5 -9 -15 14.58 2.79 -5 -9 15 15.76 3.58 5 9 -15 11.85 2.96 5 9 -15 8.44 2.63 4 -9 -15 57.60 5.17 4 -9 -15 47.36 7.60 -4 -9 15 65.02 6.78 4 9 -15 54.17 5.48 -4 9 15 54.59 4.76 4 9 -15 50.95 5.41 3 -9 -15 25.11 3.97 -3 -9 15 18.83 3.78 3 -9 -15 32.82 3.82 3 -9 -15 25.73 4.23 3 9 -15 22.46 3.51 3 9 -15 30.20 4.23 -3 9 15 31.06 3.64 2 -9 -15 39.41 5.13 -2 -9 15 47.58 5.73 2 -9 -15 43.20 4.35 2 9 -15 52.71 5.05 2 9 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1.95 -7 -10 15 4.69 2.70 7 10 -15 0.17 1.75 7 10 -15 1.53 2.15 -6 -10 15 115.72 8.48 6 -10 -15 130.95 7.40 6 10 -15 127.85 8.27 6 10 -15 119.25 8.09 5 -10 -15 21.24 3.16 -5 -10 15 23.58 4.36 5 10 -15 27.98 4.34 5 10 -15 26.56 4.32 4 -10 -15 633.34 22.94 -4 -10 15 622.97 25.13 4 10 -15 661.15 24.22 4 10 -15 654.23 24.19 3 -10 -15 21.10 3.22 -3 -10 15 18.99 3.81 3 10 -15 21.56 3.49 3 10 -15 16.25 3.22 2 -10 -15 330.26 13.40 -2 -10 15 346.90 15.47 2 10 -15 331.36 14.09 -2 10 15 300.09 12.76 2 10 -15 330.78 13.98 -1 -10 15 40.15 5.17 1 -10 -15 37.74 4.13 1 -10 -15 49.73 5.72 1 10 -15 42.19 4.69 1 10 -15 44.04 4.89 -1 10 15 37.90 4.15 0 -10 -15 89.18 6.58 0 -10 -15 94.91 6.00 0 -10 15 105.54 7.40 0 10 15 95.00 5.20 0 10 -15 98.05 6.11 0 10 15 91.74 5.93 0 10 -15 86.61 6.02 -1 -10 -15 131.44 8.07 1 -10 15 131.77 8.53 -1 -10 -15 126.59 7.23 1 10 15 115.46 7.12 -1 10 -15 137.69 7.30 -1 10 -15 121.84 7.22 1 10 15 124.51 6.44 -2 -10 -15 196.35 9.59 -2 -10 -15 177.32 10.06 2 -10 15 182.97 10.49 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20.70 4.79 12 -12 15 22.80 5.67 -12 -13 15 4.71 2.97 12 -13 -15 7.00 2.99 12 13 -15 4.00 3.63 11 -13 -15 43.40 5.48 -11 -13 15 42.69 6.72 11 13 -15 40.25 6.82 10 -13 -15 17.59 3.58 -10 -13 15 10.60 3.73 10 13 -15 17.58 4.99 -9 -13 15 1.95 2.54 9 -13 -15 -0.02 1.61 9 13 -15 -1.63 2.39 -8 -13 15 82.81 8.66 8 -13 -15 96.18 6.54 8 13 -15 92.88 9.31 -7 -13 15 24.17 4.65 7 -13 -15 30.06 4.11 7 13 -15 27.87 5.04 -6 -13 15 298.74 15.32 6 -13 -15 296.56 12.89 6 13 -15 307.79 15.31 5 -13 -15 52.10 5.09 -5 -13 15 55.70 6.73 5 13 -15 44.20 6.12 -4 -13 15 52.70 6.34 4 -13 -15 51.87 5.07 4 13 -15 68.75 7.14 3 -13 -15 71.65 5.18 -3 -13 15 70.15 7.48 3 13 -15 67.10 7.03 -2 -13 15 119.75 8.45 2 -13 -15 108.44 6.60 2 13 -15 125.22 8.16 1 -13 -15 28.16 3.63 -1 -13 15 20.97 4.13 -1 13 15 27.07 3.55 1 13 -15 27.03 4.27 0 -13 15 20.71 3.95 0 -13 -15 16.27 2.90 0 13 15 15.63 3.00 0 13 -15 22.08 3.81 1 -13 15 7.43 2.77 -1 -13 -15 7.50 2.23 1 13 15 7.21 2.32 -1 13 -15 9.30 2.71 2 -13 15 369.24 17.13 -2 -13 -15 386.36 15.88 2 13 15 378.60 15.81 -2 13 -15 391.91 16.24 3 -13 15 95.75 8.62 -3 -13 -15 100.26 6.92 3 13 15 99.91 6.79 -4 -13 -15 162.22 9.36 4 -13 15 160.76 10.10 4 13 15 171.70 9.53 -5 -13 -15 5.62 2.59 5 -13 15 2.68 2.25 5 13 15 8.20 2.79 -6 -13 -15 256.35 12.88 6 -13 15 237.09 13.25 6 13 15 251.90 12.78 -7 -13 -15 5.36 2.87 7 -13 15 5.41 2.82 7 13 15 9.12 3.18 -8 -13 -15 142.68 9.64 8 -13 15 151.89 10.34 8 13 15 141.84 9.68 -9 -13 -15 72.61 7.90 9 -13 15 52.37 7.42 9 -13 15 66.02 7.96 9 13 15 74.93 8.09 -10 -13 -15 92.10 9.33 10 -13 15 100.64 9.71 10 -13 15 87.22 9.40 10 13 15 88.81 9.17 11 -13 15 77.98 9.54 11 -13 15 85.01 9.36 -11 -13 -15 90.12 9.19 -12 -13 -15 94.73 10.10 12 -13 15 85.33 10.26 12 -13 15 82.91 9.49 11 -14 -15 6.26 2.69 -11 -14 15 1.81 2.59 11 14 -15 6.11 3.80 -10 -14 15 -1.29 2.13 10 -14 -15 1.76 1.94 10 14 -15 0.10 2.80 9 -14 -15 0.28 1.67 -9 -14 15 -1.88 1.74 9 14 -15 -0.14 2.65 -8 -14 15 181.02 11.70 8 -14 -15 173.47 9.32 8 14 -15 191.68 12.26 -7 -14 15 15.41 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36.57 5.58 1 1 -21 37.36 5.13 0 -1 21 195.02 11.60 0 -1 -21 175.42 10.10 0 1 21 167.06 10.86 0 1 -21 166.92 9.98 -1 -1 -21 0.02 1.75 1 -1 21 0.97 2.12 1 1 21 -0.55 1.96 -1 1 -21 0.18 1.76 2 -1 21 53.05 6.83 -2 -1 -21 35.83 4.93 -2 1 -21 50.42 5.82 2 1 21 43.31 6.43 3 -1 21 99.38 9.76 -3 -1 -21 109.94 7.84 3 1 21 97.28 9.59 -3 1 -21 115.40 7.78 -4 -1 -21 45.99 5.69 4 -1 21 46.51 6.72 4 1 21 59.58 7.59 -4 1 -21 64.53 6.71 5 -1 21 10.52 3.82 -5 -1 -21 10.39 3.10 5 1 21 10.29 3.55 -5 1 -21 6.08 2.53 -6 -1 -21 17.97 3.85 6 -1 21 17.11 4.42 6 1 21 14.28 4.22 -6 1 -21 16.72 3.76 -7 -1 -21 18.27 4.08 7 -1 21 6.56 3.38 -7 1 -21 10.17 3.14 7 1 21 6.40 3.35 8 -1 21 15.66 4.49 -8 -1 -21 7.73 3.14 8 -1 21 3.28 3.24 -8 1 -21 12.75 3.44 8 1 21 10.27 3.91 8 1 21 14.24 5.00 9 -1 21 50.97 7.91 -9 -1 -21 53.68 7.00 9 -1 21 39.52 7.18 -9 1 -21 40.57 6.12 9 1 21 36.43 6.62 9 1 21 46.88 7.46 10 -1 21 17.66 5.23 10 -1 21 37.00 6.92 -10 -1 -21 39.73 6.20 10 1 21 39.46 6.89 -10 1 -21 28.99 5.14 10 1 21 22.99 5.82 11 -1 21 39.19 7.20 11 -1 21 45.52 7.51 -11 -1 -21 38.07 6.11 11 1 21 34.50 7.51 -11 1 -21 29.65 5.33 11 1 21 33.56 6.74 -12 -1 -21 1.53 2.58 12 -1 21 2.00 4.01 12 1 21 3.76 3.37 -12 1 -21 4.68 2.96 13 -2 -21 58.10 8.05 13 2 -21 37.51 6.72 -12 -2 21 13.75 6.44 12 -2 -21 11.29 3.94 12 2 -21 17.01 4.81 11 -2 -21 -2.57 1.97 -11 -2 21 6.60 3.09 11 2 -21 5.64 3.17 10 -2 -21 24.94 4.80 -10 -2 21 19.34 4.51 10 2 -21 11.74 3.62 -9 -2 21 1.83 2.48 9 -2 -21 -0.85 1.92 9 2 -21 -0.97 2.00 -8 -2 21 33.11 5.47 8 -2 -21 43.47 5.97 8 2 -21 25.50 4.69 -8 2 21 31.63 5.12 7 -2 -21 41.55 5.70 -7 -2 21 47.65 6.61 7 2 -21 39.22 5.67 -7 2 21 41.37 5.69 -6 -2 21 0.48 1.87 6 -2 -21 0.55 2.07 6 2 -21 -0.30 1.93 -6 2 21 0.71 1.93 -5 -2 21 -1.09 1.92 5 -2 -21 -0.79 1.73 -5 2 21 1.58 2.07 5 2 -21 1.67 2.13 -4 -2 21 103.97 9.73 4 -2 -21 102.75 8.95 4 2 -21 98.45 8.82 -4 2 21 100.11 9.35 -3 -2 21 1.45 2.06 3 -2 -21 0.85 1.87 -3 2 21 -2.29 1.44 3 2 -21 3.22 2.26 -2 -2 21 24.68 4.63 2 -2 -21 34.24 5.06 2 2 -21 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5.14 -2 -8 21 92.24 9.41 2 -8 -21 106.79 7.58 2 8 -21 106.15 9.22 1 -8 -21 33.93 4.98 -1 -8 21 38.97 6.15 1 8 -21 35.44 5.14 0 -8 -21 39.33 5.22 0 -8 21 38.87 6.19 0 8 -21 31.60 4.98 1 -8 21 77.50 8.87 -1 -8 -21 53.63 6.06 -1 8 -21 56.00 6.53 2 -8 21 47.25 6.75 -2 -8 -21 52.90 6.15 -2 8 -21 59.91 6.61 3 -8 21 9.88 3.60 -3 -8 -21 15.16 3.65 -3 8 -21 13.87 3.35 -4 -8 -21 221.63 12.01 4 -8 21 204.31 13.04 -4 8 -21 208.62 11.56 -5 -8 -21 11.85 3.46 5 -8 21 11.20 3.78 5 8 21 13.94 6.14 -6 -8 -21 22.64 4.46 6 -8 21 14.67 4.51 7 -8 21 3.01 3.07 -7 -8 -21 6.33 2.89 8 -8 21 101.10 10.64 -8 -8 -21 106.18 10.16 9 -8 21 12.84 4.51 -9 -8 -21 -0.94 2.42 -10 -8 -21 1.23 2.50 10 -8 21 3.46 3.44 -11 -8 -21 -2.66 2.13 11 -8 21 -6.06 2.32 11 -8 21 -1.66 2.81 11 -9 -21 5.58 3.04 -11 -9 21 3.96 3.25 11 9 -21 0.28 2.83 -10 -9 21 77.69 9.22 10 -9 -21 68.07 7.95 10 9 -21 81.95 9.44 -9 -9 21 4.02 3.05 9 -9 -21 2.16 2.39 9 9 -21 -0.10 2.33 -8 -9 21 19.31 4.73 8 -9 -21 24.83 4.66 8 9 -21 29.52 5.65 -7 -9 21 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3 -25 96.56 9.72 -4 -3 25 40.48 6.86 4 -3 -25 33.65 5.66 4 3 -25 25.58 5.18 3 -3 -25 18.67 4.48 -3 -3 25 10.64 3.90 -3 3 25 12.92 4.34 3 3 -25 13.06 3.77 -2 -3 25 -0.14 2.76 2 -3 -25 2.12 2.60 -2 3 25 7.77 3.40 2 3 -25 -0.06 2.34 -1 -3 25 11.90 4.21 1 -3 -25 11.44 3.55 -1 3 25 5.47 3.17 1 3 -25 13.85 3.86 0 -3 25 5.91 3.43 0 -3 -25 6.52 3.13 0 3 25 6.14 3.47 0 3 -25 6.02 3.01 1 -3 25 12.77 4.55 -1 -3 -25 4.78 2.89 -1 3 -25 9.32 3.47 1 3 25 1.27 2.60 2 -3 25 10.60 4.04 -2 -3 -25 8.69 3.24 2 3 25 9.13 3.90 -2 3 -25 8.75 3.10 -3 -3 -25 24.95 5.05 3 -3 25 37.44 6.80 -3 3 -25 33.00 5.67 3 3 25 33.05 6.25 4 -3 25 0.88 2.65 -4 -3 -25 0.91 2.33 4 3 25 1.31 2.78 -4 3 -25 1.41 2.36 -5 -3 -25 9.54 3.40 5 -3 25 5.73 3.87 5 3 25 3.84 3.52 -5 3 -25 3.27 2.46 -6 -3 -25 13.57 4.00 6 -3 25 14.44 4.73 6 3 25 10.95 4.35 -6 3 -25 12.11 3.77 7 -3 25 -0.31 2.89 -7 -3 -25 0.88 2.56 -7 3 -25 -0.04 2.15 7 3 25 3.71 3.16 8 -3 25 0.48 2.90 -8 -3 -25 1.93 2.70 8 3 25 -2.12 2.70 -8 3 -25 -0.75 2.32 -9 -4 25 56.92 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3.72 2 -4 27 28.58 6.58 -2 -4 -27 29.55 5.59 -2 4 -27 24.36 5.33 -3 -4 -27 38.17 6.25 3 -4 27 41.31 7.57 -3 4 -27 40.32 6.42 4 -4 27 -3.35 2.33 -4 -4 -27 -2.44 2.24 -4 4 -27 0.03 2.29 5 -4 27 0.66 3.25 -5 -4 -27 2.52 2.80 -5 4 -27 0.37 2.42 -5 -5 27 10.16 4.23 5 -5 -27 20.36 4.79 5 5 -27 15.13 4.30 4 -5 -27 -2.93 2.02 -4 -5 27 -1.38 2.53 4 5 -27 2.08 2.67 -3 -5 27 -1.06 2.79 3 -5 -27 2.96 2.76 3 5 -27 1.52 2.73 -2 -5 27 9.98 4.58 2 -5 -27 24.32 5.44 2 5 -27 30.43 5.62 -1 -5 27 4.28 3.44 1 -5 -27 4.05 2.82 1 5 -27 0.60 2.51 0 -5 -27 30.62 5.64 0 -5 27 33.79 6.64 0 5 -27 31.64 5.87 1 -5 27 9.35 4.43 -1 -5 -27 8.15 3.51 -1 5 -27 13.50 4.19 2 -5 27 9.92 4.68 -2 -5 -27 7.80 3.62 -2 5 -27 7.43 3.39 -3 -5 -27 -1.23 2.12 3 -5 27 1.06 3.41 -3 5 -27 4.79 3.27 -4 -5 -27 -0.72 2.58 4 -5 27 1.90 3.10 -4 5 -27 1.82 2.80 -4 -6 27 4.96 3.73 4 -6 -27 4.12 3.05 4 6 -27 4.66 3.33 3 -6 -27 1.96 2.84 -3 -6 27 3.71 3.57 3 6 -27 2.35 2.51 -2 -6 27 75.64 9.98 2 -6 -27 73.13 8.57 2 6 -27 77.38 9.17 1 -6 -27 37.51 6.59 -1 -6 27 52.30 7.93 1 6 -27 38.40 6.28 0 -6 -27 2.26 2.94 0 -6 27 2.63 3.53 0 6 -27 4.51 2.99 -1 -6 -27 2.64 2.81 1 -6 27 4.71 3.54 -1 6 -27 0.85 2.53 2 -6 27 26.13 6.51 -2 -6 -27 36.13 6.29 -2 6 -27 29.73 5.77 -3 -6 -27 10.10 3.86 3 -6 27 -0.02 3.17 -4 -6 -27 5.48 3.38 4 -6 27 1.23 3.51 3 -7 -27 59.57 7.80 -3 -7 27 52.57 8.65 3 7 -27 58.17 7.82 2 -7 -27 29.87 5.79 -2 -7 27 18.34 5.34 2 7 -27 13.83 4.21 -1 -7 27 1.12 2.93 1 -7 -27 0.23 2.38 1 7 -27 1.73 2.93 0 -7 27 26.64 6.23 0 -7 -27 25.34 5.13 0 7 -27 20.31 6.42 1 -7 27 -1.01 2.73 -1 -7 -27 -0.22 2.53 2 -7 27 11.70 4.79 -2 -7 -27 18.81 4.73 3 -7 27 32.95 7.21 -1 -8 27 -2.19 2.53 0 -8 27 24.70 6.01 0 -8 -27 27.04 5.54 4 0 -28 84.36 9.80 3 0 -28 0.30 2.50 -3 0 28 1.10 3.12 -2 0 28 8.76 3.93 2 0 -28 6.50 3.39 -1 0 28 2.35 2.81 1 0 -28 -1.06 2.18 0 0 28 140.89 13.15 0 0 -28 105.54 10.42 1 0 28 -1.03 2.88 -1 0 -28 0.43 2.48 2 0 28 24.14 5.93 -2 0 -28 23.96 5.46 3 0 28 1.95 3.15 -3 0 -28 -0.46 2.41 4 0 28 -0.18 3.41 -4 -1 28 13.70 4.73 4 -1 -28 20.07 5.14 4 1 -28 9.94 3.85 -3 -1 28 -0.07 3.06 3 -1 -28 1.57 2.71 3 1 -28 3.19 2.62 2 -1 -28 13.56 4.54 -2 -1 28 22.81 5.67 2 1 -28 17.20 4.88 -1 -1 28 15.99 4.70 1 -1 -28 24.36 5.45 1 1 -28 29.66 5.72 -1 1 28 21.08 5.63 0 -1 -28 20.05 5.06 0 -1 28 28.98 6.54 0 1 -28 22.36 5.27 0 1 28 18.17 5.36 1 -1 28 4.03 3.55 -1 -1 -28 2.45 2.94 -1 1 -28 7.84 3.91 1 1 28 5.19 3.59 -2 -1 -28 0.64 2.52 2 -1 28 -1.25 2.81 -2 1 -28 4.19 3.12 2 1 28 0.00 2.98 3 -1 28 28.29 6.54 -3 -1 -28 33.86 6.04 -3 1 -28 26.68 5.46 3 1 28 27.76 6.31 -4 -2 28 8.82 4.08 4 -2 -28 14.26 4.43 4 2 -28 20.32 5.29 3 -2 -28 30.90 6.14 -3 -2 28 33.56 7.04 3 2 -28 33.10 6.13 -2 -2 28 5.53 3.59 2 -2 -28 4.22 3.22 2 2 -28 3.55 3.30 -1 -2 28 13.59 4.63 1 -2 -28 11.61 4.10 1 2 -28 13.53 4.20 0 -2 -28 22.70 5.01 0 -2 28 26.53 6.13 0 2 -28 26.56 5.54 1 -2 28 30.08 6.75 -1 -2 -28 32.88 6.12 -1 2 -28 39.26 6.78 1 2 28 30.83 7.32 -2 -2 -28 23.99 5.46 2 -2 28 27.20 6.53 2 2 28 26.21 6.04 -2 2 -28 30.35 5.85 -3 -2 -28 13.50 4.31 3 -2 28 6.16 4.18 -3 2 -28 8.09 3.63 3 2 28 11.59 4.53 3 -3 -28 51.93 7.45 -3 -3 28 43.65 7.89 3 3 -28 47.32 7.06 2 -3 -28 49.34 7.15 -2 -3 28 55.65 8.45 2 3 -28 49.46 7.37 -1 -3 28 55.66 8.59 1 -3 -28 44.55 6.91 1 3 -28 57.26 7.70 0 -3 28 62.86 8.84 0 -3 -28 81.79 9.27 0 3 -28 67.32 8.59 -1 -3 -28 2.13 2.99 1 -3 28 0.91 3.11 -1 3 -28 1.39 2.72 -2 -3 -28 4.22 3.08 2 -3 28 3.82 3.78 -2 3 -28 0.53 2.67 -3 -3 -28 2.62 2.66 3 -3 28 4.70 4.05 -3 3 -28 3.34 3.21 3 -4 -28 1.51 2.84 -3 -4 28 1.26 3.26 3 4 -28 0.64 2.69 -2 -4 28 116.13 12.38 2 -4 -28 128.14 11.66 2 4 -28 141.20 12.63 1 -4 -28 4.86 3.49 -1 -4 28 5.08 3.72 1 4 -28 13.37 4.18 0 -4 -28 21.34 5.26 0 -4 28 18.55 5.41 0 4 -28 21.19 4.91 -1 -4 -28 3.63 3.30 1 -4 28 2.32 3.65 -1 4 -28 -1.73 2.42 2 -4 28 -2.08 2.92 -2 -4 -28 8.27 3.64 -2 4 -28 4.79 3.43 1 -5 -28 6.21 3.62 -1 -5 28 9.36 4.40 1 5 -28 6.57 3.56 0 -5 28 6.60 3.91 0 -5 -28 2.13 3.04 0 5 -28 9.82 4.09 1 -5 28 38.78 7.59 -1 5 -28 42.82 6.71 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.8883 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71080 15.298 18.920 22.979 90.026 90.813 90.026 ) _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 62731 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 C1 C 0.16365(11) 0.62282(8) 0.19420(7) 0.0148(3) Uani 1 1 d . . H1 H 0.2081 0.6595 0.2047 0.018 Uiso 1 1 calc R U C2 C 0.08218(11) 0.63753(9) 0.23100(7) 0.0181(4) Uani 1 1 d . . H2A H 0.0940 0.6233 0.2718 0.022 Uiso 1 1 calc R U H2B H 0.0695 0.6888 0.2306 0.022 Uiso 1 1 calc R U C3 C 0.00240(11) 0.59701(9) 0.20749(8) 0.0190(4) Uani 1 1 d . . H3 H 0.0209 0.5463 0.2075 0.023 Uiso 1 1 calc R U C4 C -0.07981(13) 0.59906(9) 0.24639(9) 0.0255(4) Uani 1 1 d . . C5 C -0.15049(14) 0.55301(11) 0.21634(10) 0.0362(5) Uani 1 1 d . . H5A H -0.1323 0.5029 0.2191 0.043 Uiso 1 1 calc R U H5B H -0.2057 0.5581 0.2379 0.043 Uiso 1 1 calc R U C6 C -0.16820(13) 0.57074(11) 0.15263(10) 0.0366(5) Uani 1 1 d . . H6A H -0.1937 0.6187 0.1497 0.044 Uiso 1 1 calc R U H6B H -0.2113 0.5369 0.1363 0.044 Uiso 1 1 calc R U C7 C -0.08470(12) 0.56766(11) 0.11726(9) 0.0303(5) Uani 1 1 d . . H7A H -0.0632 0.5183 0.1163 0.036 Uiso 1 1 calc R U H7B H -0.0979 0.5824 0.0767 0.036 Uiso 1 1 calc R U C8 C -0.01341(11) 0.61518(9) 0.14263(8) 0.0184(4) Uani 1 1 d . . C9 C 0.14175(11) 0.63208(8) 0.12887(7) 0.0145(3) Uani 1 1 d . . H9 H 0.1290 0.6834 0.1226 0.017 Uiso 1 1 calc R U C10 C 0.32019(11) 0.53874(8) 0.19295(7) 0.0164(4) Uani 1 1 d . . C11 C 0.37775(12) 0.59011(9) 0.21379(7) 0.0189(4) Uani 1 1 d . . H11 H 0.3580 0.6259 0.2395 0.023 Uiso 1 1 calc R U C12 C 0.46409(12) 0.58839(9) 0.19651(8) 0.0205(4) Uani 1 1 d . . H12 H 0.5033 0.6239 0.2100 0.025 Uiso 1 1 calc R U C13 C 0.49492(12) 0.53547(9) 0.15954(8) 0.0205(4) Uani 1 1 d . . C14 C 0.43630(13) 0.48370(9) 0.14039(8) 0.0219(4) Uani 1 1 d . . H14 H 0.4563 0.4467 0.1160 0.026 Uiso 1 1 calc R U C15 C 0.34956(12) 0.48543(9) 0.15635(8) 0.0199(4) Uani 1 1 d . . H15 H 0.3101 0.4503 0.1424 0.024 Uiso 1 1 calc R U C16 C 0.58905(13) 0.53414(10) 0.14113(9) 0.0272(4) Uani 1 1 d . . H16A H 0.6146 0.4879 0.1504 0.041 Uiso 1 1 calc R U H16B H 0.6217 0.5711 0.1619 0.041 Uiso 1 1 calc R U H16C H 0.5922 0.5425 0.0991 0.041 Uiso 1 1 calc R U C17 C 0.21438(11) 0.61270(8) 0.08790(7) 0.0151(3) Uani 1 1 d . . C18 C 0.29144(12) 0.65234(9) 0.08998(8) 0.0192(4) Uani 1 1 d . . H18 H 0.2965 0.6902 0.1169 0.023 Uiso 1 1 calc R U C19 C 0.36049(12) 0.63758(9) 0.05361(8) 0.0222(4) Uani 1 1 d . . H19 H 0.4133 0.6640 0.0558 0.027 Uiso 1 1 calc R U C20 C 0.35012(12) 0.58331(10) 0.01412(8) 0.0231(4) Uani 1 1 d . . C21 C 0.27531(12) 0.54353(9) 0.00982(8) 0.0214(4) Uani 1 1 d . . H21 H 0.2702 0.5068 -0.0182 0.026 Uiso 1 1 calc R U C22 C 0.20698(12) 0.55827(9) 0.04756(7) 0.0181(4) Uani 1 1 d . . H22 H 0.1550 0.5309 0.0457 0.022 Uiso 1 1 calc R U C23 C -0.05671(16) 0.56629(11) 0.30572(10) 0.0381(5) Uani 1 1 d . . H23A H -0.0194 0.5990 0.3280 0.057 Uiso 1 1 calc R U H23B H -0.0255 0.5217 0.2999 0.057 Uiso 1 1 calc R U H23C H -0.1105 0.5573 0.3272 0.057 Uiso 1 1 calc R U C24 C -0.11613(13) 0.67345(10) 0.25795(9) 0.0255(4) Uani 1 1 d . . H24A H -0.1403 0.6931 0.2217 0.038 Uiso 1 1 calc R U H24B H -0.0689 0.7040 0.2725 0.038 Uiso 1 1 calc R U H24C H -0.1623 0.6707 0.2871 0.038 Uiso 1 1 calc R U C25 C -0.03404(12) 0.69283(9) 0.12874(8) 0.0214(4) Uani 1 1 d . . H25A H 0.0048 0.7235 0.1517 0.032 Uiso 1 1 calc R U H25B H -0.0950 0.7030 0.1384 0.032 Uiso 1 1 calc R U H25C H -0.0251 0.7016 0.0872 0.032 Uiso 1 1 calc R U C26 C 0.35302(11) 0.43703(8) 0.34538(7) 0.0144(3) Uani 1 1 d . . H26 H 0.3071 0.4644 0.3237 0.017 Uiso 1 1 calc R U C27 C 0.43840(11) 0.44451(9) 0.31167(7) 0.0170(4) Uani 1 1 d . . H27A H 0.4342 0.4170 0.2751 0.020 Uiso 1 1 calc R U H27B H 0.4476 0.4948 0.3014 0.020 Uiso 1 1 calc R U C28 C 0.51635(11) 0.41800(8) 0.34815(7) 0.0149(3) Uani 1 1 d . . H28 H 0.5015 0.3680 0.3580 0.018 Uiso 1 1 calc R U C29 C 0.60438(11) 0.41322(9) 0.31531(7) 0.0170(4) Uani 1 1 d . . C30 C 0.67088(12) 0.37794(9) 0.35732(8) 0.0212(4) Uani 1 1 d . . H30A H 0.6538 0.3280 0.3630 0.025 Uiso 1 1 calc R U H30B H 0.7292 0.3784 0.3392 0.025 Uiso 1 1 calc R U C31 C 0.67758(12) 0.41427(9) 0.41708(8) 0.0212(4) Uani 1 1 d . . H31A H 0.7182 0.3871 0.4425 0.025 Uiso 1 1 calc R U H31B H 0.7021 0.4623 0.4122 0.025 Uiso 1 1 calc R U C32 C 0.58843(11) 0.41976(9) 0.44649(7) 0.0176(4) Uani 1 1 d . . H32A H 0.5673 0.3717 0.4561 0.021 Uiso 1 1 calc R U H32B H 0.5950 0.4465 0.4833 0.021 Uiso 1 1 calc R U C33 C 0.52113(11) 0.45660(8) 0.40734(7) 0.0151(3) Uani 1 1 d . . C34 C 0.36380(11) 0.47128(8) 0.40587(7) 0.0145(3) Uani 1 1 d . . H34 H 0.3739 0.5229 0.3995 0.017 Uiso 1 1 calc R U C35 C 0.15585(11) 0.37279(9) 0.30031(8) 0.0181(4) Uani 1 1 d . . H35 H 0.1854 0.3841 0.2654 0.022 Uiso 1 1 calc R U C36 C 0.20235(11) 0.34952(8) 0.34919(7) 0.0146(3) Uani 1 1 d . . C37 C 0.15936(12) 0.33049(8) 0.39981(8) 0.0180(4) Uani 1 1 d . . H37 H 0.1914 0.3139 0.4328 0.022 Uiso 1 1 calc R U C38 C 0.06940(12) 0.33605(9) 0.40137(8) 0.0213(4) Uani 1 1 d . . H38 H 0.0397 0.3223 0.4356 0.026 Uiso 1 1 calc R U C39 C 0.02109(12) 0.36144(9) 0.35372(9) 0.0228(4) Uani 1 1 d . . C40 C 0.06581(12) 0.37921(9) 0.30342(8) 0.0217(4) Uani 1 1 d . . H40 H 0.0339 0.3961 0.2705 0.026 Uiso 1 1 calc R U C41 C -0.07654(13) 0.36957(11) 0.35631(11) 0.0361(5) Uani 1 1 d . . H41A H -0.1047 0.3303 0.3355 0.054 Uiso 1 1 calc R U H41B H -0.0938 0.4143 0.3380 0.054 Uiso 1 1 calc R U H41C H -0.0948 0.3694 0.3970 0.054 Uiso 1 1 calc R U C42 C 0.28549(11) 0.46462(8) 0.44499(7) 0.0146(3) Uani 1 1 d . . C43 C 0.28788(11) 0.42233(8) 0.49456(7) 0.0165(4) Uani 1 1 d . . H43 H 0.3392 0.3962 0.5040 0.020 Uiso 1 1 calc R U C44 C 0.21540(11) 0.41817(9) 0.53047(8) 0.0194(4) Uani 1 1 d . . H44 H 0.2166 0.3897 0.5646 0.023 Uiso 1 1 calc R U C45 C 0.14221(12) 0.45634(9) 0.51524(8) 0.0221(4) Uani 1 1 d . . C46 C 0.13709(12) 0.49853(9) 0.46654(8) 0.0229(4) Uani 1 1 d . . H46 H 0.0852 0.5241 0.4573 0.027 Uiso 1 1 calc R U C47 C 0.20997(12) 0.50267(9) 0.43137(8) 0.0191(4) Uani 1 1 d . . H47 H 0.2083 0.5317 0.3976 0.023 Uiso 1 1 calc R U C48 C 0.59148(12) 0.36543(10) 0.26200(8) 0.0234(4) Uani 1 1 d . . H48A H 0.5584 0.3910 0.2318 0.035 Uiso 1 1 calc R U H48B H 0.5591 0.3230 0.2732 0.035 Uiso 1 1 calc R U H48C H 0.6486 0.3518 0.2468 0.035 Uiso 1 1 calc R U C49 C 0.64034(12) 0.48416(10) 0.29356(8) 0.0224(4) Uani 1 1 d . . H49A H 0.6877 0.4755 0.2661 0.034 Uiso 1 1 calc R U H49B H 0.6628 0.5116 0.3267 0.034 Uiso 1 1 calc R U H49C H 0.5934 0.5107 0.2740 0.034 Uiso 1 1 calc R U C50 C 0.53817(12) 0.53662(9) 0.40510(8) 0.0201(4) Uani 1 1 d . . H50A H 0.5037 0.5575 0.3732 0.030 Uiso 1 1 calc R U H50B H 0.6005 0.5452 0.3986 0.030 Uiso 1 1 calc R U H50C H 0.5211 0.5581 0.4421 0.030 Uiso 1 1 calc R U C51 C 0.35050(11) 0.80604(8) 0.37909(7) 0.0158(3) Uani 1 1 d . . H51 H 0.3088 0.8405 0.3608 0.019 Uiso 1 1 calc R U C52 C 0.43743(11) 0.81343(9) 0.34667(8) 0.0185(4) Uani 1 1 d . . H52A H 0.4317 0.7915 0.3077 0.022 Uiso 1 1 calc R U H52B H 0.4510 0.8641 0.3413 0.022 Uiso 1 1 calc R U C53 C 0.51244(11) 0.77778(9) 0.38076(7) 0.0171(4) Uani 1 1 d . . H53 H 0.4929 0.7278 0.3863 0.021 Uiso 1 1 calc R U C54 C 0.60012(12) 0.77207(10) 0.34757(8) 0.0216(4) Uani 1 1 d . . C55 C 0.66589(12) 0.73321(10) 0.38777(8) 0.0242(4) Uani 1 1 d . . H55A H 0.6479 0.6831 0.3908 0.029 Uiso 1 1 calc R U H55B H 0.7241 0.7343 0.3695 0.029 Uiso 1 1 calc R U C56 C 0.67417(12) 0.76401(10) 0.44904(8) 0.0239(4) Uani 1 1 d . . H56A H 0.6989 0.8123 0.4468 0.029 Uiso 1 1 calc R U H56B H 0.7148 0.7346 0.4726 0.029 Uiso 1 1 calc R U C57 C 0.58544(12) 0.76688(10) 0.47866(8) 0.0218(4) Uani 1 1 d . . H57A H 0.5634 0.7182 0.4843 0.026 Uiso 1 1 calc R U H57B H 0.5924 0.7890 0.5175 0.026 Uiso 1 1 calc R U C58 C 0.51910(11) 0.80885(9) 0.44275(8) 0.0177(4) Uani 1 1 d . . C59 C 0.19284(11) 0.72646(8) 0.38102(7) 0.0164(4) Uani 1 1 d . . C60 C 0.15758(12) 0.68912(9) 0.42723(8) 0.0198(4) Uani 1 1 d . . H60 H 0.1936 0.6597 0.4509 0.024 Uiso 1 1 calc R U C61 C 0.06903(12) 0.69548(9) 0.43823(8) 0.0220(4) Uani 1 1 d . . H61 H 0.0444 0.6693 0.4693 0.026 Uiso 1 1 calc R U C62 C 0.01536(12) 0.73952(10) 0.40464(8) 0.0233(4) Uani 1 1 d . . C63 C 0.05279(12) 0.77587(10) 0.35822(8) 0.0232(4) Uani 1 1 d . . H63 H 0.0171 0.8059 0.3348 0.028 Uiso 1 1 calc R U C64 C 0.14052(12) 0.76916(9) 0.34562(8) 0.0206(4) Uani 1 1 d . . H64 H 0.1647 0.7933 0.3133 0.025 Uiso 1 1 calc R U C65 C -0.08015(13) 0.74741(12) 0.41769(10) 0.0355(5) Uani 1 1 d . . H65A H -0.1146 0.7185 0.3904 0.053 Uiso 1 1 calc R U H65B H -0.0972 0.7971 0.4135 0.053 Uiso 1 1 calc R U H65C H -0.0909 0.7318 0.4576 0.053 Uiso 1 1 calc R U C66 C 0.28457(11) 0.81913(8) 0.48213(7) 0.0159(4) Uani 1 1 d . . C67 C 0.28603(11) 0.77145(9) 0.52834(8) 0.0183(4) Uani 1 1 d . . H67 H 0.3362 0.7429 0.5350 0.022 Uiso 1 1 calc R U C68 C 0.21468(12) 0.76541(9) 0.56470(8) 0.0213(4) Uani 1 1 d . . H68 H 0.2159 0.7336 0.5967 0.026 Uiso 1 1 calc R U C69 C 0.14233(12) 0.80642(9) 0.55349(8) 0.0205(4) Uani 1 1 d . . C70 C 0.13776(12) 0.85394(9) 0.50825(8) 0.0209(4) Uani 1 1 d . . H70 H 0.0867 0.8815 0.5014 0.025 Uiso 1 1 calc R U C71 C 0.21006(12) 0.86019(9) 0.47306(8) 0.0198(4) Uani 1 1 d . . H71 H 0.2089 0.8933 0.4420 0.024 Uiso 1 1 calc R U C72 C 0.36286(11) 0.82875(8) 0.44324(7) 0.0163(4) Uani 1 1 d . . H72 H 0.3762 0.8805 0.4428 0.020 Uiso 1 1 calc R U C73 C 0.63779(13) 0.84340(10) 0.32765(9) 0.0293(4) Uani 1 1 d . . H73A H 0.6883 0.8351 0.3028 0.044 Uiso 1 1 calc R U H73B H 0.6561 0.8710 0.3618 0.044 Uiso 1 1 calc R U H73C H 0.5929 0.8695 0.3057 0.044 Uiso 1 1 calc R U C74 C 0.58553(13) 0.72615(11) 0.29323(9) 0.0291(4) Uani 1 1 d . . H74A H 0.5498 0.7521 0.2647 0.044 Uiso 1 1 calc R U H74B H 0.5554 0.6825 0.3041 0.044 Uiso 1 1 calc R U H74C H 0.6421 0.7145 0.2762 0.044 Uiso 1 1 calc R U C75 C 0.53831(12) 0.88836(9) 0.44773(8) 0.0230(4) Uani 1 1 d . . H75A H 0.5038 0.9140 0.4183 0.034 Uiso 1 1 calc R U H75B H 0.6007 0.8968 0.4414 0.034 Uiso 1 1 calc R U H75C H 0.5226 0.9050 0.4866 0.034 Uiso 1 1 calc R U F1 F 0.41822(8) 0.56833(6) -0.02199(5) 0.0353(3) Uani 1 1 d . . F2 F 0.07084(7) 0.45177(6) 0.55038(5) 0.0337(3) Uani 1 1 d . . F3 F 0.07185(7) 0.80001(6) 0.58907(5) 0.0292(3) Uani 1 1 d . . O1 O 0.16630(8) 0.48094(6) 0.18350(5) 0.0216(3) Uani 1 1 d . . O2 O 0.20951(8) 0.53617(6) 0.27755(5) 0.0229(3) Uani 1 1 d . . O3 O 0.06512(8) 0.59431(6) 0.11188(5) 0.0174(3) Uani 1 1 d . . O4 O 0.34055(8) 0.31499(6) 0.29103(5) 0.0221(3) Uani 1 1 d . . O5 O 0.34850(8) 0.30954(6) 0.39854(5) 0.0188(3) Uani 1 1 d . . O6 O 0.43847(7) 0.44468(6) 0.43623(5) 0.0145(2) Uani 1 1 d . . O7 O 0.31273(9) 0.70721(7) 0.30445(6) 0.0319(3) Uani 1 1 d . . O8 O 0.34296(8) 0.66763(6) 0.40571(7) 0.0295(3) Uani 1 1 d . . O9 O 0.43550(8) 0.79507(6) 0.47014(5) 0.0174(3) Uani 1 1 d . . S1 S 0.20943(3) 0.53790(2) 0.21463(2) 0.01653(10) Uani 1 1 d . . S2 S 0.31785(3) 0.34518(2) 0.34670(2) 0.01441(10) Uani 1 1 d . . S3 S 0.30540(3) 0.71856(2) 0.36626(2) 0.01957(11) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0171(9) 0.0127(7) 0.0147(8) 0.0009(6) 0.0005(7) 0.0005(6) C2 0.0209(9) 0.0179(8) 0.0157(9) 0.0005(7) 0.0030(7) 0.0024(7) C3 0.0192(9) 0.0139(8) 0.0242(10) 0.0003(7) 0.0075(8) 0.0004(7) C4 0.0256(10) 0.0191(9) 0.0321(11) 0.0015(8) 0.0139(9) -0.0010(8) C5 0.0267(11) 0.0245(10) 0.0581(15) -0.0071(10) 0.0218(11) -0.0078(9) C6 0.0169(10) 0.0373(11) 0.0557(15) -0.0205(10) 0.0087(10) -0.0088(9) C7 0.0182(10) 0.0343(11) 0.0386(12) -0.0152(9) 0.0024(9) -0.0028(8) C8 0.0127(9) 0.0203(8) 0.0222(9) -0.0046(7) 0.0042(7) 0.0004(7) C9 0.0145(8) 0.0136(7) 0.0155(8) 0.0017(6) 0.0009(7) -0.0004(6) C10 0.0187(9) 0.0175(8) 0.0129(8) 0.0026(6) -0.0012(7) 0.0022(7) C11 0.0228(9) 0.0178(8) 0.0162(9) -0.0019(7) -0.0013(7) 0.0033(7) C12 0.0204(9) 0.0218(9) 0.0194(9) -0.0010(7) -0.0028(7) -0.0010(7) C13 0.0218(10) 0.0253(9) 0.0144(9) 0.0033(7) 0.0002(7) 0.0044(7) C14 0.0269(10) 0.0207(9) 0.0180(9) -0.0025(7) 0.0002(8) 0.0066(8) C15 0.0240(10) 0.0180(8) 0.0175(9) -0.0013(7) -0.0036(7) 0.0009(7) C16 0.0241(10) 0.0335(10) 0.0242(10) 0.0024(8) 0.0058(8) 0.0035(8) C17 0.0167(9) 0.0144(8) 0.0142(8) 0.0046(6) 0.0008(7) 0.0034(7) C18 0.0219(9) 0.0168(8) 0.0190(9) 0.0018(7) 0.0022(7) 0.0015(7) C19 0.0194(9) 0.0232(9) 0.0240(10) 0.0033(7) 0.0038(8) -0.0014(7) C20 0.0224(10) 0.0274(9) 0.0197(9) 0.0027(7) 0.0081(8) 0.0078(8) C21 0.0261(10) 0.0200(9) 0.0182(9) -0.0004(7) 0.0007(8) 0.0055(7) C22 0.0187(9) 0.0176(8) 0.0179(9) 0.0028(7) -0.0016(7) 0.0022(7) C23 0.0450(14) 0.0320(11) 0.0379(13) 0.0115(9) 0.0256(11) 0.0056(10) C24 0.0246(10) 0.0231(9) 0.0293(11) -0.0031(8) 0.0117(8) -0.0003(8) C25 0.0179(9) 0.0251(9) 0.0211(9) 0.0018(7) 0.0011(7) 0.0060(7) C26 0.0127(8) 0.0142(8) 0.0161(9) 0.0024(6) -0.0017(7) -0.0009(6) C27 0.0150(9) 0.0216(8) 0.0143(8) 0.0025(7) 0.0001(7) -0.0021(7) C28 0.0130(8) 0.0157(8) 0.0162(8) 0.0013(6) 0.0002(7) -0.0018(6) C29 0.0126(8) 0.0200(8) 0.0182(9) 0.0000(7) 0.0015(7) -0.0021(7) C30 0.0133(9) 0.0226(9) 0.0277(10) 0.0010(7) 0.0011(7) -0.0005(7) C31 0.0151(9) 0.0242(9) 0.0242(10) 0.0003(7) -0.0027(7) -0.0003(7) C32 0.0160(9) 0.0205(8) 0.0163(9) -0.0007(7) -0.0021(7) -0.0005(7) C33 0.0109(8) 0.0176(8) 0.0169(9) 0.0003(7) 0.0011(7) -0.0021(6) C34 0.0131(8) 0.0133(7) 0.0170(8) 0.0012(6) -0.0013(7) 0.0000(6) C35 0.0179(9) 0.0187(8) 0.0176(9) 0.0004(7) -0.0010(7) -0.0028(7) C36 0.0136(8) 0.0122(7) 0.0180(9) -0.0026(6) 0.0002(7) -0.0027(6) C37 0.0206(9) 0.0155(8) 0.0180(9) -0.0009(7) 0.0004(7) -0.0034(7) C38 0.0216(10) 0.0196(8) 0.0229(10) 0.0002(7) 0.0065(8) -0.0050(7) C39 0.0168(9) 0.0181(8) 0.0335(11) -0.0014(8) 0.0016(8) -0.0027(7) C40 0.0182(9) 0.0214(9) 0.0254(10) 0.0022(7) -0.0058(8) -0.0016(7) C41 0.0168(10) 0.0373(11) 0.0545(14) 0.0123(10) 0.0054(10) -0.0013(9) C42 0.0132(8) 0.0124(7) 0.0183(9) -0.0043(6) 0.0002(7) -0.0017(6) C43 0.0138(9) 0.0167(8) 0.0189(9) -0.0036(7) -0.0026(7) -0.0017(7) C44 0.0181(9) 0.0218(9) 0.0183(9) -0.0007(7) 0.0005(7) -0.0036(7) C45 0.0164(9) 0.0263(9) 0.0240(10) -0.0042(8) 0.0078(8) -0.0028(7) C46 0.0163(9) 0.0212(9) 0.0314(11) -0.0007(8) 0.0018(8) 0.0048(7) C47 0.0188(9) 0.0159(8) 0.0225(9) 0.0008(7) 0.0004(7) 0.0008(7) C48 0.0187(9) 0.0277(9) 0.0241(10) -0.0052(8) 0.0050(8) -0.0014(8) C49 0.0180(9) 0.0268(9) 0.0225(10) 0.0030(8) 0.0030(8) -0.0058(8) C50 0.0164(9) 0.0194(9) 0.0246(10) -0.0010(7) -0.0003(7) -0.0044(7) C51 0.0171(9) 0.0138(8) 0.0163(9) 0.0010(6) -0.0006(7) 0.0000(7) C52 0.0187(9) 0.0211(8) 0.0158(9) 0.0027(7) 0.0012(7) -0.0013(7) C53 0.0147(9) 0.0181(8) 0.0186(9) 0.0013(7) 0.0008(7) -0.0022(7) C54 0.0171(9) 0.0269(9) 0.0210(9) -0.0002(7) 0.0022(7) -0.0026(7) C55 0.0157(9) 0.0283(10) 0.0285(10) 0.0004(8) 0.0021(8) 0.0004(8) C56 0.0166(9) 0.0278(10) 0.0273(10) 0.0041(8) -0.0020(8) -0.0012(8) C57 0.0191(9) 0.0278(9) 0.0186(9) 0.0022(7) -0.0020(7) -0.0015(8) C58 0.0133(9) 0.0207(8) 0.0191(9) 0.0021(7) 0.0004(7) -0.0044(7) C59 0.0162(9) 0.0165(8) 0.0164(9) -0.0050(7) -0.0011(7) -0.0012(7) C60 0.0220(10) 0.0155(8) 0.0218(9) -0.0015(7) -0.0023(8) -0.0018(7) C61 0.0238(10) 0.0216(9) 0.0207(9) -0.0025(7) 0.0018(8) -0.0063(8) C62 0.0182(9) 0.0251(9) 0.0265(10) -0.0101(8) -0.0002(8) -0.0021(7) C63 0.0209(10) 0.0248(9) 0.0238(10) -0.0021(8) -0.0083(8) 0.0022(8) C64 0.0228(10) 0.0232(9) 0.0156(9) -0.0004(7) -0.0030(7) -0.0049(7) C65 0.0199(10) 0.0436(12) 0.0431(13) -0.0096(10) 0.0040(9) -0.0001(9) C66 0.0189(9) 0.0142(8) 0.0146(8) -0.0027(6) -0.0024(7) -0.0020(7) C67 0.0154(9) 0.0187(8) 0.0207(9) 0.0022(7) -0.0021(7) -0.0011(7) C68 0.0208(10) 0.0223(9) 0.0209(9) 0.0058(7) -0.0011(8) -0.0025(7) C69 0.0187(9) 0.0216(9) 0.0212(9) -0.0025(7) 0.0032(7) -0.0040(7) C70 0.0218(10) 0.0193(8) 0.0216(9) -0.0022(7) -0.0005(8) 0.0055(7) C71 0.0270(10) 0.0158(8) 0.0165(9) 0.0000(7) -0.0012(7) 0.0026(7) C72 0.0182(9) 0.0136(8) 0.0170(9) 0.0017(6) -0.0014(7) -0.0004(7) C73 0.0231(10) 0.0367(11) 0.0281(11) 0.0078(9) 0.0052(8) -0.0059(9) C74 0.0223(10) 0.0409(11) 0.0240(10) -0.0065(9) 0.0030(8) 0.0022(9) C75 0.0213(10) 0.0227(9) 0.0248(10) -0.0018(7) -0.0001(8) -0.0067(8) F1 0.0280(6) 0.0436(7) 0.0349(7) -0.0077(5) 0.0176(5) 0.0036(5) F2 0.0186(6) 0.0478(7) 0.0351(7) 0.0050(5) 0.0127(5) 0.0028(5) F3 0.0198(6) 0.0330(6) 0.0352(7) 0.0055(5) 0.0095(5) 0.0017(5) O1 0.0223(7) 0.0155(6) 0.0270(7) 0.0027(5) -0.0018(5) -0.0021(5) O2 0.0248(7) 0.0274(7) 0.0165(6) 0.0077(5) 0.0016(5) 0.0049(5) O3 0.0128(6) 0.0200(6) 0.0193(6) -0.0041(5) 0.0015(5) 0.0004(5) O4 0.0194(7) 0.0255(6) 0.0213(7) -0.0095(5) 0.0025(5) -0.0005(5) O5 0.0196(6) 0.0146(6) 0.0222(7) 0.0027(5) -0.0040(5) 0.0003(5) O6 0.0097(6) 0.0186(6) 0.0151(6) 0.0007(5) -0.0004(5) -0.0006(5) O7 0.0263(8) 0.0395(8) 0.0303(8) -0.0200(6) 0.0092(6) -0.0072(6) O8 0.0189(7) 0.0165(6) 0.0531(9) 0.0034(6) -0.0032(6) 0.0020(5) O9 0.0140(6) 0.0224(6) 0.0158(6) 0.0041(5) -0.0004(5) -0.0012(5) S1 0.0177(2) 0.0153(2) 0.0166(2) 0.00337(16) -0.00011(17) 0.00140(16) S2 0.0132(2) 0.01408(19) 0.0159(2) -0.00132(15) -0.00040(16) -0.00028(15) S3 0.0160(2) 0.0167(2) 0.0261(2) -0.00577(17) 0.00217(18) -0.00020(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C2 C1 C9 110.27(14) C2 C1 S1 109.31(11) C9 C1 S1 115.51(11) C2 C1 H1 107.1 C9 C1 H1 107.1 S1 C1 H1 107.1 C3 C2 C1 111.24(14) C3 C2 H2A 109.4 C1 C2 H2A 109.4 C3 C2 H2B 109.4 C1 C2 H2B 109.4 H2A C2 H2B 108.0 C2 C3 C8 109.99(14) C2 C3 C4 115.57(15) C8 C3 C4 115.60(15) C2 C3 H3 104.8 C8 C3 H3 104.8 C4 C3 H3 104.8 C23 C4 C24 107.22(16) C23 C4 C5 108.69(17) C24 C4 C5 109.97(17) C23 C4 C3 108.82(16) C24 C4 C3 114.79(14) C5 C4 C3 107.23(15) C6 C5 C4 114.82(16) C6 C5 H5A 108.6 C4 C5 H5A 108.6 C6 C5 H5B 108.6 C4 C5 H5B 108.6 H5A C5 H5B 107.5 C5 C6 C7 111.39(18) C5 C6 H6A 109.3 C7 C6 H6A 109.3 C5 C6 H6B 109.3 C7 C6 H6B 109.3 H6A C6 H6B 108.0 C8 C7 C6 111.98(16) C8 C7 H7A 109.2 C6 C7 H7A 109.2 C8 C7 H7B 109.2 C6 C7 H7B 109.2 H7A C7 H7B 107.9 O3 C8 C7 104.20(13) O3 C8 C25 109.10(13) C7 C8 C25 109.96(15) O3 C8 C3 106.75(13) C7 C8 C3 109.85(15) C25 C8 C3 116.26(14) O3 C9 C17 108.49(13) O3 C9 C1 112.13(13) C17 C9 C1 115.23(14) O3 C9 H9 106.8 C17 C9 H9 106.8 C1 C9 H9 106.8 C15 C10 C11 120.41(16) C15 C10 S1 118.74(13) C11 C10 S1 120.80(13) C12 C11 C10 119.09(16) C12 C11 H11 120.5 C10 C11 H11 120.5 C11 C12 C13 121.43(17) C11 C12 H12 119.3 C13 C12 H12 119.3 C14 C13 C12 118.26(17) C14 C13 C16 120.83(16) C12 C13 C16 120.91(17) C15 C14 C13 121.01(16) C15 C14 H14 119.5 C13 C14 H14 119.5 C14 C15 C10 119.76(17) C14 C15 H15 120.1 C10 C15 H15 120.1 C13 C16 H16A 109.5 C13 C16 H16B 109.5 H16A C16 H16B 109.5 C13 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C22 C17 C18 118.81(16) C22 C17 C9 122.80(15) C18 C17 C9 118.38(15) C19 C18 C17 121.42(16) C19 C18 H18 119.3 C17 C18 H18 119.3 C20 C19 C18 117.76(17) C20 C19 H19 121.1 C18 C19 H19 121.1 F1 C20 C21 118.88(16) F1 C20 C19 118.10(17) C21 C20 C19 123.01(17) C20 C21 C22 118.46(17) C20 C21 H21 120.8 C22 C21 H21 120.8 C17 C22 C21 120.53(17) C17 C22 H22 119.7 C21 C22 H22 119.7 C4 C23 H23A 109.5 C4 C23 H23B 109.5 H23A C23 H23B 109.5 C4 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C4 C24 H24A 109.5 C4 C24 H24B 109.5 H24A C24 H24B 109.5 C4 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C8 C25 H25A 109.5 C8 C25 H25B 109.5 H25A C25 H25B 109.5 C8 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C27 C26 C34 109.58(13) C27 C26 S2 110.51(11) C34 C26 S2 114.52(11) C27 C26 H26 107.3 C34 C26 H26 107.3 S2 C26 H26 107.3 C28 C27 C26 110.80(13) C28 C27 H27A 109.5 C26 C27 H27A 109.5 C28 C27 H27B 109.5 C26 C27 H27B 109.5 H27A C27 H27B 108.1 C27 C28 C33 110.71(13) C27 C28 C29 115.22(14) C33 C28 C29 115.07(14) C27 C28 H28 104.8 C33 C28 H28 104.8 C29 C28 H28 104.8 C48 C29 C49 107.36(14) C48 C29 C30 108.71(14) C49 C29 C30 110.19(14) C48 C29 C28 108.60(14) C49 C29 C28 115.02(14) C30 C29 C28 106.82(13) C31 C30 C29 113.58(14) C31 C30 H30A 108.8 C29 C30 H30A 108.8 C31 C30 H30B 108.8 C29 C30 H30B 108.8 H30A C30 H30B 107.7 C32 C31 C30 112.00(14) C32 C31 H31A 109.2 C30 C31 H31A 109.2 C32 C31 H31B 109.2 C30 C31 H31B 109.2 H31A C31 H31B 107.9 C33 C32 C31 111.60(14) C33 C32 H32A 109.3 C31 C32 H32A 109.3 C33 C32 H32B 109.3 C31 C32 H32B 109.3 H32A C32 H32B 108.0 O6 C33 C32 104.12(13) O6 C33 C50 108.48(13) C32 C33 C50 110.87(14) O6 C33 C28 107.31(13) C32 C33 C28 109.03(13) C50 C33 C28 116.26(14) O6 C34 C42 108.44(13) O6 C34 C26 111.66(13) C42 C34 C26 115.15(14) O6 C34 H34 107.1 C42 C34 H34 107.1 C26 C34 H34 107.1 C40 C35 C36 118.91(16) C40 C35 H35 120.5 C36 C35 H35 120.5 C37 C36 C35 120.92(16) C37 C36 S2 119.89(13) C35 C36 S2 119.18(13) C38 C37 C36 118.98(17) C38 C37 H37 120.5 C36 C37 H37 120.5 C37 C38 C39 121.49(17) C37 C38 H38 119.3 C39 C38 H38 119.3 C40 C39 C38 118.21(17) C40 C39 C41 120.52(18) C38 C39 C41 121.28(18) C35 C40 C39 121.44(17) C35 C40 H40 119.3 C39 C40 H40 119.3 C39 C41 H41A 109.5 C39 C41 H41B 109.5 H41A C41 H41B 109.5 C39 C41 H41C 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C43 C42 C47 119.57(16) C43 C42 C34 121.45(15) C47 C42 C34 118.98(15) C42 C43 C44 120.31(16) C42 C43 H43 119.8 C44 C43 H43 119.8 C45 C44 C43 118.15(17) C45 C44 H44 120.9 C43 C44 H44 120.9 F2 C45 C44 118.04(16) F2 C45 C46 118.62(16) C44 C45 C46 123.34(17) C45 C46 C47 117.96(17) C45 C46 H46 121.0 C47 C46 H46 121.0 C46 C47 C42 120.68(16) C46 C47 H47 119.7 C42 C47 H47 119.7 C29 C48 H48A 109.5 C29 C48 H48B 109.5 H48A C48 H48B 109.5 C29 C48 H48C 109.5 H48A C48 H48C 109.5 H48B C48 H48C 109.5 C29 C49 H49A 109.5 C29 C49 H49B 109.5 H49A C49 H49B 109.5 C29 C49 H49C 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 C33 C50 H50A 109.5 C33 C50 H50B 109.5 H50A C50 H50B 109.5 C33 C50 H50C 109.5 H50A C50 H50C 109.5 H50B C50 H50C 109.5 C52 C51 C72 109.95(14) C52 C51 S3 109.45(11) C72 C51 S3 116.74(11) C52 C51 H51 106.7 C72 C51 H51 106.7 S3 C51 H51 106.7 C53 C52 C51 110.95(14) C53 C52 H52A 109.4 C51 C52 H52A 109.4 C53 C52 H52B 109.4 C51 C52 H52B 109.4 H52A C52 H52B 108.0 C52 C53 C58 110.05(14) C52 C53 C54 115.06(14) C58 C53 C54 115.61(14) C52 C53 H53 105.0 C58 C53 H53 105.0 C54 C53 H53 105.0 C74 C54 C73 107.80(16) C74 C54 C55 107.66(15) C73 C54 C55 110.62(15) C74 C54 C53 108.73(15) C73 C54 C53 114.41(15) C55 C54 C53 107.42(14) C56 C55 C54 114.52(15) C56 C55 H55A 108.6 C54 C55 H55A 108.6 C56 C55 H55B 108.6 C54 C55 H55B 108.6 H55A C55 H55B 107.6 C55 C56 C57 111.16(15) C55 C56 H56A 109.4 C57 C56 H56A 109.4 C55 C56 H56B 109.4 C57 C56 H56B 109.4 H56A C56 H56B 108.0 C58 C57 C56 111.53(15) C58 C57 H57A 109.3 C56 C57 H57A 109.3 C58 C57 H57B 109.3 C56 C57 H57B 109.3 H57A C57 H57B 108.0 O9 C58 C57 104.79(13) O9 C58 C75 108.13(14) C57 C58 C75 110.19(15) O9 C58 C53 106.45(13) C57 C58 C53 109.66(14) C75 C58 C53 116.87(14) C60 C59 C64 121.01(16) C60 C59 S3 119.54(14) C64 C59 S3 119.44(13) C61 C60 C59 119.02(17) C61 C60 H60 120.5 C59 C60 H60 120.5 C60 C61 C62 121.34(17) C60 C61 H61 119.3 C62 C61 H61 119.3 C61 C62 C63 118.15(17) C61 C62 C65 121.03(18) C63 C62 C65 120.82(18) C64 C63 C62 121.54(17) C64 C63 H63 119.2 C62 C63 H63 119.2 C63 C64 C59 118.89(17) C63 C64 H64 120.6 C59 C64 H64 120.6 C62 C65 H65A 109.5 C62 C65 H65B 109.5 H65A C65 H65B 109.5 C62 C65 H65C 109.5 H65A C65 H65C 109.5 H65B C65 H65C 109.5 C71 C66 C67 118.69(16) C71 C66 C72 119.78(15) C67 C66 C72 121.51(15) C68 C67 C66 120.48(16) C68 C67 H67 119.8 C66 C67 H67 119.8 C69 C68 C67 118.61(16) C69 C68 H68 120.7 C67 C68 H68 120.7 F3 C69 C68 118.54(16) F3 C69 C70 118.51(16) C68 C69 C70 122.95(17) C69 C70 C71 117.67(17) C69 C70 H70 121.2 C71 C70 H70 121.2 C70 C71 C66 121.59(16) C70 C71 H71 119.2 C66 C71 H71 119.2 O9 C72 C66 108.10(13) O9 C72 C51 112.11(13) C66 C72 C51 116.23(14) O9 C72 H72 106.6 C66 C72 H72 106.6 C51 C72 H72 106.6 C54 C73 H73A 109.5 C54 C73 H73B 109.5 H73A C73 H73B 109.5 C54 C73 H73C 109.5 H73A C73 H73C 109.5 H73B C73 H73C 109.5 C54 C74 H74A 109.5 C54 C74 H74B 109.5 H74A C74 H74B 109.5 C54 C74 H74C 109.5 H74A C74 H74C 109.5 H74B C74 H74C 109.5 C58 C75 H75A 109.5 C58 C75 H75B 109.5 H75A C75 H75B 109.5 C58 C75 H75C 109.5 H75A C75 H75C 109.5 H75B C75 H75C 109.5 C9 O3 C8 114.36(12) C34 O6 C33 114.76(12) C72 O9 C58 114.80(12) O2 S1 O1 118.12(8) O2 S1 C10 107.05(8) O1 S1 C10 107.38(8) O2 S1 C1 105.91(7) O1 S1 C1 111.13(8) C10 S1 C1 106.66(8) O5 S2 O4 117.78(7) O5 S2 C36 107.97(8) O4 S2 C36 107.36(8) O5 S2 C26 111.58(7) O4 S2 C26 106.74(8) C36 S2 C26 104.57(7) O8 S3 O7 119.03(9) O8 S3 C59 108.54(8) O7 S3 C59 106.90(8) O8 S3 C51 111.18(8) O7 S3 C51 105.14(8) C59 S3 C51 105.13(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.540(2) C1 C9 1.543(2) C1 S1 1.8118(16) C1 H1 1.0000 C2 C3 1.533(2) C2 H2A 0.9900 C2 H2B 0.9900 C3 C8 1.544(2) C3 C4 1.553(2) C3 H3 1.0000 C4 C23 1.534(3) C4 C24 1.538(2) C4 C5 1.544(3) C5 C6 1.522(3) C5 H5A 0.9900 C5 H5B 0.9900 C6 C7 1.524(3) C6 H6A 0.9900 C6 H6B 0.9900 C7 C8 1.523(2) C7 H7A 0.9900 C7 H7B 0.9900 C8 O3 1.456(2) C8 C25 1.535(2) C9 O3 1.423(2) C9 C17 1.510(2) C9 H9 1.0000 C10 C15 1.391(2) C10 C11 1.392(2) C10 S1 1.7721(18) C11 C12 1.384(2) C11 H11 0.9500 C12 C13 1.399(2) C12 H12 0.9500 C13 C14 1.395(3) C13 C16 1.506(3) C14 C15 1.381(3) C14 H14 0.9500 C15 H15 0.9500 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 C22 1.389(2) C17 C18 1.397(2) C18 C19 1.384(2) C18 H18 0.9500 C19 C20 1.378(3) C19 H19 0.9500 C20 F1 1.370(2) C20 C21 1.372(3) C21 C22 1.395(2) C21 H21 0.9500 C22 H22 0.9500 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 C26 C27 1.534(2) C26 C34 1.540(2) C26 S2 1.8195(16) C26 H26 1.0000 C27 C28 1.532(2) C27 H27A 0.9900 C27 H27B 0.9900 C28 C33 1.544(2) C28 C29 1.555(2) C28 H28 1.0000 C29 C48 1.533(2) C29 C49 1.537(2) C29 C30 1.544(2) C30 C31 1.537(2) C30 H30A 0.9900 C30 H30B 0.9900 C31 C32 1.533(2) C31 H31A 0.9900 C31 H31B 0.9900 C32 C33 1.526(2) C32 H32A 0.9900 C32 H32B 0.9900 C33 O6 1.4532(19) C33 C50 1.537(2) C34 O6 1.422(2) C34 C42 1.512(2) C34 H34 1.0000 C35 C40 1.385(2) C35 C36 1.392(2) C35 H35 0.9500 C36 C37 1.391(2) C36 S2 1.7700(17) C37 C38 1.381(2) C37 H37 0.9500 C38 C39 1.397(3) C38 H38 0.9500 C39 C40 1.392(3) C39 C41 1.503(3) C40 H40 0.9500 C41 H41A 0.9800 C41 H41B 0.9800 C41 H41C 0.9800 C42 C43 1.392(2) C42 C47 1.393(2) C43 C44 1.393(2) C43 H43 0.9500 C44 C45 1.373(3) C44 H44 0.9500 C45 F2 1.369(2) C45 C46 1.375(3) C46 C47 1.387(2) C46 H46 0.9500 C47 H47 0.9500 C48 H48A 0.9800 C48 H48B 0.9800 C48 H48C 0.9800 C49 H49A 0.9800 C49 H49B 0.9800 C49 H49C 0.9800 C50 H50A 0.9800 C50 H50B 0.9800 C50 H50C 0.9800 C51 C52 1.539(2) C51 C72 1.544(2) C51 S3 1.8156(16) C51 H51 1.0000 C52 C53 1.536(2) C52 H52A 0.9900 C52 H52B 0.9900 C53 C58 1.542(2) C53 C54 1.555(2) C53 H53 1.0000 C54 C74 1.534(3) C54 C73 1.539(3) C54 C55 1.542(3) C55 C56 1.527(3) C55 H55A 0.9900 C55 H55B 0.9900 C56 C57 1.527(2) C56 H56A 0.9900 C56 H56B 0.9900 C57 C58 1.522(2) C57 H57A 0.9900 C57 H57B 0.9900 C58 O9 1.456(2) C58 C75 1.537(2) C59 C60 1.390(2) C59 C64 1.391(2) C59 S3 1.7653(18) C60 C61 1.386(3) C60 H60 0.9500 C61 C62 1.395(3) C61 H61 0.9500 C62 C63 1.398(3) C62 C65 1.502(3) C63 C64 1.382(3) C63 H63 0.9500 C64 H64 0.9500 C65 H65A 0.9800 C65 H65B 0.9800 C65 H65C 0.9800 C66 C71 1.392(2) C66 C67 1.393(2) C66 C72 1.514(2) C67 C68 1.388(2) C67 H67 0.9500 C68 C69 1.373(3) C68 H68 0.9500 C69 F3 1.367(2) C69 C70 1.375(3) C70 C71 1.383(2) C70 H70 0.9500 C71 H71 0.9500 C72 O9 1.415(2) C72 H72 1.0000 C73 H73A 0.9800 C73 H73B 0.9800 C73 H73C 0.9800 C74 H74A 0.9800 C74 H74B 0.9800 C74 H74C 0.9800 C75 H75A 0.9800 C75 H75B 0.9800 C75 H75C 0.9800 O1 S1 1.4474(13) O2 S1 1.4454(13) O4 S2 1.4468(12) O5 S2 1.4412(12) O7 S3 1.4414(14) O8 S3 1.4372(14)