#------------------------------------------------------------------------------ #$Date: 2016-01-09 04:27:24 +0200 (Sat, 09 Jan 2016) $ #$Revision: 173695 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/19/1541919.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_1541919 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 'C26 H28 O4 S' _chemical_formula_weight 436.54 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/6 _cell_angle_alpha 90 _cell_angle_beta 112.341(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 23.259(3) _cell_length_b 5.6619(4) _cell_length_c 17.6922(16) _cell_measurement_reflns_used 3655 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.9249 _cell_measurement_theta_min 2.8405 _cell_volume 2155.0(4) _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 0.998 _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 0.0431 _diffrn_reflns_av_unetI/netI 0.0473 _diffrn_reflns_laue_measured_fraction_full 0.999 _diffrn_reflns_laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 17485 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.387 _diffrn_reflns_theta_min 0.946 _exptl_absorpt_coefficient_mu 0.182 _exptl_absorpt_correction_T_max 0.9485 _exptl_absorpt_correction_T_min 0.8864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Blade _exptl_crystal_F_000 928 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.694 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.200 _refine_ls_extinction_coef 0.039(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.255 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 285 _refine_ls_number_reflns 4391 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.255 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0654 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+3.2513P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1875 _refine_ls_wR_factor_ref 0.2079 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3522 _reflns_number_total 4391 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol5b03696_si_005.cif _cod_data_source_block 150232LT_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_original_cell_volume 2155.0(3) _cod_database_code 1541919 _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 150232LT_a.res in P2(1)/c CELL 0.71073 23.2588 5.6619 17.6922 90.000 112.341 90.000 ZERR 4.000 0.0026 0.0004 0.0016 0.000 0.004 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C O S H UNIT 104 16 4 112 L.S. 4 ACTA BOND $H FMAP 2 PLAN 5 TEMP -173.000 WGHT 0.089500 3.251300 EXTI 0.039489 FVAR 0.42026 C1 1 0.608106 -0.053404 0.280973 11.00000 0.01601 0.01691 = 0.01871 0.00268 0.00805 -0.00129 C2 1 0.598921 -0.236958 0.225799 11.00000 0.01851 0.01361 = 0.02516 0.00098 0.00944 -0.00053 AFIX 43 H2 4 0.625961 -0.369611 0.239136 11.00000 -1.20000 AFIX 0 C3 1 0.549459 -0.223966 0.150528 11.00000 0.02008 0.02018 = 0.02202 -0.00102 0.00757 -0.00327 AFIX 43 H3 4 0.543213 -0.348556 0.112252 11.00000 -1.20000 AFIX 0 C4 1 0.509125 -0.033025 0.130251 11.00000 0.01557 0.02839 = 0.02082 0.00722 0.00813 -0.00246 C5 1 0.520546 0.153564 0.185456 11.00000 0.01964 0.01986 = 0.02825 0.00822 0.01366 0.00536 AFIX 43 H5 4 0.494558 0.289166 0.171265 11.00000 -1.20000 AFIX 0 C6 1 0.569361 0.143372 0.260748 11.00000 0.01906 0.01807 = 0.02289 0.00090 0.01082 0.00014 AFIX 43 H6 4 0.576367 0.270070 0.298406 11.00000 -1.20000 AFIX 0 C7 1 0.452090 -0.029249 0.052088 11.00000 0.02056 0.04175 = 0.02287 0.00493 0.00752 -0.00312 AFIX 137 H7A 4 0.458076 -0.137046 0.012357 11.00000 -1.50000 H7B 4 0.445314 0.131331 0.029741 11.00000 -1.50000 H7C 4 0.415845 -0.079580 0.063412 11.00000 -1.50000 AFIX 0 C8 1 0.725187 0.128003 0.398724 11.00000 0.01645 0.01544 = 0.01318 -0.00051 0.00467 0.00021 AFIX 13 H8 4 0.707042 0.282144 0.373085 11.00000 -1.20000 AFIX 0 C9 1 0.758047 0.161157 0.491012 11.00000 0.02019 0.02012 = 0.01456 0.00105 0.00747 0.00137 AFIX 23 H9A 4 0.726664 0.192467 0.515010 11.00000 -1.20000 H9B 4 0.780113 0.013590 0.515497 11.00000 -1.20000 AFIX 0 C10 1 0.804539 0.364813 0.512078 11.00000 0.01497 0.01969 = 0.01464 -0.00194 0.00500 0.00258 AFIX 13 H10 4 0.780400 0.514805 0.505413 11.00000 -1.20000 AFIX 0 C11 1 0.839474 0.377660 0.454843 11.00000 0.01302 0.01780 = 0.01406 0.00207 0.00309 0.00551 C12 1 0.885291 0.551963 0.466044 11.00000 0.01602 0.01964 = 0.01641 -0.00234 0.00230 0.00316 C13 1 0.918408 0.571641 0.415157 11.00000 0.01147 0.01712 = 0.02290 -0.00313 0.00379 -0.00128 AFIX 43 H13 4 0.948929 0.691317 0.424159 11.00000 -1.20000 AFIX 0 C14 1 0.905866 0.412415 0.350871 11.00000 0.01493 0.02605 = 0.01493 0.00244 0.00405 0.00420 C15 1 0.860039 0.242516 0.336833 11.00000 0.01498 0.01724 = 0.01349 -0.00132 0.00171 0.00230 AFIX 43 H15 4 0.851569 0.135391 0.292576 11.00000 -1.20000 AFIX 0 C16 1 0.826276 0.227334 0.387001 11.00000 0.01453 0.01478 = 0.01299 0.00251 0.00161 0.00419 C17 1 0.773019 0.045060 0.364026 11.00000 0.01484 0.01606 = 0.01372 0.00127 0.00429 0.00287 AFIX 13 H17 4 0.791132 -0.106555 0.391930 11.00000 -1.20000 AFIX 0 C18 1 0.845663 0.339575 0.603593 11.00000 0.02101 0.04059 = 0.01426 -0.00162 0.00568 0.00159 AFIX 137 H18A 4 0.871292 0.197160 0.611938 11.00000 -1.50000 H18B 4 0.819198 0.327198 0.635278 11.00000 -1.50000 H18C 4 0.872627 0.478331 0.621703 11.00000 -1.50000 AFIX 0 C19 1 0.942664 0.876894 0.545394 11.00000 0.02046 0.01998 = 0.02598 -0.00658 0.00241 -0.00102 AFIX 137 H19A 4 0.981836 0.795247 0.554165 11.00000 -1.50000 H19B 4 0.946725 0.966414 0.594573 11.00000 -1.50000 H19C 4 0.932908 0.985284 0.498994 11.00000 -1.50000 AFIX 0 C20 1 0.975077 0.611663 0.302125 11.00000 0.02785 0.03078 = 0.03333 -0.00204 0.01604 -0.00852 AFIX 137 H20A 4 0.951014 0.757848 0.294948 11.00000 -1.50000 H20B 4 0.991495 0.599041 0.258818 11.00000 -1.50000 H20C 4 1.009634 0.613787 0.355479 11.00000 -1.50000 AFIX 0 C21 1 0.745726 -0.002978 0.272747 11.00000 0.01246 0.01862 = 0.01587 0.00005 0.00632 -0.00109 C22 1 0.758137 -0.215588 0.242694 11.00000 0.01968 0.01492 = 0.02167 -0.00202 0.01016 -0.00267 AFIX 43 H22 4 0.783335 -0.330881 0.279434 11.00000 -1.20000 AFIX 0 C23 1 0.733876 -0.260495 0.159139 11.00000 0.02670 0.01854 = 0.02479 -0.00602 0.01473 -0.00527 AFIX 43 H23 4 0.743036 -0.405546 0.139131 11.00000 -1.20000 AFIX 0 C24 1 0.696584 -0.095877 0.105060 11.00000 0.02199 0.02913 = 0.01677 -0.00330 0.00854 -0.00713 AFIX 43 H24 4 0.679535 -0.128758 0.048138 11.00000 -1.20000 AFIX 0 C25 1 0.684124 0.116974 0.133988 11.00000 0.01551 0.02399 = 0.01666 0.00353 0.00503 -0.00256 AFIX 43 H25 4 0.658406 0.230612 0.096996 11.00000 -1.20000 AFIX 0 C26 1 0.709338 0.164424 0.217422 11.00000 0.01553 0.01572 = 0.01812 0.00096 0.00812 -0.00203 AFIX 43 H26 4 0.701655 0.312713 0.236905 11.00000 -1.20000 AFIX 0 O1 2 0.688856 -0.318802 0.390203 11.00000 0.02386 0.01678 = 0.02565 0.00474 0.00561 -0.00032 O2 2 0.631605 -0.015440 0.434636 11.00000 0.02546 0.02874 = 0.02011 0.00149 0.01205 -0.00229 O3 2 0.936132 0.415294 0.297972 11.00000 0.02045 0.02960 = 0.02232 -0.00562 0.01202 -0.00614 O4 2 0.893966 0.707773 0.528592 11.00000 0.02108 0.02389 = 0.02195 -0.01012 0.00685 -0.00411 S1 3 0.663172 -0.083929 0.381769 11.00000 0.01830 0.01482 = 0.01704 0.00244 0.00721 -0.00054 HKLF 4 REM 150232LT_a.res in P2(1)/c REM R1 = 0.0654 for 3522 Fo > 4sig(Fo) and 0.0841 for all 4391 data REM 285 parameters refined using 0 restraints END WGHT 0.0895 3.2512 REM Highest difference peak 0.694, deepest hole -0.648, 1-sigma level 0.200 Q1 1 0.9379 0.5389 0.2836 11.00000 0.05 0.69 Q2 1 0.9187 0.4406 0.3208 11.00000 0.05 0.63 Q3 1 0.9095 0.4108 0.2538 11.00000 0.05 0.61 Q4 1 0.9488 0.6852 0.2718 11.00000 0.05 0.57 Q5 1 0.9410 0.3069 0.2905 11.00000 0.05 0.54 ; _shelx_res_checksum 49113 _shelx_hkl_file ; -1 0 1 0.20 0.30 -1 0 1 -0.10 0.20 1 0 -1 0.00 0.20 1 0 -1 0.00 0.20 2 0 -2 -1.00 0.50 2 0 -2 2.30 0.80 -2 0 2 -0.60 0.60 -2 0 2 0.00 0.70 3 0 -3 0.00 1.30 3 0 -3 -1.70 0.90 -3 0 3 -0.40 1.10 -3 0 3 0.40 1.10 4 0 -4 152.88 6.40 4 0 -4 145.49 6.80 -4 0 4 128.89 6.50 -4 0 4 157.18 6.50 -5 0 5 -1.00 1.60 5 0 -5 0.20 2.00 -5 0 5 0.20 1.90 5 0 -5 -0.90 1.50 -6 0 6 18.20 2.90 6 0 -6 16.80 2.60 6 0 -6 10.60 2.70 7 0 -7 0.60 2.20 -7 0 7 3.00 2.00 -9 0 9 0.60 2.00 9 0 -9 -2.80 2.10 10 0 -10 536.95 21.20 -10 0 10 485.05 20.10 11 0 -11 2.50 2.80 -11 0 11 1.70 2.40 12 0 -12 48.30 6.60 -12 0 12 44.70 5.50 -13 0 13 3.50 2.70 13 0 -13 2.20 3.80 14 0 -14 38.70 7.10 -14 0 14 44.60 6.50 -15 0 15 -2.20 2.80 15 0 -15 1.00 3.80 -16 0 16 2.80 3.60 16 0 -16 2.70 4.10 17 0 -17 -1.10 3.90 -17 0 17 -0.50 3.20 18 0 -18 21.80 6.70 -18 0 18 34.60 6.80 19 0 -19 -0.30 5.10 20 0 -20 17.50 7.50 0 -1 0 -0.20 1.10 0 -1 0 -0.80 1.00 0 1 0 0.00 1.10 0 1 0 -1.40 1.10 1 -1 -1 637.34 20.00 -1 -1 1 628.54 21.00 1 -1 -1 621.24 20.90 1 -1 -1 651.03 21.00 1 -1 -1 641.14 20.00 1 1 -1 634.14 21.00 -1 1 1 641.94 21.00 -1 1 1 634.24 20.10 -1 1 1 621.24 20.10 -1 1 1 646.64 20.90 2 -1 -2 188.18 6.90 2 -1 -2 178.48 6.80 2 -1 -2 182.48 7.30 -2 -1 2 183.68 7.40 -2 1 2 186.88 7.10 2 1 -2 180.08 6.30 -2 1 2 183.78 7.30 2 1 -2 185.08 6.20 2 1 -2 188.68 7.30 -2 1 2 176.48 6.90 3 -1 -3 15.10 2.20 -3 -1 3 18.60 2.30 3 -1 -3 15.40 2.00 -3 -1 3 20.20 1.90 3 1 -3 19.50 2.20 -3 1 3 15.60 2.30 -3 1 3 19.20 2.40 3 1 -3 15.90 1.70 4 -1 -4 34.30 3.20 -4 -1 4 31.50 2.90 -4 -1 4 39.10 3.10 -4 -1 4 32.30 2.50 4 -1 -4 31.70 3.30 4 1 -4 33.10 2.80 -4 1 4 37.90 3.60 -4 1 4 31.40 3.30 4 1 -4 34.70 3.20 -5 -1 5 34.10 3.50 -5 -1 5 45.10 3.20 -5 -1 5 43.30 3.20 5 -1 -5 47.20 4.40 5 1 -5 42.10 3.90 -5 1 5 49.60 4.30 -5 1 5 31.60 3.70 5 1 -5 41.70 3.50 -6 -1 6 205.38 8.50 6 -1 -6 201.78 9.50 -6 -1 6 201.08 8.30 6 1 -6 207.18 8.80 6 1 -6 211.18 9.40 -6 1 6 201.78 9.30 -7 -1 7 148.79 7.00 -7 -1 7 137.09 6.40 7 -1 -7 141.49 7.90 7 1 -7 146.99 7.20 7 1 -7 141.99 7.90 -7 1 7 144.89 7.80 -8 -1 8 85.49 5.40 8 -1 -8 75.39 6.80 8 1 -8 73.69 6.70 -8 1 8 98.79 6.50 8 1 -8 84.29 5.60 -9 -1 9 118.39 7.00 9 -1 -9 130.29 8.20 9 1 -9 121.69 7.90 -9 1 9 118.79 7.80 -10 -1 10 479.45 18.90 10 -1 -10 477.65 20.20 -10 1 10 472.85 19.90 10 1 -10 518.05 20.40 11 -1 -11 -0.50 3.10 -11 -1 11 3.10 1.60 -11 -1 11 1.20 1.90 11 1 -11 5.10 3.20 -11 1 11 0.80 2.50 -12 -1 12 66.89 6.60 -12 -1 12 55.89 4.20 12 -1 -12 61.09 7.80 -12 1 12 65.39 7.40 12 1 -12 48.50 6.70 -13 -1 13 30.00 4.80 -13 -1 13 22.20 3.00 13 -1 -13 19.80 5.10 13 1 -13 25.90 5.60 -13 1 13 25.60 5.00 14 -1 -14 128.39 11.80 -14 -1 14 101.59 9.10 -14 -1 14 107.29 6.10 14 1 -14 90.59 10.20 -14 1 14 100.29 9.60 15 -1 -15 411.16 21.10 -15 -1 15 412.16 16.10 -15 -1 15 438.66 19.50 -15 1 15 406.86 20.20 15 1 -15 447.46 21.20 -16 -1 16 -2.00 3.50 16 -1 -16 1.90 4.40 -16 1 16 -0.10 3.20 16 1 -16 -5.20 3.60 17 -1 -17 10.00 5.70 -17 1 17 18.90 5.70 17 1 -17 1.20 4.30 18 -1 -18 50.19 9.10 -18 1 18 53.19 8.60 18 1 -18 50.79 8.90 19 -1 -19 1.50 5.00 19 1 -19 -4.10 4.20 -19 1 19 -2.70 4.00 20 -1 -20 21.80 8.20 20 1 -20 16.40 7.30 -20 1 20 22.70 7.10 0 -2 0 1.40 1.80 0 -2 0 -0.30 1.60 0 2 0 0.30 1.80 0 2 0 0.90 1.70 0 2 0 0.00 0.70 0 2 0 1.60 0.80 1 -2 -1 53.99 4.40 1 -2 -1 39.40 4.00 -1 -2 1 38.00 4.00 -1 2 1 59.59 5.10 1 2 -1 50.19 4.90 -1 2 1 47.10 2.80 -1 2 1 46.80 4.40 -1 2 1 40.80 2.60 1 2 -1 42.20 4.20 -2 -2 2 129.49 7.10 2 -2 -2 126.89 5.00 2 -2 -2 139.49 7.00 2 2 -2 126.19 7.00 -2 2 2 128.29 5.70 2 2 -2 134.59 7.10 -2 2 2 129.39 5.70 -2 2 2 132.59 6.60 -2 2 2 118.89 6.90 -3 -2 3 141.69 7.60 3 -2 -3 150.68 6.30 3 -2 -3 152.08 7.70 3 2 -3 148.89 5.40 3 2 -3 144.09 7.60 3 2 -3 156.78 5.70 -3 2 3 157.08 6.80 -3 2 3 160.58 7.80 -3 2 3 152.68 7.00 -4 -2 4 17.00 3.10 4 -2 -4 18.30 3.10 4 -2 -4 17.70 2.50 4 2 -4 22.60 2.40 -4 2 4 14.70 2.70 4 2 -4 17.90 3.00 4 2 -4 17.90 1.90 -4 2 4 21.50 3.00 -4 2 4 19.00 3.10 5 -2 -5 148.89 7.30 5 -2 -5 141.39 7.80 -5 -2 5 143.09 7.60 -5 2 5 147.29 7.40 -5 2 5 151.68 7.80 -5 2 5 143.69 7.50 5 2 -5 144.89 6.80 5 2 -5 149.19 6.30 -6 -2 6 38.00 2.10 6 -2 -6 39.10 4.20 -6 -2 6 33.20 4.00 -6 -2 6 35.50 2.30 6 2 -6 32.00 3.80 -6 2 6 31.60 4.10 -6 2 6 39.80 4.40 6 2 -6 39.50 3.50 -6 2 6 34.60 3.90 -7 -2 7 119.49 5.30 -7 -2 7 122.49 6.90 7 -2 -7 111.59 7.10 -7 2 7 122.79 7.30 7 2 -7 128.59 7.00 -7 2 7 113.29 6.70 7 2 -7 112.29 6.10 8 -2 -8 44.50 5.10 -8 -2 8 50.19 4.80 8 2 -8 41.10 4.20 -8 2 8 38.00 4.10 8 2 -8 47.60 5.10 -8 2 8 38.30 4.90 -9 -2 9 2.40 1.40 9 -2 -9 1.20 2.70 -9 -2 9 0.60 1.80 -9 2 9 0.90 2.40 9 2 -9 5.90 2.80 9 2 -9 0.60 1.80 -10 -2 10 63.89 4.90 -10 -2 10 75.99 5.60 10 -2 -10 91.89 8.30 10 2 -10 70.29 7.10 10 2 -10 72.49 6.60 -10 2 10 74.39 7.40 11 -2 -11 149.69 9.80 -11 -2 11 145.09 8.00 -11 -2 11 129.59 7.50 11 2 -11 139.19 9.40 -11 2 11 140.09 9.60 12 -2 -12 5.10 3.60 -12 -2 12 7.30 2.70 -12 -2 12 8.10 2.50 12 2 -12 4.80 3.70 -12 2 12 6.20 3.60 -12 2 12 6.90 2.20 -13 -2 13 15.70 3.30 -13 -2 13 30.10 6.60 13 -2 -13 31.80 5.90 13 2 -13 29.20 5.80 -13 2 13 27.30 3.80 -13 2 13 21.90 5.20 14 -2 -14 2.20 3.60 -14 -2 14 2.10 2.30 -14 2 14 8.20 4.00 14 2 -14 5.80 4.00 -14 2 14 2.30 2.00 15 -2 -15 -0.30 3.70 -15 2 15 1.90 3.70 15 2 -15 -1.50 3.80 16 -2 -16 79.49 10.20 -16 2 16 64.49 9.10 16 2 -16 59.39 8.40 17 -2 -17 164.88 14.90 -17 2 17 177.28 13.80 17 2 -17 200.48 14.10 18 -2 -18 0.90 4.30 -18 2 18 4.20 4.70 18 2 -18 5.80 5.10 19 -2 -19 66.19 10.30 -19 2 19 54.19 9.20 19 2 -19 61.59 10.10 0 -3 0 -0.20 1.70 0 -3 0 -1.20 1.50 0 3 0 -0.10 2.00 0 3 0 -0.80 0.80 0 3 0 -1.70 1.40 0 3 0 -0.10 1.00 1 -3 -1 20.10 3.50 -1 -3 1 18.20 3.50 1 3 -1 14.90 3.20 -1 3 1 24.30 3.70 -1 3 1 20.20 3.60 1 3 -1 25.20 3.80 -1 3 1 31.80 2.80 -1 3 1 25.50 2.50 1 3 -1 22.60 1.70 1 3 -1 21.10 1.60 -2 -3 2 24.00 3.90 2 -3 -2 39.70 4.70 -2 3 2 27.40 3.00 2 3 -2 29.40 1.70 -2 3 2 29.90 4.30 2 3 -2 28.00 4.00 -2 3 2 31.00 3.90 2 3 -2 34.80 4.70 -2 3 2 32.30 3.20 3 -3 -3 60.29 2.80 -3 -3 3 54.89 5.60 3 -3 -3 57.99 6.00 3 3 -3 52.19 2.70 -3 3 3 64.29 5.00 3 3 -3 51.09 5.70 3 3 -3 56.19 2.60 -3 3 3 54.29 4.10 -3 3 3 54.09 4.20 3 3 -3 59.69 6.10 -3 3 3 58.49 6.20 4 -3 -4 80.69 6.40 -4 -3 4 86.59 6.50 -4 3 4 80.79 7.10 -4 3 4 83.99 5.50 -4 3 4 88.19 5.40 4 3 -4 84.99 3.80 4 3 -4 81.79 6.20 4 3 -4 79.59 4.20 5 -3 -5 104.19 7.40 -5 -3 5 93.79 7.10 5 -3 -5 102.09 5.40 5 3 -5 93.19 6.70 5 3 -5 100.19 4.60 -5 3 5 94.09 6.10 5 3 -5 98.49 5.20 -5 3 5 99.49 6.50 -5 3 5 87.59 7.60 6 -3 -6 308.47 12.10 -6 -3 6 299.87 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94.89 5.60 -7 -1 8 87.29 4.70 7 1 -8 83.39 5.50 -7 1 8 86.19 6.20 7 1 -8 89.89 6.40 6 -1 -7 25.80 3.80 -6 -1 7 32.80 3.00 -6 -1 7 32.80 3.40 6 1 -7 35.60 3.70 6 1 -7 28.30 3.70 -6 1 7 36.10 4.30 -5 -1 6 13.30 2.30 5 -1 -6 13.80 2.90 -5 -1 6 14.30 2.20 -5 1 6 13.70 2.90 5 1 -6 14.90 2.90 5 1 -6 13.60 2.40 -5 1 6 13.90 3.00 4 -1 -5 9.00 2.40 -4 -1 5 13.50 2.00 -4 -1 5 5.30 1.70 -4 -1 5 10.70 1.90 -4 1 5 13.50 2.60 4 1 -5 9.70 1.90 -4 1 5 9.10 2.50 4 1 -5 5.60 2.00 3 -1 -4 326.57 12.30 -3 -1 4 345.47 11.60 -3 -1 4 326.37 11.90 3 -1 -4 341.37 12.50 3 1 -4 335.57 11.80 3 1 -4 334.97 11.60 3 1 -4 351.76 12.00 -3 1 4 337.97 12.60 -3 1 4 329.27 11.90 -3 1 4 309.67 12.40 -2 -1 3 98.59 4.80 2 -1 -3 98.99 4.90 2 -1 -3 102.69 4.70 -2 1 3 103.29 4.90 -2 1 3 99.19 4.70 2 1 -3 98.59 4.00 2 1 -3 87.69 4.10 2 1 -3 98.59 4.70 -2 1 3 98.59 4.90 1 -1 -2 3.10 1.20 1 -1 -2 2.20 1.30 1 -1 -2 2.80 1.20 -1 -1 2 3.20 1.40 1 -1 -2 3.10 1.10 -1 1 2 4.20 1.50 -1 1 2 4.70 1.30 -1 1 2 3.80 1.30 1 1 -2 3.30 1.40 0 -1 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79.09 8.20 -11 2 12 82.79 8.70 -10 -2 11 96.79 6.00 10 -2 -11 99.59 8.90 -10 -2 11 83.99 5.90 -10 2 11 94.69 8.60 10 2 -11 81.89 7.80 -10 2 11 91.09 6.00 10 2 -11 101.59 8.70 9 -2 -10 12.80 3.60 -9 -2 10 10.70 2.50 -9 -2 10 6.90 1.90 9 2 -10 7.40 2.60 -9 2 10 5.40 2.10 9 2 -10 2.80 2.60 -9 2 10 13.70 3.60 8 -2 -9 442.46 18.40 -8 -2 9 457.55 17.30 -8 2 9 458.65 17.30 8 2 -9 439.26 17.90 -8 2 9 451.15 18.70 8 2 -9 433.06 17.10 -7 -2 8 0.60 1.80 7 -2 -8 2.60 2.30 -7 -2 8 2.70 1.40 -7 2 8 2.10 1.90 -7 2 8 4.10 2.50 7 2 -8 1.50 2.20 7 2 -8 2.80 1.80 6 -2 -7 102.69 6.50 -6 -2 7 106.19 6.40 -6 -2 7 103.69 4.40 6 2 -7 102.89 5.60 -6 2 7 108.09 6.80 -6 2 7 100.49 6.10 6 2 -7 104.89 6.20 -5 -2 6 109.79 6.30 5 -2 -6 93.39 6.00 5 2 -6 104.79 5.10 -5 2 6 107.09 6.40 -5 2 6 88.09 6.20 -5 2 6 98.09 6.00 5 2 -6 87.69 5.30 4 -2 -5 18.50 3.00 4 -2 -5 17.80 2.80 -4 -2 5 19.10 3.10 4 2 -5 17.80 2.00 4 2 -5 23.40 3.30 -4 2 5 20.10 3.20 -4 2 5 19.00 3.10 -4 2 5 21.60 3.40 4 2 -5 19.50 2.50 -3 -2 4 136.19 7.30 3 -2 -4 142.19 6.50 3 -2 -4 149.29 7.40 -3 2 4 142.99 7.00 3 2 -4 137.69 5.20 -3 2 4 139.69 6.90 3 2 -4 140.39 5.50 -3 2 4 126.39 7.20 3 2 -4 135.19 7.20 2 -2 -3 2.10 1.40 -2 -2 3 6.20 2.30 2 -2 -3 5.00 1.90 2 2 -3 5.70 2.20 -2 2 3 6.00 1.90 -2 2 3 2.30 2.00 -2 2 3 3.30 1.60 1 -2 -2 7.60 1.40 1 -2 -2 8.30 2.40 1 -2 -2 9.00 1.40 1 -2 -2 5.20 2.10 -1 -2 2 10.20 2.60 -1 2 2 7.80 2.00 -1 2 2 7.30 2.50 -1 2 2 9.10 1.80 1 2 -2 5.80 2.20 1 2 -2 6.20 2.40 -1 2 2 7.70 1.80 0 -2 -1 130.29 6.60 0 -2 -1 120.49 6.80 0 -2 1 124.19 6.70 0 2 1 132.19 7.10 0 2 1 128.79 5.20 0 2 -1 124.79 7.00 0 2 1 122.89 5.30 0 2 -1 129.99 7.00 0 2 1 121.99 6.30 1 -2 0 36.60 4.10 -1 -2 0 41.00 3.80 -1 -2 0 38.60 4.30 -1 2 0 29.70 3.60 1 2 0 34.50 2.10 -1 2 0 35.70 1.80 1 2 0 38.70 3.70 -1 2 0 37.10 1.80 1 2 0 27.90 3.50 1 2 0 39.50 2.30 -1 2 0 35.60 4.00 -2 -2 1 22.20 3.40 2 -2 -1 19.20 3.10 2 2 -1 18.60 3.10 2 2 -1 19.50 1.50 -2 2 1 20.10 3.20 -2 2 1 17.00 3.00 -2 2 1 23.10 2.10 2 2 -1 22.60 1.80 -2 2 1 20.10 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7.10 2.80 -7 3 8 10.30 3.20 -7 3 8 14.80 3.80 7 3 -8 12.00 3.00 7 3 -8 9.40 2.30 6 -3 -7 84.29 5.80 -6 -3 7 89.89 6.80 6 -3 -7 91.09 7.10 6 3 -7 91.79 5.00 -6 3 7 88.69 6.60 6 3 -7 97.79 5.70 -6 3 7 88.29 6.70 5 -3 -6 35.00 4.80 -5 -3 6 34.20 4.70 5 -3 -6 33.50 3.80 5 3 -6 33.50 4.60 -5 3 6 28.60 4.20 5 3 -6 28.80 3.20 5 3 -6 26.80 2.60 -5 3 6 31.90 4.70 -5 3 6 32.20 4.40 4 -3 -5 129.99 8.30 4 -3 -5 146.59 6.80 -4 -3 5 147.89 8.60 -4 3 5 140.59 7.70 -4 3 5 150.78 8.70 -4 3 5 143.59 7.90 4 3 -5 131.49 6.00 4 3 -5 140.29 5.60 4 3 -5 142.19 8.30 3 -3 -4 50.89 5.20 -3 -3 4 40.20 5.10 -3 3 4 56.89 5.90 3 3 -4 48.70 5.30 -3 3 4 37.00 4.10 3 3 -4 46.30 5.50 -3 3 4 50.19 4.60 -2 -3 3 83.49 6.40 2 -3 -3 87.59 3.80 2 -3 -3 91.69 6.50 -2 3 3 87.99 5.30 -2 3 3 88.49 5.30 2 3 -3 85.09 7.40 -2 3 3 91.49 6.70 2 3 -3 89.79 6.80 -2 3 3 86.39 5.70 1 -3 -2 180.08 9.60 1 -3 -2 177.38 9.80 -1 -3 2 185.38 9.90 -1 3 2 189.08 10.10 -1 3 2 174.58 9.00 1 3 -2 193.98 10.20 -1 3 2 191.58 8.00 1 3 -2 188.98 10.00 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11.80 -15 3 17 117.19 13.00 14 -3 -16 59.69 8.80 -14 3 16 63.29 9.60 14 3 -16 67.19 8.60 13 -3 -15 -1.80 3.70 -13 3 15 7.10 4.10 13 3 -15 2.40 3.70 -12 -3 14 34.40 4.90 12 -3 -14 34.80 6.30 -12 3 14 49.10 7.40 12 3 -14 49.60 7.00 11 -3 -13 61.89 7.80 -11 -3 13 60.89 6.40 11 3 -13 47.80 6.60 -11 3 13 52.79 7.30 -11 3 13 55.79 6.10 -10 -3 12 30.60 4.60 10 -3 -12 20.60 4.90 10 3 -12 30.70 5.30 -10 3 12 32.10 4.80 -10 3 12 34.70 6.10 -9 -3 11 12.00 3.30 9 -3 -11 19.90 4.30 9 3 -11 12.70 3.70 -9 3 11 12.70 3.40 -9 3 11 15.90 4.30 8 -3 -10 9.30 3.20 -8 -3 10 13.20 3.50 8 -3 -10 6.70 3.20 8 3 -10 10.30 3.30 8 3 -10 8.80 2.70 -8 3 10 6.40 3.40 -8 3 10 6.40 2.80 7 -3 -9 129.19 8.00 7 -3 -9 123.79 8.50 -7 -3 9 116.29 7.90 -7 3 9 126.89 8.00 -7 3 9 117.79 8.30 7 3 -9 105.39 6.40 7 3 -9 124.99 7.40 6 -3 -8 -0.10 1.90 6 -3 -8 3.30 2.20 -6 -3 8 2.10 2.20 -6 3 8 0.40 2.00 -6 3 8 1.00 2.30 6 3 -8 1.00 1.90 6 3 -8 0.70 1.40 -5 -3 7 0.00 1.90 5 -3 -7 3.70 2.00 5 -3 -7 -1.70 1.70 5 3 -7 1.40 1.70 -5 3 7 1.90 2.40 -5 3 7 0.50 2.10 5 3 -7 2.20 1.30 5 3 -7 4.00 2.20 4 -3 -6 256.87 12.20 4 -3 -6 246.78 10.60 -4 -3 6 254.47 12.10 -4 3 6 252.07 11.80 -4 3 6 244.38 12.00 4 3 -6 252.07 9.60 4 3 -6 237.28 11.90 -4 3 6 256.57 11.60 4 3 -6 237.48 9.10 -3 -3 5 55.09 5.90 3 -3 -5 51.59 4.30 3 -3 -5 51.29 5.60 -3 3 5 52.69 5.20 3 3 -5 54.99 5.90 3 3 -5 50.59 2.80 3 3 -5 49.99 2.50 -3 3 5 49.70 5.70 -3 3 5 58.19 5.40 2 -3 -4 2.40 1.90 2 -3 -4 -0.10 0.50 -2 -3 4 -0.50 1.70 -2 3 4 0.40 1.70 -2 3 4 0.70 2.00 2 3 -4 1.60 2.30 -2 3 4 0.70 1.80 2 3 -4 0.80 2.00 1 -3 -3 45.10 4.90 1 -3 -3 45.10 5.30 1 -3 -3 43.20 2.60 -1 3 3 44.70 4.20 1 3 -3 45.50 5.60 -1 3 3 46.00 4.20 -1 3 3 50.09 4.10 -1 3 3 43.80 5.40 1 3 -3 48.90 5.50 0 -3 -2 341.57 15.30 0 -3 -2 355.46 14.70 0 3 2 349.57 14.10 0 3 2 339.67 13.30 0 3 2 362.96 15.50 0 3 -2 364.36 15.90 0 3 2 355.06 13.10 0 3 -2 367.56 15.60 1 -3 1 5.30 2.50 -1 -3 -1 4.80 2.10 -1 -3 -1 5.30 2.50 1 3 1 5.50 1.70 -1 3 -1 6.40 2.60 -1 3 -1 7.10 2.80 1 3 1 1.50 2.20 1 3 1 2.90 1.80 1 3 1 7.30 1.60 -2 -3 0 104.59 7.30 2 -3 0 113.59 7.60 -2 3 0 108.39 4.50 2 3 0 116.79 6.70 -2 3 0 111.09 4.50 2 3 0 116.09 5.40 2 3 0 103.39 4.90 -2 3 0 112.49 7.50 -2 3 0 107.39 4.60 2 3 0 109.89 7.30 -2 3 0 97.69 7.10 3 -3 -1 5.90 2.60 -3 -3 1 3.10 2.40 3 3 -1 3.00 2.20 -3 3 1 3.40 1.40 -3 3 1 5.00 2.30 3 3 -1 4.20 2.20 3 3 -1 3.90 1.50 -3 3 1 2.80 1.40 3 3 -1 3.40 1.20 -3 3 1 7.70 2.70 4 -3 -2 806.62 30.20 -4 -3 2 805.12 29.90 4 3 -2 834.02 29.10 -4 3 2 832.62 27.40 4 3 -2 797.22 29.50 4 3 -2 808.52 26.90 -4 3 2 827.52 27.10 -4 3 2 772.82 29.50 -4 3 2 844.02 30.00 4 3 -2 806.22 26.30 -5 -3 3 15.00 3.50 5 -3 -3 24.80 4.30 5 -3 -3 21.10 1.80 5 3 -3 11.70 2.30 -5 3 3 17.90 3.60 5 3 -3 21.00 3.60 -5 3 3 15.50 2.70 -5 3 3 25.70 3.10 -5 3 3 25.20 3.90 -6 -3 4 2.90 2.30 6 -3 -4 0.10 0.60 6 -3 -4 7.50 2.90 -6 3 4 1.40 1.90 -6 3 4 1.70 2.30 6 3 -4 2.70 1.30 -6 3 4 6.20 2.10 6 3 -4 1.70 1.70 -7 -3 5 33.20 4.70 7 -3 -5 30.80 3.50 7 -3 -5 24.10 4.40 7 3 -5 31.90 3.10 -7 3 5 36.30 4.30 -7 3 5 30.40 4.80 7 3 -5 34.40 4.00 -7 3 5 36.50 4.70 8 -3 -6 105.39 8.00 -8 -3 6 99.89 7.50 8 -3 -6 93.29 6.10 8 3 -6 108.69 5.70 -8 3 6 90.09 7.00 -8 3 6 90.99 6.50 8 3 -6 106.19 6.60 -8 3 6 116.39 7.60 9 -3 -7 209.48 10.20 -9 -3 7 216.08 11.50 9 -3 -7 211.58 12.00 9 3 -7 209.18 10.40 9 3 -7 191.28 9.20 -9 3 7 203.88 11.00 -9 3 7 198.88 10.60 10 -3 -8 7.50 3.40 -10 -3 8 13.30 3.70 10 -3 -8 11.30 3.20 -10 3 8 12.10 3.30 10 3 -8 11.20 3.30 -10 3 8 14.30 3.60 10 3 -8 9.40 2.60 11 -3 -9 83.29 8.80 -11 -3 9 71.69 7.40 11 -3 -9 77.19 7.30 11 3 -9 68.69 6.30 11 3 -9 59.99 6.60 -11 3 9 78.39 7.90 -11 3 9 65.99 6.80 12 -3 -10 6.60 3.60 12 -3 -10 6.30 3.40 -12 -3 10 6.00 3.00 -12 3 10 8.20 2.80 -12 3 10 5.80 3.20 12 3 -10 2.10 2.90 -13 -3 11 25.70 4.70 13 -3 -11 32.20 5.60 13 -3 -11 30.20 5.80 -13 3 11 35.10 5.70 -13 3 11 29.50 4.60 13 3 -11 21.30 4.90 -14 -3 12 219.58 12.40 14 -3 -12 226.28 14.50 14 -3 -12 212.18 12.70 -14 3 12 208.98 13.50 14 3 -12 234.68 13.50 -14 3 12 205.78 11.80 -15 -3 13 3.60 3.20 15 -3 -13 2.20 3.50 -15 3 13 12.40 4.90 -15 3 13 5.10 3.10 15 3 -13 10.60 4.60 16 -3 -14 75.89 9.10 -16 -3 14 69.89 7.80 -16 3 14 78.99 9.60 16 3 -14 74.99 9.40 17 -3 -15 -1.60 3.30 -17 3 15 4.70 4.50 17 3 -15 4.90 4.30 18 3 -16 23.90 6.60 -18 3 16 44.70 8.80 19 3 -17 68.99 10.10 -19 3 17 59.89 9.60 -15 4 17 2.30 5.10 15 4 -17 9.60 4.90 14 4 -16 8.40 4.80 -14 4 16 9.10 5.60 -13 4 15 35.90 7.30 13 4 -15 61.69 8.30 12 4 -14 4.40 3.40 -12 4 14 5.60 4.40 11 -4 -13 168.08 13.40 -11 -4 13 171.68 11.30 -11 4 13 201.58 13.40 11 4 -13 196.28 11.60 -10 -4 12 165.18 10.80 10 -4 -12 151.58 12.20 -10 4 12 181.18 12.30 10 4 -12 157.58 10.10 -9 -4 11 9.40 3.50 9 -4 -11 11.20 4.10 -9 4 11 6.20 3.50 9 4 -11 9.40 3.50 8 -4 -10 5.70 3.10 -8 -4 10 2.30 2.80 8 4 -10 -2.50 2.20 -8 4 10 3.70 3.10 -7 -4 9 21.30 4.70 7 -4 -9 31.60 5.80 7 4 -9 17.10 3.30 -7 4 9 20.70 4.60 6 -4 -8 5.00 2.40 6 -4 -8 9.00 3.40 -6 -4 8 9.00 3.50 -6 4 8 4.90 3.50 6 4 -8 8.20 2.50 -6 4 8 5.30 3.00 6 4 -8 6.00 1.80 5 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-1 4 -1 10.10 3.30 2 -4 0 0.90 2.40 -2 -4 0 2.00 2.40 -2 4 0 1.30 2.30 -2 4 0 5.50 3.00 2 4 0 3.70 2.90 -2 4 0 -0.20 1.30 2 4 0 1.10 1.60 -2 4 0 2.70 1.30 2 4 0 1.20 1.40 2 4 0 -0.80 2.00 3 -4 -1 29.60 5.20 -3 -4 1 25.70 4.70 -3 4 1 38.00 5.70 3 4 -1 38.80 3.40 -3 4 1 44.40 5.90 3 4 -1 33.70 5.20 -3 4 1 32.90 3.50 3 4 -1 36.10 3.60 3 4 -1 37.70 5.30 -3 4 1 41.80 3.60 4 -4 -2 167.38 10.70 -4 -4 2 170.88 10.50 -4 4 2 143.99 9.40 -4 4 2 141.09 7.50 4 4 -2 150.68 9.30 4 4 -2 151.28 9.80 -4 4 2 141.69 9.90 4 4 -2 142.99 6.50 -4 4 2 155.38 7.40 4 4 -2 157.18 7.30 5 -4 -3 110.49 8.70 -5 -4 3 92.39 8.90 5 4 -3 106.49 5.90 -5 4 3 113.49 10.30 -5 4 3 104.09 6.20 -5 4 3 107.79 7.80 -5 4 3 103.59 6.50 5 4 -3 106.79 7.90 5 4 -3 93.59 5.00 6 -4 -4 74.19 8.40 -6 -4 4 72.29 7.90 6 4 -4 74.39 4.40 -6 4 4 85.19 7.30 6 4 -4 88.29 8.10 -6 4 4 79.19 5.80 6 4 -4 80.49 5.40 -7 -4 5 498.85 21.70 7 -4 -5 503.35 22.40 7 -4 -5 473.25 16.10 -7 4 5 452.35 19.60 7 4 -5 494.05 21.20 7 4 -5 488.25 17.30 7 4 -5 476.65 18.40 -7 4 5 489.25 19.30 -8 -4 6 258.37 14.20 8 -4 -6 249.48 12.30 8 -4 -6 255.17 14.50 8 4 -6 247.08 10.60 8 4 -6 254.47 11.80 -8 4 6 270.57 12.70 -9 -4 7 77.19 8.60 9 -4 -7 64.09 8.20 -9 4 7 65.49 7.00 9 4 -7 68.79 6.60 -10 -4 8 74.79 8.50 10 -4 -8 78.59 9.40 10 4 -8 74.69 7.20 -10 4 8 100.39 9.00 11 -4 -9 144.69 13.50 -11 -4 9 139.39 10.40 -11 4 9 133.69 9.80 11 4 -9 141.09 9.40 12 -4 -10 79.29 9.70 -12 -4 10 81.59 8.80 -12 4 10 83.99 9.00 12 4 -10 69.79 7.60 -13 -4 11 117.59 10.80 -13 4 11 135.99 11.90 13 4 -11 127.79 9.70 -14 -4 12 -4.20 2.80 -14 4 12 1.10 3.70 14 4 -12 1.80 3.40 -15 -4 13 -0.10 3.60 -15 4 13 7.80 4.30 15 4 -13 2.30 3.90 16 4 -14 10.60 4.90 -16 4 14 2.90 4.20 -17 4 15 1.70 4.20 17 4 -15 2.00 4.30 18 4 -16 12.20 5.80 -18 4 16 6.90 5.30 13 5 -15 26.90 6.20 12 5 -14 8.80 4.30 -12 5 14 6.10 5.00 -11 5 13 12.80 5.30 11 5 -13 10.60 4.10 10 5 -12 -3.00 2.50 -10 5 12 2.00 3.70 9 -5 -11 14.30 5.40 -9 5 11 10.80 4.30 9 5 -11 10.50 3.60 8 -5 -10 59.89 8.80 -8 5 10 47.80 7.30 8 5 -10 70.09 6.50 7 -5 -9 44.30 7.60 7 5 -9 49.10 5.20 -7 5 9 51.19 7.20 6 -5 -8 10.40 4.80 6 5 -8 8.20 2.60 -6 5 8 3.60 3.10 5 -5 -7 42.30 7.00 5 5 -7 46.60 4.30 -5 5 7 46.90 6.60 5 5 -7 56.49 8.60 4 -5 -6 2.50 3.20 4 5 -6 1.00 2.80 4 5 -6 0.70 1.40 -4 5 6 3.80 2.90 3 -5 -5 33.20 6.30 -3 5 5 34.50 5.00 3 5 -5 33.80 6.40 2 -5 -4 35.10 5.90 2 5 -4 33.50 6.40 -2 5 4 34.70 4.90 1 -5 -3 505.75 22.50 1 5 -3 514.15 17.20 1 5 -3 515.95 24.00 1 5 -3 529.15 17.40 -1 5 3 542.95 20.70 0 5 2 87.29 7.20 0 5 2 89.19 6.30 0 5 -2 85.99 9.30 0 5 -2 84.19 4.40 0 5 -2 82.19 4.20 1 5 1 39.50 5.60 -1 5 -1 26.60 5.50 -1 5 -1 35.10 3.30 1 5 1 38.90 4.60 -1 5 -1 34.40 3.70 -2 -5 0 157.18 11.10 2 5 0 136.79 7.70 2 5 0 146.69 9.70 -2 5 0 141.19 6.90 -2 5 0 151.28 10.70 -3 -5 1 9.10 3.50 3 -5 -1 10.20 4.00 3 5 -1 7.40 3.30 3 5 -1 3.20 2.20 -3 5 1 4.90 3.20 -3 5 1 8.80 2.40 4 -5 -2 143.69 10.80 -4 -5 2 168.58 14.00 4 5 -2 131.09 7.50 -4 5 2 137.59 10.10 -4 5 2 138.89 7.70 4 5 -2 142.69 9.90 -5 -5 3 7.30 3.60 5 -5 -3 16.50 4.70 5 5 -3 5.50 2.40 -5 5 3 20.70 4.50 -5 5 3 13.80 3.20 6 -5 -4 31.80 6.40 -6 -5 4 23.70 5.50 -6 5 4 32.70 4.70 6 5 -4 32.00 6.00 6 5 -4 27.10 4.00 7 -5 -5 28.10 6.10 -7 -5 5 31.30 6.40 -7 5 5 26.10 4.50 7 5 -5 32.50 4.40 7 5 -5 24.60 5.50 -8 -5 6 52.19 7.70 8 -5 -6 67.39 9.20 8 5 -6 63.79 6.20 8 5 -6 60.49 8.20 -8 5 6 70.49 7.50 -9 -5 7 27.90 6.30 9 -5 -7 25.40 6.40 9 5 -7 20.30 5.60 9 5 -7 31.30 4.80 -9 5 7 23.60 4.90 -10 -5 8 32.90 6.70 10 -5 -8 24.30 6.50 -10 5 8 22.20 5.10 10 5 -8 23.70 4.80 10 5 -8 18.10 5.50 -11 -5 9 21.20 5.70 11 5 -9 28.10 5.00 -11 5 9 25.50 5.60 -12 -5 10 42.50 7.60 12 5 -10 38.90 6.10 -12 5 10 49.10 7.50 -13 -5 11 9.20 5.20 13 5 -11 10.90 4.60 -13 5 11 20.90 6.00 -14 -5 12 24.70 6.50 -14 5 12 18.60 5.60 14 5 -12 30.20 6.10 -15 -5 13 7.60 4.90 -15 5 13 19.10 6.10 15 5 -13 33.60 6.60 -9 6 11 30.40 7.20 9 6 -11 36.80 5.30 8 6 -10 98.69 7.30 -8 6 10 109.29 11.60 7 6 -9 2.30 2.30 -7 6 9 5.20 4.10 -6 6 8 60.29 8.20 6 6 -8 63.59 5.40 -5 6 7 -1.00 3.10 5 6 -7 -0.70 1.80 4 6 -6 1.60 1.60 -4 6 6 3.30 3.10 -3 6 5 -1.00 2.60 2 6 -4 88.69 5.00 -2 6 4 96.09 9.00 -1 6 3 4.40 2.90 1 6 -3 2.60 1.80 0 6 2 20.20 4.10 0 6 -2 14.80 2.80 -1 6 -1 199.18 9.20 1 6 1 194.38 10.60 2 6 0 2.30 2.70 -2 6 0 2.60 2.20 3 6 -1 47.40 5.50 -3 6 1 40.10 4.80 4 6 -2 45.60 5.50 -4 6 2 46.70 5.50 5 -6 -3 42.40 8.20 5 6 -3 49.10 5.70 -5 6 3 47.00 5.80 6 -6 -4 17.40 5.70 6 6 -4 9.20 3.30 -6 6 4 9.60 3.50 7 6 -5 44.30 5.50 -7 6 5 35.40 5.60 -8 6 6 77.59 8.30 8 6 -6 73.39 7.10 9 6 -7 6.10 3.40 -9 6 7 9.80 4.10 -10 6 8 2.90 3.50 10 6 -8 6.60 3.60 -11 6 9 0.60 3.50 11 6 -9 2.00 3.50 12 6 -10 95.29 9.30 -12 6 10 84.19 10.30 -1 7 3 29.30 5.70 0 7 2 22.90 5.20 -1 7 -1 35.30 4.70 1 7 1 32.40 5.70 -2 7 0 46.70 5.70 2 7 0 47.10 6.40 -3 7 1 0.70 2.60 3 7 -1 -3.00 3.00 -4 7 2 4.50 3.00 4 7 -2 1.00 3.10 18 0 -21 8.20 6.00 17 0 -20 6.50 5.40 16 0 -19 -6.70 4.00 -15 0 18 61.39 8.70 15 0 -18 66.09 9.60 14 0 -17 -1.50 3.60 -14 0 17 -1.60 3.20 13 0 -16 63.19 8.60 -13 0 16 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1.60 3.10 -3 -5 -5 111.69 11.20 -3 5 -5 115.19 4.90 3 5 5 124.49 9.50 -4 -5 -4 99.29 10.30 -4 5 -4 81.59 4.20 4 5 4 78.49 8.60 -5 -5 -3 30.70 6.20 -5 5 -3 31.70 3.00 5 5 3 31.60 5.80 -6 -5 -2 0.40 2.90 -6 5 -2 0.00 1.40 6 5 2 -0.70 2.70 -7 -5 -1 134.99 13.00 7 -5 1 102.49 11.40 7 5 1 105.89 9.80 -7 5 -1 99.09 6.00 8 -5 0 1.80 3.30 -8 -5 0 1.60 2.90 8 5 0 2.70 3.10 -8 5 0 1.70 2.00 -8 5 0 -0.80 1.70 9 -5 -1 14.00 5.50 -9 -5 1 10.60 4.70 -9 5 1 15.10 3.30 9 5 -1 14.30 4.50 -10 -5 2 24.70 6.20 10 5 -2 20.10 4.90 -10 5 2 24.40 4.20 -11 -5 3 7.50 4.50 -11 5 3 8.70 3.10 11 5 -3 5.60 3.80 -12 -5 4 24.50 6.30 -12 5 4 20.80 4.40 12 5 -4 23.90 5.30 -13 -5 5 -3.00 3.20 13 5 -5 0.00 3.30 -13 5 5 2.30 2.90 -14 -5 6 1.90 4.20 14 5 -6 1.50 3.80 -14 5 6 0.90 2.90 -15 5 7 -1.10 2.80 15 5 -7 -4.60 3.20 -16 5 8 26.40 5.90 16 5 -8 29.90 6.50 17 5 -9 -0.80 3.90 -17 5 9 3.50 3.80 -18 5 10 -2.40 3.50 18 5 -10 7.10 5.30 -19 5 11 32.10 7.40 19 5 -11 40.80 8.30 -3 6 11 5.20 4.70 -2 6 10 7.80 5.00 -1 6 9 7.80 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3 78.29 11.40 -19 2 -3 69.99 8.10 -20 -2 -2 1.70 3.50 20 2 2 2.80 5.10 -20 2 -2 2.10 3.40 -21 -2 -1 102.79 10.30 21 2 1 85.69 12.00 -21 2 -1 103.39 10.90 -22 -2 0 11.90 4.50 22 2 0 19.80 7.60 -22 2 0 23.40 5.70 -23 -2 1 13.60 5.00 23 2 -1 2.30 5.50 -23 2 1 17.60 5.20 -24 -2 2 1.10 3.30 -24 2 2 1.30 3.50 24 2 -2 -0.90 5.30 25 2 -3 36.80 9.20 -25 2 3 37.20 7.10 26 2 -4 7.80 6.20 -26 2 4 12.20 5.70 -27 2 5 0.80 4.40 27 2 -5 9.50 6.90 -6 -3 -16 6.60 5.10 -6 3 -16 12.70 5.00 6 3 16 2.80 6.10 -7 -3 -15 3.20 4.10 7 3 15 7.60 6.60 -7 3 -15 0.30 3.50 -8 -3 -14 103.29 11.40 -8 3 -14 89.79 9.90 8 3 14 99.59 13.40 -9 -3 -13 20.40 5.70 -9 3 -13 14.30 4.80 9 3 13 24.90 8.40 -10 -3 -12 12.10 5.00 -10 -3 -12 14.20 4.90 -10 3 -12 11.70 4.50 10 3 12 22.50 7.40 -11 -3 -11 3.10 3.90 -11 -3 -11 1.80 3.50 -11 3 -11 -0.70 2.90 11 3 11 9.50 6.30 -12 -3 -10 105.79 10.60 -12 -3 -10 98.19 10.40 -12 3 -10 100.79 9.90 12 3 10 109.79 13.60 -13 -3 -9 19.30 5.20 13 3 9 2.30 5.70 -13 3 -9 20.80 5.00 -14 -3 -8 40.80 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0.70 5.70 -20 -2 -5 7.40 4.50 20 2 5 4.30 5.60 -20 2 -5 10.10 4.40 -21 -2 -4 36.50 7.10 -21 2 -4 55.99 8.30 21 2 4 49.40 10.20 -22 -2 -3 197.68 13.50 -22 2 -3 135.79 13.00 22 2 3 179.68 17.60 -23 -2 -2 4.90 4.20 23 2 2 10.60 6.40 -23 2 -2 4.10 4.30 -24 -2 -1 67.09 9.40 -24 2 -1 70.99 10.00 24 2 1 67.39 11.80 -25 2 0 18.10 6.10 25 2 0 4.80 6.70 26 2 -1 5.40 6.50 -26 2 1 -5.30 3.40 -12 3 -13 24.40 5.80 -13 3 -12 192.28 13.70 13 3 12 233.88 21.40 -14 3 -11 3.50 4.20 14 3 11 17.80 8.00 -15 3 -10 52.59 8.00 15 3 10 67.59 12.10 16 3 9 9.70 7.20 -16 3 -9 7.30 4.50 17 3 8 54.99 11.00 -17 3 -8 53.09 7.80 -18 3 -7 11.00 4.50 18 3 7 4.90 6.60 -19 3 -6 2.80 3.60 19 3 6 -3.80 6.00 -20 3 -5 26.40 6.30 20 3 5 17.70 8.00 -21 3 -4 13.80 5.00 21 3 4 18.10 7.80 -22 3 -3 0.70 3.70 22 3 3 4.70 6.20 23 3 2 10.00 6.90 -23 3 -2 1.80 3.90 -10 0 -16 21.10 6.80 -11 0 -15 -0.30 4.60 -12 0 -14 2.00 4.30 -13 0 -13 2.50 4.30 -14 0 -12 148.89 13.60 -15 0 -11 1.40 4.30 -16 0 -10 33.10 6.60 -17 0 -9 -2.70 3.60 18 0 8 7.50 5.10 -18 0 -8 11.00 4.70 19 0 7 0.70 5.00 -19 0 -7 -2.60 3.50 -20 0 -6 133.09 13.00 20 0 6 112.79 12.80 -21 0 -5 8.50 4.80 21 0 5 -1.10 4.20 -22 0 -4 44.90 7.90 22 0 4 33.10 8.00 -23 0 -3 -7.50 3.00 23 0 3 2.70 4.90 24 0 2 14.20 6.40 -24 0 -2 3.60 4.20 -25 0 -1 -5.60 3.50 25 0 1 1.10 5.10 26 0 0 4.20 5.50 -26 0 0 -0.50 4.40 27 0 -1 -0.70 5.10 -27 0 1 1.30 4.40 -10 -1 -16 7.00 5.40 -10 1 -16 11.10 5.70 -11 -1 -15 26.00 7.10 -11 1 -15 35.00 7.70 -12 -1 -14 2.30 4.70 12 1 14 1.30 5.20 -12 1 -14 4.00 4.60 -13 -1 -13 66.39 9.70 -13 1 -13 79.09 10.20 13 1 13 77.09 12.00 -14 -1 -12 69.79 9.90 -14 1 -12 51.79 8.40 14 1 12 56.89 10.50 -15 -1 -11 101.39 11.10 15 1 11 90.69 12.30 -15 1 -11 92.59 10.70 -16 -1 -10 10.20 5.30 -16 1 -10 5.00 4.30 16 1 10 3.70 5.80 -17 -1 -9 55.89 8.50 -17 1 -9 40.60 7.40 17 1 9 47.70 9.90 -18 -1 -8 0.30 3.90 -18 1 -8 0.90 3.70 18 1 8 -0.50 5.10 -19 -1 -7 -2.40 3.40 19 1 7 6.50 5.40 -19 1 -7 4.30 3.90 -20 -1 -6 3.40 4.00 -20 1 -6 0.80 3.50 20 1 6 0.00 5.40 -21 -1 -5 23.50 6.00 -21 1 -5 25.70 6.20 21 1 5 25.60 7.40 -22 -1 -4 31.60 6.80 22 1 4 24.80 7.90 -22 1 -4 23.30 6.20 -23 -1 -3 24.00 6.10 -23 1 -3 17.80 5.90 23 1 3 4.80 5.60 -24 -1 -2 124.99 12.50 24 1 2 95.89 12.80 -24 1 -2 98.79 11.40 -25 -1 -1 39.30 7.50 25 1 1 54.99 11.00 -25 1 -1 52.89 8.60 -26 -1 0 68.99 9.70 26 1 0 82.49 12.70 -26 1 0 56.69 9.20 -27 -1 1 25.10 6.70 -27 1 1 16.40 6.10 27 1 -1 12.70 7.30 -12 -2 -14 -0.50 4.30 -12 2 -14 -2.60 4.00 12 2 14 -0.80 5.40 -13 -2 -13 1.10 4.50 -13 2 -13 1.10 3.80 13 2 13 11.80 6.60 -14 -2 -12 78.59 10.10 -14 2 -12 67.09 9.60 14 2 12 55.69 11.30 -15 -2 -11 99.49 11.30 -15 2 -11 56.59 8.60 15 2 11 61.39 11.00 -16 -2 -10 11.20 5.20 16 2 10 17.70 7.50 -16 2 -10 16.00 5.50 -17 -2 -9 167.78 14.60 17 2 9 183.88 17.90 -17 2 -9 160.78 14.20 -18 -2 -8 34.50 6.90 18 2 8 50.79 10.20 -18 2 -8 36.00 7.20 -19 -2 -7 33.60 7.00 -19 2 -7 42.40 7.50 19 2 7 32.60 9.00 -20 -2 -6 65.19 9.00 20 2 6 62.89 11.80 -20 2 -6 68.09 9.20 -21 -2 -5 93.49 10.80 -21 2 -5 98.69 11.20 21 2 5 95.79 13.10 -22 -2 -4 8.40 5.00 22 2 4 8.20 6.60 -22 2 -4 6.30 4.60 -23 -2 -3 45.30 7.90 23 2 3 47.80 10.80 -23 2 -3 42.20 7.80 -24 -2 -2 36.60 7.10 -24 2 -2 26.10 6.40 24 2 2 43.40 10.10 -25 2 -1 5.00 4.40 25 2 1 0.50 5.60 -16 3 -10 4.20 4.20 16 3 10 -0.30 6.60 17 3 9 -0.10 6.40 -17 3 -9 -2.70 3.60 -18 3 -8 9.30 4.30 18 3 8 -5.00 5.70 19 3 7 3.80 6.90 -19 3 -7 7.10 4.40 -20 3 -6 6.50 3.90 20 3 6 10.20 6.90 -21 3 -5 10.20 5.10 21 3 5 3.10 6.20 -12 0 -15 -2.20 4.90 -13 0 -14 43.70 8.20 -14 0 -13 2.90 4.40 -15 0 -12 12.70 5.70 -16 0 -11 4.40 4.10 -17 0 -10 120.49 12.80 -18 0 -9 0.20 4.20 -19 0 -8 -4.50 3.50 -20 0 -7 -5.90 3.70 -21 0 -6 -2.60 3.90 -22 0 -5 2.50 4.40 23 0 4 13.20 10.90 -23 0 -4 20.10 6.20 24 0 3 -1.90 7.30 -24 0 -3 3.70 4.90 -25 0 -2 0.80 4.30 -26 0 -1 -1.00 3.50 -13 -1 -14 5.10 5.40 -13 1 -14 14.00 5.90 -14 -1 -13 3.50 5.10 -14 1 -13 3.30 4.40 -15 -1 -12 2.10 4.70 15 1 12 16.20 6.60 -15 1 -12 12.00 5.50 -16 -1 -11 44.90 8.70 -16 1 -11 29.40 6.60 16 1 11 25.80 7.80 -17 -1 -10 16.80 5.90 -17 1 -10 9.10 5.10 17 1 10 13.90 7.10 -18 -1 -9 67.39 9.70 -18 1 -9 61.89 9.20 18 1 9 59.99 10.50 -19 -1 -8 -1.90 3.70 19 1 8 2.70 5.10 -19 1 -8 0.50 3.90 -20 -1 -7 23.20 6.40 20 1 7 18.00 7.20 -20 1 -7 31.10 7.00 -21 -1 -6 8.20 5.00 -21 1 -6 3.10 4.40 21 1 6 -1.20 4.80 -22 -1 -5 12.00 5.10 22 1 5 14.70 6.90 -22 1 -5 16.10 5.70 -23 -1 -4 80.09 10.00 -23 1 -4 67.69 9.50 23 1 4 82.49 12.10 -24 -1 -3 14.20 5.70 24 1 3 13.90 7.80 -24 1 -3 13.60 5.70 -25 -1 -2 19.20 6.30 25 1 2 13.40 6.90 -25 1 -2 12.50 5.70 -26 -1 -1 2.00 4.40 -26 1 -1 6.00 5.10 26 1 1 25.80 8.50 -15 -2 -12 164.28 15.50 -15 2 -12 142.29 13.80 15 2 12 133.09 16.00 -16 -2 -11 24.40 7.00 16 2 11 21.10 8.00 -16 2 -11 22.80 6.10 -17 -2 -10 38.60 8.00 17 2 10 47.90 10.30 -17 2 -10 47.30 8.20 -18 -2 -9 30.30 7.20 -18 2 -9 26.90 6.30 18 2 9 19.60 8.70 -19 -2 -8 28.40 6.60 -19 2 -8 34.10 7.00 19 2 8 17.40 8.40 -20 -2 -7 26.50 6.80 20 2 7 42.60 10.20 -20 2 -7 38.00 7.40 -21 -2 -6 25.00 6.50 -21 2 -6 28.60 6.40 21 2 6 39.90 9.40 -22 -2 -5 2.70 4.30 22 2 5 8.10 6.70 -22 2 -5 -0.40 3.80 -23 -2 -4 26.10 6.60 23 2 4 17.10 8.30 -23 2 -4 21.70 6.10 -24 -2 -3 41.00 7.90 -24 2 -3 35.90 7.60 24 2 3 31.10 9.10 -15 0 -13 4.00 4.80 -16 0 -12 0.60 4.00 -17 0 -11 0.80 4.20 -18 0 -10 47.10 8.50 -19 0 -9 3.00 4.80 -20 0 -8 25.60 6.50 -21 0 -7 6.40 4.80 -22 0 -6 183.58 15.90 -23 0 -5 -1.40 4.00 -24 0 -4 66.39 9.90 -25 0 -3 -1.20 4.40 -16 -1 -12 24.70 6.80 -16 1 -12 35.20 7.80 -17 -1 -11 74.79 10.50 -17 1 -11 85.69 11.10 17 1 11 52.39 11.00 -18 -1 -10 21.40 6.60 -18 1 -10 19.10 6.20 18 1 10 14.90 7.50 -19 -1 -9 104.19 11.90 19 1 9 90.19 13.30 -19 1 -9 97.69 11.90 -20 -1 -8 77.69 10.90 20 1 8 51.19 9.40 -20 1 -8 47.40 8.40 -21 -1 -7 55.89 9.10 -21 1 -7 56.69 9.00 21 1 7 53.69 10.30 -22 -1 -6 1.20 4.40 -22 1 -6 11.70 5.30 22 1 6 -0.60 5.10 -23 -1 -5 72.69 10.50 23 1 5 59.29 11.10 -23 1 -5 64.49 9.80 -24 -1 -4 0.10 4.50 24 1 4 10.20 7.10 -24 1 -4 -2.00 4.20 -20 0 -9 4.50 5.00 -21 0 -8 38.20 8.00 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 8877 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.60811(15) -0.0534(6) 0.2810(2) 0.0168(7) Uani 1 1 d . . C2 C 0.59892(16) -0.2370(6) 0.2258(2) 0.0188(7) Uani 1 1 d . . H2 H 0.6260 -0.3696 0.2391 0.023 Uiso 1 1 calc R U C3 C 0.54946(16) -0.2240(6) 0.1505(2) 0.0209(8) Uani 1 1 d . . H3 H 0.5432 -0.3486 0.1123 0.025 Uiso 1 1 calc R U C4 C 0.50912(16) -0.0330(7) 0.1303(2) 0.0212(8) Uani 1 1 d . . C5 C 0.52055(16) 0.1536(6) 0.1855(2) 0.0212(8) Uani 1 1 d . . H5 H 0.4946 0.2892 0.1713 0.025 Uiso 1 1 calc R U C6 C 0.56936(16) 0.1434(6) 0.2607(2) 0.0192(7) Uani 1 1 d . . H6 H 0.5764 0.2701 0.2984 0.023 Uiso 1 1 calc R U C7 C 0.45209(17) -0.0292(8) 0.0521(2) 0.0286(9) Uani 1 1 d . . H7A H 0.4581 -0.1370 0.0124 0.043 Uiso 1 1 calc R U H7B H 0.4453 0.1313 0.0297 0.043 Uiso 1 1 calc R U H7C H 0.4158 -0.0796 0.0634 0.043 Uiso 1 1 calc R U C8 C 0.72519(15) 0.1280(6) 0.39872(19) 0.0153(7) Uani 1 1 d . . H8 H 0.7070 0.2821 0.3731 0.018 Uiso 1 1 calc R U C9 C 0.75805(16) 0.1612(6) 0.4910(2) 0.0180(7) Uani 1 1 d . . H9A H 0.7267 0.1925 0.5150 0.022 Uiso 1 1 calc R U H9B H 0.7801 0.0136 0.5155 0.022 Uiso 1 1 calc R U C10 C 0.80454(15) 0.3648(6) 0.5121(2) 0.0166(7) Uani 1 1 d . . H10 H 0.7804 0.5148 0.5054 0.020 Uiso 1 1 calc R U C11 C 0.83947(15) 0.3777(6) 0.4548(2) 0.0156(7) Uani 1 1 d . . C12 C 0.88529(15) 0.5520(6) 0.4660(2) 0.0185(7) Uani 1 1 d . . C13 C 0.91841(15) 0.5716(6) 0.4152(2) 0.0180(7) Uani 1 1 d . . H13 H 0.9489 0.6913 0.4242 0.022 Uiso 1 1 calc R U C14 C 0.90587(15) 0.4124(6) 0.3509(2) 0.0191(7) Uani 1 1 d . . C15 C 0.86004(15) 0.2425(6) 0.3368(2) 0.0163(7) Uani 1 1 d . . H15 H 0.8516 0.1354 0.2926 0.020 Uiso 1 1 calc R U C16 C 0.82628(15) 0.2273(6) 0.3870(2) 0.0152(7) Uani 1 1 d . . C17 C 0.77302(15) 0.0451(6) 0.3640(2) 0.0152(7) Uani 1 1 d . . H17 H 0.7911 -0.1066 0.3919 0.018 Uiso 1 1 calc R U C18 C 0.84566(17) 0.3396(8) 0.6036(2) 0.0256(8) Uani 1 1 d . . H18A H 0.8713 0.1972 0.6119 0.038 Uiso 1 1 calc R U H18B H 0.8192 0.3272 0.6353 0.038 Uiso 1 1 calc R U H18C H 0.8726 0.4783 0.6217 0.038 Uiso 1 1 calc R U C19 C 0.94266(17) 0.8769(6) 0.5454(2) 0.0240(8) Uani 1 1 d . . H19A H 0.9818 0.7952 0.5542 0.036 Uiso 1 1 calc R U H19B H 0.9467 0.9664 0.5946 0.036 Uiso 1 1 calc R U H19C H 0.9329 0.9853 0.4990 0.036 Uiso 1 1 calc R U C20 C 0.97508(18) 0.6117(7) 0.3021(3) 0.0293(9) Uani 1 1 d . . H20A H 0.9510 0.7578 0.2949 0.044 Uiso 1 1 calc R U H20B H 0.9915 0.5990 0.2588 0.044 Uiso 1 1 calc R U H20C H 1.0096 0.6138 0.3555 0.044 Uiso 1 1 calc R U C21 C 0.74573(15) -0.0030(6) 0.2727(2) 0.0154(7) Uani 1 1 d . . C22 C 0.75814(16) -0.2156(6) 0.2427(2) 0.0181(7) Uani 1 1 d . . H22 H 0.7833 -0.3309 0.2794 0.022 Uiso 1 1 calc R U C23 C 0.73388(17) -0.2605(6) 0.1591(2) 0.0219(8) Uani 1 1 d . . H23 H 0.7430 -0.4055 0.1391 0.026 Uiso 1 1 calc R U C24 C 0.69658(16) -0.0959(7) 0.1051(2) 0.0223(8) Uani 1 1 d . . H24 H 0.6795 -0.1288 0.0481 0.027 Uiso 1 1 calc R U C25 C 0.68412(16) 0.1170(6) 0.1340(2) 0.0190(7) Uani 1 1 d . . H25 H 0.6584 0.2306 0.0970 0.023 Uiso 1 1 calc R U C26 C 0.70934(15) 0.1644(6) 0.2174(2) 0.0159(7) Uani 1 1 d . . H26 H 0.7017 0.3127 0.2369 0.019 Uiso 1 1 calc R U O1 O 0.68886(12) -0.3188(4) 0.39020(15) 0.0232(6) Uani 1 1 d . . O2 O 0.63160(12) -0.0154(5) 0.43464(15) 0.0238(6) Uani 1 1 d . . O3 O 0.93613(11) 0.4153(5) 0.29797(15) 0.0230(6) Uani 1 1 d . . O4 O 0.89397(11) 0.7078(4) 0.52859(15) 0.0227(6) Uani 1 1 d . . S1 S 0.66317(4) -0.08393(14) 0.38177(5) 0.0166(3) 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 0.0160(16) 0.0169(17) 0.0187(17) 0.0027(13) 0.0081(13) -0.0013(13) C2 0.0185(17) 0.0136(16) 0.0252(19) 0.0010(14) 0.0094(15) -0.0005(13) C3 0.0201(18) 0.0202(18) 0.0220(19) -0.0010(14) 0.0076(15) -0.0033(14) C4 0.0156(17) 0.0284(19) 0.0208(18) 0.0072(15) 0.0081(14) -0.0025(14) C5 0.0196(17) 0.0199(17) 0.028(2) 0.0082(15) 0.0137(15) 0.0054(14) C6 0.0191(17) 0.0181(17) 0.0229(18) 0.0009(14) 0.0108(15) 0.0001(14) C7 0.0206(19) 0.042(2) 0.023(2) 0.0049(17) 0.0075(16) -0.0031(17) C8 0.0165(16) 0.0154(16) 0.0132(16) -0.0005(12) 0.0047(13) 0.0002(13) C9 0.0202(17) 0.0201(17) 0.0146(17) 0.0010(13) 0.0075(14) 0.0014(14) C10 0.0150(16) 0.0197(17) 0.0146(16) -0.0019(13) 0.0050(13) 0.0026(13) C11 0.0130(15) 0.0178(17) 0.0141(16) 0.0021(13) 0.0031(13) 0.0055(13) C12 0.0160(16) 0.0196(18) 0.0164(17) -0.0023(13) 0.0023(13) 0.0032(14) C13 0.0115(15) 0.0171(16) 0.0229(18) -0.0031(14) 0.0038(14) -0.0013(13) C14 0.0149(16) 0.0261(19) 0.0149(16) 0.0024(14) 0.0040(13) 0.0042(14) C15 0.0150(16) 0.0172(16) 0.0135(16) -0.0013(13) 0.0017(13) 0.0023(13) C16 0.0145(16) 0.0148(16) 0.0130(16) 0.0025(12) 0.0016(13) 0.0042(13) C17 0.0148(16) 0.0161(17) 0.0137(16) 0.0013(13) 0.0043(13) 0.0029(13) C18 0.0210(18) 0.041(2) 0.0143(17) -0.0016(16) 0.0057(14) 0.0016(16) C19 0.0205(18) 0.0200(18) 0.0260(19) -0.0066(15) 0.0024(15) -0.0010(14) C20 0.028(2) 0.031(2) 0.033(2) -0.0020(17) 0.0160(18) -0.0085(17) C21 0.0125(15) 0.0186(16) 0.0159(16) 0.0000(13) 0.0063(13) -0.0011(13) C22 0.0197(17) 0.0149(16) 0.0217(18) -0.0020(13) 0.0102(14) -0.0027(13) C23 0.0267(19) 0.0185(17) 0.0248(19) -0.0060(15) 0.0147(16) -0.0053(15) C24 0.0220(18) 0.029(2) 0.0168(17) -0.0033(15) 0.0085(15) -0.0071(15) C25 0.0155(16) 0.0240(18) 0.0167(17) 0.0035(14) 0.0050(13) -0.0026(14) C26 0.0155(16) 0.0157(16) 0.0181(17) 0.0010(13) 0.0081(13) -0.0020(13) O1 0.0239(13) 0.0168(13) 0.0257(14) 0.0047(10) 0.0056(11) -0.0003(10) O2 0.0255(13) 0.0287(14) 0.0201(13) 0.0015(11) 0.0121(11) -0.0023(11) O3 0.0205(13) 0.0296(14) 0.0223(13) -0.0056(11) 0.0120(11) -0.0061(11) O4 0.0211(13) 0.0239(13) 0.0219(13) -0.0101(10) 0.0068(11) -0.0041(10) S1 0.0183(4) 0.0148(4) 0.0170(4) 0.0024(3) 0.0072(3) -0.0005(3) 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' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 '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 C6 120.5(3) C2 C1 S1 119.8(3) C6 C1 S1 119.2(3) C1 C2 C3 119.0(3) C1 C2 H2 120.5 C3 C2 H2 120.5 C4 C3 C2 121.4(3) C4 C3 H3 119.3 C2 C3 H3 119.3 C3 C4 C5 118.7(3) C3 C4 C7 121.4(3) C5 C4 C7 119.9(3) C6 C5 C4 120.7(3) C6 C5 H5 119.6 C4 C5 H5 119.6 C5 C6 C1 119.7(3) C5 C6 H6 120.2 C1 C6 H6 120.2 C4 C7 H7A 109.5 C4 C7 H7B 109.5 H7A C7 H7B 109.5 C4 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C9 C8 C17 108.7(3) C9 C8 S1 107.6(2) C17 C8 S1 112.6(2) C9 C8 H8 109.3 C17 C8 H8 109.3 S1 C8 H8 109.3 C10 C9 C8 111.9(3) C10 C9 H9A 109.2 C8 C9 H9A 109.2 C10 C9 H9B 109.2 C8 C9 H9B 109.2 H9A C9 H9B 107.9 C11 C10 C9 112.4(3) C11 C10 C18 115.3(3) C9 C10 C18 106.6(3) C11 C10 H10 107.4 C9 C10 H10 107.4 C18 C10 H10 107.4 C16 C11 C12 116.8(3) C16 C11 C10 122.7(3) C12 C11 C10 120.4(3) O4 C12 C13 121.5(3) O4 C12 C11 115.8(3) C13 C12 C11 122.6(3) C14 C13 C12 118.7(3) C14 C13 H13 120.7 C12 C13 H13 120.7 O3 C14 C15 116.5(3) O3 C14 C13 123.3(3) C15 C14 C13 120.2(3) C14 C15 C16 120.6(3) C14 C15 H15 119.7 C16 C15 H15 119.7 C15 C16 C11 120.9(3) C15 C16 C17 117.6(3) C11 C16 C17 121.5(3) C21 C17 C8 114.0(3) C21 C17 C16 111.7(3) C8 C17 C16 108.7(3) C21 C17 H17 107.4 C8 C17 H17 107.4 C16 C17 H17 107.4 C10 C18 H18A 109.5 C10 C18 H18B 109.5 H18A C18 H18B 109.5 C10 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 O4 C19 H19A 109.5 O4 C19 H19B 109.5 H19A C19 H19B 109.5 O4 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 O3 C20 H20A 109.5 O3 C20 H20B 109.5 H20A C20 H20B 109.5 O3 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 C22 C21 C26 118.6(3) C22 C21 C17 119.9(3) C26 C21 C17 121.5(3) C21 C22 C23 120.4(3) C21 C22 H22 119.8 C23 C22 H22 119.8 C24 C23 C22 120.5(3) C24 C23 H23 119.8 C22 C23 H23 119.8 C23 C24 C25 119.8(3) C23 C24 H24 120.1 C25 C24 H24 120.1 C24 C25 C26 119.9(3) C24 C25 H25 120.1 C26 C25 H25 120.1 C25 C26 C21 120.8(3) C25 C26 H26 119.6 C21 C26 H26 119.6 C14 O3 C20 117.3(3) C12 O4 C19 117.6(3) O1 S1 O2 118.23(16) O1 S1 C1 107.93(15) O2 S1 C1 106.01(15) O1 S1 C8 108.74(15) O2 S1 C8 106.48(15) C1 S1 C8 109.20(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C2 1.386(5) C1 C6 1.391(5) C1 S1 1.765(3) C2 C3 1.392(5) C2 H2 0.9500 C3 C4 1.386(5) C3 H3 0.9500 C4 C5 1.394(5) C4 C7 1.509(5) C5 C6 1.385(5) C5 H5 0.9500 C6 H6 0.9500 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 C9 1.529(4) C8 C17 1.534(4) C8 S1 1.811(3) C8 H8 1.0000 C9 C10 1.527(5) C9 H9A 0.9900 C9 H9B 0.9900 C10 C11 1.522(5) C10 C18 1.543(5) C10 H10 1.0000 C11 C16 1.407(5) C11 C12 1.410(5) C12 O4 1.369(4) C12 C13 1.394(5) C13 C14 1.393(5) C13 H13 0.9500 C14 O3 1.368(4) C14 C15 1.386(5) C15 C16 1.393(5) C15 H15 0.9500 C16 C17 1.543(5) C17 C21 1.518(4) C17 H17 1.0000 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 O4 1.426(4) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 O3 1.418(4) C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 C22 1.390(5) C21 C26 1.394(5) C22 C23 1.391(5) C22 H22 0.9500 C23 C24 1.380(5) C23 H23 0.9500 C24 C25 1.382(5) C24 H24 0.9500 C25 C26 1.392(5) C25 H25 0.9500 C26 H26 0.9500 O1 S1 1.442(3) O2 S1 1.444(3)