#------------------------------------------------------------------------------ #$Date: 2020-07-06 06:42:57 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253969 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157530.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_7157530 loop_ _publ_author_name 'Terashima, Kyu' 'Kawasaki-Takasuka, Tomoko' 'Agou, Tomohiro' 'Kubota, Toshio' 'Yamazaki, Takashi' _publ_section_title ; Syntheses of \a-CF3-\a-quaternary ketones via p-quinone methides and their derivatization to compounds with successively congested stereogenic centers. ; _journal_issue 24 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 4638 _journal_page_last 4644 _journal_paper_doi 10.1039/d0ob00951b _journal_volume 18 _journal_year 2020 _chemical_formula_moiety 'C22 H18 Cl F3 O2, C4 H8 O2' _chemical_formula_sum 'C26 H26 Cl F3 O4' _chemical_formula_weight 494.92 _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 103.931(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.0518(6) _cell_length_b 11.0358(4) _cell_length_c 18.5393(9) _cell_measurement_reflns_used 12255 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 30.248 _cell_measurement_theta_min 2.65 _cell_volume 2393.22(19) _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 0.994 _diffrn_measured_fraction_theta_max 0.994 _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 0.0376 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 28431 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.495 _diffrn_reflns_theta_min 2.602 _diffrn_source 'Rigaku VariMax' _exptl_absorpt_coefficient_mu 0.214 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76561 _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 1.374 _exptl_crystal_description block _exptl_crystal_F_000 1032 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.110 _refine_diff_density_max 0.726 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 312 _refine_ls_number_reflns 4433 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0458 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+1.5111P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1285 _refine_ls_wR_factor_ref 0.1330 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3822 _reflns_number_total 4433 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00951b2.cif _cod_data_source_block Kyu4 _cod_depositor_comments 'Adding full bibliography for 7157528--7157531.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7157530 _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 0.957 _shelx_estimated_absorpt_t_max 0.977 _oxdiff_exptl_absorpt_empirical_full_min 0.817 _oxdiff_exptl_absorpt_empirical_full_max 1.327 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; Kyu4.res created by SHELXL-2014/7 TITL Kyu4_a.res in P2(1)/n REM Yadorkari-X generated CELL 0.71073 12.0518 11.0358 18.5393 90.0000 103.9310 90.0000 ZERR 4.0 0.0006 0.0004 0.0009 0.0000 0.0050 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H O F Cl UNIT 104 104 16 12 4 SIZE 0.21 0.18 0.11 TEMP -100.0 L.S. 20 FMAP 2 PLAN -20 ACTA CONF HTAB LIST 4 BOND $H OMIT -10.000000 51.000000 OMIT 1 1 0 OMIT 1 0 1 EQIV $1 1-X, 2-Y, -Z EQIV $2 -1/2+X, 3/2-Y, -1/2+Z EQIV $3 1-X, 1-Y, 1-Z EQIV $4 1/2+X, 3/2-Y, 1/2+Z HTAB C2 F3_$1 HTAB O1 O2_$2 HTAB C23 O2 HTAB C23 O4_$3 WGHT 0.072900 1.511100 FVAR 1.94858 CL1 5 0.448272 1.310899 0.215588 11.00000 0.05403 0.02711 = 0.06676 -0.01074 0.02784 -0.00278 C1 1 0.464893 1.162366 0.187515 11.00000 0.02899 0.02444 = 0.04133 -0.00450 0.01393 -0.00275 C2 1 0.433747 1.134160 0.113020 11.00000 0.03454 0.02577 = 0.03660 0.00716 0.01142 0.00201 AFIX 43 H1 2 0.403234 1.194762 0.077361 11.00000 -1.20000 AFIX 0 C3 1 0.447438 1.015924 0.090505 11.00000 0.02972 0.02873 = 0.02265 0.00363 0.00630 -0.00057 AFIX 43 H2 2 0.426355 0.997146 0.038998 11.00000 -1.20000 AFIX 0 C4 1 0.491039 0.924226 0.141019 11.00000 0.02070 0.02507 = 0.02160 0.00141 0.00460 -0.00059 C5 1 0.523947 0.957177 0.216343 11.00000 0.02819 0.03249 = 0.02107 0.00048 0.00103 0.00468 AFIX 43 H3 2 0.555453 0.897401 0.252331 11.00000 -1.20000 AFIX 0 C6 1 0.511553 1.074920 0.239460 11.00000 0.03028 0.03620 = 0.02774 -0.00846 0.00505 -0.00069 AFIX 43 H4 2 0.534969 1.095371 0.290656 11.00000 -1.20000 AFIX 0 C7 1 0.498032 0.793074 0.112113 11.00000 0.02343 0.02637 = 0.01415 0.00285 0.00292 0.00065 O1 3 0.481114 0.796054 0.033414 11.00000 0.02835 0.03321 = 0.01429 0.00137 0.00322 0.00065 AFIX 147 H5 2 0.412331 0.811945 0.013706 11.00000 -1.50000 AFIX 0 C8 1 0.402621 0.715143 0.131410 11.00000 0.02167 0.02576 = 0.02537 0.00557 0.00376 0.00264 C9 1 0.367991 0.727026 0.197811 11.00000 0.03083 0.03607 = 0.02964 0.00845 0.00983 0.00491 AFIX 43 H6 2 0.405765 0.783992 0.233854 11.00000 -1.20000 AFIX 0 C10 1 0.280281 0.658065 0.212331 11.00000 0.03769 0.04994 = 0.04698 0.01605 0.02243 0.00592 AFIX 43 H7 2 0.259122 0.667366 0.258181 11.00000 -1.20000 AFIX 0 C11 1 0.223251 0.575724 0.160540 11.00000 0.03830 0.05042 = 0.07875 0.01271 0.02529 -0.00851 AFIX 43 H8 2 0.162649 0.528456 0.170344 11.00000 -1.20000 AFIX 0 C12 1 0.255327 0.562765 0.094145 11.00000 0.03947 0.04451 = 0.06593 -0.00235 0.00943 -0.01536 AFIX 43 H9 2 0.216378 0.506293 0.058185 11.00000 -1.20000 AFIX 0 C13 1 0.343772 0.631428 0.079620 11.00000 0.03119 0.03371 = 0.03628 -0.00098 0.00517 -0.00463 AFIX 43 H10 2 0.364681 0.621393 0.033739 11.00000 -1.20000 AFIX 0 C14 1 0.625959 0.740828 0.139408 11.00000 0.02345 0.02573 = 0.02082 0.00221 0.00558 0.00070 C15 1 0.707081 0.834292 0.116952 11.00000 0.02642 0.03566 = 0.02962 0.00680 0.00873 -0.00178 AFIX 137 H11 2 0.704413 0.910255 0.143861 11.00000 -1.50000 H12 2 0.682933 0.849316 0.063352 11.00000 -1.50000 H13 2 0.785331 0.802566 0.129406 11.00000 -1.50000 AFIX 0 C16 1 0.643286 0.623304 0.097680 11.00000 0.03118 0.03198 = 0.02460 0.00124 0.00667 0.00594 F1 4 0.747266 0.575385 0.128508 11.00000 0.03362 0.04083 = 0.04365 -0.00253 0.00557 0.01277 F2 4 0.568149 0.534966 0.099367 11.00000 0.04068 0.02960 = 0.04231 -0.01024 0.00915 -0.00308 F3 4 0.642968 0.639398 0.026052 11.00000 0.06396 0.04908 = 0.02613 -0.00021 0.01744 0.01659 C17 1 0.660549 0.712217 0.223036 11.00000 0.02038 0.02218 = 0.02093 0.00207 0.00300 0.00264 C18 1 0.745964 0.778287 0.271218 11.00000 0.02208 0.02441 = 0.02802 0.00299 0.00350 -0.00150 AFIX 43 H14 2 0.783795 0.841322 0.251681 11.00000 -1.20000 AFIX 0 C19 1 0.777175 0.754412 0.346946 11.00000 0.02358 0.02892 = 0.02616 -0.00268 -0.00274 -0.00053 AFIX 43 H15 2 0.835472 0.800891 0.378595 11.00000 -1.20000 AFIX 0 C20 1 0.723126 0.662828 0.376064 11.00000 0.02363 0.03227 = 0.01816 0.00120 0.00041 0.00630 C21 1 0.638651 0.594234 0.329461 11.00000 0.02250 0.02699 = 0.02418 0.00604 0.00389 0.00071 AFIX 43 H16 2 0.601528 0.530971 0.349323 11.00000 -1.20000 AFIX 0 C22 1 0.608792 0.618537 0.253853 11.00000 0.02016 0.02279 = 0.02374 0.00168 0.00082 0.00004 AFIX 43 H17 2 0.551849 0.570423 0.222255 11.00000 -1.20000 AFIX 0 O2 3 0.755741 0.642305 0.451296 11.00000 0.03471 0.04982 = 0.01868 0.00509 -0.00215 -0.00260 AFIX 147 H18 2 0.713523 0.588895 0.462925 11.00000 -1.50000 AFIX 0 C27 1 0.656423 0.555316 0.617347 11.00000 0.06511 0.06062 = 0.04191 -0.00877 0.01658 -0.01515 AFIX 137 H19 2 0.683190 0.626254 0.594593 11.00000 -1.50000 H20 2 0.715959 0.529255 0.660466 11.00000 -1.50000 H21 2 0.587063 0.576444 0.633341 11.00000 -1.50000 AFIX 0 O5 3 0.636837 0.462290 0.498198 11.00000 0.05033 0.05889 = 0.03167 0.00283 0.01349 -0.00341 C24 1 0.630761 0.455334 0.562270 11.00000 0.03768 0.04578 = 0.03459 0.00403 0.01281 0.00303 O4 3 0.597208 0.355122 0.590089 11.00000 0.10452 0.04236 = 0.04928 0.00225 0.04035 -0.00144 C25 1 0.568262 0.250190 0.539782 11.00000 0.19492 0.04675 = 0.08465 -0.00979 0.07154 -0.00426 AFIX 23 H26 2 0.520723 0.276952 0.491134 11.00000 -1.20000 H27 2 0.639082 0.213344 0.531529 11.00000 -1.20000 AFIX 0 C26 1 0.507471 0.163449 0.571843 11.00000 0.06151 0.06176 = 0.12281 -0.02646 0.02134 0.00853 AFIX 137 H23 2 0.554915 0.137198 0.619938 11.00000 -1.50000 H24 2 0.488761 0.093367 0.538673 11.00000 -1.50000 H25 2 0.436779 0.199913 0.579047 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM Kyu4_a.res in P2(1)/n REM R1 = 0.0458 for 3822 Fo > 4sig(Fo) and 0.0523 for all 4433 data REM 312 parameters refined using 0 restraints END WGHT 0.0679 1.5978 REM Instructions for potential hydrogen bonds HTAB C2 F3_$1 HTAB O1 O2_$2 HTAB O2 O5 REM Highest difference peak 0.726, deepest hole -0.389, 1-sigma level 0.058 Q1 1 0.6422 0.2374 0.5773 11.00000 0.05 0.73 Q2 1 0.6600 0.3525 0.6207 11.00000 0.05 0.41 Q3 1 0.5510 0.2722 0.5333 11.00000 0.05 0.33 Q4 1 0.3940 1.3014 0.2510 11.00000 0.05 0.29 Q5 1 0.6339 0.6964 0.1166 11.00000 0.05 0.28 Q6 1 0.5611 0.7644 0.1249 11.00000 0.05 0.28 Q7 1 0.5364 0.2250 0.5370 11.00000 0.05 0.28 Q8 1 0.6137 0.2567 0.5019 11.00000 0.05 0.28 Q9 1 0.4434 1.2219 0.2032 11.00000 0.05 0.28 Q10 1 0.4925 1.2892 0.2577 11.00000 0.05 0.25 Q11 1 0.6651 0.7882 0.1292 11.00000 0.05 0.23 Q12 1 0.4478 0.7613 0.1246 11.00000 0.05 0.22 Q13 1 0.4675 1.1143 0.2124 11.00000 0.05 0.22 Q14 1 0.4942 1.3050 0.1812 11.00000 0.05 0.22 Q15 1 0.4165 1.0679 0.1109 11.00000 0.05 0.20 Q16 1 0.3958 0.7147 0.1651 11.00000 0.05 0.20 Q17 1 0.2332 0.6467 0.1753 11.00000 0.05 0.20 Q18 1 0.6183 0.6860 0.2428 11.00000 0.05 0.19 Q19 1 0.7746 0.6791 0.3553 11.00000 0.05 0.19 Q20 1 0.4969 0.8644 0.1271 11.00000 0.05 0.19 ; _shelx_res_checksum 95817 _shelx_hkl_file ; 0 0 3 12.2918 5.23079 0 0 -4 23440.6 643.474 0 0 4 22770.0 643.479 0 0 5 5.72922 7.90053 0 0 -5-0.49927 8.40258 0 0 -6 33931.4 938.785 0 0 6 33463.9 938.996 0 0 7-6.24813 10.9204 0 0 -7-5.90465 10.4663 0 0 8 30044.1 830.105 0 0 -8 29331.7 830.074 0 0 9-7.89705 14.4351 0 0 9 30.8222 31.4860 0 0 -9 2.20442 14.2939 0 0 -10 2763.28 91.7932 0 0 10 3078.55 93.0391 0 0 10 2918.95 107.815 0 0 11-1.06728 14.8552 0 0 11 11.5461 23.5960 0 0 -11 26.6987 15.7600 0 0 12 9405.68 276.987 0 0 12 9780.42 298.002 0 0 -12 9621.62 277.515 0 0 13-1.20252 15.7971 0 0 -13-7.17482 17.6873 0 0 13 6.06500 30.9788 0 0 14 31.6870 17.9790 0 0 14 55.2542 32.3724 0 0 -14 37.8015 19.2194 0 0 -15 10.2582 19.3707 0 0 15-1.35936 19.3406 0 0 15-15.8076 35.2309 0 0 -16 1683.47 64.8045 0 0 16 1672.61 88.1941 0 0 16 1806.52 65.9177 0 0 -16 1504.59 87.9802 0 0 -17-16.5387 45.0098 0 0 17 8.00448 39.8247 0 0 17-8.06414 23.7112 0 0 -17 1.42867 22.8949 0 0 -18 2.19427 45.7709 0 0 18-12.7082 43.5380 0 0 18 25.1449 23.1977 0 0 -18 32.7477 23.6712 0 0 -19 10.4432 23.4052 0 0 -19 30.2588 49.3826 0 0 19-11.7709 22.7268 0 0 19 15.5313 42.2943 0 0 -20 116.632 26.1330 0 0 20 101.819 25.3223 0 0 -20 135.779 50.1587 0 0 20 148.698 52.0276 0 0 21 19.8434 49.9095 0 0 21-14.2260 23.2272 0 0 -21-10.3515 52.8735 0 0 22 174.992 58.4861 0 0 -23-11.5436 60.9709 0 1 -2 5831.45 167.046 0 1 -3 1168.23 40.1113 0 1 -4 900.619 33.4422 0 -1 4 876.747 33.3843 0 1 -5 982.406 38.1061 0 -1 5 1080.94 39.4510 0 1 6 18342.4 510.109 0 1 -6 18102.7 516.898 0 1 -7 3007.31 93.2858 0 -1 7 2960.23 93.5460 0 -1 -7 2985.52 86.1143 0 1 7 2951.58 86.3433 0 -1 -8 3065.08 89.4363 0 -1 8 2939.04 96.2615 0 1 -8 2915.70 96.7932 0 1 8 3144.81 89.7437 0 -1 9 525.116 29.8424 0 1 9 570.844 23.3566 0 1 -9 554.960 30.6879 0 -1 9 502.655 36.2757 0 -1 -9 566.465 22.6196 0 -1 -10 8358.37 248.794 0 -1 10 8580.86 256.679 0 -1 10 8664.76 267.918 0 1 -10 8166.42 255.952 0 1 11 108.807 13.7921 0 1 -11 114.046 19.8894 0 -1 11 119.384 20.0799 0 -1 11 141.633 27.4755 0 -1 -11 116.747 13.2859 0 1 12 5014.70 149.189 0 -1 -12 5104.25 149.024 0 1 -12 5149.61 156.883 0 -1 12 5124.14 171.434 0 -1 12 5078.90 157.606 0 1 12 4639.17 172.898 0 -1 13 78.6557 22.5688 0 1 13 66.8326 15.0515 0 1 -13 51.4603 21.6361 0 1 13 19.1049 35.2587 0 -1 13 60.6793 27.9209 0 -1 -13 61.3905 13.9199 0 1 14 106.643 16.1627 0 1 -14 110.118 24.5457 0 -1 -14 124.879 16.3103 0 -1 14 110.387 36.2657 0 1 14 98.6872 37.0038 0 -1 14 70.9973 22.0447 0 1 -14 88.0609 37.9562 0 -1 15 263.084 42.3528 0 -1 15 277.086 29.5491 0 -1 -15 286.925 21.5090 0 1 15 300.816 21.2309 0 1 -15 284.771 44.2035 0 1 -15 309.069 31.0049 0 1 15 303.080 45.0799 0 1 16 1697.58 89.2597 0 1 -16 1640.49 89.0695 0 1 -16 1537.65 66.1875 0 1 16 1683.07 58.4787 0 -1 16 1719.38 68.7099 0 -1 -16 1684.86 58.6951 0 -1 16 1720.43 87.9981 0 1 -17 2595.65 94.7177 0 -1 -17 2680.25 85.1164 0 1 -17 2612.64 119.859 0 -1 17 2581.52 94.5496 0 -1 17 2915.20 121.842 0 1 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58.3318 52.3964 -14 -2 2 118.107 56.2818 -14 -2 2 55.7995 50.7992 -14 2 2 81.6776 53.9172 -14 -2 1 43.2902 52.0136 -14 -2 1-30.5519 53.4898 -14 -2 0 45.9008 53.2926 -14 -2 0-9.47692 50.8963 -14 2 -1 27.8101 54.5299 -14 -2 -1-39.2591 54.8890 -14 2 -1 4.99026 53.5250 -14 -2 -1 14.2149 50.4043 -14 2 -2 95.1852 56.9858 -14 -2 -2 87.1879 57.3361 -14 2 -2 100.946 55.1717 -14 -2 -2 192.474 59.8660 -14 2 -3 26.3708 58.0204 -14 -2 -3-5.09760 56.6577 -14 -2 -3-48.6269 56.5994 -14 2 -4-43.0100 59.4569 -14 -2 -4-25.6970 57.2747 -14 -2 -5 65.1992 61.3676 -14 3 16 215.474 59.2775 -14 3 16 238.681 61.2300 -14 -3 16 243.706 67.2430 -14 3 15 573.140 72.5169 -14 3 15 646.360 70.9405 -14 3 14 58.4134 54.0316 -14 3 14 26.0610 52.5515 -14 -3 14 102.200 59.1974 -14 3 13 103.843 53.9874 -14 3 13 38.8977 50.3019 -14 -3 13-16.5074 56.0380 14 3 -13-5.02316 58.2699 -14 3 12 202.019 59.3917 -14 3 12 191.486 56.7782 -14 -3 12 164.176 59.9904 14 3 -12 171.071 62.2657 -14 3 11 1250.36 86.9196 -14 -3 11 1442.94 95.7404 -14 3 11 1542.66 94.7981 14 3 -11 1557.64 99.6391 -14 3 10-6.77820 54.4549 -14 3 10 45.7466 53.4602 -14 -3 10-2.39838 53.9205 14 3 -10-52.7938 59.3988 -14 3 9 755.944 72.1854 -14 -3 9 799.302 76.5740 -14 3 9 849.307 78.9274 14 3 -9 712.122 77.7477 -14 3 8 169.132 60.4139 -14 3 8 51.4582 52.6689 -14 -3 8 159.212 58.5941 -14 3 7 377.796 65.1087 -14 3 7 332.448 61.1618 -14 -3 7 392.810 65.1310 -14 3 6 547.156 67.6674 -14 -3 6 514.967 70.7605 -14 -3 6 585.671 70.8674 -14 3 6 513.674 67.7518 -14 3 5 1144.58 85.4144 -14 3 5 1062.75 81.4050 -14 3 4 344.819 63.5158 -14 3 4 344.818 62.6934 -14 3 3 96.9979 53.0993 -14 -3 3 72.4180 55.4476 -14 -3 3 59.7855 54.8002 -14 3 3 79.1812 55.5076 -14 3 2 134.716 56.5729 -14 -3 2 26.5950 52.1362 -14 -3 2 146.055 55.2742 -14 3 2 56.3264 51.7265 -14 -3 1 452.242 63.7522 -14 3 1 414.602 66.1130 -14 -3 1 528.286 68.8091 -14 3 1 430.495 64.7825 -14 -3 0 7.40713 54.1118 -14 -3 0 16.6556 52.0781 -14 -3 -1 241.214 61.5905 -14 -3 -1 248.518 60.5720 -14 3 -2 36.9924 58.5290 -14 -3 -2 74.7507 54.4994 -14 -3 -2 45.2396 56.5229 -14 3 -3 332.201 68.6568 -14 -3 -3 490.794 70.7536 -14 -3 -4-12.6970 59.2525 -14 -3 -5 122.581 64.5029 -14 4 15 793.809 72.6246 -14 4 15 862.900 74.7122 -14 4 14-23.9086 53.1034 -14 -4 14-25.2469 61.8292 -14 4 14 29.1633 53.2643 -14 4 13 50.1963 54.2224 -14 -4 13-4.98695 56.8214 -14 4 13-12.7324 53.4732 -14 4 12 84.3202 52.9693 -14 -4 12 104.625 58.1416 -14 4 12 131.697 56.5906 -14 4 11 25.3725 55.7349 -14 -4 11 2.44341 56.8456 -14 4 10 73.3848 55.2694 -14 -4 10 66.3666 56.4494 -14 4 10 62.2748 54.3287 14 4 -10 71.4902 58.9123 -14 4 9 153.149 54.7875 -14 -4 9 123.409 59.7900 -14 4 9 238.996 60.3732 14 4 -9 153.547 58.9851 -14 4 8 456.040 63.3728 -14 -4 8 459.839 69.7844 -14 4 8 563.988 68.2142 14 4 -8 502.494 70.3266 -14 4 7-20.0426 52.4442 -14 -4 7-66.2805 56.8181 -14 4 7-11.6921 54.6298 14 4 -7-2.56258 54.2208 -14 4 6 106.791 53.8610 -14 4 6 65.4013 55.1797 -14 4 5 11.4411 53.9471 -14 4 5 39.8389 54.5575 -14 4 4-46.7214 52.9148 -14 -4 4-17.5306 54.9612 -14 -4 4-29.6078 56.2967 -14 4 4-4.76497 54.4270 -14 4 3 1001.46 82.0964 -14 -4 3 977.459 83.5541 -14 -4 3 1149.04 86.9399 -14 4 3 860.716 78.9560 -14 4 2-27.0239 53.6288 -14 -4 2 31.4055 52.3167 -14 -4 2-15.0449 55.4546 -14 4 2 34.6808 55.7619 -14 4 1 9.96140 53.5717 -14 -4 1 25.2064 54.1495 -14 4 1 19.8680 53.5694 -14 -4 1 34.4140 54.8535 -14 4 0 71.8069 59.0566 -14 -4 0 48.8817 55.1673 -14 -4 0 20.0403 55.7696 -14 -4 -1-62.7117 60.8088 -14 -4 -2-22.6264 59.3366 -14 -4 -3 75.4108 59.2276 -14 -4 -4 166.680 66.4507 -14 5 14 66.4840 50.7550 -14 5 14 79.9174 50.3809 -14 5 13 70.2684 51.2381 -14 5 13 98.2837 55.2872 -14 5 12 60.0116 53.3129 -14 5 12 102.481 54.9494 -14 5 11 401.520 61.4162 -14 5 11 448.244 66.8357 -14 -5 11 316.488 69.2357 -14 5 10 263.526 56.3259 -14 5 10 241.924 62.4098 -14 -5 10 248.354 63.0970 -14 5 9 269.048 59.6912 -14 5 9 225.853 61.0864 -14 -5 9 162.983 60.2839 -14 5 8 139.085 55.5520 -14 5 8 232.315 61.6522 -14 -5 8 212.299 63.8426 -14 5 7 55.3651 52.5603 -14 5 7 136.251 58.4075 -14 5 6 9.03274 51.5830 -14 5 6-16.5873 55.2259 -14 -5 5 865.220 83.3257 -14 5 5 902.871 80.5264 -14 5 5 848.250 77.0669 -14 5 4 242.182 60.4618 -14 5 4 168.080 59.2109 -14 -5 4 212.797 64.5987 -14 5 3 490.052 70.7110 -14 5 3 452.682 69.2759 -14 -5 3 442.852 70.7894 -14 5 2 15.6336 56.5843 -14 -5 2 45.3985 58.3087 -14 -5 1 196.443 61.1849 -14 5 1 188.173 61.8541 -14 -5 0 59.1491 59.4109 -14 5 0 84.1466 61.0574 -14 -5 -1 311.004 67.5783 -14 -5 -2 103.585 63.6826 -14 6 13 8.08863 51.3087 -14 6 13 28.0657 53.0387 -14 6 12 611.896 67.5879 -14 6 12 539.651 71.1045 -14 6 11 468.328 65.1036 -14 6 11 421.612 68.8205 -14 6 10 264.569 59.4245 -14 6 10 276.158 65.1966 -14 6 9 71.3530 55.7505 -14 6 9 82.3791 57.6795 -14 6 8 335.831 61.8049 -14 6 8 347.775 67.1419 -14 6 7 26.8353 53.0807 -14 6 7 31.6532 56.0251 -14 6 6 298.104 61.7318 -14 6 6 393.606 68.8094 -14 6 5 398.930 65.0598 -14 6 4-17.6060 57.7981 -14 -6 4 2.60476 58.0487 -14 -6 3 1138.28 91.6749 -14 6 3 1283.00 93.6147 -14 6 2 122.592 61.2341 -14 7 12-8.05167 51.2717 -14 7 11 156.115 63.0617 -14 7 11 148.497 53.8043 -14 7 10 541.527 74.7460 -14 7 10 395.684 62.4961 -14 7 9 443.882 74.1035 -14 7 9 408.132 63.6588 -14 7 8 94.8330 53.2185 -14 7 7 262.387 60.2977 -14 7 6 400.307 68.1008 -14 7 5 151.319 62.1516 -14 8 11 102.953 56.9075 -14 8 10-25.3725 54.1721 -14 8 9 256.390 60.2460 -15 0 16 13.9409 59.0682 -15 0 15-4.73472 58.0974 -15 0 14 72.2063 59.3618 -15 0 13 110.935 58.4865 -15 0 12 54.9822 59.3551 -15 0 11 468.908 68.6848 -15 0 11 327.069 62.7028 -15 0 10 100.009 55.0769 -15 0 10 32.9347 52.6594 -15 0 9-43.0575 56.3282 -15 0 9 21.4036 53.0668 -15 0 8 150.643 59.7675 -15 0 8 144.654 58.8740 -15 0 7 203.575 58.7022 -15 0 7 259.937 59.8966 -15 0 6 126.643 57.9586 -15 0 6 178.175 58.5338 -15 0 5 661.899 72.7999 -15 0 5 686.950 74.0131 -15 0 4 40.9040 55.2264 -15 0 1 148.256 61.6225 -15 1 17 233.092 64.1997 -15 1 16 27.4706 58.1442 -15 1 15-18.0421 56.2637 -15 -1 15 43.2786 60.5864 -15 1 14 8.97733 55.2826 -15 1 14 16.2721 59.5260 -15 -1 14 172.455 63.6691 -15 1 13 138.341 57.6202 -15 1 13 123.351 58.8357 -15 -1 13 166.746 63.0924 -15 1 12 275.051 61.5796 -15 1 12 252.384 61.4363 -15 -1 12 214.078 63.5647 -15 1 11 342.212 65.6925 -15 1 11 386.288 63.2118 -15 -1 11 281.199 63.5789 -15 1 10 167.341 60.2085 -15 -1 10 140.624 59.0630 -15 1 10 95.7231 57.5380 -15 1 9 47.6813 53.8239 -15 -1 9 63.8669 57.8004 -15 1 9 70.3600 56.3052 -15 1 8 352.549 63.7178 -15 -1 8 316.680 65.1325 -15 1 8 360.385 62.3356 -15 1 7 782.230 75.3784 -15 -1 7 722.465 75.6081 -15 1 7 681.226 75.3105 -15 1 6 329.384 63.2397 -15 -1 6 384.876 64.4416 -15 1 6 326.185 65.7088 -15 1 5 405.213 70.4966 -15 1 5 290.945 64.7562 -15 1 4 255.335 62.5059 -15 1 3 55.9609 58.2648 -15 -1 1 224.423 61.2764 -15 2 16-19.6440 57.2955 -15 2 15 218.610 64.2162 -15 2 14 958.138 82.7736 -15 2 14 1020.75 85.0120 -15 2 13 414.115 65.5577 -15 2 13 505.498 71.0511 -15 2 12 128.851 55.2524 -15 -2 12 32.6074 59.1924 -15 2 12 130.855 59.9822 -15 2 11 110.878 56.9656 -15 -2 11 67.0013 57.4624 -15 2 11 208.318 63.5694 -15 2 10 133.526 57.7147 -15 -2 10 69.7007 56.9129 -15 2 10 49.2821 53.7243 -15 2 9 86.8420 54.8252 -15 2 9 143.830 58.5221 -15 -2 9 175.491 60.8773 -15 2 8 210.114 61.1415 -15 2 8 170.731 60.9616 -15 -2 8 50.8776 58.3838 -15 2 7 315.113 63.8687 -15 2 7 179.068 61.4241 -15 2 6 146.653 61.0355 -15 2 6 117.869 60.0534 -15 -2 6 27.8849 59.5489 -15 2 5 188.271 59.8541 -15 2 4 339.039 65.2617 -15 2 3 48.6075 54.6710 -15 2 2 427.379 70.5213 -15 -2 2 429.785 68.0485 -15 -2 1-42.3651 58.9448 -15 3 15 74.8746 61.3381 -15 3 15 26.2970 56.4248 -15 3 14 336.761 66.1530 -15 3 14 146.570 59.7791 -15 3 13 63.2271 59.7925 -15 3 13 72.9734 56.6830 -15 3 12 4.75122 59.0358 -15 3 12 65.3934 55.3495 -15 3 11 86.3328 58.3054 -15 3 11-4.48413 53.8119 -15 3 10-21.7650 56.2308 -15 3 10 20.9574 56.6667 -15 3 9 46.3332 58.2154 -15 3 9 111.719 58.0455 -15 -3 9-7.67372 58.0934 -15 3 8 636.795 74.7139 -15 -3 8 700.692 79.2358 -15 3 8 820.297 80.1392 -15 3 7 142.065 57.1022 -15 -3 7 167.830 63.2780 -15 3 6 1565.78 98.8662 -15 -3 6 1352.03 100.648 -15 3 5 24.8344 57.6143 -15 3 4 164.943 64.1048 -15 3 3-7.81790 57.3357 -15 4 15 148.740 56.9328 -15 4 14 73.1711 55.9057 -15 4 14 74.8165 59.3829 -15 4 13 24.1391 56.0738 -15 4 13 80.7755 61.6896 -15 4 12 81.6308 56.6033 -15 4 12 42.2385 58.0340 -15 4 11-36.6778 54.4153 -15 4 10 2.30740 57.6800 -15 4 9 502.452 68.7613 -15 4 8 263.085 63.6310 -15 4 7 74.4340 56.6410 -15 4 6 186.523 62.3616 -15 4 5 174.458 63.0059 -15 5 13 45.2223 54.5450 -15 5 12 45.2927 58.4183 -15 5 11 160.500 58.7427 -15 5 10 47.1774 55.4917 -15 5 9 242.695 62.4019 -15 5 8-25.9596 57.8596 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 91200 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 Cl1 Cl 0.44827(5) 1.31090(5) 0.21559(4) 0.04704(19) Uani 1 1 d . . . . . C1 C 0.46489(17) 1.16237(18) 0.18752(12) 0.0307(4) Uani 1 1 d . . . . . C2 C 0.43375(18) 1.13416(18) 0.11302(12) 0.0318(4) Uani 1 1 d . . . . . H1 H 0.4032 1.1948 0.0774 0.038 Uiso 1 1 calc R U . . . C3 C 0.44744(16) 1.01592(18) 0.09050(10) 0.0270(4) Uani 1 1 d . . . . . H2 H 0.4264 0.9971 0.0390 0.032 Uiso 1 1 calc R U . . . C4 C 0.49104(15) 0.92423(16) 0.14102(10) 0.0225(4) Uani 1 1 d . . . . . C5 C 0.52395(16) 0.95718(18) 0.21634(10) 0.0281(4) Uani 1 1 d . . . . . H3 H 0.5555 0.8974 0.2523 0.034 Uiso 1 1 calc R U . . . C6 C 0.51155(17) 1.07492(19) 0.23946(11) 0.0317(4) Uani 1 1 d . . . . . H4 H 0.5350 1.0954 0.2907 0.038 Uiso 1 1 calc R U . . . C7 C 0.49803(15) 0.79307(17) 0.11211(9) 0.0216(4) Uani 1 1 d . . . . . O1 O 0.48111(11) 0.79605(12) 0.03341(6) 0.0256(3) Uani 1 1 d . . . . . H5 H 0.4123 0.8119 0.0137 0.038 Uiso 1 1 calc R U . . . C8 C 0.40262(15) 0.71514(17) 0.13141(10) 0.0246(4) Uani 1 1 d . . . . . C9 C 0.36799(17) 0.7270(2) 0.19781(11) 0.0317(4) Uani 1 1 d . . . . . H6 H 0.4058 0.7840 0.2339 0.038 Uiso 1 1 calc R U . . . C10 C 0.2803(2) 0.6581(2) 0.21233(14) 0.0428(6) Uani 1 1 d . . . . . H7 H 0.2591 0.6674 0.2582 0.051 Uiso 1 1 calc R U . . . C11 C 0.2233(2) 0.5757(2) 0.16054(17) 0.0539(7) Uani 1 1 d . . . . . H8 H 0.1626 0.5285 0.1703 0.065 Uiso 1 1 calc R U . . . C12 C 0.2553(2) 0.5628(2) 0.09415(16) 0.0505(6) Uani 1 1 d . . . . . H9 H 0.2164 0.5063 0.0582 0.061 Uiso 1 1 calc R U . . . C13 C 0.34377(18) 0.63143(19) 0.07962(12) 0.0342(5) Uani 1 1 d . . . . . H10 H 0.3647 0.6214 0.0337 0.041 Uiso 1 1 calc R U . . . C14 C 0.62596(15) 0.74083(17) 0.13941(10) 0.0233(4) Uani 1 1 d . . . . . C15 C 0.70708(17) 0.83429(19) 0.11695(11) 0.0302(4) Uani 1 1 d . . . . . H11 H 0.7044 0.9103 0.1439 0.045 Uiso 1 1 calc R U . . . H12 H 0.6829 0.8493 0.0634 0.045 Uiso 1 1 calc R U . . . H13 H 0.7853 0.8026 0.1294 0.045 Uiso 1 1 calc R U . . . C16 C 0.64329(17) 0.62330(18) 0.09768(11) 0.0293(4) Uani 1 1 d . . . . . F1 F 0.74727(10) 0.57538(12) 0.12851(7) 0.0400(3) Uani 1 1 d . . . . . F2 F 0.56815(10) 0.53497(11) 0.09937(7) 0.0377(3) Uani 1 1 d . . . . . F3 F 0.64297(12) 0.63940(12) 0.02605(7) 0.0453(3) Uani 1 1 d . . . . . C17 C 0.66055(15) 0.71222(16) 0.22304(10) 0.0215(4) Uani 1 1 d . . . . . C18 C 0.74596(15) 0.77829(17) 0.27122(10) 0.0253(4) Uani 1 1 d . . . . . H14 H 0.7838 0.8413 0.2517 0.030 Uiso 1 1 calc R U . . . C19 C 0.77718(16) 0.75441(18) 0.34695(10) 0.0277(4) Uani 1 1 d . . . . . H15 H 0.8355 0.8009 0.3786 0.033 Uiso 1 1 calc R U . . . C20 C 0.72313(16) 0.66283(18) 0.37606(10) 0.0255(4) Uani 1 1 d . . . . . C21 C 0.63865(15) 0.59423(17) 0.32946(10) 0.0249(4) Uani 1 1 d . . . . . H16 H 0.6015 0.5310 0.3493 0.030 Uiso 1 1 calc R U . . . C22 C 0.60879(15) 0.61854(16) 0.25385(10) 0.0230(4) Uani 1 1 d . . . . . H17 H 0.5518 0.5704 0.2223 0.028 Uiso 1 1 calc R U . . . O2 O 0.75574(12) 0.64231(15) 0.45130(7) 0.0359(4) Uani 1 1 d . . . . . H18 H 0.7135 0.5889 0.4629 0.054 Uiso 1 1 calc R U . . . C27 C 0.6564(3) 0.5553(3) 0.61735(14) 0.0553(7) Uani 1 1 d . . . . . H19 H 0.6832 0.6263 0.5946 0.083 Uiso 1 1 calc R U . . . H20 H 0.7160 0.5293 0.6605 0.083 Uiso 1 1 calc R U . . . H21 H 0.5871 0.5764 0.6333 0.083 Uiso 1 1 calc R U . . . O5 O 0.63684(15) 0.46229(16) 0.49820(8) 0.0463(4) Uani 1 1 d . . . . . C24 C 0.63076(19) 0.4553(2) 0.56227(12) 0.0386(5) Uani 1 1 d . . . . . O4 O 0.5972(2) 0.35512(17) 0.59009(10) 0.0617(5) Uani 1 1 d . . . . . C25 C 0.5683(5) 0.2502(3) 0.5398(2) 0.1023(16) Uani 1 1 d . . . . . H26 H 0.5207 0.2770 0.4911 0.123 Uiso 1 1 calc R U . . . H27 H 0.6391 0.2133 0.5315 0.123 Uiso 1 1 calc R U . . . C26 C 0.5075(3) 0.1634(3) 0.5718(2) 0.0822(11) Uani 1 1 d . . . . . H23 H 0.5549 0.1372 0.6199 0.123 Uiso 1 1 calc R U . . . H24 H 0.4888 0.0934 0.5387 0.123 Uiso 1 1 calc R U . . . H25 H 0.4368 0.1999 0.5790 0.123 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 Cl1 0.0540(4) 0.0271(3) 0.0668(4) -0.0107(2) 0.0278(3) -0.0028(2) C1 0.0290(10) 0.0244(10) 0.0413(11) -0.0045(8) 0.0139(8) -0.0028(8) C2 0.0345(11) 0.0258(10) 0.0366(11) 0.0072(8) 0.0114(9) 0.0020(8) C3 0.0297(10) 0.0287(10) 0.0227(9) 0.0036(7) 0.0063(7) -0.0006(8) C4 0.0207(9) 0.0251(9) 0.0216(9) 0.0014(7) 0.0046(7) -0.0006(7) C5 0.0282(10) 0.0325(10) 0.0211(9) 0.0005(7) 0.0010(7) 0.0047(8) C6 0.0303(10) 0.0362(11) 0.0277(10) -0.0085(8) 0.0050(8) -0.0007(8) C7 0.0234(9) 0.0264(9) 0.0142(8) 0.0029(7) 0.0029(6) 0.0006(7) O1 0.0283(7) 0.0332(7) 0.0143(6) 0.0014(5) 0.0032(5) 0.0006(6) C8 0.0217(9) 0.0258(9) 0.0254(9) 0.0056(7) 0.0038(7) 0.0026(7) C9 0.0308(10) 0.0361(11) 0.0296(10) 0.0085(8) 0.0098(8) 0.0049(8) C10 0.0377(12) 0.0499(14) 0.0470(13) 0.0160(11) 0.0224(10) 0.0059(10) C11 0.0383(13) 0.0504(15) 0.0788(19) 0.0127(14) 0.0253(13) -0.0085(11) C12 0.0395(13) 0.0445(14) 0.0659(17) -0.0023(12) 0.0094(12) -0.0154(11) C13 0.0312(11) 0.0337(11) 0.0363(11) -0.0010(9) 0.0052(8) -0.0046(8) C14 0.0235(9) 0.0257(9) 0.0208(9) 0.0022(7) 0.0056(7) 0.0007(7) C15 0.0264(10) 0.0357(11) 0.0296(10) 0.0068(8) 0.0087(8) -0.0018(8) C16 0.0312(10) 0.0320(10) 0.0246(9) 0.0012(8) 0.0067(8) 0.0059(8) F1 0.0336(7) 0.0408(7) 0.0436(7) -0.0025(6) 0.0056(5) 0.0128(5) F2 0.0407(7) 0.0296(6) 0.0423(7) -0.0102(5) 0.0091(5) -0.0031(5) F3 0.0640(9) 0.0491(8) 0.0261(6) -0.0002(5) 0.0174(6) 0.0166(7) C17 0.0204(9) 0.0222(9) 0.0209(9) 0.0021(7) 0.0030(7) 0.0026(7) C18 0.0221(9) 0.0244(9) 0.0280(9) 0.0030(7) 0.0035(7) -0.0015(7) C19 0.0236(9) 0.0289(10) 0.0262(10) -0.0027(7) -0.0027(7) -0.0005(7) C20 0.0236(9) 0.0323(10) 0.0182(9) 0.0012(7) 0.0004(7) 0.0063(7) C21 0.0225(9) 0.0270(9) 0.0242(9) 0.0060(7) 0.0039(7) 0.0007(7) C22 0.0202(9) 0.0228(9) 0.0237(9) 0.0017(7) 0.0008(7) 0.0000(7) O2 0.0347(8) 0.0498(9) 0.0187(7) 0.0051(6) -0.0022(6) -0.0026(7) C27 0.0651(17) 0.0606(17) 0.0419(14) -0.0088(12) 0.0166(12) -0.0152(13) O5 0.0503(10) 0.0589(11) 0.0317(8) 0.0028(7) 0.0135(7) -0.0034(8) C24 0.0377(12) 0.0458(13) 0.0346(12) 0.0040(10) 0.0128(9) 0.0030(9) O4 0.1045(16) 0.0424(10) 0.0493(11) 0.0022(8) 0.0403(11) -0.0014(10) C25 0.195(5) 0.0468(19) 0.085(3) -0.0098(17) 0.072(3) -0.004(2) C26 0.062(2) 0.062(2) 0.123(3) -0.026(2) 0.0213(19) 0.0085(16) 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' Cl Cl 0.1484 0.1585 '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 C2 C1 C6 120.50(18) . . ? C2 C1 Cl1 119.22(16) . . ? C6 C1 Cl1 120.26(16) . . ? C1 C2 C3 119.30(18) . . ? C1 C2 H1 120.3 . . ? C3 C2 H1 120.3 . . ? C2 C3 C4 122.16(17) . . ? C2 C3 H2 118.9 . . ? C4 C3 H2 118.9 . . ? C3 C4 C5 116.80(17) . . ? C3 C4 C7 119.22(16) . . ? C5 C4 C7 123.96(16) . . ? C6 C5 C4 121.59(18) . . ? C6 C5 H3 119.2 . . ? C4 C5 H3 119.2 . . ? C1 C6 C5 119.61(18) . . ? C1 C6 H4 120.2 . . ? C5 C6 H4 120.2 . . ? O1 C7 C8 108.61(14) . . ? O1 C7 C4 109.01(14) . . ? C8 C7 C4 109.49(14) . . ? O1 C7 C14 102.73(13) . . ? C8 C7 C14 115.96(14) . . ? C4 C7 C14 110.67(14) . . ? C7 O1 H5 109.5 . . ? C13 C8 C9 117.23(18) . . ? C13 C8 C7 119.47(16) . . ? C9 C8 C7 123.24(17) . . ? C10 C9 C8 121.7(2) . . ? C10 C9 H6 119.2 . . ? C8 C9 H6 119.2 . . ? C11 C10 C9 120.3(2) . . ? C11 C10 H7 119.9 . . ? C9 C10 H7 119.9 . . ? C10 C11 C12 119.2(2) . . ? C10 C11 H8 120.4 . . ? C12 C11 H8 120.4 . . ? C11 C12 C13 120.6(2) . . ? C11 C12 H9 119.7 . . ? C13 C12 H9 119.7 . . ? C12 C13 C8 121.0(2) . . ? C12 C13 H10 119.5 . . ? C8 C13 H10 119.5 . . ? C17 C14 C15 111.90(15) . . ? C17 C14 C16 107.15(15) . . ? C15 C14 C16 104.72(15) . . ? C17 C14 C7 113.40(14) . . ? C15 C14 C7 107.24(14) . . ? C16 C14 C7 112.14(15) . . ? C14 C15 H11 109.5 . . ? C14 C15 H12 109.5 . . ? H11 C15 H12 109.5 . . ? C14 C15 H13 109.5 . . ? H11 C15 H13 109.5 . . ? H12 C15 H13 109.5 . . ? F2 C16 F3 106.25(16) . . ? F2 C16 F1 105.60(16) . . ? F3 C16 F1 104.59(15) . . ? F2 C16 C14 115.18(16) . . ? F3 C16 C14 114.55(16) . . ? F1 C16 C14 109.79(16) . . ? C18 C17 C22 117.24(16) . . ? C18 C17 C14 121.14(16) . . ? C22 C17 C14 121.61(16) . . ? C19 C18 C17 121.79(17) . . ? C19 C18 H14 119.1 . . ? C17 C18 H14 119.1 . . ? C20 C19 C18 119.72(17) . . ? C20 C19 H15 120.1 . . ? C18 C19 H15 120.1 . . ? O2 C20 C19 118.10(17) . . ? O2 C20 C21 121.94(18) . . ? C19 C20 C21 119.96(16) . . ? C22 C21 C20 119.73(17) . . ? C22 C21 H16 120.1 . . ? C20 C21 H16 120.1 . . ? C21 C22 C17 121.54(17) . . ? C21 C22 H17 119.2 . . ? C17 C22 H17 119.2 . . ? C20 O2 H18 109.5 . . ? C24 C27 H19 109.5 . . ? C24 C27 H20 109.5 . . ? H19 C27 H20 109.5 . . ? C24 C27 H21 109.5 . . ? H19 C27 H21 109.5 . . ? H20 C27 H21 109.5 . . ? O5 C24 O4 122.1(2) . . ? O5 C24 C27 125.2(2) . . ? O4 C24 C27 112.7(2) . . ? C24 O4 C25 117.2(2) . . ? C26 C25 O4 109.4(3) . . ? C26 C25 H26 109.8 . . ? O4 C25 H26 109.8 . . ? C26 C25 H27 109.8 . . ? O4 C25 H27 109.8 . . ? H26 C25 H27 108.2 . . ? C25 C26 H23 109.5 . . ? C25 C26 H24 109.5 . . ? H23 C26 H24 109.5 . . ? C25 C26 H25 109.5 . . ? H23 C26 H25 109.5 . . ? H24 C26 H25 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 Cl1 C1 1.746(2) . ? C1 C2 1.377(3) . ? C1 C6 1.384(3) . ? C2 C3 1.392(3) . ? C2 H1 0.9500 . ? C3 C4 1.393(3) . ? C3 H2 0.9500 . ? C4 C5 1.405(3) . ? C4 C7 1.553(3) . ? C5 C6 1.388(3) . ? C5 H3 0.9500 . ? C6 H4 0.9500 . ? C7 O1 1.424(2) . ? C7 C8 1.545(3) . ? C7 C14 1.609(2) . ? O1 H5 0.8400 . ? C8 C13 1.397(3) . ? C8 C9 1.398(3) . ? C9 C10 1.381(3) . ? C9 H6 0.9500 . ? C10 C11 1.379(4) . ? C10 H7 0.9500 . ? C11 C12 1.384(4) . ? C11 H8 0.9500 . ? C12 C13 1.386(3) . ? C12 H9 0.9500 . ? C13 H10 0.9500 . ? C14 C17 1.538(2) . ? C14 C15 1.546(3) . ? C14 C16 1.550(3) . ? C15 H11 0.9800 . ? C15 H12 0.9800 . ? C15 H13 0.9800 . ? C16 F2 1.336(2) . ? C16 F3 1.339(2) . ? C16 F1 1.353(2) . ? C17 C18 1.395(3) . ? C17 C22 1.399(3) . ? C18 C19 1.388(3) . ? C18 H14 0.9500 . ? C19 C20 1.381(3) . ? C19 H15 0.9500 . ? C20 O2 1.374(2) . ? C20 C21 1.390(3) . ? C21 C22 1.387(3) . ? C21 H16 0.9500 . ? C22 H17 0.9500 . ? O2 H18 0.8400 . ? C27 C24 1.484(3) . ? C27 H19 0.9800 . ? C27 H20 0.9800 . ? C27 H21 0.9800 . ? O5 C24 1.210(3) . ? C24 O4 1.324(3) . ? O4 C25 1.475(4) . ? C25 C26 1.420(5) . ? C25 H26 0.9900 . ? C25 H27 0.9900 . ? C26 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 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 C2 H1 F3 0.95 2.61 3.550(2) 169.3 3_675 O1 H5 O2 0.84 2.03 2.8578(19) 170.6 4_575 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 C6 C1 C2 C3 1.3(3) . . . . ? Cl1 C1 C2 C3 179.70(15) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C2 C3 C4 C5 -1.7(3) . . . . ? C2 C3 C4 C7 176.88(17) . . . . ? C3 C4 C5 C6 1.2(3) . . . . ? C7 C4 C5 C6 -177.32(17) . . . . ? C2 C1 C6 C5 -1.8(3) . . . . ? Cl1 C1 C6 C5 179.82(15) . . . . ? C4 C5 C6 C1 0.5(3) . . . . ? C3 C4 C7 O1 13.5(2) . . . . ? C5 C4 C7 O1 -168.02(16) . . . . ? C3 C4 C7 C8 -105.21(18) . . . . ? C5 C4 C7 C8 73.3(2) . . . . ? C3 C4 C7 C14 125.76(17) . . . . ? C5 C4 C7 C14 -55.7(2) . . . . ? O1 C7 C8 C13 21.1(2) . . . . ? C4 C7 C8 C13 140.03(18) . . . . ? C14 C7 C8 C13 -93.9(2) . . . . ? O1 C7 C8 C9 -156.28(17) . . . . ? C4 C7 C8 C9 -37.3(2) . . . . ? C14 C7 C8 C9 88.7(2) . . . . ? C13 C8 C9 C10 0.8(3) . . . . ? C7 C8 C9 C10 178.22(19) . . . . ? C8 C9 C10 C11 -0.7(3) . . . . ? C9 C10 C11 C12 0.3(4) . . . . ? C10 C11 C12 C13 0.1(4) . . . . ? C11 C12 C13 C8 0.0(4) . . . . ? C9 C8 C13 C12 -0.4(3) . . . . ? C7 C8 C13 C12 -178.0(2) . . . . ? O1 C7 C14 C17 -172.27(14) . . . . ? C8 C7 C14 C17 -54.0(2) . . . . ? C4 C7 C14 C17 71.49(18) . . . . ? O1 C7 C14 C15 63.69(17) . . . . ? C8 C7 C14 C15 -178.02(15) . . . . ? C4 C7 C14 C15 -52.55(18) . . . . ? O1 C7 C14 C16 -50.73(18) . . . . ? C8 C7 C14 C16 67.55(19) . . . . ? C4 C7 C14 C16 -166.98(14) . . . . ? C17 C14 C16 F2 71.24(19) . . . . ? C15 C14 C16 F2 -169.77(15) . . . . ? C7 C14 C16 F2 -53.8(2) . . . . ? C17 C14 C16 F3 -165.07(15) . . . . ? C15 C14 C16 F3 -46.1(2) . . . . ? C7 C14 C16 F3 69.9(2) . . . . ? C17 C14 C16 F1 -47.8(2) . . . . ? C15 C14 C16 F1 71.23(18) . . . . ? C7 C14 C16 F1 -172.81(14) . . . . ? C15 C14 C17 C18 8.1(2) . . . . ? C16 C14 C17 C18 122.31(18) . . . . ? C7 C14 C17 C18 -113.41(19) . . . . ? C15 C14 C17 C22 -171.31(17) . . . . ? C16 C14 C17 C22 -57.1(2) . . . . ? C7 C14 C17 C22 67.2(2) . . . . ? C22 C17 C18 C19 -1.4(3) . . . . ? C14 C17 C18 C19 179.25(17) . . . . ? C17 C18 C19 C20 0.2(3) . . . . ? C18 C19 C20 O2 -179.60(17) . . . . ? C18 C19 C20 C21 0.6(3) . . . . ? O2 C20 C21 C22 -179.99(17) . . . . ? C19 C20 C21 C22 -0.2(3) . . . . ? C20 C21 C22 C17 -1.0(3) . . . . ? C18 C17 C22 C21 1.8(3) . . . . ? C14 C17 C22 C21 -178.84(16) . . . . ? O5 C24 O4 C25 0.7(4) . . . . ? C27 C24 O4 C25 179.4(3) . . . . ? C24 O4 C25 C26 -165.2(3) . . . . ?