#------------------------------------------------------------------------------ #$Date: 2020-06-04 06:54:28 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252640 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157531.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_7157531 loop_ _publ_author_name 'Terashima, Kyu' 'Kawasaki-Takasuka, Tomoko' 'Agou, Tomohiro' 'Kubota, Toshio' 'Yamazaki, Takashi' _publ_section_title ; Construction of quaternary carbon centers with a CF3 group by NHC-catalyzed 1,6-addition of aldehydes to p-quinone methides and their application to construct successively congested stereogenic centers ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D0OB00951B _journal_year 2020 _chemical_formula_moiety 'C23 H21 F3 O4 S' _chemical_formula_sum 'C23 H21 F3 O4 S' _chemical_formula_weight 450.46 _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' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-03-27 deposited with the CCDC. 2020-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.237(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.8943(4) _cell_length_b 9.9889(3) _cell_length_c 15.0537(4) _cell_measurement_reflns_used 14703 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 30.2440 _cell_measurement_theta_min 2.5940 _cell_volume 2062.19(10) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrystalClear-SM Expert ver 2.1' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Yadokari-XG (Wakita, Nemoto, et al., 2019)' _computing_publication_material 'Yadokari-XG (Wakita, Nemoto, et al., 2019)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXTL-2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Pilatus P200' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_unetI/netI 0.0164 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 24059 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.499 _diffrn_reflns_theta_min 2.457 _diffrn_source 'Rigaku VariMax' _exptl_absorpt_coefficient_mu 0.212 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.451 _exptl_crystal_description block _exptl_crystal_F_000 936 _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.256 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.038 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 3833 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0320 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.7299P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.0912 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3453 _reflns_number_total 3833 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00951b2.cif _cod_data_source_block Kyu2 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7157531 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.981 _shelx_estimated_absorpt_t_max 0.987 _oxdiff_exptl_absorpt_empirical_full_min 0.843 _oxdiff_exptl_absorpt_empirical_full_max 1.284 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _shelx_res_file ; Kyu2.res created by SHELXL-2014/7 TITL Kyu2_a.res in P2(1)/n REM Yadorkari-X generated CELL 0.71073 13.8943 9.9889 15.0537 90.0000 99.2370 90.0000 ZERR 4.0 0.0004 0.0003 0.0004 0.0000 0.0030 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H F S O UNIT 92 84 12 4 16 SIZE 0.09 0.08 0.06 TEMP -100.0 L.S. 10 FMAP 2 PLAN -20 ACTA CONF HTAB LIST 4 BOND $H OMIT -10.000000 51.000000 OMIT 1 1 0 EQIV $1 1-X, 1-Y, 1-Z EQIV $2 2-X, 1-Y, 1-Z HTAB O4 O2_$1 HTAB C14 O4_$1 HTAB C15 O1_$2 WGHT 0.049200 0.729900 FVAR 2.54539 S1 4 0.834656 0.562246 0.389729 11.00000 0.02924 0.03839 = 0.03129 0.00363 0.01055 -0.00089 F1 3 0.517488 0.705258 0.728967 11.00000 0.07569 0.02951 = 0.06857 -0.00236 0.03718 0.01232 F2 3 0.503316 0.582485 0.842472 11.00000 0.06975 0.04236 = 0.06105 -0.01237 0.04336 -0.00751 O1 5 0.860145 0.608508 0.492711 11.00000 0.02714 0.03811 = 0.03507 -0.00147 0.00965 -0.00698 F3 3 0.640994 0.674415 0.832161 11.00000 0.07079 0.04694 = 0.06798 -0.02932 0.02534 -0.02409 O2 5 0.742562 0.617735 0.351014 11.00000 0.03980 0.04479 = 0.03717 0.00607 0.00527 0.00559 O3 5 0.920712 0.597703 0.354943 11.00000 0.04117 0.05299 = 0.04606 0.00618 0.02210 -0.00603 O4 5 0.459578 0.497464 0.613626 11.00000 0.02902 0.03527 = 0.07441 0.00193 -0.00548 0.00456 AFIX 147 H1 2 0.404809 0.466311 0.591483 11.00000 -1.50000 AFIX 0 C1 1 0.667015 0.526040 0.673788 11.00000 0.02592 0.02354 = 0.02955 -0.00522 0.00631 -0.00398 C2 1 0.792621 0.580992 0.552039 11.00000 0.02632 0.02852 = 0.02969 -0.00416 0.00783 -0.00538 C3 1 0.524399 0.276739 0.655155 11.00000 0.02478 0.02679 = 0.03293 -0.00226 0.00286 -0.00263 C4 1 0.757271 0.462552 0.679901 11.00000 0.02957 0.03129 = 0.03182 0.00243 0.00462 0.00213 AFIX 43 H2 2 0.776223 0.399813 0.726883 11.00000 -1.20000 AFIX 0 C5 1 0.823047 0.387834 0.395532 11.00000 0.02700 0.03785 = 0.02683 -0.00219 0.01008 0.00000 C6 1 0.595410 0.487061 0.737707 11.00000 0.03116 0.02574 = 0.03491 -0.00425 0.01116 -0.00264 C7 1 0.820200 0.488872 0.618875 11.00000 0.02480 0.03558 = 0.03497 -0.00055 0.00433 0.00327 AFIX 43 H3 2 0.881057 0.443950 0.623395 11.00000 -1.20000 AFIX 0 C8 1 0.705291 0.649847 0.544871 11.00000 0.03254 0.02623 = 0.03304 0.00180 0.00593 0.00056 AFIX 43 H4 2 0.688490 0.715507 0.499370 11.00000 -1.20000 AFIX 0 C9 1 0.642698 0.620983 0.605574 11.00000 0.02785 0.02695 = 0.03594 -0.00247 0.00670 0.00299 AFIX 43 H5 2 0.582110 0.666680 0.600658 11.00000 -1.20000 AFIX 0 C10 1 0.573071 0.257460 0.582301 11.00000 0.03912 0.03310 = 0.03257 -0.00307 0.00707 -0.00656 AFIX 43 H6 2 0.590025 0.332170 0.548947 11.00000 -1.20000 AFIX 0 C11 1 0.502238 0.415791 0.686462 11.00000 0.02564 0.02885 = 0.04634 -0.00427 0.01101 -0.00176 AFIX 13 H7 2 0.454264 0.406899 0.729032 11.00000 -1.20000 AFIX 0 C12 1 0.803972 0.111004 0.402091 11.00000 0.04281 0.03976 = 0.03520 -0.00551 0.01882 -0.00002 C13 1 0.642398 0.393908 0.814381 11.00000 0.03985 0.04054 = 0.03175 0.00142 0.00855 -0.00833 AFIX 137 H8 2 0.698456 0.439015 0.849782 11.00000 -1.50000 H9 2 0.664159 0.311230 0.788705 11.00000 -1.50000 H10 2 0.594414 0.372336 0.853340 11.00000 -1.50000 AFIX 0 C14 1 0.736772 0.328248 0.356020 11.00000 0.02816 0.04539 = 0.03560 -0.00228 0.00368 0.00224 AFIX 43 H11 2 0.684109 0.381196 0.327090 11.00000 -1.20000 AFIX 0 C15 1 0.900624 0.311184 0.437580 11.00000 0.02657 0.04405 = 0.04173 -0.00178 0.00296 0.00082 AFIX 43 H12 2 0.960022 0.352610 0.463666 11.00000 -1.20000 AFIX 0 C16 1 0.497049 0.165314 0.700403 11.00000 0.04211 0.03432 = 0.03815 -0.00179 0.00975 -0.01124 AFIX 43 H13 2 0.461971 0.177015 0.749068 11.00000 -1.20000 AFIX 0 C17 1 0.564052 0.613226 0.783914 11.00000 0.04855 0.03224 = 0.04722 -0.00966 0.02430 -0.00830 C18 1 0.728417 0.190188 0.359319 11.00000 0.03421 0.04733 = 0.04138 -0.00978 0.00693 -0.00696 AFIX 43 H14 2 0.669617 0.148796 0.331666 11.00000 -1.20000 AFIX 0 C19 1 0.571000 0.019579 0.605026 11.00000 0.04726 0.02898 = 0.06200 -0.01291 -0.00241 0.00239 AFIX 43 H15 2 0.588200 -0.067971 0.588546 11.00000 -1.20000 AFIX 0 C20 1 0.520371 0.037082 0.675348 11.00000 0.05226 0.02870 = 0.04782 0.00330 -0.00322 -0.00962 AFIX 43 H16 2 0.501341 -0.038394 0.706789 11.00000 -1.20000 AFIX 0 C21 1 0.890160 0.174162 0.440897 11.00000 0.03658 0.04411 = 0.04250 0.00104 0.00682 0.00817 AFIX 43 H17 2 0.942774 0.121514 0.470247 11.00000 -1.20000 AFIX 0 C22 1 0.596812 0.128808 0.558447 11.00000 0.04852 0.04596 = 0.04659 -0.01778 0.01449 -0.00389 AFIX 43 H18 2 0.631244 0.116089 0.509443 11.00000 -1.20000 AFIX 0 C23 1 0.791810 -0.038244 0.406720 11.00000 0.06277 0.03993 = 0.06773 -0.00680 0.02618 -0.00196 AFIX 137 H19 2 0.729234 -0.058838 0.425759 11.00000 -1.50000 H20 2 0.844987 -0.075904 0.450189 11.00000 -1.50000 H21 2 0.793281 -0.077289 0.347230 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM Kyu2_a.res in P2(1)/n REM R1 = 0.0320 for 3453 Fo > 4sig(Fo) and 0.0352 for all 3833 data REM 283 parameters refined using 0 restraints END WGHT 0.0492 0.7305 REM Instructions for potential hydrogen bonds HTAB O4 O2_$1 HTAB C14 O4_$1 HTAB C15 O1_$2 REM Highest difference peak 0.256, deepest hole -0.354, 1-sigma level 0.038 Q1 1 0.5792 0.5449 0.7553 11.00000 0.05 0.26 Q2 1 0.6262 0.5043 0.7038 11.00000 0.05 0.22 Q3 1 0.4275 0.4399 0.7407 11.00000 0.05 0.22 Q4 1 0.5543 0.4489 0.7082 11.00000 0.05 0.22 Q5 1 0.7185 -0.0726 0.3693 11.00000 0.05 0.21 Q6 1 0.7861 -0.0628 0.4744 11.00000 0.05 0.21 Q7 1 0.8415 -0.0860 0.3874 11.00000 0.05 0.21 Q8 1 0.5231 0.3434 0.6730 11.00000 0.05 0.20 Q9 1 0.8281 0.4641 0.3922 11.00000 0.05 0.19 Q10 1 0.5778 0.4396 0.8775 11.00000 0.05 0.18 Q11 1 0.7576 0.6331 0.5603 11.00000 0.05 0.18 Q12 1 0.7031 0.5387 0.8635 11.00000 0.05 0.17 Q13 1 0.7181 0.5122 0.6867 11.00000 0.05 0.16 Q14 1 0.5265 0.2274 0.6805 11.00000 0.05 0.16 Q15 1 0.5479 0.2698 0.6176 11.00000 0.05 0.16 Q16 1 0.7959 0.5195 0.5772 11.00000 0.05 0.15 Q17 1 0.8545 0.3540 0.4327 11.00000 0.05 0.15 Q18 1 0.7928 0.3616 0.3665 11.00000 0.05 0.14 Q19 1 0.7460 0.2549 0.3395 11.00000 0.05 0.14 Q20 1 0.8400 0.1434 0.4241 11.00000 0.05 0.14 ; _shelx_res_checksum 22262 _shelx_hkl_file ; 0 0 -2 17489.3 415.068 0 0 3-0.31224 10.4054 0 0 3 10.6128 8.16247 0 0 -3 18.1761 7.59930 0 0 4 255793. 6023.60 0 0 -4 256966. 6018.70 0 0 4 254782. 6018.51 0 0 -5 0.35476 10.2238 0 0 5-5.42924 11.2602 0 0 5 8.96888 15.0988 0 0 -6 4129.48 111.896 0 0 6 4343.34 118.780 0 0 6 4438.04 111.686 0 0 -7 11.4489 18.0501 0 0 7-0.73749 18.1345 0 0 -7 14.7233 13.0889 0 0 7 7.48493 12.0134 0 0 -8 972.037 39.7136 0 0 -8 1050.14 47.3059 0 0 8 998.773 39.7380 0 0 8 993.881 46.7705 0 0 -9 26.0802 16.8265 0 0 9 14.0849 21.3173 0 0 -9-9.30861 21.2211 0 0 9 7.24487 15.7223 0 0 -10 41.4119 18.0684 0 0 10 34.5961 22.1247 0 0 -10 37.1956 22.5672 0 0 10 26.1031 17.3536 0 0 -11-1.15109 22.7766 0 0 11-2.31032 22.3043 0 0 -11 0.79786 19.2166 0 0 11 2.23402 19.0157 0 0 -12 491.124 40.4437 0 0 -12 487.326 34.9961 0 0 12 426.920 40.6738 0 0 12 460.186 32.4151 0 0 -13 14.2821 23.9621 0 0 13-10.5343 20.9060 0 0 13-6.95046 29.1267 0 0 -13-11.0397 27.8030 0 0 -14 3419.47 107.627 0 0 14 3195.71 103.931 0 0 14 3101.05 118.410 0 0 -14 3091.31 117.277 0 0 15-1.61375 33.9804 0 0 -15-1.10408 25.9933 0 0 15 29.9890 25.8085 0 0 15 19.1958 31.6430 0 0 16 12.8098 25.8147 0 0 -16 27.4655 27.5294 0 0 16 68.3042 35.7113 0 0 16 17.4925 35.9913 0 0 -17-23.8226 31.8755 0 0 17 22.5183 38.6034 0 0 17 1.72453 37.7562 0 0 -18 3045.13 112.240 0 0 18 3113.89 130.253 0 0 18 3115.44 124.188 0 0 18 2988.93 107.308 0 0 19-7.60074 32.5974 0 0 19-6.43353 47.1624 0 0 -19 28.5400 33.6805 0 -1 1 63612.0 1497.93 0 -1 2 10214.7 245.699 0 -1 3 5936.99 140.055 0 -1 -3 5341.72 133.952 0 -1 3 5906.95 138.663 0 1 3 5410.31 133.732 0 1 -4 40821.0 1000.92 0 -1 4 42073.2 1001.68 0 -1 4 42474.9 1000.40 0 -1 -4 43252.5 995.603 0 1 4 41529.4 995.180 0 1 -5 10884.6 276.573 0 -1 -5 11257.4 271.206 0 1 5 11486.9 270.786 0 -1 5 11143.7 275.896 0 -1 5 10997.8 276.306 0 -1 5 11039.8 278.558 0 -1 6 2855.21 87.5810 0 -1 -6 2772.18 79.0209 0 1 -6 3083.68 87.7359 0 1 6 2922.37 78.8205 0 1 -6 3000.40 85.6571 0 -1 6 3095.80 84.8298 0 -1 7 11783.9 273.820 0 1 -7 11115.8 277.474 0 1 7 10959.8 267.358 0 1 -7 11340.4 274.097 0 -1 7 11355.8 278.822 0 -1 8 4176.41 121.084 0 1 -8 4352.79 116.207 0 -1 8 4224.57 115.058 0 -1 -8 3927.30 109.389 0 1 8 3658.04 119.188 0 1 -8 4221.89 120.255 0 1 8 3884.73 108.382 0 1 9 13987.4 351.796 0 -1 9 13665.8 341.326 0 -1 9 13927.6 350.217 0 -1 -9 13418.0 337.642 0 1 -9 13687.3 342.342 0 1 9 14022.6 336.563 0 -1 10 1753.57 70.8187 0 1 -10 1789.50 64.9918 0 -1 10 1678.77 67.2791 0 -1 10 1764.32 63.6711 0 -1 -10 1775.87 71.2643 0 1 10 1801.87 58.8092 0 -1 -10 1776.26 60.5632 0 1 10 1742.64 71.7991 0 -1 11 689.355 39.5696 0 1 11 738.623 46.4527 0 -1 -11 760.699 36.4776 0 -1 -11 738.447 46.1603 0 1 11 754.453 35.3522 0 1 -11 734.700 40.3135 0 -1 11 713.061 42.1260 0 -1 11 669.654 45.5329 0 -1 -12 537.044 33.6978 0 -1 12 440.206 33.8108 0 1 12 511.727 31.5955 0 1 -12 496.688 36.6522 0 -1 12 492.257 41.6550 0 1 12 514.805 43.4497 0 -1 12 551.829 40.6552 0 -1 -12 521.474 41.9614 0 -1 13 2468.96 93.6817 0 -1 13 2428.94 86.4386 0 -1 -13 2541.36 83.8867 0 1 13 2520.84 98.2941 0 1 -13 2387.92 88.4889 0 -1 -13 2491.36 97.7399 0 -1 13 2331.54 96.0955 0 1 13 2422.22 81.1124 0 -1 -14 1074.82 51.5487 0 -1 14 1107.16 55.4258 0 1 14 991.850 62.4776 0 1 14 1054.25 49.6075 0 -1 -14 1029.22 62.8876 0 1 -14 1055.33 56.2481 0 -1 14 1112.45 63.9319 0 -1 14 1022.48 60.8416 0 -1 -15 702.260 43.1353 0 -1 15 626.798 53.2386 0 -1 15 649.800 50.8922 0 1 15 606.296 53.2104 0 -1 15 569.173 43.2636 0 -1 -15 654.911 55.3415 0 1 15 679.480 40.7140 0 1 -15 659.764 46.1673 0 -1 16 384.370 51.1253 0 -1 16 460.992 40.7631 0 -1 -16 402.833 37.4045 0 1 16 359.433 48.9107 0 -1 16 459.147 47.6891 0 1 16 417.216 36.6535 0 1 -16 515.735 42.0893 0 -1 -16 440.631 49.4477 0 -1 -17 2673.51 96.0649 0 -1 17 2560.44 112.081 0 1 17 2618.25 113.880 0 -1 17 2740.66 109.275 0 1 17 2528.43 91.4843 0 1 -17 2437.64 98.1339 0 -1 -18-13.4839 28.1742 0 1 18-3.73696 41.7589 0 1 -18-5.75957 31.2393 0 -1 18 30.2763 43.1069 0 1 18 6.46532 28.5299 0 1 18 2.03752 45.9288 0 -1 18 15.8264 43.5717 0 -1 19 278.672 40.1934 0 1 19 300.151 38.6523 0 1 -19 341.971 46.5806 0 -1 -19 321.353 39.2667 0 -1 19 347.792 57.2973 0 1 -20 171.556 45.0271 0 -1 20 184.964 41.8203 0 2 0 102163. 2348.87 0 -2 0 102733. 2350.16 0 2 1 1791.20 54.0202 0 -2 1 1905.15 53.5227 0 -2 -1 1995.52 54.9569 0 2 -1 1863.14 53.7482 0 -2 1 2092.40 52.9658 0 2 1 2025.70 49.6643 0 2 -1 2002.90 53.0979 0 2 -2 1278.62 36.5540 0 -2 2 1245.24 36.1323 0 -2 2 1252.90 38.0087 0 2 -3 206.189 13.4153 0 -2 3 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0 -4-18.0329 22.4378 -17 0 4 12.6690 28.9849 -17 0 3 1984.15 80.6883 17 0 -3 1943.53 79.3250 17 0 -2 28.1281 27.1372 -17 0 2-1.78565 37.9058 -17 0 2 34.9702 39.5684 -17 0 2 20.8983 29.2754 -17 0 1 896.934 68.9801 -17 0 1 789.987 50.5980 -17 0 1 734.907 59.5690 17 0 -1 765.951 49.0853 17 0 0 6.84749 34.1214 -17 0 0 24.5599 27.3839 17 0 0-8.55747 27.9413 -17 0 0-1.77713 37.8419 -17 0 -1 1293.85 62.9316 17 0 1 1347.57 75.0029 17 0 2-25.7171 39.4104 17 0 3 1411.33 80.0078 -17 1 13 400.832 59.3125 -17 1 12 2103.84 106.087 -17 1 12 1856.74 89.6966 -17 -1 11 37.3563 40.4633 -17 1 11 17.1690 39.6492 -17 -1 11 24.4105 41.4245 -17 1 11 44.5506 36.9530 -17 -1 10 408.684 55.4397 -17 1 10 397.965 51.1926 -17 1 10 348.673 42.1053 -17 -1 10 360.149 47.5959 -17 1 9 308.039 48.6934 -17 1 9 329.661 53.2449 -17 -1 9 243.205 45.8812 -17 1 9 306.860 42.1995 17 1 -8 3410.07 129.995 -17 1 8 3914.57 135.345 -17 1 8 3782.35 146.062 -17 -1 8 3738.56 144.007 -17 -1 8 3603.52 130.590 -17 1 8 3668.55 124.498 17 1 -7 7.24168 31.3263 -17 1 7 1.54426 36.1644 -17 1 7-8.03229 41.3797 -17 -1 7 20.4427 41.5505 -17 -1 7 9.56096 34.4908 -17 1 7-4.74739 28.5855 17 1 -6 64.1601 33.2831 -17 1 6 90.5740 34.2807 -17 1 6 39.5621 41.0580 -17 1 6 79.2177 40.2609 -17 -1 6 18.7123 33.8528 -17 1 6 48.2138 30.0783 17 -1 -5 596.812 45.3945 -17 1 5 637.941 61.5112 -17 -1 5 594.622 49.7580 -17 1 5 651.003 45.5185 17 1 -5 608.529 50.1832 -17 1 5 662.531 57.7629 17 -1 -4 2683.13 95.5024 -17 -1 4 2655.96 110.860 -17 1 4 2770.78 117.925 -17 -1 4 2368.28 112.925 -17 1 4 2709.25 94.9664 -17 -1 4 2623.84 100.258 -17 1 4 2828.16 112.804 17 1 -4 2691.01 102.306 -17 1 3 135.369 41.2110 -17 -1 3 130.910 42.0928 -17 -1 3 180.295 42.2129 -17 1 3 135.803 32.1960 -17 -1 3 181.912 37.1620 17 1 -3 162.009 32.5625 -17 1 2 563.965 41.4426 -17 -1 2 610.902 49.0230 17 1 -2 691.575 48.1607 -17 -1 2 701.650 57.6814 17 -1 -2 591.206 41.1274 -17 -1 1 14.3123 38.3102 -17 -1 1 24.4747 37.8640 -17 -1 1 9.86236 28.9531 -17 -1 0 228.030 42.9685 -17 -1 0 214.614 48.9973 -17 -1 0 233.498 36.4835 17 -1 1 64.5503 35.9083 -17 -1 -1 99.7760 31.8776 17 1 1 130.807 29.4232 -17 -1 -2 303.643 40.3758 17 1 2 305.822 43.9337 17 -1 2 336.307 46.8264 17 1 2 365.537 37.8821 17 1 3 104.292 40.1660 17 2 -10 33.6739 39.3828 -17 2 10 1.76021 39.1710 -17 -2 10 16.4784 35.7532 17 2 -9 896.254 64.5247 -17 2 9 1014.38 67.3566 -17 2 9 993.124 74.3765 -17 -2 9 913.345 63.6087 17 2 -8 74.6735 40.7016 -17 2 8 83.2910 36.3308 -17 2 8 82.0285 45.7004 -17 -2 8 50.3941 36.9544 -17 2 7 1038.23 60.8142 -17 2 7 1034.66 73.5164 -17 -2 7 979.254 62.4546 17 2 -7 980.788 65.9358 17 2 -6 46.3883 35.0109 -17 2 6 44.8184 32.9174 -17 2 6 22.2597 42.5458 -17 -2 6 10.2473 40.1097 -17 -2 6 24.3614 37.5571 17 2 -5 1.49377 32.5582 -17 2 5 32.3961 42.2168 -17 2 5 36.9386 37.9293 -17 -2 5 6.36214 39.7454 -17 -2 5 4.18220 33.8682 -17 2 4 69.2213 36.6245 -17 -2 4 121.018 45.5501 -17 -2 4 101.964 39.5960 -17 -2 4 81.4591 39.2801 17 2 -4 50.7599 32.1877 -17 -2 3 1191.17 72.9780 -17 -2 3 1181.34 77.0471 -17 -2 3 1161.79 66.8787 -17 2 3 1186.40 73.8170 17 2 -3 1138.43 64.9561 -17 -2 2 243.436 47.7987 -17 -2 2 230.556 45.3001 -17 -2 2 214.992 42.5473 17 -2 -2 254.837 43.0379 17 2 -2 199.765 37.5098 -17 2 2 264.254 44.3081 -17 -2 1 10.2493 39.7322 -17 -2 1-1.81061 34.7570 -17 -2 1-8.08902 33.3061 17 -2 -1 32.5579 37.1200 17 2 -1-17.8163 33.4557 -17 -2 0 41.1246 40.6467 -17 -2 0-4.05682 40.3576 -17 -2 0 1.39513 33.4773 -17 -2 -1 130.658 45.6319 -17 -2 -1 162.900 35.9718 -17 -2 -2 49.3883 46.1433 -17 -2 -2 61.8673 33.7653 -17 -2 -3 17.6751 30.3029 17 2 3 14.4070 28.2870 -17 -2 -4 274.162 40.5873 17 2 4 374.226 39.8391 17 3 -10 174.580 47.0445 17 3 -9 257.410 45.6520 17 3 -8 200.193 42.9701 -17 3 8 227.374 50.2092 -17 -3 8 167.205 43.5054 -17 3 7 142.019 48.2609 -17 -3 7 108.957 39.2982 -17 3 6 157.035 48.7661 -17 -3 6 219.513 47.0839 -17 -3 6 179.447 43.7476 -17 3 5 42.9028 46.9143 -17 -3 5 69.6050 42.2103 -17 -3 5 60.9053 37.5989 17 3 -5 64.4936 35.4875 -17 3 4 20.6050 42.6053 -17 -3 4-2.08051 44.0918 -17 -3 4-18.2745 39.5278 17 3 -4 53.7070 35.9602 17 -3 -3 465.109 52.9695 -17 -3 3 478.762 57.6916 -17 -3 3 447.559 50.9057 17 3 -3 449.651 50.6051 -17 -3 2 70.8335 45.1272 -17 -3 2 53.6439 38.6246 17 -3 -2 51.6696 38.5243 17 3 -2 90.0602 39.1388 -17 -3 1 69.1366 44.5559 -17 -3 1 82.9128 40.9647 17 3 -1 60.1768 36.5930 17 -3 -1 62.5516 38.5695 -17 -3 0 145.561 48.2017 -17 -3 0 193.270 43.9391 17 -3 0 165.296 42.9610 17 3 0 191.730 41.1446 -17 -3 -1 235.887 50.0310 -17 -3 -1 183.346 41.8694 17 3 1 180.738 38.7890 -17 -3 -2 142.102 49.8598 -17 -3 -2 110.831 42.5162 17 3 2 88.6368 37.0687 -17 -3 -3 139.810 48.4686 -17 -3 -3 128.932 39.2120 17 3 3 165.434 37.6698 -17 -3 -4 54.9398 49.3120 -17 -3 -4 6.64612 37.7709 17 3 4-16.0290 35.8722 17 4 -8 102.199 43.3742 -17 4 8 78.3333 43.1206 17 4 -7 719.885 62.4007 -17 4 6 228.143 50.2755 -17 -4 6 233.134 48.1112 17 4 -6 308.148 47.8873 -17 4 5 831.401 69.0492 -17 -4 5 956.608 68.7440 17 4 -5 813.491 63.2113 -17 -4 4 14.3607 44.2425 17 -4 -4 45.4045 41.5423 -17 -4 4 35.1524 42.3246 -17 -4 3 2034.14 100.204 -17 -4 3 2076.36 95.3006 17 -4 -3 1848.00 91.4780 17 4 -3 1963.36 94.1482 17 -4 -2 8.94571 39.7554 -17 -4 2 8.37302 44.0757 -17 -4 2-19.5900 40.9446 17 4 -2 40.6549 39.6507 -17 -4 1-12.2205 42.0416 -17 -4 1 3.22860 37.4556 17 4 -1 14.7232 39.7418 -17 -4 0 261.353 50.1069 -17 -4 0 294.860 49.9137 17 4 0 308.682 44.0131 -17 -4 -1 415.937 57.7205 -17 -4 -1 495.111 54.7159 17 4 1 480.593 52.5301 -17 -4 -2 23.3503 44.0595 -17 -4 -2 57.8969 41.4205 -17 -4 -3 85.5123 45.4107 -17 -4 -3 20.9867 38.0195 -17 -4 -4 854.621 65.9459 17 4 4 923.104 65.0797 17 4 5 44.4633 39.6768 17 5 -5 500.292 59.7496 17 5 -4 201.170 49.5333 17 5 -3 25.3028 40.0463 17 5 -2 23.0351 43.2591 -17 -5 1 2606.62 118.461 17 5 -1 2674.68 113.396 17 5 0 397.738 53.5542 -17 -5 -1 236.517 51.2054 17 5 2 102.733 42.9319 -18 0 11-22.8561 45.5627 -18 0 10 49.3917 44.7385 -18 0 9-24.7750 40.4522 -18 0 9 33.7449 38.0399 -18 0 8 92.9689 42.3346 -18 0 8 68.6066 29.4884 18 0 -7 9.98783 34.2373 -18 0 7-10.7163 34.4316 18 0 -6 492.292 43.0433 -18 0 6 442.048 45.2523 -18 0 5 2.51931 31.1561 -18 -1 10 509.294 60.7476 -18 -1 9 119.395 40.2571 -18 -1 8 601.652 54.9777 18 1 -7 47.5027 37.0686 -18 -1 7 66.6740 36.4194 -18 -1 6 51.4425 34.0845 18 1 -5 258.287 39.7579 -18 -1 5 309.231 45.2302 18 1 -4 206.836 35.8884 -18 -1 4 199.974 37.8534 -18 -1 3 180.425 39.1991 18 1 -3 233.976 34.6942 -18 -1 2 60.9078 31.3608 18 2 -9 59.1960 42.0865 18 2 -8 478.527 51.7088 -18 -2 8 458.550 53.6475 18 2 -7 294.627 48.5312 -18 -2 7 248.654 46.6841 18 2 -6-16.1983 36.9761 -18 -2 6 7.46595 35.8296 -18 -2 5 7.49137 36.3542 -18 -2 4 179.619 43.0567 -18 -2 3 218.552 41.6923 18 2 -3 310.858 41.8865 -18 -2 2 1.42895 31.4256 18 2 -2-5.84016 34.4156 -18 -2 1-1.46224 34.6012 18 2 -1-4.22429 34.9095 -18 -2 0 240.567 38.9082 18 2 0 213.877 38.4199 18 3 -8 723.653 62.2686 18 3 -7 457.012 52.4904 -18 -3 6 585.816 56.9738 18 3 -6 698.074 59.2424 -18 -3 5-1.61725 37.5239 18 3 -5 3.37133 40.8505 -18 -3 4 14.8959 40.8407 18 3 -4-3.26802 38.0649 -18 -3 3-4.75823 40.3672 -18 -3 2 1583.22 84.7061 18 3 -2 1653.86 82.8707 -18 -3 1 164.765 45.2212 18 3 -1 129.979 41.8575 -18 -3 0 723.185 62.2377 -18 -3 -1 933.447 66.1986 18 3 1 893.809 62.5206 18 4 -5 10.8446 40.3372 18 4 -4 5.37241 36.7145 18 4 -3 48.4574 41.3343 -18 -4 2 294.213 49.6118 18 4 -2 330.022 48.9343 -18 -4 1 705.116 63.7781 18 4 -1 720.381 63.3829 18 4 1 163.817 42.1965 18 4 2 33.2975 41.7633 19 3 -5 235.624 50.5386 19 3 -4 25.7121 38.9167 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 84425 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.83466(3) 0.56225(4) 0.38973(2) 0.03235(12) Uani 1 1 d . . . . . F1 F 0.51749(8) 0.70526(10) 0.72897(8) 0.0551(3) Uani 1 1 d . . . . . F2 F 0.50332(8) 0.58248(10) 0.84247(7) 0.0541(3) Uani 1 1 d . . . . . O1 O 0.86014(7) 0.60851(10) 0.49271(7) 0.0329(2) Uani 1 1 d . . . . . F3 F 0.64099(9) 0.67441(11) 0.83216(8) 0.0603(3) Uani 1 1 d . . . . . O2 O 0.74256(8) 0.61773(12) 0.35101(7) 0.0407(3) Uani 1 1 d . . . . . O3 O 0.92071(8) 0.59770(13) 0.35494(8) 0.0451(3) Uani 1 1 d . . . . . O4 O 0.45958(8) 0.49746(11) 0.61363(9) 0.0477(3) Uani 1 1 d . . . . . H1 H 0.4048 0.4663 0.5915 0.072 Uiso 1 1 calc R U . . . C1 C 0.66701(10) 0.52604(13) 0.67379(9) 0.0261(3) Uani 1 1 d . . . . . C2 C 0.79262(10) 0.58099(14) 0.55204(9) 0.0278(3) Uani 1 1 d . . . . . C3 C 0.52440(10) 0.27674(14) 0.65515(9) 0.0284(3) Uani 1 1 d . . . . . C4 C 0.75727(10) 0.46255(14) 0.67990(10) 0.0309(3) Uani 1 1 d . . . . . H2 H 0.7762 0.3998 0.7269 0.037 Uiso 1 1 calc R U . . . C5 C 0.82305(10) 0.38783(15) 0.39553(9) 0.0299(3) Uani 1 1 d . . . . . C6 C 0.59541(10) 0.48706(14) 0.73771(10) 0.0300(3) Uani 1 1 d . . . . . C7 C 0.82020(10) 0.48887(15) 0.61888(10) 0.0318(3) Uani 1 1 d . . . . . H3 H 0.8811 0.4440 0.6234 0.038 Uiso 1 1 calc R U . . . C8 C 0.70529(10) 0.64985(14) 0.54487(10) 0.0305(3) Uani 1 1 d . . . . . H4 H 0.6885 0.7155 0.4994 0.037 Uiso 1 1 calc R U . . . C9 C 0.64270(10) 0.62098(14) 0.60557(10) 0.0301(3) Uani 1 1 d . . . . . H5 H 0.5821 0.6667 0.6007 0.036 Uiso 1 1 calc R U . . . C10 C 0.57307(11) 0.25746(15) 0.58230(10) 0.0348(3) Uani 1 1 d . . . . . H6 H 0.5900 0.3322 0.5489 0.042 Uiso 1 1 calc R U . . . C11 C 0.50224(10) 0.41579(15) 0.68646(11) 0.0330(3) Uani 1 1 d . . . . . H7 H 0.4543 0.4069 0.7290 0.040 Uiso 1 1 calc R U . . . C12 C 0.80397(12) 0.11100(16) 0.40209(10) 0.0379(3) Uani 1 1 d . . . . . C13 C 0.64240(11) 0.39391(16) 0.81438(10) 0.0371(3) Uani 1 1 d . . . . . H8 H 0.6985 0.4390 0.8498 0.056 Uiso 1 1 calc R U . . . H9 H 0.6642 0.3112 0.7887 0.056 Uiso 1 1 calc R U . . . H10 H 0.5944 0.3723 0.8533 0.056 Uiso 1 1 calc R U . . . C14 C 0.73677(11) 0.32825(17) 0.35602(10) 0.0365(3) Uani 1 1 d . . . . . H11 H 0.6841 0.3812 0.3271 0.044 Uiso 1 1 calc R U . . . C15 C 0.90062(11) 0.31118(17) 0.43758(11) 0.0377(3) Uani 1 1 d . . . . . H12 H 0.9600 0.3526 0.4637 0.045 Uiso 1 1 calc R U . . . C16 C 0.49705(12) 0.16531(16) 0.70040(11) 0.0378(3) Uani 1 1 d . . . . . H13 H 0.4620 0.1770 0.7491 0.045 Uiso 1 1 calc R U . . . C17 C 0.56405(12) 0.61323(16) 0.78391(11) 0.0408(4) Uani 1 1 d . . . . . C18 C 0.72842(12) 0.19019(17) 0.35932(11) 0.0409(4) Uani 1 1 d . . . . . H14 H 0.6696 0.1488 0.3317 0.049 Uiso 1 1 calc R U . . . C19 C 0.57100(13) 0.01958(17) 0.60503(13) 0.0473(4) Uani 1 1 d . . . . . H15 H 0.5882 -0.0680 0.5885 0.057 Uiso 1 1 calc R U . . . C20 C 0.52037(13) 0.03708(16) 0.67535(12) 0.0442(4) Uani 1 1 d . . . . . H16 H 0.5013 -0.0384 0.7068 0.053 Uiso 1 1 calc R U . . . C21 C 0.89016(12) 0.17416(17) 0.44090(11) 0.0410(4) Uani 1 1 d . . . . . H17 H 0.9428 0.1215 0.4702 0.049 Uiso 1 1 calc R U . . . C22 C 0.59681(13) 0.12881(18) 0.55845(12) 0.0463(4) Uani 1 1 d . . . . . H18 H 0.6312 0.1161 0.5094 0.056 Uiso 1 1 calc R U . . . C23 C 0.79181(15) -0.03824(18) 0.40672(15) 0.0551(5) Uani 1 1 d . . . . . H19 H 0.7292 -0.0588 0.4258 0.083 Uiso 1 1 calc R U . . . H20 H 0.8450 -0.0759 0.4502 0.083 Uiso 1 1 calc R U . . . H21 H 0.7933 -0.0773 0.3472 0.083 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0292(2) 0.0384(2) 0.0313(2) 0.00363(15) 0.01055(14) -0.00089(14) F1 0.0757(7) 0.0295(5) 0.0686(7) -0.0024(5) 0.0372(6) 0.0123(5) F2 0.0697(7) 0.0424(5) 0.0610(6) -0.0124(5) 0.0434(5) -0.0075(5) O1 0.0271(5) 0.0381(6) 0.0351(5) -0.0015(4) 0.0097(4) -0.0070(4) F3 0.0708(7) 0.0469(6) 0.0680(7) -0.0293(5) 0.0253(6) -0.0241(5) O2 0.0398(6) 0.0448(6) 0.0372(6) 0.0061(5) 0.0053(5) 0.0056(5) O3 0.0412(6) 0.0530(7) 0.0461(6) 0.0062(5) 0.0221(5) -0.0060(5) O4 0.0290(6) 0.0353(6) 0.0744(8) 0.0019(6) -0.0055(5) 0.0046(5) C1 0.0259(7) 0.0235(6) 0.0295(7) -0.0052(5) 0.0063(5) -0.0040(5) C2 0.0263(7) 0.0285(7) 0.0297(7) -0.0042(5) 0.0078(5) -0.0054(5) C3 0.0248(6) 0.0268(7) 0.0329(7) -0.0023(6) 0.0029(5) -0.0026(5) C4 0.0296(7) 0.0313(7) 0.0318(7) 0.0024(6) 0.0046(5) 0.0021(6) C5 0.0270(7) 0.0378(8) 0.0268(7) -0.0022(6) 0.0101(5) 0.0000(6) C6 0.0312(7) 0.0257(7) 0.0349(7) -0.0043(6) 0.0112(6) -0.0026(6) C7 0.0248(7) 0.0356(8) 0.0350(7) -0.0006(6) 0.0043(6) 0.0033(6) C8 0.0325(7) 0.0262(7) 0.0330(7) 0.0018(6) 0.0059(6) 0.0006(6) C9 0.0278(7) 0.0270(7) 0.0359(7) -0.0025(6) 0.0067(6) 0.0030(5) C10 0.0391(8) 0.0331(8) 0.0326(7) -0.0031(6) 0.0071(6) -0.0066(6) C11 0.0256(7) 0.0288(7) 0.0463(8) -0.0043(6) 0.0110(6) -0.0018(6) C12 0.0428(8) 0.0398(8) 0.0352(8) -0.0055(6) 0.0188(7) 0.0000(7) C13 0.0398(8) 0.0405(8) 0.0318(7) 0.0014(6) 0.0086(6) -0.0083(7) C14 0.0282(7) 0.0454(9) 0.0356(8) -0.0023(7) 0.0037(6) 0.0022(6) C15 0.0266(7) 0.0440(9) 0.0417(8) -0.0018(7) 0.0030(6) 0.0008(6) C16 0.0421(8) 0.0343(8) 0.0382(8) -0.0018(6) 0.0097(6) -0.0112(7) C17 0.0485(9) 0.0322(8) 0.0472(9) -0.0097(7) 0.0243(7) -0.0083(7) C18 0.0342(8) 0.0473(9) 0.0414(8) -0.0098(7) 0.0069(6) -0.0070(7) C19 0.0473(10) 0.0290(8) 0.0620(11) -0.0129(8) -0.0024(8) 0.0024(7) C20 0.0523(10) 0.0287(8) 0.0478(9) 0.0033(7) -0.0032(8) -0.0096(7) C21 0.0366(8) 0.0441(9) 0.0425(9) 0.0010(7) 0.0068(6) 0.0082(7) C22 0.0485(9) 0.0460(10) 0.0466(9) -0.0178(8) 0.0145(7) -0.0039(8) C23 0.0628(12) 0.0399(10) 0.0677(12) -0.0068(9) 0.0262(10) -0.0020(8) 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 S1 O2 120.18(7) . . ? O3 S1 O1 102.46(6) . . ? O2 S1 O1 109.09(6) . . ? O3 S1 C5 110.77(7) . . ? O2 S1 C5 108.79(7) . . ? O1 S1 C5 104.26(6) . . ? C2 O1 S1 119.10(8) . . ? C11 O4 H1 109.5 . . ? C4 C1 C9 117.73(13) . . ? C4 C1 C6 120.50(12) . . ? C9 C1 C6 121.71(12) . . ? C7 C2 C8 121.92(13) . . ? C7 C2 O1 117.09(12) . . ? C8 C2 O1 120.90(12) . . ? C16 C3 C10 118.78(14) . . ? C16 C3 C11 119.80(13) . . ? C10 C3 C11 121.41(13) . . ? C7 C4 C1 121.61(13) . . ? C7 C4 H2 119.2 . . ? C1 C4 H2 119.2 . . ? C14 C5 C15 120.92(15) . . ? C14 C5 S1 119.09(11) . . ? C15 C5 S1 119.97(11) . . ? C17 C6 C1 109.51(11) . . ? C17 C6 C13 105.82(12) . . ? C1 C6 C13 112.41(12) . . ? C17 C6 C11 108.88(12) . . ? C1 C6 C11 111.87(11) . . ? C13 C6 C11 108.12(12) . . ? C2 C7 C4 118.68(13) . . ? C2 C7 H3 120.7 . . ? C4 C7 H3 120.7 . . ? C2 C8 C9 118.64(13) . . ? C2 C8 H4 120.7 . . ? C9 C8 H4 120.7 . . ? C8 C9 C1 121.38(13) . . ? C8 C9 H5 119.3 . . ? C1 C9 H5 119.3 . . ? C22 C10 C3 119.86(14) . . ? C22 C10 H6 120.1 . . ? C3 C10 H6 120.1 . . ? O4 C11 C3 111.58(13) . . ? O4 C11 C6 109.21(12) . . ? C3 C11 C6 112.13(11) . . ? O4 C11 H7 107.9 . . ? C3 C11 H7 107.9 . . ? C6 C11 H7 107.9 . . ? C18 C12 C21 118.09(15) . . ? C18 C12 C23 120.30(16) . . ? C21 C12 C23 121.60(16) . . ? C6 C13 H8 109.5 . . ? C6 C13 H9 109.5 . . ? H8 C13 H9 109.5 . . ? C6 C13 H10 109.5 . . ? H8 C13 H10 109.5 . . ? H9 C13 H10 109.5 . . ? C5 C14 C18 118.97(14) . . ? C5 C14 H11 120.5 . . ? C18 C14 H11 120.5 . . ? C21 C15 C5 119.03(14) . . ? C21 C15 H12 120.5 . . ? C5 C15 H12 120.5 . . ? C20 C16 C3 120.78(15) . . ? C20 C16 H13 119.6 . . ? C3 C16 H13 119.6 . . ? F1 C17 F3 106.70(13) . . ? F1 C17 F2 105.67(13) . . ? F3 C17 F2 106.13(13) . . ? F1 C17 C6 115.44(13) . . ? F3 C17 C6 111.11(13) . . ? F2 C17 C6 111.20(12) . . ? C14 C18 C12 121.50(15) . . ? C14 C18 H14 119.2 . . ? C12 C18 H14 119.2 . . ? C20 C19 C22 119.99(15) . . ? C20 C19 H15 120.0 . . ? C22 C19 H15 120.0 . . ? C19 C20 C16 119.85(16) . . ? C19 C20 H16 120.1 . . ? C16 C20 H16 120.1 . . ? C15 C21 C12 121.47(15) . . ? C15 C21 H17 119.3 . . ? C12 C21 H17 119.3 . . ? C19 C22 C10 120.68(16) . . ? C19 C22 H18 119.7 . . ? C10 C22 H18 119.7 . . ? C12 C23 H19 109.5 . . ? C12 C23 H20 109.5 . . ? H19 C23 H20 109.5 . . ? C12 C23 H21 109.5 . . ? H19 C23 H21 109.5 . . ? H20 C23 H21 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O3 1.4249(11) . ? S1 O2 1.4300(11) . ? S1 O1 1.6019(11) . ? S1 C5 1.7531(16) . ? F1 C17 1.333(2) . ? F2 C17 1.3499(18) . ? O1 C2 1.4221(16) . ? F3 C17 1.340(2) . ? O4 C11 1.4179(19) . ? O4 H1 0.8400 . ? C1 C4 1.395(2) . ? C1 C9 1.399(2) . ? C1 C6 1.5410(19) . ? C2 C7 1.372(2) . ? C2 C8 1.384(2) . ? C3 C16 1.389(2) . ? C3 C10 1.391(2) . ? C3 C11 1.5142(19) . ? C4 C7 1.391(2) . ? C4 H2 0.9500 . ? C5 C14 1.384(2) . ? C5 C15 1.389(2) . ? C6 C17 1.536(2) . ? C6 C13 1.543(2) . ? C6 C11 1.5675(19) . ? C7 H3 0.9500 . ? C8 C9 1.389(2) . ? C8 H4 0.9500 . ? C9 H5 0.9500 . ? C10 C22 1.388(2) . ? C10 H6 0.9500 . ? C11 H7 1.0000 . ? C12 C18 1.388(2) . ? C12 C21 1.396(2) . ? C12 C23 1.503(2) . ? C13 H8 0.9800 . ? C13 H9 0.9800 . ? C13 H10 0.9800 . ? C14 C18 1.386(2) . ? C14 H11 0.9500 . ? C15 C21 1.378(2) . ? C15 H12 0.9500 . ? C16 C20 1.388(2) . ? C16 H13 0.9500 . ? C18 H14 0.9500 . ? C19 C20 1.373(3) . ? C19 C22 1.375(3) . ? C19 H15 0.9500 . ? C20 H16 0.9500 . ? C21 H17 0.9500 . ? C22 H18 0.9500 . ? C23 H19 0.9800 . ? C23 H20 0.9800 . ? C23 H21 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H1 O2 0.84 2.49 3.1584(17) 136.8 3_666 C14 H11 O4 0.95 2.61 3.3291(19) 132.6 3_666 C15 H12 O1 0.95 2.51 3.4167(17) 159.7 3_766 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O1 C2 -175.92(10) . . . . ? O2 S1 O1 C2 55.68(12) . . . . ? C5 S1 O1 C2 -60.39(11) . . . . ? S1 O1 C2 C7 111.66(12) . . . . ? S1 O1 C2 C8 -71.59(15) . . . . ? C9 C1 C4 C7 -2.0(2) . . . . ? C6 C1 C4 C7 175.24(13) . . . . ? O3 S1 C5 C14 -127.41(12) . . . . ? O2 S1 C5 C14 6.76(13) . . . . ? O1 S1 C5 C14 123.05(11) . . . . ? O3 S1 C5 C15 51.13(14) . . . . ? O2 S1 C5 C15 -174.69(11) . . . . ? O1 S1 C5 C15 -58.41(13) . . . . ? C4 C1 C6 C17 127.19(14) . . . . ? C9 C1 C6 C17 -55.69(17) . . . . ? C4 C1 C6 C13 9.87(18) . . . . ? C9 C1 C6 C13 -173.01(12) . . . . ? C4 C1 C6 C11 -112.00(14) . . . . ? C9 C1 C6 C11 65.12(16) . . . . ? C8 C2 C7 C4 1.3(2) . . . . ? O1 C2 C7 C4 178.00(12) . . . . ? C1 C4 C7 C2 0.9(2) . . . . ? C7 C2 C8 C9 -2.2(2) . . . . ? O1 C2 C8 C9 -178.78(12) . . . . ? C2 C8 C9 C1 1.0(2) . . . . ? C4 C1 C9 C8 1.1(2) . . . . ? C6 C1 C9 C8 -176.14(12) . . . . ? C16 C3 C10 C22 -2.6(2) . . . . ? C11 C3 C10 C22 176.54(14) . . . . ? C16 C3 C11 O4 -132.39(14) . . . . ? C10 C3 C11 O4 48.50(18) . . . . ? C16 C3 C11 C6 104.75(15) . . . . ? C10 C3 C11 C6 -74.37(17) . . . . ? C17 C6 C11 O4 67.49(15) . . . . ? C1 C6 C11 O4 -53.68(15) . . . . ? C13 C6 C11 O4 -177.98(12) . . . . ? C17 C6 C11 C3 -168.32(12) . . . . ? C1 C6 C11 C3 70.51(15) . . . . ? C13 C6 C11 C3 -53.79(16) . . . . ? C15 C5 C14 C18 0.3(2) . . . . ? S1 C5 C14 C18 178.87(12) . . . . ? C14 C5 C15 C21 -1.1(2) . . . . ? S1 C5 C15 C21 -179.60(12) . . . . ? C10 C3 C16 C20 2.0(2) . . . . ? C11 C3 C16 C20 -177.17(14) . . . . ? C1 C6 C17 F1 61.39(17) . . . . ? C13 C6 C17 F1 -177.22(12) . . . . ? C11 C6 C17 F1 -61.21(17) . . . . ? C1 C6 C17 F3 -60.27(17) . . . . ? C13 C6 C17 F3 61.12(16) . . . . ? C11 C6 C17 F3 177.13(12) . . . . ? C1 C6 C17 F2 -178.25(13) . . . . ? C13 C6 C17 F2 -56.86(17) . . . . ? C11 C6 C17 F2 59.15(17) . . . . ? C5 C14 C18 C12 0.7(2) . . . . ? C21 C12 C18 C14 -1.0(2) . . . . ? C23 C12 C18 C14 178.36(15) . . . . ? C22 C19 C20 C16 -1.3(3) . . . . ? C3 C16 C20 C19 0.0(2) . . . . ? C5 C15 C21 C12 0.8(2) . . . . ? C18 C12 C21 C15 0.3(2) . . . . ? C23 C12 C21 C15 -179.13(15) . . . . ? C20 C19 C22 C10 0.7(3) . . . . ? C3 C10 C22 C19 1.3(2) . . . . ?