#------------------------------------------------------------------------------ #$Date: 2020-06-04 06:54:28 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252640 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/75/7157529.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_7157529 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 'C17 H17 F3 O2' _chemical_formula_sum 'C17 H17 F3 O2' _chemical_formula_weight 310.30 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _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 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.3360(11) _cell_length_b 7.1684(3) _cell_length_c 16.7513(8) _cell_measurement_reflns_used 8196 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.9280 _cell_measurement_theta_min 2.5560 _cell_volume 2922.3(2) _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0608 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 20991 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.499 _diffrn_reflns_theta_min 2.432 _diffrn_source 'Rigaku VariMax' _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.24460 _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 1.411 _exptl_crystal_description block _exptl_crystal_F_000 1296 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.130 _refine_diff_density_max 0.200 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.040 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 203 _refine_ls_number_reflns 2724 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0369 _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^)+(0.0422P)^2^+0.9146P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.0989 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2283 _reflns_number_total 2724 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ob00951b2.cif _cod_data_source_block Kyu3 _cod_database_code 7157529 _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 0.975 _shelx_estimated_absorpt_t_max 0.985 _oxdiff_exptl_absorpt_empirical_full_min 0.338 _oxdiff_exptl_absorpt_empirical_full_max 2.154 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; Kyu3.res created by SHELXL-2014/7 TITL Kyu3_a.res in Pbcn REM Yadorkari-X generated CELL 0.71073 24.3360 7.1684 16.7513 90.0000 90.0000 90.0000 ZERR 8.0 0.0011 0.0003 0.0008 0.0000 0.0000 0.0000 LATT 1 SYMM 1/2-X, 1/2-Y, 1/2+Z SYMM 1/2+X, 1/2-Y, -Z SYMM -X, +Y, 1/2-Z REM SPGR Pbcn orthorhombic SFAC C H O F UNIT 136 136 16 24 SIZE 0.22 0.19 0.13 TEMP -100.0 L.S. 20 FMAP 2 PLAN -20 ACTA CONF HTAB LIST 4 BOND $H OMIT -10.000000 51.000000 EQIV $1 +X, -Y, -1/2+Z EQIV $2 1-X, -Y, 1-Z HTAB O1 O2_$1 HTAB O2 O1_$2 HTAB C16 F2 WGHT 0.042200 0.914600 FVAR 0.95723 F1 4 0.313841 0.500284 0.713328 11.00000 0.04573 0.04024 = 0.03043 0.00048 0.01417 0.01736 F2 4 0.288953 0.305776 0.623548 11.00000 0.02454 0.05513 = 0.03869 0.00084 0.00102 0.00609 F3 4 0.330994 0.558070 0.590660 11.00000 0.05819 0.04040 = 0.03287 0.01327 0.01284 0.02192 O1 3 0.480048 0.126986 0.349727 11.00000 0.03009 0.04363 = 0.02337 -0.01025 0.00493 -0.00236 AFIX 147 H1 2 0.456742 0.077089 0.319524 11.00000 -1.50000 AFIX 0 O2 3 0.438495 0.089088 0.726157 11.00000 0.02803 0.04592 = 0.02184 -0.00003 0.00303 0.01602 AFIX 147 H2 2 0.454610 0.044697 0.686087 11.00000 -1.50000 AFIX 0 C1 1 0.409483 0.279339 0.568290 11.00000 0.02347 0.02235 = 0.02090 -0.00030 0.00180 0.00146 C2 1 0.354188 0.170379 0.784681 11.00000 0.02471 0.02277 = 0.02162 0.00179 0.00013 0.00301 C3 1 0.455191 0.178805 0.419903 11.00000 0.02928 0.02435 = 0.02066 -0.00343 0.00523 0.00042 C4 1 0.386737 0.325812 0.651987 11.00000 0.02416 0.02413 = 0.02114 -0.00098 0.00246 0.00061 C5 1 0.383069 0.138891 0.704869 11.00000 0.02385 0.02458 = 0.02150 -0.00012 -0.00076 0.00407 C6 1 0.398845 0.183468 0.430026 11.00000 0.02794 0.03461 = 0.02271 -0.00530 -0.00493 0.00290 AFIX 43 H3 2 0.375278 0.153836 0.386630 11.00000 -1.20000 AFIX 0 C7 1 0.376690 0.231372 0.503483 11.00000 0.01976 0.03528 = 0.02872 -0.00405 0.00044 0.00437 AFIX 43 H4 2 0.337891 0.231421 0.509731 11.00000 -1.20000 AFIX 0 C8 1 0.381976 0.253326 0.848252 11.00000 0.02306 0.03430 = 0.02589 -0.00233 0.00089 0.00081 AFIX 43 H5 2 0.418994 0.292174 0.841352 11.00000 -1.20000 AFIX 0 C9 1 0.300255 0.113942 0.797216 11.00000 0.02811 0.03221 = 0.02965 0.00148 -0.00039 -0.00428 AFIX 43 H6 2 0.280469 0.056838 0.754874 11.00000 -1.20000 AFIX 0 C10 1 0.466088 0.278772 0.555474 11.00000 0.02576 0.03789 = 0.02329 -0.00577 -0.00058 -0.00451 AFIX 43 H7 2 0.489826 0.314004 0.597897 11.00000 -1.20000 AFIX 0 C11 1 0.488724 0.228475 0.482878 11.00000 0.02173 0.04191 = 0.02909 -0.00681 0.00514 -0.00413 AFIX 43 H8 2 0.527499 0.228103 0.476320 11.00000 -1.20000 AFIX 0 C12 1 0.330382 0.419434 0.644959 11.00000 0.03419 0.03259 = 0.02416 0.00386 0.00714 0.00696 C13 1 0.356570 0.279888 0.921016 11.00000 0.03601 0.03998 = 0.02415 -0.00724 0.00033 0.00355 AFIX 43 H9 2 0.376069 0.337773 0.963445 11.00000 -1.20000 AFIX 0 C14 1 0.302773 0.222586 0.932530 11.00000 0.03789 0.04033 = 0.02805 0.00004 0.01174 0.00647 AFIX 43 H10 2 0.285325 0.240348 0.982689 11.00000 -1.20000 AFIX 0 C15 1 0.423701 0.472646 0.692786 11.00000 0.04156 0.03199 = 0.02706 -0.00783 0.00884 -0.00869 AFIX 137 H11 2 0.429093 0.578642 0.656678 11.00000 -1.50000 H12 2 0.459377 0.416657 0.705527 11.00000 -1.50000 H13 2 0.406095 0.515833 0.742049 11.00000 -1.50000 AFIX 0 C16 1 0.358820 -0.025713 0.659125 11.00000 0.04733 0.02467 = 0.02938 -0.00179 0.00217 -0.00081 AFIX 137 H14 2 0.382495 -0.055706 0.613574 11.00000 -1.50000 H15 2 0.322037 0.007033 0.639873 11.00000 -1.50000 H16 2 0.356352 -0.134197 0.694545 11.00000 -1.50000 AFIX 0 C17 1 0.274854 0.139504 0.870365 11.00000 0.02717 0.04018 = 0.03870 0.00339 0.00857 -0.00331 AFIX 43 H17 2 0.237982 0.099568 0.877758 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM Kyu3_a.res in Pbcn REM R1 = 0.0369 for 2283 Fo > 4sig(Fo) and 0.0468 for all 2724 data REM 203 parameters refined using 0 restraints END WGHT 0.0379 1.0281 REM Instructions for potential hydrogen bonds HTAB O1 O2_$1 HTAB O2 O1_$2 HTAB C16 F2 REM Highest difference peak 0.200, deepest hole -0.260, 1-sigma level 0.040 Q1 1 0.3802 0.2415 0.6800 11.00000 0.05 0.20 Q2 1 0.4295 0.2497 0.4182 11.00000 0.05 0.19 Q3 1 0.3737 0.5848 0.6016 11.00000 0.05 0.18 Q4 1 0.3627 0.3734 0.6491 11.00000 0.05 0.18 Q5 1 0.3373 0.0914 0.7992 11.00000 0.05 0.18 Q6 1 0.3667 0.1650 0.7447 11.00000 0.05 0.17 Q7 1 0.4393 0.2211 0.5645 11.00000 0.05 0.17 Q8 1 0.3221 0.2120 0.7823 11.00000 0.05 0.16 Q9 1 0.4272 0.1198 0.4352 11.00000 0.05 0.15 Q10 1 0.3937 0.3170 0.6087 11.00000 0.05 0.15 Q11 1 0.4004 0.6188 0.6253 11.00000 0.05 0.14 Q12 1 0.4318 0.3263 0.5606 11.00000 0.05 0.14 Q13 1 0.3600 0.5618 0.7238 11.00000 0.05 0.13 Q14 1 0.3367 0.1961 0.9334 11.00000 0.05 0.13 Q15 1 0.4793 0.2002 0.5246 11.00000 0.05 0.13 Q16 1 0.5272 0.1364 0.4950 11.00000 0.05 0.12 Q17 1 0.4569 0.5026 0.6804 11.00000 0.05 0.12 Q18 1 0.4720 0.1519 0.4612 11.00000 0.05 0.12 Q19 1 0.3675 0.2411 0.8046 11.00000 0.05 0.12 Q20 1 0.4005 0.3938 0.6740 11.00000 0.05 0.12 ; _shelx_res_checksum 11734 _shelx_hkl_file ; 0 0 -2 3209.44 346.433 0 0 2 3925.31 347.427 0 0 3 2.93695 3.63288 0 0 -3-1.56823 3.38783 0 0 3-2.79378 8.21055 0 0 4 14506.7 1463.11 0 0 4 13848.4 1461.68 0 0 -4 14638.2 1461.54 0 0 5-2.34391 10.6963 0 0 5 0.39833 4.91738 0 0 -5 0.32314 4.49411 0 0 -5-15.1866 9.56619 0 0 6 187.600 26.2779 0 0 -6 225.172 26.5207 0 0 -6 208.609 22.6390 0 0 6 188.464 22.8466 0 0 -7-1.13833 11.5131 0 0 7 2.83128 6.31660 0 0 7-7.63796 11.8036 0 0 -7 2.60783 5.15817 0 0 -8 1325.41 143.196 0 0 8 1301.93 143.251 0 0 -8 1360.30 139.811 0 0 8 1356.75 140.541 0 0 -9-11.8847 14.2227 0 0 -9 4.94778 6.52460 0 0 9-7.02139 15.0846 0 0 9 5.59474 8.37111 0 0 10 124.631 24.3325 0 0 10 125.150 18.8106 0 0 -10 152.593 18.0130 0 0 -10 140.923 24.0617 0 0 -11-5.72082 7.49022 0 0 11-1.71698 15.6867 0 0 -11 7.33399 15.2016 0 0 11-1.97507 9.32807 0 0 12-4.38327 9.86364 0 0 12-7.48600 17.2646 0 0 -12 4.36071 8.05296 0 0 -12 12.0505 15.6287 0 0 -13 17.4454 20.1214 0 0 13-1.23742 11.9075 0 0 -13 5.13465 8.00309 0 0 -14 18189.5 2040.52 0 0 -14 20171.2 2043.25 0 0 -14 20609.9 2036.49 0 0 -15-2.53845 22.1491 0 0 -15 10.4905 18.5047 0 0 -16 568.113 69.3004 0 0 -16 511.903 66.6858 0 0 -17 11.5282 24.2067 0 0 -17 12.2619 22.4369 0 0 -18 30.7097 27.6144 0 0 -18 75.9351 27.8498 0 0 -19 22.2981 23.7005 0 0 -19 6.48994 27.8881 0 0 -20 23.9073 29.1380 0 0 -20 35.6444 28.9716 0 0 -21-14.2187 28.9390 0 0 -21 12.6602 28.1972 0 0 -22 693.276 91.1836 0 1 0 0.24301 2.70113 0 -1 0 1.49773 1.13502 0 1 0 2.89771 0.95452 0 -1 1-0.16072 1.66088 0 1 -1-4.44378 0.74178 0 1 1 1.61184 3.44427 0 1 1 0.56552 1.63081 0 1 2-1.72025 8.00646 0 1 -2-16.4282 2.23957 0 -1 2 3.42164 4.15399 0 -1 3 7.05656 6.92357 0 1 -3-6.81692 2.96280 0 -1 -3 3.58622 9.39979 0 1 3-9.65530 10.2048 0 -1 -4 3.14011 3.71738 0 1 -4-20.7696 3.86681 0 -1 4-0.46355 6.78088 0 1 4-0.71981 9.90061 0 -1 4 0.67857 9.86379 0 -1 -4-2.89773 8.91807 0 -1 -5-7.00300 10.2640 0 -1 5 8.27737 9.73432 0 1 -5-2.31595 4.69552 0 1 5 11.1813 4.68031 0 1 5 15.3402 10.1402 0 -1 -5 2.76956 3.65269 0 -1 -6-1.10823 4.52855 0 1 6-3.95231 11.1307 0 -1 6 2.94488 11.5805 0 -1 -6 1.04686 9.89015 0 1 -6-8.20077 5.68889 0 1 6-6.40821 5.35766 0 1 -6 1.93834 5.16098 0 1 -7 2.64036 5.40365 0 1 7 10.0908 12.5875 0 1 -7 1.14793 10.9911 0 1 7-2.30225 5.53838 0 -1 7 7.90445 12.4699 0 -1 -7-0.41976 5.09856 0 -1 -7-1.20610 11.9032 0 1 -7 15.9202 8.31695 0 1 -8 2.05328 9.60611 0 -1 8 2.52081 13.0988 0 1 8-2.52052 12.3833 0 1 -8-5.23128 12.2941 0 1 -8-1.92504 6.29347 0 1 8 2.67171 6.86216 0 -1 -8 2.73470 12.1815 0 -1 -8-0.46929 5.33592 0 -1 -9 4.14653 6.10924 0 1 -9 10.3556 12.3444 0 1 -9 4.30924 6.06089 0 1 9 4.64815 6.47405 0 1 -9 2.34640 10.8823 0 1 9-2.80891 14.2097 0 -1 -9 4.55144 12.8072 0 -1 9-4.08721 13.6740 0 1 -10 9.23862 12.8026 0 1 -10-1.75372 6.62577 0 -1 -10 3.32903 14.3631 0 1 -10 3.29269 14.5151 0 -1 -10 1.70036 6.38313 0 -1 10 3.09403 14.1329 0 1 10-13.9722 15.8879 0 1 10-1.77722 7.49747 0 1 -11 0.65490 6.80633 0 1 -11-10.2695 14.8962 0 -1 -11-0.59468 6.13360 0 -1 -11 1.78857 13.9176 0 1 11 4.09801 8.84058 0 1 11-8.52921 15.5074 0 1 -11 5.45056 15.5044 0 -1 11 10.2623 16.3734 0 1 12 7.86769 9.48449 0 1 -12-0.69161 7.56110 0 1 -12 1.98980 16.7891 0 1 -12-6.45566 15.3123 0 -1 -12 1.99952 15.4543 0 -1 -12 2.60644 6.56567 0 1 12-13.0425 18.3087 0 1 13 20.7499 12.7520 0 1 -13 10.7704 19.6256 0 -1 -13 22.1759 18.7556 0 1 -13 11.2356 9.95130 0 1 -13-12.3891 19.4543 0 -1 -14-7.24191 19.8960 0 1 14-4.07945 12.1811 0 1 -14-5.79258 9.20400 0 1 -14 18.5461 21.4903 0 1 -14-11.5612 17.1694 0 1 15 13.7275 13.6776 0 -1 -15 7.79503 21.5535 0 1 -15 12.4947 20.8528 0 1 -15 4.35525 8.87405 0 1 -15-6.27744 20.3106 0 1 -16-6.70547 21.8694 0 -1 -16 5.56649 22.7979 0 1 16 4.91829 15.1233 0 1 -16-10.7076 22.9715 0 -1 -17 2.96377 23.8546 0 1 -17 28.6152 25.1204 0 1 17 7.17840 16.0269 0 1 -17 9.50081 22.9670 0 -1 -18-12.5062 27.4253 0 -1 -18 7.54971 21.7221 0 1 -18 2.51010 21.1851 0 1 -18-24.3218 28.0504 0 1 -19-7.90929 24.9093 0 -1 -19 9.90411 25.5257 0 -1 -19 19.0765 24.5390 0 1 -19 6.44649 25.9253 0 -1 -20-6.91955 27.8164 0 1 -20-17.1382 28.5854 0 -1 -20 8.79589 26.5215 0 1 -20 11.0319 26.8695 0 1 -21-39.6863 34.6924 0 -1 -21 14.4328 31.4762 0 -1 -21 18.6490 27.6914 0 -1 -22-9.83652 27.3798 0 1 -22 11.3646 33.6031 0 -1 -22 41.4809 34.8143 0 -1 -23 24.2603 32.5229 0 2 0 20133.9 2097.69 0 2 0 20552.1 2096.25 0 -2 0 20945.1 2096.22 0 -2 0 19403.2 2097.64 0 2 -1 41.9084 8.51402 0 2 -1 35.7035 4.20104 0 -2 -1 34.1835 4.79149 0 2 1 32.8615 7.78967 0 2 1 32.8005 4.75150 0 -2 -1 42.4112 8.40467 0 -2 1 26.8102 4.51793 0 2 2 55637.2 116.394 0 -2 -2 56116.2 163.224 0 -2 2 55751.6 103.029 0 -2 -2 56043.9 108.484 0 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20.0913 -10 -1 3 131.819 21.5310 -10 -1 3 159.054 18.0303 -10 1 -3 158.074 17.5172 -10 -1 -3 132.324 16.8161 -10 1 3 182.130 23.7768 10 -1 3 148.177 15.5840 10 1 -3 148.337 17.3760 10 -1 4 145.688 15.2900 10 -1 -4 125.831 15.1076 10 -1 -4 138.200 18.3274 10 1 4 194.389 16.5916 10 -1 4 169.262 21.0525 -10 -1 -4 106.594 20.5732 -10 1 -4 170.665 20.5010 -10 1 -4 151.357 16.8666 10 1 4 135.261 21.7179 10 -1 -4 149.831 22.3610 10 -1 -4 118.236 15.3035 -10 -1 4 163.202 18.6651 -10 -1 -4 153.974 16.6144 10 1 -4 136.562 17.5528 10 -1 -5 78.0829 12.4912 -10 1 5 88.5133 10.3560 10 1 5 76.9830 16.2486 -10 -1 -5 84.3758 16.2192 10 1 5 63.1122 8.93265 10 -1 5 74.0032 16.3639 10 -1 -5 75.3447 9.72431 -10 1 -5 72.5713 9.47254 -10 1 -5 100.527 16.2748 10 -1 -5 58.3681 15.1000 -10 -1 5 69.9331 12.7800 10 -1 5 71.5632 8.16538 10 1 -5 85.9479 12.1089 -10 -1 -5 61.0025 9.64043 -10 -1 -6 1959.13 203.427 10 1 6 2032.85 208.159 -10 -1 6 1954.98 208.476 10 -1 -6 1781.20 207.634 -10 1 6 2234.86 204.908 10 1 -6 1876.89 207.143 -10 1 -6 1995.45 207.586 10 1 6 1961.10 203.439 10 -1 -6 1941.90 204.132 -10 -1 6 1889.05 205.407 -10 -1 -6 2013.53 208.779 10 -1 6 2063.08 202.866 10 -1 -6 1716.33 204.914 10 -1 6 1935.32 207.397 -10 1 -6 1949.24 203.036 10 1 -6 1994.32 205.099 10 1 7 599.397 62.1811 -10 -1 -7 542.202 54.8281 10 -1 -7 465.432 60.0228 -10 -1 7 481.666 60.8077 -10 1 7 550.181 57.1615 -10 -1 7 497.528 57.6947 10 1 -7 539.009 59.8530 10 -1 -7 479.276 56.8198 -10 1 -7 483.550 59.8736 10 -1 -7 457.234 55.8564 10 -1 7 465.066 59.6899 10 1 7 508.724 54.8186 -10 -1 -7 520.762 61.1135 10 1 -7 513.237 56.9401 -10 1 -7 545.921 54.1964 10 -1 7 524.495 54.3098 -10 1 -8 1653.83 178.437 10 1 8 2051.93 186.441 -10 -1 -8 1757.69 179.143 10 -1 8 1905.97 179.170 -10 1 -8 1797.33 184.882 10 -1 8 1625.01 184.065 -10 -1 -8 1849.24 186.172 10 1 -8 1903.62 184.790 10 -1 -8 1575.91 180.707 -10 -1 8 1869.47 186.064 -10 1 8 1849.49 181.697 10 1 -8 1761.83 181.687 10 1 8 1688.86 179.378 -10 -1 8 1750.91 182.432 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-5-3.00601 16.2728 29 2 5 12.3388 12.0396 29 -2 -5 8.20303 17.6978 29 2 6 292.709 34.1873 29 -2 -6 236.513 38.8929 29 2 -6 272.987 37.9363 29 2 -7 56.2947 21.0084 29 2 7 99.5282 16.6483 29 -2 -7 85.3821 23.7363 29 2 8 14.5266 10.5229 29 -2 -8 5.96117 21.9067 29 -2 -9 61.0747 24.1499 29 3 0 318.371 39.0919 29 3 -1 13.1170 12.6937 29 3 1 20.0529 12.9387 29 3 -2 47.1056 14.8043 29 3 2 28.4132 13.1348 29 3 -3 18.2961 15.6417 29 3 3 8.57131 10.8640 29 3 -4 29.3349 16.1650 29 3 4 24.4285 13.9359 29 3 -5 108.953 22.5443 29 3 5 115.958 18.9112 29 -3 -5 112.830 24.8699 29 3 6 72.8200 15.9852 29 -3 -6 47.2610 21.3683 29 3 7 8.59504 11.2784 29 -3 -7 27.1063 21.3436 29 -3 -8 83.1899 25.8641 29 3 8 97.0382 17.6884 29 -3 -9 30.3934 25.2529 29 3 9 36.6241 14.6474 29 4 0-2.41026 13.7911 29 4 2 33.3144 14.4786 29 4 3 132.955 23.4861 30 0 0 178.594 25.6496 30 0 -1-18.6873 15.4994 30 0 1 4.98921 11.6052 30 0 2 179.963 24.9344 30 0 -2 205.696 28.2182 30 0 -3-5.39677 15.4854 30 0 3 2.57150 10.1094 30 0 -4 43.2072 18.3529 30 0 -5-6.21121 18.2708 30 0 -6 343.446 45.4846 30 0 -7-16.1511 20.1466 30 0 -8 254.918 38.9220 30 -1 0 10.4499 12.7173 30 1 0-7.80210 12.9901 30 -1 -1 29.9916 13.9683 30 1 -1 42.6391 15.9858 30 1 1 31.7115 13.2890 30 -1 -2 22.5251 14.4305 30 1 -2 30.7829 14.7351 30 1 2 19.4858 11.3703 30 1 -3 59.9243 17.6949 30 1 3 53.7053 13.7998 30 -1 -3 74.6233 19.1851 30 1 -4-4.31388 16.0985 30 1 4 9.93138 10.9709 30 -1 -4 5.95241 17.3518 30 1 -5 126.980 26.0837 30 1 5 152.647 21.1621 30 -1 -5 120.007 26.0658 30 -1 -6 24.1915 20.6014 30 1 -6 51.2905 19.8163 30 -1 -7 255.886 37.4923 30 1 -7 252.719 37.2359 30 -1 -8 79.6205 24.4290 30 2 0 167.868 24.5567 30 2 -1 26.2086 13.5191 30 2 1 27.0920 12.1931 30 2 -2 65.5829 17.2242 30 2 2 37.6328 13.5038 30 2 -3 21.0853 14.3926 30 2 3 29.6397 12.1812 30 -2 -3 35.0565 17.5805 30 2 -4 109.146 20.5014 30 2 4 61.6537 15.6710 30 -2 -4 61.8209 21.3002 30 2 -5 86.9852 23.1567 30 2 5 128.705 20.1074 30 -2 -5 127.338 24.6795 30 2 -6 114.860 27.5746 30 2 6 208.914 24.1825 30 -2 -6 127.447 28.6908 30 2 7 6.85117 11.1025 30 -2 -7-3.73326 21.2287 30 -2 -8 203.429 34.6133 30 3 0-10.6851 13.2415 30 3 -1-7.31961 13.8717 30 3 1 3.42116 11.5341 30 3 -2 43.4600 15.3439 30 3 2 35.8391 14.0658 30 3 -3 10.9205 15.0500 30 3 3 25.4853 12.7526 30 3 4 37.8754 14.8663 30 3 5 9.89786 12.1850 30 3 7 8.83954 12.2025 30 -3 -7-18.9267 22.3233 30 -3 -8 14.2782 19.8397 31 0 0-2.23462 11.5699 31 0 -1 15.1185 13.1631 31 0 1 1.00174 12.2167 31 0 -2 26.2559 17.0465 31 0 2 46.3105 13.4110 31 0 -3 24.5624 15.9571 31 0 -4 186.525 29.9303 31 0 -5-1.56176 17.0119 31 0 -7-16.0890 20.5836 31 1 0 23.4770 13.9617 31 -1 -1 70.1446 18.5404 31 1 -1 80.3674 18.6579 31 1 1 98.8255 17.1286 31 -1 -2 3.74298 13.7108 31 1 -2-2.49557 14.2588 31 1 2 20.1081 12.3333 31 1 -3 36.4321 19.3755 31 1 3 20.1049 11.7575 31 -1 -3 62.5838 18.3400 31 1 -4 14.6884 17.1891 31 1 4 8.40260 10.7131 31 -1 -4-1.47471 18.3083 31 1 -5 263.962 34.3583 31 -1 -5 198.953 34.2346 31 1 -6 25.8946 18.0837 31 -1 -6 19.3603 19.1832 31 -1 -7 58.3087 23.0774 31 2 0 10.4553 12.6985 31 2 -1 9.68831 12.7797 31 2 1-3.35168 12.3820 31 2 2 172.201 26.7527 31 2 -2 241.231 30.3816 31 2 3 265.957 32.6943 31 2 -3 239.824 34.4278 31 2 4 281.053 33.6760 31 -2 -4 266.188 37.4148 31 2 -4 246.833 35.9036 31 2 5 370.374 44.5459 31 -2 -5 379.936 48.8813 31 2 6-1.99249 11.3992 31 -2 -6 10.5211 20.0009 31 -2 -7 20.5554 20.7394 31 3 2 28.9137 14.4187 31 3 3 15.0382 12.2989 31 3 4 281.657 35.7613 32 0 0 181.978 27.1560 32 0 -1 8.17387 13.3866 32 0 -2 45.2640 17.5405 32 0 -3 2.77953 15.0357 32 0 -4 314.480 41.6090 32 0 -5 1.56094 16.9442 32 1 0 11.3579 12.9660 32 1 -1 9.08710 14.7620 32 1 1-2.14844 11.7030 32 -1 -2 34.4578 16.3100 32 1 -2 31.0963 16.1753 32 1 2 12.4899 12.6991 32 -1 -3 139.693 26.1393 32 1 -3 174.853 26.5207 32 1 3 161.102 23.0225 32 1 -4-19.6871 18.4955 32 -1 -4 5.92926 17.9047 32 2 0 28.4631 14.2857 32 2 -1 64.0381 17.3384 32 2 1 70.5105 15.9405 32 2 2 93.7664 18.1262 32 2 3 35.6552 13.7128 32 2 4 15.7339 12.6358 32 2 5 65.9756 16.4108 32 -2 -6 29.7035 20.9486 33 0 -1-12.1163 13.8751 33 0 -2 6.36835 15.5136 33 0 -3-8.59107 17.8274 33 0 -4 28.0828 17.3598 33 1 0-4.61413 14.9107 33 1 1 241.934 30.9292 33 1 -1 222.033 31.8608 33 1 -2 51.1896 17.6921 33 1 2 47.4302 14.2520 33 -1 -4 48.2716 19.0308 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 82877 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, 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 F1 F 0.31384(4) 0.50028(13) 0.71333(5) 0.0388(3) Uani 1 1 d . . . . . F2 F 0.28895(4) 0.30578(14) 0.62355(6) 0.0395(3) Uani 1 1 d . . . . . F3 F 0.33099(4) 0.55807(13) 0.59066(6) 0.0438(3) Uani 1 1 d . . . . . O1 O 0.48005(4) 0.12699(16) 0.34973(6) 0.0324(3) Uani 1 1 d . . . . . H1 H 0.4567 0.0771 0.3195 0.049 Uiso 1 1 calc R U . . . O2 O 0.43849(4) 0.08909(16) 0.72616(6) 0.0319(3) Uani 1 1 d . . . . . H2 H 0.4546 0.0447 0.6861 0.048 Uiso 1 1 calc R U . . . C1 C 0.40948(6) 0.27934(19) 0.56829(8) 0.0222(3) Uani 1 1 d . . . . . C2 C 0.35419(6) 0.1704(2) 0.78468(8) 0.0230(3) Uani 1 1 d . . . . . C3 C 0.45519(6) 0.1788(2) 0.41990(9) 0.0248(3) Uani 1 1 d . . . . . C4 C 0.38674(6) 0.3258(2) 0.65199(8) 0.0231(3) Uani 1 1 d . . . . . C5 C 0.38307(6) 0.1389(2) 0.70487(8) 0.0233(3) Uani 1 1 d . . . . . C6 C 0.39885(6) 0.1835(2) 0.43003(9) 0.0284(4) Uani 1 1 d . . . . . H3 H 0.3753 0.1538 0.3866 0.034 Uiso 1 1 calc R U . . . C7 C 0.37669(6) 0.2314(2) 0.50348(9) 0.0279(3) Uani 1 1 d . . . . . H4 H 0.3379 0.2314 0.5097 0.034 Uiso 1 1 calc R U . . . C8 C 0.38198(6) 0.2533(2) 0.84825(9) 0.0277(3) Uani 1 1 d . . . . . H5 H 0.4190 0.2922 0.8414 0.033 Uiso 1 1 calc R U . . . C9 C 0.30026(6) 0.1139(2) 0.79722(10) 0.0300(4) Uani 1 1 d . . . . . H6 H 0.2805 0.0568 0.7549 0.036 Uiso 1 1 calc R U . . . C10 C 0.46609(6) 0.2788(2) 0.55547(9) 0.0290(4) Uani 1 1 d . . . . . H7 H 0.4898 0.3140 0.5979 0.035 Uiso 1 1 calc R U . . . C11 C 0.48872(6) 0.2285(2) 0.48288(9) 0.0309(4) Uani 1 1 d . . . . . H8 H 0.5275 0.2281 0.4763 0.037 Uiso 1 1 calc R U . . . C12 C 0.33038(7) 0.4194(2) 0.64496(9) 0.0303(4) Uani 1 1 d . . . . . C13 C 0.35657(7) 0.2799(2) 0.92102(10) 0.0334(4) Uani 1 1 d . . . . . H9 H 0.3761 0.3378 0.9634 0.040 Uiso 1 1 calc R U . . . C14 C 0.30277(7) 0.2226(2) 0.93253(10) 0.0354(4) Uani 1 1 d . . . . . H10 H 0.2853 0.2403 0.9827 0.043 Uiso 1 1 calc R U . . . C15 C 0.42370(7) 0.4726(2) 0.69279(9) 0.0335(4) Uani 1 1 d . . . . . H11 H 0.4291 0.5786 0.6567 0.050 Uiso 1 1 calc R U . . . H12 H 0.4594 0.4167 0.7055 0.050 Uiso 1 1 calc R U . . . H13 H 0.4061 0.5158 0.7420 0.050 Uiso 1 1 calc R U . . . C16 C 0.35882(7) -0.0257(2) 0.65912(10) 0.0338(4) Uani 1 1 d . . . . . H14 H 0.3825 -0.0557 0.6136 0.051 Uiso 1 1 calc R U . . . H15 H 0.3220 0.0070 0.6399 0.051 Uiso 1 1 calc R U . . . H16 H 0.3564 -0.1342 0.6945 0.051 Uiso 1 1 calc R U . . . C17 C 0.27485(7) 0.1395(2) 0.87036(10) 0.0354(4) Uani 1 1 d . . . . . H17 H 0.2380 0.0996 0.8778 0.042 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 F1 0.0457(6) 0.0402(5) 0.0304(5) 0.0005(4) 0.0142(4) 0.0174(5) F2 0.0245(5) 0.0551(6) 0.0387(6) 0.0008(5) 0.0010(4) 0.0061(4) F3 0.0582(6) 0.0404(6) 0.0329(5) 0.0133(4) 0.0128(5) 0.0219(5) O1 0.0301(6) 0.0436(7) 0.0234(6) -0.0102(5) 0.0049(4) -0.0024(5) O2 0.0280(6) 0.0459(7) 0.0218(6) 0.0000(5) 0.0030(4) 0.0160(5) C1 0.0235(7) 0.0223(7) 0.0209(7) -0.0003(6) 0.0018(6) 0.0015(6) C2 0.0247(8) 0.0228(7) 0.0216(8) 0.0018(6) 0.0001(6) 0.0030(6) C3 0.0293(8) 0.0244(7) 0.0207(8) -0.0034(6) 0.0052(6) 0.0004(6) C4 0.0242(8) 0.0241(7) 0.0211(7) -0.0010(6) 0.0025(6) 0.0006(6) C5 0.0239(8) 0.0246(7) 0.0215(8) -0.0001(6) -0.0008(6) 0.0041(6) C6 0.0279(8) 0.0346(8) 0.0227(8) -0.0053(7) -0.0049(6) 0.0029(6) C7 0.0198(7) 0.0353(8) 0.0287(8) -0.0041(7) 0.0004(6) 0.0044(6) C8 0.0231(8) 0.0343(8) 0.0259(8) -0.0023(6) 0.0009(6) 0.0008(6) C9 0.0281(8) 0.0322(8) 0.0296(9) 0.0015(7) -0.0004(7) -0.0043(7) C10 0.0258(8) 0.0379(8) 0.0233(8) -0.0058(7) -0.0006(6) -0.0045(7) C11 0.0217(8) 0.0419(9) 0.0291(9) -0.0068(7) 0.0051(6) -0.0041(7) C12 0.0342(9) 0.0326(8) 0.0242(8) 0.0039(7) 0.0071(7) 0.0070(7) C13 0.0360(9) 0.0400(9) 0.0242(9) -0.0072(7) 0.0003(7) 0.0036(7) C14 0.0379(9) 0.0403(9) 0.0281(9) 0.0000(7) 0.0117(7) 0.0065(7) C15 0.0416(9) 0.0320(8) 0.0271(8) -0.0078(7) 0.0088(7) -0.0087(7) C16 0.0473(10) 0.0247(8) 0.0294(9) -0.0018(7) 0.0022(7) -0.0008(7) C17 0.0272(8) 0.0402(9) 0.0387(10) 0.0034(8) 0.0086(7) -0.0033(7) 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' 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 C3 O1 H1 109.5 . . ? C5 O2 H2 109.5 . . ? C7 C1 C10 116.50(13) . . ? C7 C1 C4 123.82(12) . . ? C10 C1 C4 119.65(13) . . ? C9 C2 C8 117.83(14) . . ? C9 C2 C5 121.60(13) . . ? C8 C2 C5 120.55(13) . . ? O1 C3 C11 117.61(13) . . ? O1 C3 C6 123.27(13) . . ? C11 C3 C6 119.11(13) . . ? C12 C4 C15 104.89(12) . . ? C12 C4 C1 110.23(12) . . ? C15 C4 C1 109.89(12) . . ? C12 C4 C5 110.96(12) . . ? C15 C4 C5 110.88(12) . . ? C1 C4 C5 109.89(11) . . ? O2 C5 C16 107.15(12) . . ? O2 C5 C2 104.53(11) . . ? C16 C5 C2 112.08(12) . . ? O2 C5 C4 106.91(11) . . ? C16 C5 C4 112.90(12) . . ? C2 C5 C4 112.61(11) . . ? C3 C6 C7 120.04(14) . . ? C3 C6 H3 120.0 . . ? C7 C6 H3 120.0 . . ? C6 C7 C1 122.06(13) . . ? C6 C7 H4 119.0 . . ? C1 C7 H4 119.0 . . ? C13 C8 C2 121.07(14) . . ? C13 C8 H5 119.5 . . ? C2 C8 H5 119.5 . . ? C17 C9 C2 121.13(15) . . ? C17 C9 H6 119.4 . . ? C2 C9 H6 119.4 . . ? C11 C10 C1 121.99(14) . . ? C11 C10 H7 119.0 . . ? C1 C10 H7 119.0 . . ? C3 C11 C10 120.25(14) . . ? C3 C11 H8 119.9 . . ? C10 C11 H8 119.9 . . ? F2 C12 F1 105.29(12) . . ? F2 C12 F3 105.97(13) . . ? F1 C12 F3 105.09(12) . . ? F2 C12 C4 115.24(13) . . ? F1 C12 C4 113.04(13) . . ? F3 C12 C4 111.42(12) . . ? C8 C13 C14 120.36(15) . . ? C8 C13 H9 119.8 . . ? C14 C13 H9 119.8 . . ? C17 C14 C13 119.25(15) . . ? C17 C14 H10 120.4 . . ? C13 C14 H10 120.4 . . ? C4 C15 H11 109.5 . . ? C4 C15 H12 109.5 . . ? H11 C15 H12 109.5 . . ? C4 C15 H13 109.5 . . ? H11 C15 H13 109.5 . . ? H12 C15 H13 109.5 . . ? C5 C16 H14 109.5 . . ? C5 C16 H15 109.5 . . ? H14 C16 H15 109.5 . . ? C5 C16 H16 109.5 . . ? H14 C16 H16 109.5 . . ? H15 C16 H16 109.5 . . ? C14 C17 C9 120.37(15) . . ? C14 C17 H17 119.8 . . ? C9 C17 H17 119.8 . . ? 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 F1 C12 1.3452(17) . ? F2 C12 1.3450(19) . ? F3 C12 1.3473(18) . ? O1 C3 1.3732(17) . ? O1 H1 0.8400 . ? O2 C5 1.4401(17) . ? O2 H2 0.8400 . ? C1 C7 1.391(2) . ? C1 C10 1.394(2) . ? C1 C4 1.5437(19) . ? C2 C9 1.389(2) . ? C2 C8 1.395(2) . ? C2 C5 1.5272(19) . ? C3 C11 1.380(2) . ? C3 C6 1.382(2) . ? C4 C12 1.531(2) . ? C4 C15 1.544(2) . ? C4 C5 1.6088(19) . ? C5 C16 1.526(2) . ? C6 C7 1.387(2) . ? C6 H3 0.9500 . ? C7 H4 0.9500 . ? C8 C13 1.380(2) . ? C8 H5 0.9500 . ? C9 C17 1.385(2) . ? C9 H6 0.9500 . ? C10 C11 1.383(2) . ? C10 H7 0.9500 . ? C11 H8 0.9500 . ? C13 C14 1.386(2) . ? C13 H9 0.9500 . ? C14 C17 1.379(2) . ? C14 H10 0.9500 . ? C15 H11 0.9800 . ? C15 H12 0.9800 . ? C15 H13 0.9800 . ? C16 H14 0.9800 . ? C16 H15 0.9800 . ? C16 H16 0.9800 . ? C17 H17 0.9500 . ? 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 O1 H1 O2 0.84 2.02 2.7761(15) 150.2 8 O2 H2 O1 0.84 2.10 2.8186(14) 143.6 5_656 C16 H15 F2 0.98 2.30 2.9821(19) 125.5 . 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 C7 C1 C4 C12 -32.40(19) . . . . ? C10 C1 C4 C12 149.59(14) . . . . ? C7 C1 C4 C15 -147.53(14) . . . . ? C10 C1 C4 C15 34.46(18) . . . . ? C7 C1 C4 C5 90.20(16) . . . . ? C10 C1 C4 C5 -87.82(16) . . . . ? C9 C2 C5 O2 -141.33(14) . . . . ? C8 C2 C5 O2 37.08(17) . . . . ? C9 C2 C5 C16 -25.61(19) . . . . ? C8 C2 C5 C16 152.79(14) . . . . ? C9 C2 C5 C4 102.99(16) . . . . ? C8 C2 C5 C4 -78.61(16) . . . . ? C12 C4 C5 O2 -164.85(11) . . . . ? C15 C4 C5 O2 -48.71(15) . . . . ? C1 C4 C5 O2 72.98(13) . . . . ? C12 C4 C5 C16 77.57(15) . . . . ? C15 C4 C5 C16 -166.29(13) . . . . ? C1 C4 C5 C16 -44.60(16) . . . . ? C12 C4 C5 C2 -50.61(16) . . . . ? C15 C4 C5 C2 65.54(15) . . . . ? C1 C4 C5 C2 -172.78(11) . . . . ? O1 C3 C6 C7 177.87(14) . . . . ? C11 C3 C6 C7 -2.2(2) . . . . ? C3 C6 C7 C1 1.3(2) . . . . ? C10 C1 C7 C6 0.6(2) . . . . ? C4 C1 C7 C6 -177.42(14) . . . . ? C9 C2 C8 C13 -0.5(2) . . . . ? C5 C2 C8 C13 -179.00(14) . . . . ? C8 C2 C9 C17 0.1(2) . . . . ? C5 C2 C9 C17 178.57(14) . . . . ? C7 C1 C10 C11 -1.7(2) . . . . ? C4 C1 C10 C11 176.49(14) . . . . ? O1 C3 C11 C10 -178.86(14) . . . . ? C6 C3 C11 C10 1.2(2) . . . . ? C1 C10 C11 C3 0.8(2) . . . . ? C15 C4 C12 F2 -169.00(12) . . . . ? C1 C4 C12 F2 72.76(15) . . . . ? C5 C4 C12 F2 -49.21(16) . . . . ? C15 C4 C12 F1 -47.85(16) . . . . ? C1 C4 C12 F1 -166.10(12) . . . . ? C5 C4 C12 F1 71.93(16) . . . . ? C15 C4 C12 F3 70.23(15) . . . . ? C1 C4 C12 F3 -48.02(17) . . . . ? C5 C4 C12 F3 -169.99(12) . . . . ? C2 C8 C13 C14 0.6(2) . . . . ? C8 C13 C14 C17 -0.3(2) . . . . ? C13 C14 C17 C9 -0.1(2) . . . . ? C2 C9 C17 C14 0.2(2) . . . . ?