#------------------------------------------------------------------------------ #$Date: 2019-11-11 16:42:54 +0200 (Mon, 11 Nov 2019) $ #$Revision: 226599 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/51/4035113.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_4035113 loop_ _publ_author_name 'Zhou, Wen' 'Zhang, Yan-Xue' 'Nie, Xiao-Di' 'Si, Chang-Mei' 'Sun, Xun' 'Wei, Bang-Guo' _publ_section_title ; Approach to Chiral 1-Substituted Isoquinolone and 3-Substituted Isoindolin-1-one by Addition-Cyclization Process. ; _journal_issue 17 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 9879 _journal_page_last 9889 _journal_paper_doi 10.1021/acs.joc.8b01282 _journal_volume 83 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_sum 'C19 H20 F N O2 S' _chemical_formula_weight 345.42 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.4084(8) _cell_length_b 13.5716(13) _cell_length_c 15.4024(17) _cell_measurement_reflns_used 3586 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 51.763 _cell_measurement_theta_min 5.290 _cell_volume 1757.7(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_unetI/netI 0.0498 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 8211 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_min 2.760 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.305 _exptl_crystal_description prismatic _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.173 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.041 _refine_ls_abs_structure_details ; Flack x determined using 950 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.06(5) _refine_ls_extinction_coef 0.0109(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 221 _refine_ls_number_reflns 3428 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0447 _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^)+(0.0384P)^2^+0.4554P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.1008 _reflns_Friedel_coverage 0.728 _reflns_Friedel_fraction_full 0.984 _reflns_Friedel_fraction_max 0.980 _reflns_number_gt 2736 _reflns_number_total 3428 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b01282_si_001.cif _cod_data_source_block mo_d8v17574_0m _cod_database_code 4035113 _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 0.964 _shelx_estimated_absorpt_t_max 0.980 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_d8v17574_0m_a.res in P2(1)2(1)2(1) CELL 0.71073 8.4084 13.5716 15.4024 90 90 90 ZERR 4 0.0008 0.0013 0.0017 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O S F UNIT 76 80 4 8 4 4 OMIT 0 1 1 OMIT 0 0 2 OMIT -3.00 52.00 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 wpdb -1 size 0.18 0.15 0.10 mpla c10 > c15 mpla c1 > c6 htab conf TEMP 23 WGHT 0.038400 0.455400 EXTI 0.010883 FVAR 0.73170 S1 5 1.070425 0.605590 0.606623 11.00000 0.03740 0.04324 = 0.03741 -0.00073 0.00195 -0.00280 F1 6 0.409511 0.807641 0.798941 11.00000 0.05611 0.08052 = 0.14371 -0.02060 0.00123 0.02741 N1 3 0.975665 0.560198 0.700633 11.00000 0.03556 0.02965 = 0.03645 -0.00073 0.00344 0.00217 O1 4 1.102726 0.415685 0.678176 11.00000 0.06256 0.04147 = 0.06099 -0.00844 0.00465 0.01497 O2 4 1.079811 0.713048 0.620509 11.00000 0.06867 0.04016 = 0.04566 0.00059 0.00510 -0.01696 C1 1 0.972718 0.618236 0.852114 11.00000 0.02920 0.03826 = 0.03735 0.00179 -0.00083 0.00069 C2 1 0.997979 0.698386 0.906781 11.00000 0.06149 0.04562 = 0.05216 -0.00659 -0.01338 0.00545 AFIX 43 H2 2 0.970587 0.761418 0.888412 11.00000 -1.20000 AFIX 0 C3 1 1.063274 0.684905 0.987885 11.00000 0.10023 0.06700 = 0.05591 -0.01194 -0.03022 0.00670 AFIX 43 H3 2 1.080960 0.738967 1.023708 11.00000 -1.20000 AFIX 0 C4 1 1.102299 0.592380 1.016079 11.00000 0.07736 0.08719 = 0.04806 0.00243 -0.02812 0.01160 AFIX 43 H4 2 1.144742 0.583762 1.071317 11.00000 -1.20000 AFIX 0 C5 1 1.079096 0.512269 0.963225 11.00000 0.05310 0.05711 = 0.05182 0.01362 -0.00732 0.00726 AFIX 43 H5 2 1.106839 0.449595 0.982373 11.00000 -1.20000 AFIX 0 C6 1 1.013991 0.524969 0.880937 11.00000 0.03305 0.04258 = 0.03935 0.00647 0.00189 0.00186 C7 1 0.991024 0.440189 0.819188 11.00000 0.06181 0.03183 = 0.05537 0.01060 0.00348 0.00242 AFIX 23 H7A 2 1.059405 0.386049 0.836418 11.00000 -1.20000 H7B 2 0.881734 0.417613 0.822466 11.00000 -1.20000 AFIX 0 C8 1 1.028465 0.468871 0.727472 11.00000 0.03702 0.03101 = 0.05033 -0.00139 -0.00228 0.00259 C9 1 0.904926 0.631880 0.762174 11.00000 0.02921 0.02601 = 0.03703 0.00123 0.00145 0.00075 AFIX 13 H9 2 0.937641 0.697539 0.742624 11.00000 -1.20000 AFIX 0 C10 1 0.723310 0.631233 0.762703 11.00000 0.02867 0.03532 = 0.03584 0.00091 -0.00209 -0.00101 C11 1 0.632964 0.548124 0.746998 11.00000 0.04185 0.03775 = 0.05942 -0.00324 -0.00271 -0.00150 AFIX 43 H11 2 0.682889 0.488865 0.733710 11.00000 -1.20000 AFIX 0 C12 1 0.467834 0.552433 0.750919 11.00000 0.03663 0.06944 = 0.07007 0.00001 -0.00397 -0.01472 AFIX 43 H12 2 0.408424 0.495780 0.740820 11.00000 -1.20000 AFIX 0 C13 1 0.391619 0.639242 0.769500 11.00000 0.02975 0.07270 = 0.07255 -0.00581 0.00063 0.00119 AFIX 43 H13 2 0.281316 0.642549 0.772862 11.00000 -1.20000 AFIX 0 C14 1 0.483551 0.720353 0.782831 11.00000 0.04286 0.05373 = 0.06572 -0.00625 0.00008 0.01728 C15 1 0.646326 0.719816 0.780353 11.00000 0.03472 0.03848 = 0.05440 -0.00240 -0.00249 0.00500 AFIX 43 H15 2 0.704024 0.777197 0.790216 11.00000 -1.20000 AFIX 0 C16 1 0.917660 0.587365 0.521868 11.00000 0.04937 0.04903 = 0.03948 -0.00370 -0.00651 -0.00023 C17 1 0.882946 0.477590 0.515629 11.00000 0.08740 0.06075 = 0.07953 -0.00990 -0.03519 -0.00916 AFIX 137 H17A 2 0.833765 0.455619 0.568441 11.00000 -1.50000 H17B 2 0.980576 0.442310 0.506810 11.00000 -1.50000 H17C 2 0.812591 0.465564 0.467699 11.00000 -1.50000 AFIX 0 C18 1 1.001935 0.624676 0.439878 11.00000 0.08263 0.09860 = 0.04071 0.00144 -0.00442 -0.01121 AFIX 137 H18A 2 0.932334 0.617700 0.390854 11.00000 -1.50000 H18B 2 1.096802 0.586839 0.430332 11.00000 -1.50000 H18C 2 1.029407 0.692837 0.447137 11.00000 -1.50000 AFIX 0 C19 1 0.772217 0.649705 0.540539 11.00000 0.06514 0.08430 = 0.05290 0.00464 -0.01563 0.01626 AFIX 137 H19A 2 0.705520 0.651687 0.489983 11.00000 -1.50000 H19B 2 0.804799 0.715384 0.555342 11.00000 -1.50000 H19C 2 0.714147 0.621554 0.588127 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_d8v17574_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0447 for 2736 Fo > 4sig(Fo) and 0.0669 for all 3428 data REM 221 parameters refined using 0 restraints END WGHT 0.0273 0.4084 REM Instructions for potential hydrogen bonds HTAB C9 O2 EQIV $1 -x+2, y+1/2, -z+3/2 HTAB C15 O1_$1 HTAB C19 O2 REM Highest difference peak 0.173, deepest hole -0.184, 1-sigma level 0.041 Q1 1 0.4064 0.4589 0.7442 11.00000 0.05 0.17 Q2 1 0.4675 0.8996 0.7797 11.00000 0.05 0.17 Q3 1 0.6444 0.6723 0.6787 11.00000 0.05 0.15 Q4 1 1.1171 0.6046 0.7058 11.00000 0.05 0.15 Q5 1 1.0812 0.7567 0.6160 11.00000 0.05 0.15 Q6 1 0.9908 0.7781 0.8430 11.00000 0.05 0.15 Q7 1 1.1629 0.7593 0.9984 11.00000 0.05 0.14 Q8 1 1.1302 0.4798 0.6595 11.00000 0.05 0.14 Q9 1 1.0763 0.5409 0.6149 11.00000 0.05 0.13 Q10 1 1.1453 0.6647 0.5502 11.00000 0.05 0.13 Q11 1 0.9261 0.5603 0.9062 11.00000 0.05 0.13 Q12 1 1.0029 0.5789 0.8611 11.00000 0.05 0.13 Q13 1 1.0250 0.6054 0.5765 11.00000 0.05 0.13 Q14 1 0.3603 0.7578 0.7327 11.00000 0.05 0.13 Q15 1 1.0265 0.6656 0.6863 11.00000 0.05 0.13 Q16 1 0.2216 0.5612 0.7259 11.00000 0.05 0.13 Q17 1 0.3069 0.6271 0.8993 11.00000 0.05 0.13 Q18 1 0.9900 0.5200 0.9532 11.00000 0.05 0.13 Q19 1 0.6084 0.5414 0.6573 11.00000 0.05 0.13 Q20 1 0.9396 0.5584 0.6355 11.00000 0.05 0.13 ; _shelx_res_checksum 1078 _shelx_hkl_file ; 1 0 0 6.40 0.90 3 0 0 2.00 1.50 -3 0 0 1.30 2.30 -4 0 0 4.70 2.80 4 0 0 3.80 1.60 5 0 0 9.10 2.20 -5 0 0 -2.00 3.20 6 0 0 608.84 15.50 -6 0 0 608.54 18.80 7 0 0 6.00 2.60 -1 1 0 67.79 3.00 -2 1 0 63.09 4.20 2 -1 0 56.79 3.60 -3 1 0 2274.17 31.60 3 -1 0 2273.27 31.50 -4 1 0 77.99 6.20 4 -1 0 75.99 5.00 5 -1 0 302.77 10.70 -5 1 0 322.67 12.60 6 -1 0 -0.40 2.10 -6 1 0 2.90 4.50 -7 1 0 -0.80 4.90 7 -1 0 1.50 3.90 -8 1 0 -4.20 4.50 8 -1 0 -0.90 2.40 9 -1 0 26.00 5.40 0 2 0 2273.67 26.30 0 -2 0 2043.20 26.00 -1 2 0 7050.09 76.79 -2 2 0 1090.39 18.80 2 -2 0 1106.09 19.00 -3 2 0 1603.84 26.20 3 -2 0 1643.24 26.60 -4 2 0 13.40 3.60 4 -2 0 13.70 3.10 -5 2 0 218.88 10.80 5 -2 0 216.28 9.60 -6 2 0 17.00 6.00 6 -2 0 19.90 4.40 -7 2 0 362.86 16.10 7 -2 0 357.46 14.10 8 -2 0 5.00 2.60 -8 2 0 4.00 5.20 9 -2 0 54.39 7.10 -9 2 0 62.99 15.80 -10 2 0 -10.30 5.30 10 -2 0 3.10 3.90 0 -3 0 0.60 1.00 0 3 0 0.40 1.00 -1 -3 0 154.38 4.80 1 -3 0 159.38 6.30 1 3 0 150.98 4.70 -1 3 0 157.78 6.30 2 -3 0 38.60 3.70 -2 3 0 43.10 4.10 -3 3 0 222.38 9.20 3 -3 0 233.58 9.30 -4 3 0 41.30 5.50 4 -3 0 47.10 4.90 -5 3 0 101.99 8.70 5 -3 0 112.29 7.70 6 -3 0 -3.60 2.20 -6 3 0 -0.10 4.50 8 -3 0 44.10 6.70 -8 3 0 55.89 12.20 9 -3 0 2.20 3.50 -9 3 0 8.60 6.30 10 -3 0 25.10 5.70 0 4 0 1193.88 20.10 0 -4 0 1219.68 20.40 1 4 0 1463.45 21.50 -1 -4 0 1473.25 21.80 -1 4 0 1470.05 24.70 1 -4 0 1488.95 24.90 -2 4 0 28.00 3.70 2 -4 0 35.60 3.90 -3 4 0 2.00 2.30 3 -4 0 3.10 2.00 -4 4 0 9.00 3.60 4 -4 0 8.90 2.60 -5 4 0 42.90 6.80 5 -4 0 41.10 5.30 6 -4 0 702.33 21.50 -6 4 0 716.93 23.00 -7 4 0 1.00 6.20 7 -4 0 1.90 3.00 -8 4 0 78.09 10.90 8 -4 0 71.09 8.20 9 -4 0 26.70 5.40 0 -5 0 -1.50 1.00 0 5 0 -1.20 1.10 1 -5 0 285.57 10.30 1 5 0 297.67 8.80 -1 -5 0 294.07 9.00 -1 5 0 292.17 10.40 2 5 0 619.14 12.30 2 -5 0 633.64 16.90 -2 5 0 627.64 16.80 -3 5 0 375.96 13.70 3 -5 0 369.76 13.60 4 -5 0 3.90 2.70 -4 5 0 8.80 3.60 -5 5 0 131.29 10.40 5 -5 0 129.99 9.10 6 -5 0 225.98 12.70 -6 5 0 210.48 14.10 -7 5 0 105.39 11.30 7 -5 0 100.09 9.30 8 -5 0 28.90 5.90 9 -5 0 53.89 8.80 10 -5 0 11.80 5.20 0 -6 0 747.03 17.60 0 6 0 732.03 19.90 -1 6 0 642.34 17.00 1 6 0 621.84 14.70 -1 -6 0 616.14 15.00 1 -6 0 624.84 16.90 -2 6 0 549.15 16.60 -2 -6 0 548.85 13.20 2 -6 0 579.54 17.20 2 6 0 562.04 12.80 3 -6 0 67.69 6.40 -3 6 0 54.89 6.40 -4 6 0 55.29 7.50 4 -6 0 60.59 6.40 5 -6 0 10.50 3.40 -5 6 0 1.90 4.30 6 -6 0 6.10 3.80 -6 6 0 13.60 6.10 7 -6 0 43.80 7.10 8 -6 0 7.80 4.50 9 -6 0 38.70 7.40 10 -6 0 -0.20 4.80 0 -7 0 3.20 2.00 0 7 0 1.40 1.90 -1 -7 0 147.69 7.70 1 -7 0 142.09 8.90 -1 7 0 151.88 8.70 -2 7 0 15.20 3.80 2 -7 0 16.90 4.20 -2 -7 0 22.70 3.40 2 7 0 20.30 3.20 -3 7 0 13.20 4.40 3 -7 0 15.50 4.10 4 -7 0 127.39 9.60 -4 7 0 134.99 10.50 5 -7 0 135.89 10.60 -5 7 0 161.08 12.40 6 -7 0 196.88 13.10 -6 7 0 197.58 14.60 7 -7 0 8.20 4.20 8 -7 0 9.10 4.10 9 -7 0 10.60 4.70 10 -7 0 16.60 7.20 0 8 0 13.50 3.50 -1 -8 0 746.23 19.40 1 -8 0 762.62 21.40 -1 8 0 750.02 20.90 1 8 0 768.62 19.20 2 -8 0 178.78 10.70 2 8 0 178.18 8.40 -2 8 0 173.48 10.60 -2 -8 0 180.58 8.70 3 -8 0 1.90 2.90 -3 8 0 8.40 4.40 3 8 0 5.90 2.50 4 -8 0 -1.00 2.40 -4 8 0 -1.30 4.20 -5 8 0 151.38 12.90 5 -8 0 157.48 11.90 6 -8 0 77.29 9.20 7 -8 0 87.89 10.20 8 -8 0 17.80 5.60 9 -8 0 8.10 5.10 0 -9 0 -0.30 1.90 0 9 0 2.40 2.80 1 -9 0 71.69 7.10 1 9 0 77.69 6.70 -1 9 0 71.29 7.40 -1 -9 0 72.09 6.60 -2 9 0 2.40 3.60 -2 -9 0 7.70 3.10 2 9 0 6.50 2.90 2 -9 0 9.10 3.40 -3 -9 0 426.06 13.80 -3 9 0 426.06 18.40 3 9 0 421.06 13.00 3 -9 0 442.26 18.60 4 -9 0 14.20 4.80 -4 9 0 18.60 5.80 5 -9 0 213.08 14.10 6 -9 0 -4.60 3.50 7 -9 0 4.70 3.60 8 -9 0 -0.80 4.30 9 -9 0 16.80 7.20 0 -10 0 377.26 15.90 0 10 0 356.56 15.40 -1 -10 0 32.50 5.80 -1 10 0 43.60 6.90 1 10 0 20.70 4.70 1 -10 0 30.90 5.80 2 10 0 213.88 10.60 2 -10 0 216.68 13.00 -2 -10 0 186.68 10.30 -2 10 0 188.78 12.80 3 -10 0 39.70 7.10 -3 -10 0 37.00 5.10 -3 10 0 36.90 6.70 4 -10 0 162.28 12.40 5 -10 0 28.00 7.20 6 -10 0 203.88 14.80 7 -10 0 2.20 4.80 8 -10 0 62.49 10.10 0 -11 0 6.20 3.40 0 11 0 -1.40 5.70 1 -11 0 180.38 12.30 -1 11 0 199.08 13.20 -1 -11 0 187.18 11.30 1 11 0 187.08 11.70 -2 -11 0 261.27 12.80 -2 11 0 256.07 16.00 2 -11 0 245.48 14.70 2 11 0 264.37 12.70 -3 -11 0 43.20 5.80 3 11 0 42.40 6.20 3 -11 0 48.30 8.10 4 -11 0 101.69 11.80 5 -11 0 -5.20 3.00 6 -11 0 -1.90 3.60 7 -11 0 22.10 6.50 8 -11 0 28.60 6.70 0 12 0 442.26 19.00 0 -12 0 427.46 18.90 -1 -12 0 511.35 19.90 1 12 0 489.05 21.10 1 -12 0 485.05 20.70 2 12 0 79.49 8.80 -2 -12 0 78.29 7.90 2 -12 0 84.49 9.60 3 12 0 27.90 5.50 -3 -12 0 26.80 5.40 3 -12 0 17.30 5.70 4 -12 0 39.70 8.40 5 -12 0 9.90 5.00 6 -12 0 8.40 5.20 7 -12 0 -3.70 4.10 0 -13 0 -4.80 3.10 -1 -13 0 3.50 3.40 1 13 0 6.10 4.50 1 -13 0 2.70 3.20 2 -13 0 27.90 6.40 -2 -13 0 36.90 6.00 2 13 0 40.70 6.90 3 13 0 9.10 4.40 3 -13 0 1.20 3.80 -3 -13 0 0.30 2.80 4 -13 0 93.39 10.80 5 -13 0 7.50 5.40 6 -13 0 -7.70 4.30 7 -13 0 6.20 5.70 0 -14 0 -4.30 3.70 1 -14 0 14.60 5.30 -1 -14 0 18.40 5.30 2 14 0 46.60 7.90 2 -14 0 31.20 7.20 -2 -14 0 52.29 7.50 3 14 0 -5.50 4.00 -3 -14 0 6.90 3.30 3 -14 0 5.90 4.40 4 -14 0 12.70 4.80 5 -14 0 5.80 4.90 6 -14 0 -1.60 5.50 0 -15 0 -3.00 3.30 1 -15 0 24.80 6.50 -1 -15 0 26.20 6.50 2 -15 0 11.50 4.70 -2 -15 0 6.40 4.10 -3 -15 0 52.09 8.80 3 -15 0 54.39 8.80 4 15 0 6.90 5.40 -4 -15 0 -1.30 3.60 4 -15 0 17.70 4.80 5 -15 0 83.29 11.20 0 -16 0 12.50 4.80 -1 -16 0 2.60 3.60 1 -16 0 -7.30 3.60 2 -16 0 -0.60 4.10 -2 -16 0 2.00 3.40 3 -16 0 12.70 4.60 -3 -16 0 -4.50 4.00 4 -16 0 30.70 7.40 0 -17 0 4.00 4.70 1 -17 0 4.80 5.00 -1 -17 0 -2.10 4.40 -2 -17 0 53.19 9.50 1 0 1 3345.57 36.20 1 0 -1 3399.06 37.50 2 0 -1 215.68 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7.00 -2 -5 -16 21.80 8.20 2 -5 -16 14.40 9.10 -2 5 -16 9.30 7.50 -3 -5 -16 -1.20 6.60 3 5 -16 -3.20 5.70 3 -5 -16 -9.40 7.50 -3 5 -16 0.90 5.50 4 5 -16 20.00 8.20 4 -5 -16 13.80 7.60 -5 -5 -16 -1.70 7.10 5 5 -16 23.10 8.80 -5 5 -16 3.80 6.20 5 -5 -16 0.80 8.00 0 6 -16 -3.00 4.90 0 -6 -16 -1.30 7.40 1 6 -16 13.20 6.80 -1 -6 -16 13.30 8.00 -1 6 -16 19.10 7.10 1 -6 -16 12.30 8.60 2 6 -16 16.30 8.00 -2 -6 -16 5.60 7.30 2 -6 -16 8.60 7.80 -2 6 -16 24.20 7.90 3 6 -16 16.00 8.50 -3 -6 -16 23.50 9.20 -3 6 -16 19.10 7.80 3 -6 -16 3.30 8.60 4 6 -16 14.40 8.90 4 -6 -16 30.70 13.90 -4 6 -16 20.40 8.00 -5 -6 -16 17.00 7.40 5 6 -16 8.50 9.20 5 -6 -16 7.20 8.30 -5 6 -16 17.60 7.30 0 7 -16 0.10 5.50 0 -7 -16 1.40 7.30 1 7 -16 40.80 9.90 -1 -7 -16 42.70 9.50 -1 7 -16 37.50 10.30 1 -7 -16 26.80 9.30 2 7 -16 10.50 6.50 -2 -7 -16 8.70 7.30 -2 7 -16 -4.90 5.20 2 -7 -16 10.30 7.30 3 7 -16 12.20 7.20 -3 -7 -16 17.10 8.10 -3 7 -16 17.10 6.80 3 -7 -16 33.40 10.00 -4 -7 -16 27.00 13.90 4 7 -16 8.90 9.10 4 -7 -16 11.20 8.10 -4 7 -16 3.70 6.90 0 -8 -16 -6.70 6.90 0 8 -16 8.90 6.90 -1 -8 -16 22.80 8.30 1 8 -16 2.60 6.20 1 -8 -16 3.10 6.50 -1 8 -16 -2.40 5.20 2 8 -16 1.30 7.00 -2 -8 -16 3.10 7.00 -2 8 -16 23.70 7.50 2 -8 -16 5.20 7.10 -3 -8 -16 1.60 6.30 3 8 -16 -1.20 7.90 3 -8 -16 -1.30 12.40 -4 -8 -16 11.80 8.80 4 -8 -16 16.40 8.60 -4 8 -16 9.60 7.40 0 -9 -16 10.30 8.40 -1 -9 -16 13.70 7.70 1 -9 -16 0.00 7.20 -1 9 -16 4.30 6.80 -2 -9 -16 44.90 9.60 2 -9 -16 44.30 13.50 -2 9 -16 48.10 10.60 -3 -9 -16 5.70 6.90 3 9 -16 18.90 7.40 3 -9 -16 1.40 6.80 0 -10 -16 12.00 7.70 0 10 -16 17.40 6.90 -1 -10 -16 -2.40 7.00 1 10 -16 24.50 8.30 -1 10 -16 9.40 7.00 1 -10 -16 8.90 8.60 -2 -10 -16 6.40 7.30 2 10 -16 10.20 8.40 2 -10 -16 15.90 8.00 -2 10 -16 15.80 8.50 0 0 -17 3.20 6.80 1 0 -17 24.60 8.50 -1 0 -17 27.30 9.00 2 0 -17 74.19 13.80 -2 0 -17 88.59 13.30 -3 0 -17 -7.80 5.60 3 0 -17 -1.90 7.60 -4 0 -17 36.80 9.50 4 0 -17 55.49 11.60 -5 0 -17 3.10 6.80 5 0 -17 -9.30 9.70 0 1 -17 9.90 6.80 0 -1 -17 8.70 7.30 1 1 -17 -3.30 6.50 -1 -1 -17 -5.50 6.20 1 -1 -17 2.30 7.80 -1 1 -17 20.00 8.10 2 1 -17 104.19 13.70 -2 -1 -17 96.39 13.30 2 -1 -17 98.69 14.90 -2 1 -17 87.39 12.60 3 1 -17 17.40 8.00 -3 -1 -17 29.20 8.90 3 -1 -17 17.00 8.90 -3 1 -17 40.10 9.10 -4 -1 -17 89.09 12.40 4 1 -17 65.39 12.80 4 -1 -17 46.90 11.90 -4 1 -17 87.09 11.90 5 1 -17 10.60 12.30 -5 -1 -17 18.70 7.70 -5 1 -17 7.90 6.50 5 -1 -17 -1.60 8.70 0 2 -17 40.40 9.80 0 -2 -17 31.10 9.30 1 2 -17 31.50 9.00 -1 -2 -17 14.70 8.40 1 -2 -17 30.60 9.50 -1 2 -17 28.50 8.20 -2 -2 -17 5.70 6.90 2 2 -17 3.40 6.70 2 -2 -17 13.70 8.70 -2 2 -17 -4.00 5.60 -3 -2 -17 4.00 7.10 3 2 -17 9.90 7.80 3 -2 -17 -9.30 7.90 -3 2 -17 2.40 5.90 -4 -2 -17 -8.10 5.70 4 2 -17 -3.80 7.10 4 -2 -17 3.30 7.50 -4 2 -17 5.30 6.50 5 2 -17 -12.20 10.50 -5 -2 -17 17.70 7.40 -5 2 -17 -11.40 5.50 5 -2 -17 -1.10 8.60 0 3 -17 -2.20 5.40 0 -3 -17 16.90 8.90 1 3 -17 32.10 9.20 -1 -3 -17 49.80 11.40 -1 3 -17 53.49 11.00 1 -3 -17 47.80 10.80 -2 -3 -17 -9.10 6.20 2 3 -17 6.40 6.80 2 -3 -17 -0.10 6.20 -2 3 -17 -6.50 4.90 3 3 -17 74.69 13.30 -3 -3 -17 96.79 13.80 -3 3 -17 95.09 13.00 3 -3 -17 114.19 16.50 -4 -3 -17 0.40 7.10 4 3 -17 -10.10 7.50 4 -3 -17 2.60 10.10 -4 3 -17 4.20 6.30 5 3 -17 0.90 9.70 -5 -3 -17 18.10 8.50 -5 3 -17 22.90 7.90 5 -3 -17 27.70 10.00 0 -4 -17 6.70 7.10 0 4 -17 6.10 5.90 1 4 -17 14.90 7.00 -1 -4 -17 5.00 8.60 1 -4 -17 8.40 8.30 -1 4 -17 29.30 9.20 -2 -4 -17 6.80 7.60 2 4 -17 -1.70 6.10 2 -4 -17 9.50 8.30 -2 4 -17 1.90 6.30 3 4 -17 19.00 8.40 -3 -4 -17 -3.90 6.20 -3 4 -17 -4.10 6.10 3 -4 -17 8.20 8.90 4 4 -17 21.50 9.60 -4 -4 -17 20.80 8.50 -4 4 -17 2.70 6.50 4 -4 -17 22.90 13.20 5 4 -17 16.10 8.30 -5 -4 -17 -4.40 7.30 5 -4 -17 -11.30 7.60 -5 4 -17 8.80 7.10 0 -5 -17 -3.00 7.50 0 5 -17 -7.10 5.00 1 5 -17 -2.10 5.10 -1 -5 -17 8.00 7.80 1 -5 -17 -0.30 7.20 -2 -5 -17 53.29 11.50 2 5 -17 45.30 10.10 -2 5 -17 50.79 10.00 2 -5 -17 56.69 11.50 3 5 -17 -6.20 6.80 3 -5 -17 5.20 7.70 -3 5 -17 16.80 6.20 -4 -5 -17 65.99 11.60 -4 5 -17 45.70 9.80 4 -5 -17 32.50 10.90 0 6 -17 53.79 10.70 -1 -6 -17 0.70 8.20 1 6 -17 25.50 7.50 1 -6 -17 11.50 9.10 -1 6 -17 3.30 6.10 -2 -6 -17 16.10 8.40 2 6 -17 13.10 7.70 -2 6 -17 10.90 7.80 2 -6 -17 21.10 8.50 -3 -6 -17 8.30 7.40 3 -6 -17 -7.60 11.10 -3 6 -17 -9.20 5.60 4 6 -17 8.50 8.80 -4 -6 -17 11.20 7.40 4 -6 -17 7.60 8.10 -4 6 -17 3.90 10.10 0 7 -17 17.80 8.70 0 -7 -17 4.60 7.40 1 7 -17 6.40 10.90 -1 -7 -17 6.90 7.40 1 -7 -17 4.10 7.70 -1 7 -17 4.10 9.50 -2 -7 -17 25.20 8.70 2 -7 -17 21.70 9.60 3 7 -17 51.59 11.50 -3 -7 -17 24.10 9.00 3 -7 -17 19.00 9.90 -3 7 -17 36.10 9.90 0 8 -17 30.40 9.60 0 -8 -17 42.40 10.30 1 8 -17 9.70 8.00 -1 8 -17 16.20 7.80 1 -8 -17 18.30 8.70 -2 -8 -17 23.40 9.00 2 8 -17 6.10 7.00 2 -8 -17 8.70 8.90 -2 8 -17 27.20 8.40 0 9 -17 5.80 7.10 0 -9 -17 18.70 7.90 -1 -9 -17 36.20 9.30 1 9 -17 41.90 11.40 -1 9 -17 50.59 10.80 1 -9 -17 44.50 15.10 0 0 -18 27.60 9.20 -1 0 -18 -1.40 6.10 1 0 -18 -13.90 6.90 2 0 -18 25.70 9.20 -2 0 -18 17.90 7.90 3 0 -18 -2.00 11.30 4 0 -18 1.50 8.10 -4 0 -18 -7.00 6.80 0 -1 -18 4.30 6.60 0 1 -18 6.20 6.70 1 1 -18 4.90 7.40 -1 -1 -18 25.70 7.90 1 -1 -18 18.00 8.70 -1 1 -18 9.00 6.50 -2 -1 -18 28.00 9.30 2 1 -18 15.00 7.40 2 -1 -18 18.30 8.80 -2 1 -18 12.50 6.80 3 1 -18 57.39 18.10 -3 -1 -18 30.10 8.40 -3 1 -18 35.40 8.90 3 -1 -18 62.99 17.90 4 1 -18 20.90 10.20 -4 -1 -18 20.70 8.10 -4 1 -18 11.80 7.50 4 -1 -18 34.90 11.60 0 -2 -18 -5.60 7.70 1 2 -18 17.70 8.70 -1 -2 -18 1.10 7.20 -1 2 -18 23.10 7.40 -2 -2 -18 -1.60 6.20 2 2 -18 -1.90 6.90 2 -2 -18 20.50 8.40 -2 2 -18 -5.10 5.30 -3 -2 -18 -5.50 6.50 -3 2 -18 19.60 7.20 4 2 -18 10.40 9.00 -4 -2 -18 11.90 7.50 4 -2 -18 31.40 10.60 -4 2 -18 8.90 6.40 0 3 -18 5.40 7.20 0 -3 -18 16.70 8.50 -1 -3 -18 2.30 7.50 1 3 -18 12.60 8.30 -1 3 -18 1.30 6.30 1 -3 -18 16.70 8.60 2 3 -18 12.70 9.40 -2 -3 -18 2.70 7.70 2 -3 -18 17.60 8.60 -2 3 -18 14.80 6.50 -3 -3 -18 8.20 7.50 3 3 -18 13.90 9.80 -3 3 -18 20.50 7.10 3 -3 -18 -5.50 8.80 -4 -3 -18 38.50 10.00 4 3 -18 10.10 9.20 -4 3 -18 16.60 8.80 4 -3 -18 18.60 10.10 0 4 -18 -5.60 5.20 0 -4 -18 1.80 7.60 -1 -4 -18 -8.60 6.70 1 4 -18 21.40 8.00 1 -4 -18 -9.90 7.40 -1 4 -18 -2.50 6.00 2 4 -18 16.60 15.70 -2 -4 -18 8.40 7.20 -2 4 -18 -2.30 6.40 2 -4 -18 -1.00 8.40 -3 -4 -18 24.40 8.80 3 4 -18 39.20 10.50 -3 4 -18 9.70 7.60 3 -4 -18 -11.30 7.80 -4 -4 -18 24.30 8.00 4 -4 -18 15.50 9.60 0 5 -18 36.00 13.90 0 -5 -18 19.40 9.30 -1 -5 -18 4.70 7.90 -1 5 -18 -5.50 10.30 1 -5 -18 7.00 9.30 -2 -5 -18 -8.40 6.70 2 5 -18 -7.00 7.00 -2 5 -18 5.20 10.30 2 -5 -18 2.20 12.20 -3 -5 -18 20.10 8.20 3 5 -18 25.90 9.70 3 -5 -18 16.60 10.60 -3 5 -18 8.00 9.10 0 6 -18 5.20 6.70 -1 -6 -18 30.20 9.80 1 6 -18 10.20 8.50 -1 6 -18 15.30 8.10 1 -6 -18 -5.60 9.90 -2 -6 -18 -10.70 7.40 2 6 -18 -6.90 6.40 -2 6 -18 11.40 7.10 2 -6 -18 2.30 8.00 0 -7 -18 16.60 8.60 0 7 -18 30.50 9.20 1 7 -18 8.00 6.50 -1 -7 -18 -4.30 7.20 -1 7 -18 -10.20 6.00 1 -7 -18 -17.20 9.30 0 0 -19 9.70 6.60 -1 0 -19 -0.50 6.60 -2 0 -19 9.10 7.50 2 0 -19 18.40 8.90 -3 0 -19 12.80 7.00 3 0 -19 7.10 9.10 0 -1 -19 19.30 8.50 0 1 -19 37.90 14.40 1 1 -19 35.60 13.30 -1 -1 -19 23.20 8.40 -1 1 -19 24.60 9.30 2 1 -19 -0.80 7.80 -2 -1 -19 4.30 7.20 -2 1 -19 10.10 6.90 -3 -1 -19 -7.50 6.50 3 1 -19 -7.40 8.30 -3 1 -19 8.90 7.80 3 -1 -19 16.30 8.50 0 -2 -19 3.00 7.80 0 2 -19 14.80 14.20 -1 -2 -19 2.10 7.30 1 2 -19 5.50 7.70 -1 2 -19 29.10 12.50 -2 -2 -19 1.20 7.30 2 2 -19 -1.50 6.60 2 -2 -19 4.90 9.10 -2 2 -19 23.30 11.10 3 2 -19 19.80 10.50 -3 -2 -19 28.00 9.10 3 -2 -19 44.40 11.20 0 -3 -19 45.40 11.00 0 3 -19 49.99 11.90 1 3 -19 -9.90 5.80 -1 -3 -19 3.50 8.20 1 -3 -19 0.20 10.00 -1 3 -19 -12.00 6.60 -2 -3 -19 46.00 10.60 2 3 -19 20.80 9.50 2 -3 -19 18.40 9.20 -2 3 -19 20.50 8.40 0 -4 -19 19.90 13.90 0 4 -19 20.60 9.70 1 4 -19 -12.10 6.50 -1 -4 -19 18.60 9.40 -1 4 -19 4.80 7.10 1 -4 -19 7.80 9.10 -2 -4 -19 8.40 8.50 2 4 -19 19.30 9.10 2 -4 -19 1.30 8.60 -2 4 -19 13.00 7.10 0 5 -19 20.60 8.70 1 5 -19 10.10 8.10 -1 -5 -19 -2.40 8.30 -1 5 -19 24.40 8.30 1 -5 -19 -7.70 8.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 12704 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 S1 S 1.07042(12) 0.60559(7) 0.60662(6) 0.0393(3) Uani 1 1 d . . F1 F 0.4095(4) 0.8076(2) 0.7989(2) 0.0934(11) Uani 1 1 d . . N1 N 0.9757(3) 0.5602(2) 0.70063(19) 0.0339(7) Uani 1 1 d . . O1 O 1.1027(4) 0.41568(19) 0.67818(19) 0.0550(8) Uani 1 1 d . . O2 O 1.0798(4) 0.71305(18) 0.62051(17) 0.0515(7) Uani 1 1 d . . C1 C 0.9727(4) 0.6182(3) 0.8521(2) 0.0349(9) Uani 1 1 d . . C2 C 0.9980(5) 0.6984(3) 0.9068(3) 0.0531(12) Uani 1 1 d . . H2 H 0.9706 0.7614 0.8884 0.064 Uiso 1 1 calc R U C3 C 1.0633(7) 0.6849(4) 0.9879(3) 0.0744(16) Uani 1 1 d . . H3 H 1.0810 0.7390 1.0237 0.089 Uiso 1 1 calc R U C4 C 1.1023(6) 0.5924(4) 1.0161(3) 0.0709(14) Uani 1 1 d . . H4 H 1.1447 0.5838 1.0713 0.085 Uiso 1 1 calc R U C5 C 1.0791(6) 0.5123(3) 0.9632(3) 0.0540(11) Uani 1 1 d . . H5 H 1.1068 0.4496 0.9824 0.065 Uiso 1 1 calc R U C6 C 1.0140(4) 0.5250(3) 0.8809(3) 0.0383(9) Uani 1 1 d . . C7 C 0.9910(6) 0.4402(3) 0.8192(3) 0.0497(11) Uani 1 1 d . . H7A H 1.0594 0.3860 0.8364 0.060 Uiso 1 1 calc R U H7B H 0.8817 0.4176 0.8225 0.060 Uiso 1 1 calc R U C8 C 1.0285(4) 0.4689(3) 0.7275(3) 0.0395(9) Uani 1 1 d . . C9 C 0.9049(4) 0.6319(2) 0.7622(2) 0.0307(8) Uani 1 1 d . . H9 H 0.9376 0.6975 0.7426 0.037 Uiso 1 1 calc R U C10 C 0.7233(4) 0.6312(3) 0.7627(2) 0.0333(9) Uani 1 1 d . . C11 C 0.6330(5) 0.5481(3) 0.7470(3) 0.0463(10) Uani 1 1 d . . H11 H 0.6829 0.4889 0.7337 0.056 Uiso 1 1 calc R U C12 C 0.4678(5) 0.5524(4) 0.7509(3) 0.0587(13) Uani 1 1 d . . H12 H 0.4084 0.4958 0.7408 0.070 Uiso 1 1 calc R U C13 C 0.3916(5) 0.6392(3) 0.7695(3) 0.0583(13) Uani 1 1 d . . H13 H 0.2813 0.6425 0.7729 0.070 Uiso 1 1 calc R U C14 C 0.4836(5) 0.7204(3) 0.7828(3) 0.0541(12) Uani 1 1 d . . C15 C 0.6463(5) 0.7198(3) 0.7804(3) 0.0425(10) Uani 1 1 d . . H15 H 0.7040 0.7772 0.7902 0.051 Uiso 1 1 calc R U C16 C 0.9177(5) 0.5874(3) 0.5219(2) 0.0460(10) Uani 1 1 d . . C17 C 0.8829(7) 0.4776(3) 0.5156(3) 0.0759(17) Uani 1 1 d . . H17A H 0.8338 0.4556 0.5684 0.114 Uiso 1 1 calc R U H17B H 0.9806 0.4423 0.5068 0.114 Uiso 1 1 calc R U H17C H 0.8126 0.4656 0.4677 0.114 Uiso 1 1 calc R U C18 C 1.0019(6) 0.6247(4) 0.4399(3) 0.0740(16) Uani 1 1 d . . H18A H 0.9323 0.6177 0.3909 0.111 Uiso 1 1 calc R U H18B H 1.0968 0.5868 0.4303 0.111 Uiso 1 1 calc R U H18C H 1.0294 0.6928 0.4471 0.111 Uiso 1 1 calc R U C19 C 0.7722(6) 0.6497(4) 0.5405(3) 0.0674(14) Uani 1 1 d . . H19A H 0.7055 0.6517 0.4900 0.101 Uiso 1 1 calc R U H19B H 0.8048 0.7154 0.5553 0.101 Uiso 1 1 calc R U H19C H 0.7141 0.6216 0.5881 0.101 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 0.0374(5) 0.0432(5) 0.0374(5) -0.0007(4) 0.0020(5) -0.0028(5) F1 0.0561(19) 0.081(2) 0.144(3) -0.0206(19) 0.001(2) 0.0274(17) N1 0.0356(18) 0.0296(15) 0.0364(17) -0.0007(13) 0.0034(13) 0.0022(13) O1 0.063(2) 0.0415(15) 0.0610(19) -0.0084(14) 0.0047(16) 0.0150(15) O2 0.0687(19) 0.0402(14) 0.0457(16) 0.0006(12) 0.0051(16) -0.0170(15) C1 0.0292(19) 0.038(2) 0.037(2) 0.0018(17) -0.0008(15) 0.0007(17) C2 0.061(3) 0.046(2) 0.052(3) -0.007(2) -0.013(2) 0.005(2) C3 0.100(4) 0.067(3) 0.056(3) -0.012(2) -0.030(3) 0.007(3) C4 0.077(4) 0.087(4) 0.048(3) 0.002(3) -0.028(3) 0.012(3) C5 0.053(3) 0.057(3) 0.052(3) 0.014(2) -0.007(2) 0.007(3) C6 0.033(2) 0.043(2) 0.039(2) 0.0065(18) 0.0019(17) 0.0019(17) C7 0.062(3) 0.0318(19) 0.055(3) 0.0106(19) 0.003(2) 0.002(2) C8 0.037(2) 0.0310(19) 0.050(2) -0.0014(18) -0.0023(18) 0.0026(18) C9 0.0292(19) 0.0260(16) 0.037(2) 0.0012(14) 0.0015(16) 0.0008(15) C10 0.0287(18) 0.035(2) 0.036(2) 0.0009(16) -0.0021(15) -0.0010(16) C11 0.042(2) 0.038(2) 0.059(3) -0.003(2) -0.003(2) -0.0015(19) C12 0.037(3) 0.069(3) 0.070(3) 0.000(3) -0.004(2) -0.015(2) C13 0.030(2) 0.073(3) 0.073(3) -0.006(3) 0.001(2) 0.001(2) C14 0.043(3) 0.054(3) 0.066(3) -0.006(2) 0.000(2) 0.017(2) C15 0.035(2) 0.038(2) 0.054(3) -0.0024(19) -0.0025(19) 0.0050(19) C16 0.049(2) 0.049(2) 0.039(2) -0.0037(17) -0.007(2) 0.000(2) C17 0.087(4) 0.061(3) 0.080(4) -0.010(3) -0.035(3) -0.009(3) C18 0.083(3) 0.099(4) 0.041(3) 0.001(3) -0.004(2) -0.011(3) C19 0.065(3) 0.084(3) 0.053(3) 0.005(3) -0.016(2) 0.016(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O2 S1 N1 104.49(15) O2 S1 C16 105.77(18) N1 S1 C16 102.66(17) C8 N1 C9 121.8(3) C8 N1 S1 114.5(2) C9 N1 S1 118.5(2) C6 C1 C2 118.8(3) C6 C1 C9 120.0(3) C2 C1 C9 121.1(3) C3 C2 C1 120.4(4) C3 C2 H2 119.8 C1 C2 H2 119.8 C4 C3 C2 120.4(4) C4 C3 H3 119.8 C2 C3 H3 119.8 C3 C4 C5 120.3(4) C3 C4 H4 119.8 C5 C4 H4 119.8 C4 C5 C6 119.9(4) C4 C5 H5 120.1 C6 C5 H5 120.1 C1 C6 C5 120.2(4) C1 C6 C7 117.6(3) C5 C6 C7 122.1(4) C8 C7 C6 111.7(3) C8 C7 H7A 109.3 C6 C7 H7A 109.3 C8 C7 H7B 109.3 C6 C7 H7B 109.3 H7A C7 H7B 107.9 O1 C8 N1 120.7(4) O1 C8 C7 122.7(3) N1 C8 C7 116.6(3) N1 C9 C1 110.8(3) N1 C9 C10 113.6(3) C1 C9 C10 111.8(3) N1 C9 H9 106.7 C1 C9 H9 106.7 C10 C9 H9 106.7 C11 C10 C15 118.9(4) C11 C10 C9 123.6(3) C15 C10 C9 117.5(3) C10 C11 C12 120.5(4) C10 C11 H11 119.8 C12 C11 H11 119.8 C13 C12 C11 120.8(4) C13 C12 H12 119.6 C11 C12 H12 119.6 C14 C13 C12 117.5(4) C14 C13 H13 121.3 C12 C13 H13 121.3 F1 C14 C13 118.2(4) F1 C14 C15 117.8(4) C13 C14 C15 124.0(4) C14 C15 C10 118.3(4) C14 C15 H15 120.8 C10 C15 H15 120.8 C19 C16 C17 113.8(4) C19 C16 C18 110.2(4) C17 C16 C18 111.1(4) C19 C16 S1 110.6(3) C17 C16 S1 108.0(3) C18 C16 S1 102.5(3) C16 C17 H17A 109.5 C16 C17 H17B 109.5 H17A C17 H17B 109.5 C16 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C16 C18 H18A 109.5 C16 C18 H18B 109.5 H18A C18 H18B 109.5 C16 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C16 C19 H19A 109.5 C16 C19 H19B 109.5 H19A C19 H19B 109.5 C16 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O2 1.476(3) S1 N1 1.764(3) S1 C16 1.848(4) F1 C14 1.361(5) N1 C8 1.380(4) N1 C9 1.483(4) O1 C8 1.220(4) C1 C6 1.386(5) C1 C2 1.392(5) C1 C9 1.509(5) C2 C3 1.377(6) C2 H2 0.9300 C3 C4 1.369(6) C3 H3 0.9300 C4 C5 1.372(6) C4 H4 0.9300 C5 C6 1.391(6) C5 H5 0.9300 C6 C7 1.505(5) C7 C8 1.499(6) C7 H7A 0.9700 C7 H7B 0.9700 C9 C10 1.527(5) C9 H9 0.9800 C10 C11 1.381(5) C10 C15 1.392(5) C11 C12 1.391(6) C11 H11 0.9300 C12 C13 1.371(6) C12 H12 0.9300 C13 C14 1.361(6) C13 H13 0.9300 C14 C15 1.369(5) C15 H15 0.9300 C16 C19 1.515(6) C16 C17 1.521(6) C16 C18 1.534(6) C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 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 O2 S1 N1 C8 -145.1(3) C16 S1 N1 C8 104.6(3) O2 S1 N1 C9 9.7(3) C16 S1 N1 C9 -100.5(3) C6 C1 C2 C3 0.2(6) C9 C1 C2 C3 -178.5(4) C1 C2 C3 C4 -0.8(9) C2 C3 C4 C5 1.1(9) C3 C4 C5 C6 -0.7(8) C2 C1 C6 C5 0.2(6) C9 C1 C6 C5 178.9(4) C2 C1 C6 C7 -177.8(4) C9 C1 C6 C7 1.0(5) C4 C5 C6 C1 0.1(7) C4 C5 C6 C7 177.9(4) C1 C6 C7 C8 36.9(5) C5 C6 C7 C8 -141.0(4) C9 N1 C8 O1 -171.4(3) S1 N1 C8 O1 -17.5(5) C9 N1 C8 C7 8.0(5) S1 N1 C8 C7 162.0(3) C6 C7 C8 O1 137.9(4) C6 C7 C8 N1 -41.5(5) C8 N1 C9 C1 29.2(4) S1 N1 C9 C1 -123.7(3) C8 N1 C9 C10 -97.7(4) S1 N1 C9 C10 109.4(3) C6 C1 C9 N1 -33.8(4) C2 C1 C9 N1 144.9(4) C6 C1 C9 C10 94.1(4) C2 C1 C9 C10 -87.2(4) N1 C9 C10 C11 31.7(5) C1 C9 C10 C11 -94.6(4) N1 C9 C10 C15 -148.5(3) C1 C9 C10 C15 85.2(4) C15 C10 C11 C12 -1.6(7) C9 C10 C11 C12 178.2(4) C10 C11 C12 C13 0.7(7) C11 C12 C13 C14 0.7(7) C12 C13 C14 F1 178.2(4) C12 C13 C14 C15 -1.3(8) F1 C14 C15 C10 -179.1(4) C13 C14 C15 C10 0.4(8) C11 C10 C15 C14 1.1(6) C9 C10 C15 C14 -178.7(4) O2 S1 C16 C19 -45.4(3) N1 S1 C16 C19 63.8(3) O2 S1 C16 C17 -170.6(3) N1 S1 C16 C17 -61.4(3) O2 S1 C16 C18 72.0(3) N1 S1 C16 C18 -178.7(3)